Open-access and free articles in Acta Crystallographica Section E: Crystallographic Communications
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Acta Crystallographica Section E: Crystallographic Communications is the IUCr's popular open-access structural journal. It provides a simple and easily accessible publication mechanism for inorganic, metal-organic and organic crystal structure determinations. The electronic submission, validation, refereeing and publication facilities of the journal ensure very rapid and high-quality publication, whilst key indicators and validation reports provide measures of structural reliability. The average publication time is less than one month.en-gbhttps://creativecommons.org/licenses/by/4.0/International Union of CrystallographyInternational Union of Crystallographyhttps://journals.iucr.orgtext/htmlurn:issn:1600-5368Open-access and free articles in Acta Crystallographica Section E Crystallographic CommunicationsActa Crystallographica Section E: Crystallographic Communications is the IUCr's popular open-access structural journal. It provides a simple and easily accessible publication mechanism for inorganic, metal-organic and organic crystal structure determinations. The electronic submission, validation, refereeing and publication facilities of the journal ensure very rapid and high-quality publication, whilst key indicators and validation reports provide measures of structural reliability. The average publication time is less than one month.textmonthly2002-01-01T00:00+00:001urn:issn:1600-5368Acta Crystallographica Section E Crystallographic Communicationsmed@iucr.orgOpen-access and free articles in Acta Crystallographica Section E: Crystallographic Communicationshttp://journals.iucr.org/logos/rss10e.gif
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Still imageSynthesis and crystal structure of tetramethyl (E)-4,4′-(ethene-1,2-diyl)bis(5-nitrobenzene-1,2-dicarboxylate)
http://scripts.iucr.org/cgi-bin/paper?wm5712
The title compound, C22H18N2O12, was obtained as a by-product during the planned synthesis of 1,2-bis(2-nitro-4,5-dimethyl phthalate)ethane by oxidative dimerization starting from dimethyl-4-methyl-5-nitro phthalate. To identify this compound unambiguously, a single-crystal structure analysis was performed. The asymmetric unit consists of half a molecule that is located at a centre of inversion. As a result of symmetry restrictions, the molecule shows an E configuration around the double bond. Both phenyl rings are coplanar, whereas the nitro and the two methyl ester groups are rotated out of the ring plane by 32.6 (1), 56.5 (2) and 49.5 (2)°, respectively. In the crystal, molecules are connected into chains extending parallel to the a axis by pairs of C—H⋯O hydrogen bonds that are connected into a tri-periodic network by additional C—H⋯O hydrogen-bonding interactions.urn:issn:2056-9890Businski, A.Ta, T.C.Gindullis, N.Näther, C.Herges, R.text/htmlIn the crystal structure of the title compound the two phenyl rings are coplanar, whereas the nitro and the two methyl ester groups are rotated out of the ring plane. The molecules are linked by intermolecular C—H⋯O hydrogen bonding into a tri-periodic network.doi:10.1107/S2056989024002676CRYSTAL STRUCTURE; SYNTHESIS; STILBENE DERIVATIVE; DIAZOCINE2024-03-28Synthesis and crystal structure of tetramethyl (E)-4,4′-(ethene-1,2-diyl)bis(5-nitrobenzene-1,2-dicarboxylate)The title compound, C22H18N2O12, was obtained as a by-product during the planned synthesis of 1,2-bis(2-nitro-4,5-dimethyl phthalate)ethane by oxidative dimerization starting from dimethyl-4-methyl-5-nitro phthalate. To identify this compound unambiguously, a single-crystal structure analysis was performed. The asymmetric unit consists of half a molecule that is located at a centre of inversion. As a result of symmetry restrictions, the molecule shows an E configuration around the double bond. Both phenyl rings are coplanar, whereas the nitro and the two methyl ester groups are rotated out of the ring plane by 32.6 (1), 56.5 (2) and 49.5 (2)°, respectively. In the crystal, molecules are connected into chains extending parallel to the a axis by pairs of C—H⋯O hydrogen bonds that are connected into a tri-periodic network by additional C—H⋯O hydrogen-bonding interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext802024-03-28435research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsMarch 202442056-98902056-9890med@iucr.org438Synthesis, crystal structure and Hirshfeld surface analysis of bromidotetrakis[5-(prop-2-en-1-ylsulfanyl)-1,3,4-thiadiazol-2-amine-κN3]copper(II) bromide
http://scripts.iucr.org/cgi-bin/paper?ny2003
A novel cationic complex, bromidotetrakis[5-(prop-2-en-1-ylsulfanyl)-1,3,4-thiadiazol-2-amine-κN3]copper(II) bromide, [CuBr](C5H7N3S2)4Br, was synthesized. The complex crystallizes with fourfold molecular symmetry in the tetragonal space group P4/n. The CuII atom exhibits a square-pyramidal coordination geometry. The Cu atom is located centrally within the complex, being coordinated by four nitrogen atoms from four AAT molecules, while a bromine anion is located at the apex of the pyramid. The amino H atoms of AAT interact with bromine from the inner and outer spheres, forming a two-dimensional network in the [100] and [010] directions. Hirshfeld surface analysis reveals that 33.7% of the intermolecular interactions are from H⋯H contacts, 21.2% are from S⋯H/H⋯S contacts, 13.4% are from S⋯S contacts and 11.0% are from C⋯H/H⋯C, while other contributions are from Br⋯H/H⋯Br and N⋯H/H⋯N contacts.urn:issn:2056-9890Atashov, A.Azamova, M.Ziyatov, D.Uzakbergenova, Z.Torambetov, B.Holczbauer, T.Ashurov, J.Kadirova, S.text/htmlThe molecular and crystal structure of the bromidotetrakis[5-(prop-2-en-1-ylsulfanyl)-1,3,4-thiadiazol-2-amine-κN3]copper(II) bromide complex was studied and Hirshfeld surfaces and fingerprint plots were generated to investigate the various intermolecular interactions.doi:10.1107/S2056989024002652CRYSTAL STRUCTURE; COPPER(II); 1,3,4-THIADIAZOLE; HYDROGEN BONDING; HIRSHFELD SURFACE ANALYSIS2024-03-26Synthesis, crystal structure and Hirshfeld surface analysis of bromidotetrakis[5-(prop-2-en-1-ylsulfanyl)-1,3,4-thiadiazol-2-amine-κN3]copper(II) bromideA novel cationic complex, bromidotetrakis[5-(prop-2-en-1-ylsulfanyl)-1,3,4-thiadiazol-2-amine-κN3]copper(II) bromide, [CuBr](C5H7N3S2)4Br, was synthesized. The complex crystallizes with fourfold molecular symmetry in the tetragonal space group P4/n. The CuII atom exhibits a square-pyramidal coordination geometry. The Cu atom is located centrally within the complex, being coordinated by four nitrogen atoms from four AAT molecules, while a bromine anion is located at the apex of the pyramid. The amino H atoms of AAT interact with bromine from the inner and outer spheres, forming a two-dimensional network in the [100] and [010] directions. Hirshfeld surface analysis reveals that 33.7% of the intermolecular interactions are from H⋯H contacts, 21.2% are from S⋯H/H⋯S contacts, 13.4% are from S⋯S contacts and 11.0% are from C⋯H/H⋯C, while other contributions are from Br⋯H/H⋯Br and N⋯H/H⋯N contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98904412med@iucr.org80research communicationshttps://creativecommons.org/licenses/by/4.0/March 2024Acta Crystallographica Section E: Crystallographic Communications4082024-03-26Crystal structure and Hirshfeld surface analysis of ethyl 2-(7-chloro-3-methyl-2-oxo-1,2-dihydroquinoxalin-1-yl)acetate
http://scripts.iucr.org/cgi-bin/paper?vm2299
The quinoxaline moiety in the title molecule, C13H13ClN2O3, is almost planar (r.m.s. deviation of the fitted atoms = 0.033 Å). In the crystal, C—H⋯O hydrogen bonds plus slipped π-stacking and C—H⋯π(ring) interactions generate chains of molecules extending along the b-axis direction. The chains are connected by additional C—H⋯O hydrogen bonds. Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from H⋯H (37.6%), H⋯O/O⋯H (22.7%) and H⋯Cl/Cl⋯H (13.1%) interactions.urn:issn:2056-9890Mustaphi, N.E.H.Aboutofil, F.E.El Houssni, L.Saif, E.Mague, J.T.Chkirate, K.Essassi, E.M.text/htmlThe quinoxaline moiety is almost planar and the dihedral angle between the mean planes through the two constituent six-membered rings is 2.1 (2)°. In the crystal, C—H⋯O hydrogen bonds together with slipped π-stacking and C—H⋯π(ring) interactions generate chains of molecules extending along the b-axis direction. The chains are connected by additional C—H⋯O hydrogen bonds.doi:10.1107/S2056989024002664CRYSTAL STRUCTURE; C-H...[PI](RING) INTERACTION; [PI]-STACKING; HYDROGEN BOND; QUINOXALINE2024-03-26Crystal structure and Hirshfeld surface analysis of ethyl 2-(7-chloro-3-methyl-2-oxo-1,2-dihydroquinoxalin-1-yl)acetateThe quinoxaline moiety in the title molecule, C13H13ClN2O3, is almost planar (r.m.s. deviation of the fitted atoms = 0.033 Å). In the crystal, C—H⋯O hydrogen bonds plus slipped π-stacking and C—H⋯π(ring) interactions generate chains of molecules extending along the b-axis direction. The chains are connected by additional C—H⋯O hydrogen bonds. Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from H⋯H (37.6%), H⋯O/O⋯H (22.7%) and H⋯Cl/Cl⋯H (13.1%) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org43442056-98902056-98902024-03-26430Acta Crystallographica Section E: Crystallographic CommunicationsMarch 2024research communicationshttps://creativecommons.org/licenses/by/4.0/80Synthesis, characterization and supramolecular analysis for (E)-3-(pyridin-4-yl)acrylic acid
http://scripts.iucr.org/cgi-bin/paper?ex2082
The title compound, C8H7NO2, crystallizes as prismatic colourless crystals in space group P\overline{1}, with one molecule in the asymmetric unit. The pyridine ring is fused to acrylic acid, forming an almost planar structure with an E-configuration about the double bond with a torsion angle of −6.1 (2)°. In the crystal, strong O—H⋯N interactions link the molecules, forming chains along the [101] direction. Weak C—H⋯O interactions link adjacent chains along the [100] direction, generating an R22(14) homosynthon. Finally, π–π stacking interactions lead to the formation of the three-dimensional structure. The supramolecular analysis was supported by Hirshfeld surface and two-dimensional fingerprint plot analysis, indicating that the most abundant contacts are associated with H⋯H, O⋯H/H⋯O, N⋯H/H⋯N and C⋯H/H⋯C interactions.urn:issn:2056-9890Florez-Muñoz, V.Guerrero, A.F.Macias, M.Illicachi, L.A.D'Vries, R.text/htmlIn the title compound, the pyridine ring is fused to acrylic acid, forming an almost planar structure with an E-configuration about the double bond. In the crystal, O—H⋯N and C—H⋯O interactions together with π–π stacking interactions lead to the formation of the three-dimensional structure.doi:10.1107/S2056989024002627CRYSTAL STRUCTURE; (E)-3-(PYRIDIN-4-YL)ACRYLIC ACID; SUPRAMOLECULAR ANALYSIS2024-03-26Synthesis, characterization and supramolecular analysis for (E)-3-(pyridin-4-yl)acrylic acidThe title compound, C8H7NO2, crystallizes as prismatic colourless crystals in space group P\overline{1}, with one molecule in the asymmetric unit. The pyridine ring is fused to acrylic acid, forming an almost planar structure with an E-configuration about the double bond with a torsion angle of −6.1 (2)°. In the crystal, strong O—H⋯N interactions link the molecules, forming chains along the [101] direction. Weak C—H⋯O interactions link adjacent chains along the [100] direction, generating an R22(14) homosynthon. Finally, π–π stacking interactions lead to the formation of the three-dimensional structure. The supramolecular analysis was supported by Hirshfeld surface and two-dimensional fingerprint plot analysis, indicating that the most abundant contacts are associated with H⋯H, O⋯H/H⋯O, N⋯H/H⋯N and C⋯H/H⋯C interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext803882024-03-26https://creativecommons.org/licenses/by/4.0/research communicationsMarch 2024Acta Crystallographica Section E: Crystallographic Communications42056-98902056-9890med@iucr.org391Synthesis, crystal structure and Hirshfeld surface analysis of 2-phenyl-3-(prop-2-yn-1-yloxy)quinoxaline
http://scripts.iucr.org/cgi-bin/paper?vm2298
In the title compound, C17H12N2O, the quinoxaline moiety shows deviations of 0.0288 (7) to −0.0370 (7) Å from the mean plane (r.m.s. deviation of fitted atoms = 0.0223 Å). In the crystal, corrugated layers two molecules thick are formed by C—H⋯N hydrogen bonds and π-stacking interactions.urn:issn:2056-9890Abad, N.Mague, J.T.Alsubari, A.Essassi, E.M.Pourayoubi, M.Yahya Abdullah Alzahrani, A.Ramli, Y.text/htmlIn the title compound, the quinoxaline moiety shows deviations of 0.0288 (7) to −0.0370 (7) Å from the mean plane (r.m.s. deviation of fitted atoms = 0.0223 Å). In the crystal, corrugated layers two molecules thick are formed by C—H⋯N hydrogen bonds and π-stacking interactions.doi:10.1107/S2056989024002585CRYSTAL STRUCTURE; QUINOXALINE; ALKYLATION; HYDROGEN BOND; [PI]-STACKING2024-03-21Synthesis, crystal structure and Hirshfeld surface analysis of 2-phenyl-3-(prop-2-yn-1-yloxy)quinoxalineIn the title compound, C17H12N2O, the quinoxaline moiety shows deviations of 0.0288 (7) to −0.0370 (7) Å from the mean plane (r.m.s. deviation of fitted atoms = 0.0223 Å). In the crystal, corrugated layers two molecules thick are formed by C—H⋯N hydrogen bonds and π-stacking interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org38742056-98902056-98903832024-03-21Acta Crystallographica Section E: Crystallographic CommunicationsMarch 2024https://creativecommons.org/licenses/by/4.0/research communications80Crystal structure of 2,4-diamino-5-(4-hydroxy-3-methoxyphenyl)-8,8-dimethyl-6-oxo-6,7,8,9-tetrahydro-5H-chromeno[2,3-b]pyridine-3-carbonitrile–dimethylformamide–water (1/1/1)
http://scripts.iucr.org/cgi-bin/paper?yz2052
In the structure of the title compound, C22H22N4O4·C3H7NO·H2O, the entire tricyclic system is approximately planar except for the carbon atom bearing the two methyl groups; the methoxyphenyl ring is approximately perpendicular to the tricycle. All seven potential hydrogen-bond donors take part in classical hydrogen bonds. The main molecule and the DMF combine to form broad ribbons parallel to the a axis and roughly parallel to the ab plane; the water molecules connect the residues in the third dimension.urn:issn:2056-9890Metwally, N.H.Elgemeie, G.H.Abd Al-latif, E.S.M.Jones, P.G.text/htmlThe heterocyclic system of the title compound is approximately planar except for the carbon atom of the CMe2 group; the residues are connected by extensive classical hydrogen bonding.doi:10.1107/S2056989024002615CRYSTAL STRUCTURE; CHROMENOPYRIDINE; SOLVATE; SECONDARY INTERACTIONS2024-03-26Crystal structure of 2,4-diamino-5-(4-hydroxy-3-methoxyphenyl)-8,8-dimethyl-6-oxo-6,7,8,9-tetrahydro-5H-chromeno[2,3-b]pyridine-3-carbonitrile–dimethylformamide–water (1/1/1)In the structure of the title compound, C22H22N4O4·C3H7NO·H2O, the entire tricyclic system is approximately planar except for the carbon atom bearing the two methyl groups; the methoxyphenyl ring is approximately perpendicular to the tricycle. All seven potential hydrogen-bond donors take part in classical hydrogen bonds. The main molecule and the DMF combine to form broad ribbons parallel to the a axis and roughly parallel to the ab plane; the water molecules connect the residues in the third dimension.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext42056-98902056-9890med@iucr.org400803962024-03-26https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsMarch 2024Synthesis and crystal structure of N-phenyl-2-(phenylsulfanyl)acetamide
http://scripts.iucr.org/cgi-bin/paper?yz2049
N-Phenyl-2-(phenylsulfanyl)acetamide, C14H13NOS, was synthesized and structurally characterized. In the crystal, N—H⋯O hydrogen bonding leads to the formation of chains of molecules along the [100] direction. The chains are linked by C—H⋯π interactions, forming a three-dimensional network. The crystal studied was twinned by a twofold rotation around [100].urn:issn:2056-9890Mohamed-Ezzat, R.A.Kariuki, B.M.Elgemeie, G.H.text/htmlIn the crystal of the title compound, N—H⋯O hydrogen bonds form chains of molecules along the [100] direction. The chains are linked by C—H⋯π interactions, forming a three-dimensional network.doi:10.1107/S2056989024002573CRYSTAL STRUCTURE; ACETAMIDE; SULFIDE; SYNTHESIS2024-03-26Synthesis and crystal structure of N-phenyl-2-(phenylsulfanyl)acetamideN-Phenyl-2-(phenylsulfanyl)acetamide, C14H13NOS, was synthesized and structurally characterized. In the crystal, N—H⋯O hydrogen bonding leads to the formation of chains of molecules along the [100] direction. The chains are linked by C—H⋯π interactions, forming a three-dimensional network. The crystal studied was twinned by a twofold rotation around [100].https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org39542056-98902056-98903922024-03-26research communicationshttps://creativecommons.org/licenses/by/4.0/March 2024Acta Crystallographica Section E: Crystallographic Communications80Crystal structure and Hirshfeld surface analysis of 6-imino-8-(4-methylphenyl)-1,3,4,6-tetrahydro-2H-pyrido[1,2-a]pyrimidine-7,9-dicarbonitrile
http://scripts.iucr.org/cgi-bin/paper?nx2006
In the ten-membered 1,3,4,6-tetrahydro-2H-pyrido[1,2-a]pyrimidine ring system of the title compound, C17H15N5, the 1,2-dihydropyridine ring is essentially planar (r.m.s. deviation = 0.001 Å), while the 1,3-diazinane ring has a distorted twist-boat conformation. In the crystal, molecules are linked by N—H⋯N and C—H⋯N hydrogen bonds, forming a three-dimensional network. In addition, C—H⋯π interactions form layers parallel to the (100) plane. Thus, crystal-structure cohesion is ensured. According to a Hirshfeld surface study, H⋯H (40.4%), N⋯H/H⋯N (28.6%) and C⋯H/H⋯C (24.1%) interactions are the most important contributors to the crystal packing.urn:issn:2056-9890Naghiyev, F.N.Khrustalev, V.N.Akkurt, M.Dobrokhotova, E.V.Bhattarai, A.Khalilov, A.N.Mamedov, İ.G.text/htmlIn the crystal, molecules are linked by N—H⋯N and C–H⋯N hydrogen bonds, forming a three-dimensional network. In addition, C—H⋯π interactions form layers parallel to the (100) plane. Thus, crystal-structure cohesion is ensured.doi:10.1107/S2056989024002500CRYSTAL STRUCTURE; 1,2-DIHYDROPYRIDINE RING; 1,3-DIAZINANE RING; HYDROGEN BONDS; C-H...[PI] INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2024-03-21Crystal structure and Hirshfeld surface analysis of 6-imino-8-(4-methylphenyl)-1,3,4,6-tetrahydro-2H-pyrido[1,2-a]pyrimidine-7,9-dicarbonitrileIn the ten-membered 1,3,4,6-tetrahydro-2H-pyrido[1,2-a]pyrimidine ring system of the title compound, C17H15N5, the 1,2-dihydropyridine ring is essentially planar (r.m.s. deviation = 0.001 Å), while the 1,3-diazinane ring has a distorted twist-boat conformation. In the crystal, molecules are linked by N—H⋯N and C—H⋯N hydrogen bonds, forming a three-dimensional network. In addition, C—H⋯π interactions form layers parallel to the (100) plane. Thus, crystal-structure cohesion is ensured. According to a Hirshfeld surface study, H⋯H (40.4%), N⋯H/H⋯N (28.6%) and C⋯H/H⋯C (24.1%) interactions are the most important contributors to the crystal packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org38242056-98902056-98902024-03-21378https://creativecommons.org/licenses/by/4.0/research communicationsMarch 2024Acta Crystallographica Section E: Crystallographic Communications80Lithium and sodium 3-(3,4-dihydroxyphenyl)propenoate hydrate
http://scripts.iucr.org/cgi-bin/paper?wm5710
Treatment of 3-(3,4-dihydroxyphenyl)propenoic acid (caffeic acid or 3,4-dihydroxycinnamic acid) with the alkali hydroxides MOH (M = Li, Na) in aqueous solution led to the formation of poly[aqua[μ-3-(3,4-dihydroxyphenyl)propenoato]lithium], [Li(C9H7O4)(H2O)]n, 1, and poly[aqua[μ-3-(3,4-dihydroxyphenyl)propenoato]sodium], [Na(C9H7O4)(H2O)]n, 2. The crystal structure of 1 consists of a lithium cation that is coordinated nearly tetrahedrally by three carboxylate oxygen atoms and a water molecule. The carboxylate groups adopt a μ3-κ3O:O′:O′ coordination mode that leads to a chain-like catenation of Li cations and carboxylate units parallel to the b axis. Moreover, the lithium carboxylate chains are connected by hydrogen bonds between water molecules attached to lithium and catechol OH groups. The crystal structure of 2 shows a sevenfold coordination of the sodium cation by one water molecule, two monodentately binding carboxylate groups and four oxygen atoms from two catechol groups. The coordination polyhedra are linked by face- and edge-sharing into chains extending parallel to the b axis. The chains are interlinked by the bridging 3-(3,4-dihydroxyphenyl)propenoate units and by intermolecular hydrogen bonds to form the tri-periodic network.urn:issn:2056-9890Bieler, I.Wagner, C.Merzweiler, K.text/htmlThe Li cation in the crystal structure of the lithium salt LiC9H7O4·H2O shows a coordination number of four whereas the Na cation in the crystal structure of the sodium salt NaC9H7O4·H2O shows a coordination number of seven.doi:10.1107/S2056989024002494CRYSTAL STRUCTURE; CAFFEIC ACID; LITHIUM; SODIUM; HYDROGEN-BONDING2024-03-26Lithium and sodium 3-(3,4-dihydroxyphenyl)propenoate hydrateTreatment of 3-(3,4-dihydroxyphenyl)propenoic acid (caffeic acid or 3,4-dihydroxycinnamic acid) with the alkali hydroxides MOH (M = Li, Na) in aqueous solution led to the formation of poly[aqua[μ-3-(3,4-dihydroxyphenyl)propenoato]lithium], [Li(C9H7O4)(H2O)]n, 1, and poly[aqua[μ-3-(3,4-dihydroxyphenyl)propenoato]sodium], [Na(C9H7O4)(H2O)]n, 2. The crystal structure of 1 consists of a lithium cation that is coordinated nearly tetrahedrally by three carboxylate oxygen atoms and a water molecule. The carboxylate groups adopt a μ3-κ3O:O′:O′ coordination mode that leads to a chain-like catenation of Li cations and carboxylate units parallel to the b axis. Moreover, the lithium carboxylate chains are connected by hydrogen bonds between water molecules attached to lithium and catechol OH groups. The crystal structure of 2 shows a sevenfold coordination of the sodium cation by one water molecule, two monodentately binding carboxylate groups and four oxygen atoms from two catechol groups. The coordination polyhedra are linked by face- and edge-sharing into chains extending parallel to the b axis. The chains are interlinked by the bridging 3-(3,4-dihydroxyphenyl)propenoate units and by intermolecular hydrogen bonds to form the tri-periodic network.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext42056-98902056-9890med@iucr.org407804012024-03-26March 2024Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/Crystal structure, Hirshfeld surface analysis, calculations of crystal voids, interaction energy and energy frameworks as well as density functional theory (DFT) calculations of 3-[2-(morpholin-4-yl)ethyl]-5,5-diphenylimidazolidine-2,4-dione
http://scripts.iucr.org/cgi-bin/paper?wm5711
In the title molecule, C21H23N3O3, the imidazolidine ring slightly deviates from planarity and the morpholine ring exhibits the chair conformation. In the crystal, N—H⋯O and C—H⋯O hydrogen bonds form helical chains of molecules extending parallel to the c axis that are connected by C—H⋯π(ring) interactions. A Hirshfeld surface analysis reveals that the most important contributions for the crystal packing are from H⋯H (55.2%), H⋯C/C⋯H (22.6%) and H⋯O/O⋯H (20.5%) interactions. The volume of the crystal voids and the percentage of free space were calculated to be 236.78 Å3 and 12.71%, respectively. Evaluation of the electrostatic, dispersion and total energy frameworks indicates that the stabilization is dominated by the nearly equal electrostatic and dispersion energy contributions. The DFT-optimized molecular structure at the B3LYP/6-311 G(d,p) level is compared with the experimentally determined molecular structure in the solid state. Moreover, the HOMO–LUMO behaviour was elucidated to determine the energy gap.urn:issn:2056-9890Lamssane, H.Haoudi, A.Kartah, B.E.Mazzah, A.Mague, J.T.Hökelek, T.Kandri Rodi, Y.Sebbar, N.K.text/htmlIn the title molecule, the imidazolidine ring slightly deviates from planarity and the morpholine ring exhibits the usual chair conformation. In the crystal, N—H⋯O and C—H⋯O hydrogen bonds form helical chains of molecules extending parallel to the c axis that are connected by C—H⋯π(ring) interactions into a tri-periodic network.doi:10.1107/S2056989024002445CRYSTAL STRUCTURE; IMIDAZOLIDINEDIONE; HYDROGEN BOND; C-H...[PI](RING) INTERACTION2024-03-26Crystal structure, Hirshfeld surface analysis, calculations of crystal voids, interaction energy and energy frameworks as well as density functional theory (DFT) calculations of 3-[2-(morpholin-4-yl)ethyl]-5,5-diphenylimidazolidine-2,4-dioneIn the title molecule, C21H23N3O3, the imidazolidine ring slightly deviates from planarity and the morpholine ring exhibits the chair conformation. In the crystal, N—H⋯O and C—H⋯O hydrogen bonds form helical chains of molecules extending parallel to the c axis that are connected by C—H⋯π(ring) interactions. A Hirshfeld surface analysis reveals that the most important contributions for the crystal packing are from H⋯H (55.2%), H⋯C/C⋯H (22.6%) and H⋯O/O⋯H (20.5%) interactions. The volume of the crystal voids and the percentage of free space were calculated to be 236.78 Å3 and 12.71%, respectively. Evaluation of the electrostatic, dispersion and total energy frameworks indicates that the stabilization is dominated by the nearly equal electrostatic and dispersion energy contributions. The DFT-optimized molecular structure at the B3LYP/6-311 G(d,p) level is compared with the experimentally determined molecular structure in the solid state. Moreover, the HOMO–LUMO behaviour was elucidated to determine the energy gap.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98904429med@iucr.org80research communicationshttps://creativecommons.org/licenses/by/4.0/March 2024Acta Crystallographica Section E: Crystallographic Communications4232024-03-26Crystal structure and Hirshfeld surface analysis of 4,4′-dimethoxybiphenyl-3,3′,5,5′-tetracarboxylic acid dihydrate
http://scripts.iucr.org/cgi-bin/paper?ex2080
In the crystal of the title compound, C18H14O10·2H2O, the arene rings of the biphenyl moiety are tilted at an angle of 24.3 (1)°, while the planes passing through the carboxyl groups are rotated at angles of 8.6 (1) and 7.7 (1)° out of the plane of the benzene ring to which they are attached. The crystal structure is essentially stabilized by O—H⋯O bonds. Here, the carboxyl groups of neighbouring host molecules are connected by cyclic R22(8) synthons, leading to the formation of a three-dimensional network. The water molecules in turn form helical supramolecular strands running in the direction of the crystallographic c-axis (chain-like water clusters). The second H atom of each water molecule provides a link to a methoxy O atom of the host molecule. A Hirshfeld surface analysis was performed to quantify the contributions of the different intermolecular interactions, indicating that the most important contributions to the crystal packing are from H⋯O/O⋯H (37.0%), H⋯H (26.3%), H⋯C/C⋯H (18.5%) and C⋯O/O⋯C (9.5%) interactions.urn:issn:2056-9890Hanauer, T.Seichter, W.Mazik, M.text/htmlThe crystal structure is essentially stabilized by O—H⋯O bonds. Here, the carboxyl groups of neighbouring host molecules are connected by cyclic R_{2}^{2}(8) synthons, leading to the formation of a three-dimensional network. The water molecules in turn form helical supramolecular strands running in the c-axis direction (chain-like water clusters). The second H atom of each water molecule provides a link to a methoxy O atom of the host molecule.doi:10.1107/S2056989024002305BIPHENYL DERIVATIVE; O-H...O HYDROGEN BONDS; SUPRAMOLECULAR MOTIFS; WATER CLUSTER; HELICAL SUPRAMOLECULAR STRANDS; HIRSHFELD SURFACE; CRYSTAL STRUCTURE2024-03-26Crystal structure and Hirshfeld surface analysis of 4,4′-dimethoxybiphenyl-3,3′,5,5′-tetracarboxylic acid dihydrateIn the crystal of the title compound, C18H14O10·2H2O, the arene rings of the biphenyl moiety are tilted at an angle of 24.3 (1)°, while the planes passing through the carboxyl groups are rotated at angles of 8.6 (1) and 7.7 (1)° out of the plane of the benzene ring to which they are attached. The crystal structure is essentially stabilized by O—H⋯O bonds. Here, the carboxyl groups of neighbouring host molecules are connected by cyclic R22(8) synthons, leading to the formation of a three-dimensional network. The water molecules in turn form helical supramolecular strands running in the direction of the crystallographic c-axis (chain-like water clusters). The second H atom of each water molecule provides a link to a methoxy O atom of the host molecule. A Hirshfeld surface analysis was performed to quantify the contributions of the different intermolecular interactions, indicating that the most important contributions to the crystal packing are from H⋯O/O⋯H (37.0%), H⋯H (26.3%), H⋯C/C⋯H (18.5%) and C⋯O/O⋯C (9.5%) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98904417med@iucr.org80Acta Crystallographica Section E: Crystallographic CommunicationsMarch 2024https://creativecommons.org/licenses/by/4.0/research communications2024-03-26413Crystal structure and Hirshfeld surface analysis of 8-benzyl-1-[(4-methylphenyl)sulfonyl]-2,7,8,9-tetrahydro-1H-3,6:10,13-diepoxy-1,8-benzodiazacyclopentadecine ethanol hemisolvate
http://scripts.iucr.org/cgi-bin/paper?vm2297
The asymmetric unit of the title compound, 2C31H28N2O4S·C2H6O, contains a parent molecule and a half molecule of ethanol solvent. The main compound stabilizes its molecular conformation by forming a ring with an R12(7) motif with the ethanol solvent molecule. In the crystal, molecules are connected by C—H⋯O and O—H⋯O hydrogen bonds, forming a three-dimensional network. In addition, C—H⋯π interactions also strengthen the molecular packing.urn:issn:2056-9890Burkin, G.M.Kvyatkovskaya, E.A.Khrustalev, V.N.Hasanov, K.I.Sadikhova, N.D.Akkurt, M.Bhattarai, A.text/htmlIn the crystal, molecules are connected by C—H⋯O and O—H⋯O hydrogen bonds, forming a three-dimensional network. In addition, C—H⋯π interactions also strengthen the molecular packing.doi:10.1107/S2056989024002275CRYSTAL STRUCTURE; FURAN; SULFONAMIDE; MACROCYCLES; HYDROGEN BONDS; C-H...[PI] INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2024-03-26Crystal structure and Hirshfeld surface analysis of 8-benzyl-1-[(4-methylphenyl)sulfonyl]-2,7,8,9-tetrahydro-1H-3,6:10,13-diepoxy-1,8-benzodiazacyclopentadecine ethanol hemisolvateThe asymmetric unit of the title compound, 2C31H28N2O4S·C2H6O, contains a parent molecule and a half molecule of ethanol solvent. The main compound stabilizes its molecular conformation by forming a ring with an R12(7) motif with the ethanol solvent molecule. In the crystal, molecules are connected by C—H⋯O and O—H⋯O hydrogen bonds, forming a three-dimensional network. In addition, C—H⋯π interactions also strengthen the molecular packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext422med@iucr.org2056-98902056-98904https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsMarch 20242024-03-2641880Crystal structure of tetraphenyl phosphate tetrakis[dimethyl (2,2,2-trichloroacetyl)phosphoramidato]lutetium(III), PPh4[LuL4]
http://scripts.iucr.org/cgi-bin/paper?dj2075
A lutetium(III) complex based on the anion of the ligand dimethyl (2,2,2-trichloroacetyl)phosphoramidate (HL) and tetraphenylphosphonium, of composition PPh4[LuL4] (L = CAPh = carbacylamidophosphate), or (C24H20)[Lu(C4H6Cl3NO4P)4], has been synthesized and structurally characterized. The X-ray diffraction study of the compound revealed that the lutetium ion is surrounded by four bis-chelating CAPh ligands, forming the complex anion [LuL4]− with a coordination number of 8[O] for LuIII, while PPh4+ serves as a counter-ion. The coordination geometry around the Lu3+ ion was determined to be a nearly perfect triangular dodecahedron. The complex crystallizes in the monoclinic crystal system, space group P21/c, with four molecules in the unit cell. Weak hydrogen bonds O⋯HC(Ph), Cl⋯HC(Ph) and N⋯HC(Ph) are formed between the cations and anions. For a comparative study, HL-based structures were retrieved from the Cambridge Structural Database (CSD) and their geometries and conformations are discussed. A Hirshfeld surface analysis was also performed.urn:issn:2056-9890Struhatska, M.B.Ovchynnikov, V.A.Kariaka, N.S.Gawryszewska, P.Amirkhanov, V.M.text/htmlThe crystal structure of the anionic lutetium(III) tetrakis-CAPh complex (CAPh = carbacylamidophosphate) with tetraphenyl phosphate as the cation, PPh4[LuL4], is presented and discussed.doi:10.1107/S205698902400210XCRYSTAL STRUCTURE; LANTHANIDE; CARBACYLAMIDOPHOSPHATE CAPH; RARE-EARTH METALS; COORDINATION COMPOUND; TETRAKIS COMPLEX; CHELATE LIGAND; LUTETIUM; TETRAPHENYLPHOSPHONIUM CATION2024-03-12Crystal structure of tetraphenyl phosphate tetrakis[dimethyl (2,2,2-trichloroacetyl)phosphoramidato]lutetium(III), PPh4[LuL4]A lutetium(III) complex based on the anion of the ligand dimethyl (2,2,2-trichloroacetyl)phosphoramidate (HL) and tetraphenylphosphonium, of composition PPh4[LuL4] (L = CAPh = carbacylamidophosphate), or (C24H20)[Lu(C4H6Cl3NO4P)4], has been synthesized and structurally characterized. The X-ray diffraction study of the compound revealed that the lutetium ion is surrounded by four bis-chelating CAPh ligands, forming the complex anion [LuL4]− with a coordination number of 8[O] for LuIII, while PPh4+ serves as a counter-ion. The coordination geometry around the Lu3+ ion was determined to be a nearly perfect triangular dodecahedron. The complex crystallizes in the monoclinic crystal system, space group P21/c, with four molecules in the unit cell. Weak hydrogen bonds O⋯HC(Ph), Cl⋯HC(Ph) and N⋯HC(Ph) are formed between the cations and anions. For a comparative study, HL-based structures were retrieved from the Cambridge Structural Database (CSD) and their geometries and conformations are discussed. A Hirshfeld surface analysis was also performed.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext42056-98902056-9890med@iucr.org374803702024-03-12https://creativecommons.org/licenses/by/4.0/research communicationsMarch 2024Acta Crystallographica Section E: Crystallographic CommunicationsCoII-catalysed synthesis of N-(4-methoxyphenyl)-5-(pyridin-4-yl)-1,3,4-oxadiazol-2-amine hemihydrochloride monohydrate
http://scripts.iucr.org/cgi-bin/paper?hb8088
The title compound, C14H12N4O2·0.5HCl·H2O or H(C14H12N4O2)2+·Cl−·2H2O, arose from the unexpected cyclization of isonicotinoyl-N-phenyl hydrazine carbothioamide catalysed by cobalt(II) acetate. The organic molecule is almost planar and a symmetric N⋯H+⋯N hydrogen bond links two of them together, with the H atom lying on a crystallographic twofold axis. The extended structure features N—H⋯O and O—H⋯Cl hydrogen bonds, which generate [001] chains. Weak C—H⋯Cl interactions cross-link the chains. The chloride ion has site symmetry 2. The major contributions to the Hirshfeld surface are from H⋯H (47.1%), Cl⋯H/H⋯Cl (total 10.8%), O⋯H/H⋯O (7.4%) and N⋯H/H⋯N (6.7%) interactions.urn:issn:2056-9890Gautam, R.N.Sonkar, S.P.Yadav, S.Nath, P.Bharty, M.K.text/htmlThe CoII-catalysed synthesis and crystal structure is reported for the title compound, which features a symmetric N⋯H+⋯N unit.doi:10.1107/S20569890240020441,3,4-OXADIAZOLE; CYCLO-DESULFURIZATION; HIRSHFELD SURFACE ANALYSIS; CRYSTAL STRUCTURE2024-03-12CoII-catalysed synthesis of N-(4-methoxyphenyl)-5-(pyridin-4-yl)-1,3,4-oxadiazol-2-amine hemihydrochloride monohydrateThe title compound, C14H12N4O2·0.5HCl·H2O or H(C14H12N4O2)2+·Cl−·2H2O, arose from the unexpected cyclization of isonicotinoyl-N-phenyl hydrazine carbothioamide catalysed by cobalt(II) acetate. The organic molecule is almost planar and a symmetric N⋯H+⋯N hydrogen bond links two of them together, with the H atom lying on a crystallographic twofold axis. The extended structure features N—H⋯O and O—H⋯Cl hydrogen bonds, which generate [001] chains. Weak C—H⋯Cl interactions cross-link the chains. The chloride ion has site symmetry 2. The major contributions to the Hirshfeld surface are from H⋯H (47.1%), Cl⋯H/H⋯Cl (total 10.8%), O⋯H/H⋯O (7.4%) and N⋯H/H⋯N (6.7%) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext42056-98902056-9890med@iucr.org354802024-03-12351March 2024Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/Crystal structures of ten phosphane chalcogenide complexes of gold(III) chloride and bromide
http://scripts.iucr.org/cgi-bin/paper?yz2051
The structures of ten phosphane chalcogenide complexes of gold(III) halides, with general formula R13–nR2nPEAuX3 (R1 = t-butyl; R2 = i-propyl; n = 0 to 3; E = S or Se; X = Cl or Br) are presented. The eight possible chlorido derivatives are: 9a, n = 3, E = S; 10a, n = 2, E = S; 11a, n = 1, E = S; 12a, n = 0, E = S; 13a, n = 3, E = Se; 14a, n = 2, E = Se; 15a, n = 1, E = Se; and 16a, n = 0, E = Se, and the corresponding bromido derivatives are 9b–16b in the same order. Structures were obtained for 9a, 10a (and a second polymorph 10aa), 11a (and its deuterochloroform monosolvate 11aa), 12a (as its dichloromethane monosolvate), 14a, 15a (as its deuterochloroform monosolvate 15aa, in which the solvent molecule is disordered over two positions), 9b, 11b, 13b and 15b. The structures of 11a, 15a, 11b and 15b form an isotypic set, and those of compounds 10aa and 14a form an isotypic pair. All structures have Z′ = 1. The gold(III) centres show square-planar coordination geometry and the chalcogenide atoms show approximately tetrahedral angles (except for the very wide angle in 12a, probably associated with the bulky t-butyl groups). The bond lengths at the gold atoms are lengthened with respect to the known gold(I) derivatives, and demonstrate a considerable trans influence of S and Se donor atoms on a trans Au—Cl bond. Each compound with an isopropyl group shows a short intramolecular contact of the type C—Hmethine⋯Xcis; these may be regarded as intramolecular ‘weak’ hydrogen bonds, and they determine the orientation of the AuX3 groups. The molecular packing is analysed in terms of various short contacts such as weak hydrogen bonds C—H⋯X and contacts between the heavier atoms, such as X⋯X (9a, 10aa, 11aa, 15aa and 9b), S⋯S (10aa, 11a and 12a) and S⋯Cl (10a). The packing of the polymorphs 10a and 10aa is thus quite different. The solvent molecules take part in C—H⋯Cl hydrogen bonds; for 15aa, a disordered solvent region at z ≃ 0 is observed. Structure 13b involves unusual inversion-symmetric dimers with Se⋯Au and Se⋯Br contacts, further connected by Br⋯Br contacts.urn:issn:2056-9890Upmann, D.Bockfeld, D.Jones, P.G.Târcoveanu, E.text/htmlThe structures of ten phosphane chalcogenide complexes of gold(III) halides are presented and compared.doi:10.1107/S2056989024002032CRYSTAL STRUCTURE; GOLD(III) HALIDES; PHOSPHANE CHALCOGENIDES; SECONDARY INTERACTIONS2024-03-12Crystal structures of ten phosphane chalcogenide complexes of gold(III) chloride and bromideThe structures of ten phosphane chalcogenide complexes of gold(III) halides, with general formula R13–nR2nPEAuX3 (R1 = t-butyl; R2 = i-propyl; n = 0 to 3; E = S or Se; X = Cl or Br) are presented. The eight possible chlorido derivatives are: 9a, n = 3, E = S; 10a, n = 2, E = S; 11a, n = 1, E = S; 12a, n = 0, E = S; 13a, n = 3, E = Se; 14a, n = 2, E = Se; 15a, n = 1, E = Se; and 16a, n = 0, E = Se, and the corresponding bromido derivatives are 9b–16b in the same order. Structures were obtained for 9a, 10a (and a second polymorph 10aa), 11a (and its deuterochloroform monosolvate 11aa), 12a (as its dichloromethane monosolvate), 14a, 15a (as its deuterochloroform monosolvate 15aa, in which the solvent molecule is disordered over two positions), 9b, 11b, 13b and 15b. The structures of 11a, 15a, 11b and 15b form an isotypic set, and those of compounds 10aa and 14a form an isotypic pair. All structures have Z′ = 1. The gold(III) centres show square-planar coordination geometry and the chalcogenide atoms show approximately tetrahedral angles (except for the very wide angle in 12a, probably associated with the bulky t-butyl groups). The bond lengths at the gold atoms are lengthened with respect to the known gold(I) derivatives, and demonstrate a considerable trans influence of S and Se donor atoms on a trans Au—Cl bond. Each compound with an isopropyl group shows a short intramolecular contact of the type C—Hmethine⋯Xcis; these may be regarded as intramolecular ‘weak’ hydrogen bonds, and they determine the orientation of the AuX3 groups. The molecular packing is analysed in terms of various short contacts such as weak hydrogen bonds C—H⋯X and contacts between the heavier atoms, such as X⋯X (9a, 10aa, 11aa, 15aa and 9b), S⋯S (10aa, 11a and 12a) and S⋯Cl (10a). The packing of the polymorphs 10a and 10aa is thus quite different. The solvent molecules take part in C—H⋯Cl hydrogen bonds; for 15aa, a disordered solvent region at z ≃ 0 is observed. Structure 13b involves unusual inversion-symmetric dimers with Se⋯Au and Se⋯Br contacts, further connected by Br⋯Br contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext802024-03-12355research communicationshttps://creativecommons.org/licenses/by/4.0/March 2024Acta Crystallographica Section E: Crystallographic Communications42056-98902056-9890med@iucr.org369Crystal structure of (S)-5-(3-acetyl-5-chloro-2-ethoxy-6-fluorophenyl)-2-oxazolidinone
http://scripts.iucr.org/cgi-bin/paper?jy2039
The structure of (S)-5-(3-acetyl-5-chloro-2-ethoxy-6-fluorophenyl)-2-oxazolidinone, C13H13ClFNO4, at 100 K has monoclinic (P21) symmetry. The compound has a polymeric structure propagated by a screw axis parallel to the b axis with N—H⋯O hydrogen bonding. It is of interest with respect to efforts in the synthesis of a candidate anticancer drug, parsaclisib.urn:issn:2056-9890Li, V.Yap, G.P.A.Ni, C.text/htmlThe structure of (S)-5-(3-acetyl-5-chloro-2-ethoxy-6-fluorophenyl)-2-oxazolidinone has been determined to establish its absolute configuration in efforts to synthesize an anticancer drug candidate, parsaclisib.doi:10.1107/S2056989024001920CRYSTAL STRUCTURE; OXAZOLIDINONE; PARSACLIB; PHARMACEUTICAL; KINASE INHIBITOR; ANTI-CANCER; DRUG2024-03-19Crystal structure of (S)-5-(3-acetyl-5-chloro-2-ethoxy-6-fluorophenyl)-2-oxazolidinoneThe structure of (S)-5-(3-acetyl-5-chloro-2-ethoxy-6-fluorophenyl)-2-oxazolidinone, C13H13ClFNO4, at 100 K has monoclinic (P21) symmetry. The compound has a polymeric structure propagated by a screw axis parallel to the b axis with N—H⋯O hydrogen bonding. It is of interest with respect to efforts in the synthesis of a candidate anticancer drug, parsaclisib.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98904377med@iucr.org80research communicationshttps://creativecommons.org/licenses/by/4.0/March 2024Acta Crystallographica Section E: Crystallographic Communications3752024-03-19The unanticipated oxidation of a tertiary amine in a tetracyclic glyoxal-cyclam condensate yielding zinc(II) coordinated to a sterically hindered amine oxide
http://scripts.iucr.org/cgi-bin/paper?pk2704
The complex, trichlorido(1,4,11-triaza-8-azoniatetracyclo[6.6.2.04,16.011,15]hexadecane 1-oxide-κO)zinc(II) monohydrate, [ZnCl3(C12H23N4O)]·H2O, (I), has monoclinic symmetry (space group P21/n) at 120 K. The zinc(II) center adopts a slightly distorted tetrahedral coordination geometry and is coordinated by three chlorine atoms and the oxygen atom of the oxidized tertiary amine of the tetracycle. The amine nitrogen atom, inside the ligand cleft, is protonated and forms a hydrogen bond to the oxygen of the amine oxide. Additional hydrogen-bonding interactions involve the protonated amine, the water solvate oxygen atom, and one of the chloro ligands.urn:issn:2056-9890Hubin, D.J.Cunningham, B.M.Hubin, T.J.Ebel, J.P.Krause, J.A.Oliver, A.G.text/htmlThe crystal structure of the first reported glyoxal–tetraazamacrocycle condensate amine oxide is presented. The sterically hindered oxidized amine binds zinc(II) through the oxygen atom in its folded cleft, with an internal hydrogen bond across the cleft between the oxygen and a protonated tertiary nitrogen.doi:10.1107/S2056989024001889CRYSTAL STRUCTURE; ZINC(II); GLYOXAL-CYCLAM2024-03-06The unanticipated oxidation of a tertiary amine in a tetracyclic glyoxal-cyclam condensate yielding zinc(II) coordinated to a sterically hindered amine oxideThe complex, trichlorido(1,4,11-triaza-8-azoniatetracyclo[6.6.2.04,16.011,15]hexadecane 1-oxide-κO)zinc(II) monohydrate, [ZnCl3(C12H23N4O)]·H2O, (I), has monoclinic symmetry (space group P21/n) at 120 K. The zinc(II) center adopts a slightly distorted tetrahedral coordination geometry and is coordinated by three chlorine atoms and the oxygen atom of the oxidized tertiary amine of the tetracycle. The amine nitrogen atom, inside the ligand cleft, is protonated and forms a hydrogen bond to the oxygen of the amine oxide. Additional hydrogen-bonding interactions involve the protonated amine, the water solvate oxygen atom, and one of the chloro ligands.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext80research communicationshttps://creativecommons.org/licenses/by/4.0/March 2024Acta Crystallographica Section E: Crystallographic Communications2024-03-062056-98902056-98904med@iucr.orgCrystal structure of 1-{4-[bis(4-methylphenyl)amino]phenyl}ethene-1,2,2-tricarbonitrile
http://scripts.iucr.org/cgi-bin/paper?nx2005
The title compound, C25H18N4, crystallizes in the centrosymmetric orthorhombic space group Pbca, with eight molecules in the unit cell. The main feature noticeable in the structure is the impact of the tricyanovinyl (TCV) group in forcing partial planarity of the portion of the molecule carrying the TCV group and directing the molecular packing in the solid state, resulting in the formation of π-stacks of dimers within the unit cell. Short π–π stack closest atom-to-atom distances of 3.444 Å are observed. Such motif patterns are favorable as they are thought to be conducive for better charge transport in organic semiconductors, which results in enhanced device performance. Intramolecular charge transfer is evident from the shortening in the observed experimental bond lengths. The nitrogen atoms (of the cyano groups) are involved in extensive short contacts, primarily through C—H⋯NC interactions with distances of 2.637 Å.urn:issn:2056-9890Bader, M.M.Pham, P.-T.text/htmlThe title compound crystallizes in the centrosymmetric orthorhombic space group Pbca, with 8 molecules in the unit cell. The main feature noticeable in the structure is the impact of the tricyanovinyl (TCV) group in forcing partial planarity of the portion of the molecule carrying the TCV group and directing the molecular packing in the solid state, resulting in the formation of π-stacks of dimers within the unit cell.doi:10.1107/S2056989024001804CRYSTAL STRUCTURE; DONOR/ACCEPTOR; DYES; TRIPHENYLAMINE; TRICYANOVINYL2024-02-29Crystal structure of 1-{4-[bis(4-methylphenyl)amino]phenyl}ethene-1,2,2-tricarbonitrileThe title compound, C25H18N4, crystallizes in the centrosymmetric orthorhombic space group Pbca, with eight molecules in the unit cell. The main feature noticeable in the structure is the impact of the tricyanovinyl (TCV) group in forcing partial planarity of the portion of the molecule carrying the TCV group and directing the molecular packing in the solid state, resulting in the formation of π-stacks of dimers within the unit cell. Short π–π stack closest atom-to-atom distances of 3.444 Å are observed. Such motif patterns are favorable as they are thought to be conducive for better charge transport in organic semiconductors, which results in enhanced device performance. Intramolecular charge transfer is evident from the shortening in the observed experimental bond lengths. The nitrogen atoms (of the cyano groups) are involved in extensive short contacts, primarily through C—H⋯NC interactions with distances of 2.637 Å.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext32056-98902056-9890med@iucr.org342802024-02-29339March 2024Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/‘Young crystallographers’ rejuvenate crystallography in Germany
http://scripts.iucr.org/cgi-bin/paper?dj2076
Since its founding in 2013, the Young Crystallographers (YC) have become one of the most active working groups not only within their parent organization, the German Crystallographic Society (DGK), but also among other young crystallographers' groups in Europe and the world. The aim of the YC is and always has been to support early-career researchers in the diverse fields of crystallography and the rejuvenation of the field on a national scale. Over the past decade, we have curated events, platforms, and educational content tailored to foster collaboration and knowledge transfer among young crystallographers. In this article, we introduce our group and show how this active and diverse community has shaped the rejuvenation of crystallography in Germany, strengthened by the support of our national society.urn:issn:2056-9890Meurer, F.Möbs, J.Nentwich, M.Weigel, T.Wöhrle, J.-P.text/htmlThe Young Crystallographers were founded in 2013 within the German Crystallographic Association and have revitalized the field of crystallography by establishing collaboration and support among early career researchers, organizing educational events, and promoting scientific contributions on national and international stages.doi:10.1107/S2056989024001695EDUCATION; TEACHING; YOUNG SCIENTISTS; CRYSTALLOGRAPHIC ASSOCIATIONS2024-02-27‘Young crystallographers’ rejuvenate crystallography in GermanySince its founding in 2013, the Young Crystallographers (YC) have become one of the most active working groups not only within their parent organization, the German Crystallographic Society (DGK), but also among other young crystallographers' groups in Europe and the world. The aim of the YC is and always has been to support early-career researchers in the diverse fields of crystallography and the rejuvenation of the field on a national scale. Over the past decade, we have curated events, platforms, and educational content tailored to foster collaboration and knowledge transfer among young crystallographers. In this article, we introduce our group and show how this active and diverse community has shaped the rejuvenation of crystallography in Germany, strengthened by the support of our national society.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext80March 2024Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2522024-02-272056-98902056-98903255med@iucr.orgCrystal structure of tetrakis(μ-2-hydroxy-3,5-diisopropylbenzoato)bis[(dimethyl sulfoxide)copper(II)]
http://scripts.iucr.org/cgi-bin/paper?ev2003
Metal complexes of 3,5-diisopropylsalicylate are reported to have anti-inflammatory and anti-convulsant activities. The title binuclear copper complex, [Cu2(C13H17O3)4(C2H6OS)2] or [Cu(II)2(3,5-DIPS)4(DMSO)2], contains two five-coordinate copper atoms that are bridged by four 3,5-diisopropylsalicylate ligands and capped by two axial dimethyl sulfoxide (DMSO) moieties. Each copper atom is attached to four oxygen atoms in an almost square-planar fashion, with the addition of a DMSO ligand in an apical position leading to a square-pyramidal arrangement. The hydroxy group of the diisopropylsalicylate ligands participates in intramolecular O—H⋯O hydrogen-bonding interactions.urn:issn:2056-9890Shlian, D.G.Summers, R.H.Martinez, K.Upmacis, R.K.text/htmlA solution of 2-hydroxy-3,5-bis(1-methylethyl)benzoic acid copper(II) hydrate (C26H34CuO6·xH2O), also known as copper(II) 3,5-diisopropylsalicylate hydrate, in dimethyl sulfoxide (DMSO) affords crystals of tetrakis-3,5-diisopropylsalicylatobis-dimethylsulfoxidodicopper(II), [Cu(II)2(3,5-DIPS)4(DMSO)2], upon evaporation. The structure has an empirical formula of [Cu2(C13H17O3)4(C2H6OS)2] and consists of a centrosymmetric binuclear copper complex surrounded by four 3,5-diisopropylsalicylate ligands. Each copper atom is attached to four oxygen atoms in an almost square-planar fashion, with the addition of a DMSO ligand in an apical position leading to a square-pyramidal arrangement.doi:10.1107/S205698902400166XCRYSTAL STRUCTURE; BINUCLEAR COPPER; 3,5-DIISOPROPYLSALICYLATE; DIMETHYL SULFOXIDE.2024-02-27Crystal structure of tetrakis(μ-2-hydroxy-3,5-diisopropylbenzoato)bis[(dimethyl sulfoxide)copper(II)]Metal complexes of 3,5-diisopropylsalicylate are reported to have anti-inflammatory and anti-convulsant activities. The title binuclear copper complex, [Cu2(C13H17O3)4(C2H6OS)2] or [Cu(II)2(3,5-DIPS)4(DMSO)2], contains two five-coordinate copper atoms that are bridged by four 3,5-diisopropylsalicylate ligands and capped by two axial dimethyl sulfoxide (DMSO) moieties. Each copper atom is attached to four oxygen atoms in an almost square-planar fashion, with the addition of a DMSO ligand in an apical position leading to a square-pyramidal arrangement. The hydroxy group of the diisopropylsalicylate ligands participates in intramolecular O—H⋯O hydrogen-bonding interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext338med@iucr.org2056-98902056-98903Acta Crystallographica Section E: Crystallographic CommunicationsMarch 2024research communicationshttps://creativecommons.org/licenses/by/4.0/2024-02-2733580Crystal structure and Hirshfeld surface analysis of 4-oxo-3-phenyl-2-sulfanylidene-5-(thiophen-2-yl)-3,4,7,8,9,10-hexahydro-2H-pyrido[1,6-a:2,3-d′]dipyrimidine-6-carbonitrile
http://scripts.iucr.org/cgi-bin/paper?tx2082
In the title compound, C21H15N5OS2, molecular pairs are linked by N—H⋯N hydrogen bonds along the c-axis direction and C—H⋯S and C—H⋯O hydrogen bonds along the b-axis direction, with R22(12) and R22(16) motifs, respectively, thus forming layers parallel to the (10\overline{4}) plane. In addition, C=S⋯π and C≡N⋯π interactions between the layers ensure crystal cohesion. The Hirshfeld surface analysis indicates that the major contributions to the crystal packing are H⋯H (43.0%), C⋯H/H⋯C (16.9%), N⋯H/H⋯N (11.3%) and S⋯H/H⋯S (10.9%) interactions.urn:issn:2056-9890Naghiyev, F.N.Khrustalev, V.N.Akkurt, M.Mamedov, H.M.Bhattarai, A.Khalilov, A.N.Mamedov, İ.G.text/htmlIn the title compound, molecular pairs are linked by N—H⋯N hydrogen bonds along the c-axis direction and C—H⋯S and C—H⋯O hydrogen bonds along the b-axis direction, with R_{2}^{2}(12) and R_{2}^{2}(16) motifs, respectively, thus forming layers parallel to the (10\overline{4}) plane. In addition, C=S⋯π and C≡N⋯π interactions between the layers ensure crystal cohesion.doi:10.1107/S2056989024001658CRYSTAL STRUCTURE; HYDROGEN BONDS; HETEROCYCLE; HIRSHFELD SURFACE ANALYSIS2024-02-20Crystal structure and Hirshfeld surface analysis of 4-oxo-3-phenyl-2-sulfanylidene-5-(thiophen-2-yl)-3,4,7,8,9,10-hexahydro-2H-pyrido[1,6-a:2,3-d′]dipyrimidine-6-carbonitrileIn the title compound, C21H15N5OS2, molecular pairs are linked by N—H⋯N hydrogen bonds along the c-axis direction and C—H⋯S and C—H⋯O hydrogen bonds along the b-axis direction, with R22(12) and R22(16) motifs, respectively, thus forming layers parallel to the (10\overline{4}) plane. In addition, C=S⋯π and C≡N⋯π interactions between the layers ensure crystal cohesion. The Hirshfeld surface analysis indicates that the major contributions to the crystal packing are H⋯H (43.0%), C⋯H/H⋯C (16.9%), N⋯H/H⋯N (11.3%) and S⋯H/H⋯S (10.9%) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98903329med@iucr.org80research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsMarch 20243252024-02-20Synthesis, crystal structure and Hirshfeld surface analysis of N-(6-acetyl-1-nitronaphthalen-2-yl)acetamide
http://scripts.iucr.org/cgi-bin/paper?zn2035
The title compound, C14H12N2O4, was obtained from 2-acetyl-6-aminonaphthalene through two-step reactions of acetylation and nitration. The molecule comprises the naphthalene ring system consisting of functional systems bearing a acetyl group (C-2), a nitro group (C-5), and an acetylamino group (C-6). In the crystal, the molecules are assembled into two-dimensional sheet-like structures by intermolecular N—H⋯O and C—H⋯O hydrogen-bonding interactions. Hirshfeld surface analysis illustrates that the most important contributions to the crystal packing are from O⋯H/H⋯O (43.7%), H⋯H (31.0%), and C⋯H/H⋯C (8.5%) contacts.urn:issn:2056-9890Shi, X.-W.Zheng, S.-J.Lu, Q.-Q.Li, G.Zhou, Y.text/htmlThe title compound, C14H12N2O4, obtained from 2-acetyl-6-aminonaphthalene through two-step reactions of acetylation and nitration, is a Prodane fluorescent dye. In the crystal, the molecules are assembled into two-dimensional sheet-like structures by intermolecular N—H⋯O hydrogen bonding and π–π stacking interactions. Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from O⋯H/H⋯O (43.7%), H⋯H (31.0%), and C⋯H/H⋯C (8.5%) contacts.doi:10.1107/S2056989024001609CRYSTAL STRUCTURE; NAPHTHALENE RING; HYDROGEN BONDING; HIRSHFELD SURFACE ANALYSIS2024-03-06Synthesis, crystal structure and Hirshfeld surface analysis of N-(6-acetyl-1-nitronaphthalen-2-yl)acetamideThe title compound, C14H12N2O4, was obtained from 2-acetyl-6-aminonaphthalene through two-step reactions of acetylation and nitration. The molecule comprises the naphthalene ring system consisting of functional systems bearing a acetyl group (C-2), a nitro group (C-5), and an acetylamino group (C-6). In the crystal, the molecules are assembled into two-dimensional sheet-like structures by intermolecular N—H⋯O and C—H⋯O hydrogen-bonding interactions. Hirshfeld surface analysis illustrates that the most important contributions to the crystal packing are from O⋯H/H⋯O (43.7%), H⋯H (31.0%), and C⋯H/H⋯C (8.5%) contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98904med@iucr.org80Acta Crystallographica Section E: Crystallographic CommunicationsMarch 2024research communicationshttps://creativecommons.org/licenses/by/4.0/2024-03-06Synthesis and crystal structures of bis[1-oxopyridin-2-olato(1−)]bis(pentafluorophenyl)silicon(IV)–tetrahydrofuran–pentane (2/1/1), bis[1-oxopyridin-2-olato(1−)]bis(p-tolyl)silicon(IV), and dimesitylbis[1-oxopyridin-2-olato(1−)]silicon(IV)
http://scripts.iucr.org/cgi-bin/paper?ee2004
The neutral organosilicon(IV) complex, (C6F5)2Si(OPO)2 (OPO = 1-oxopyridin-2-one, C5H4NO2), was synthesized from (C6F5)2Si(OCH3)2 and 2 equiv. of 1-hydroxypyridin-2-one in tetrahydrofuran (THF). Single crystals grown from the diffusion of n-pentane into a THF solution were identified as a THF hemisolvate and an n-pentane hemisolvate, (C6F5)2Si(OPO)2·0.5THF·0.5C5H12 (1). p-Tolyl2Si(OPO)2 (2) and mesityl2Si(OPO)2 (3) crystallized directly from reaction mixtures of 2 equiv. of Me3Si(OPO) with p-tolyl2SiCl2 and mesityl2SiCl2, respectively, in acetonitrile. The oxygen-bonded carbon and nitrogen atoms of the OPO ligands in 1, 2, and 3 were modeled as disordered indicating co-crystallization of up to three possible diastereomers in each. Solution NMR studies support the presence of exclusively the all-cis isomer in 1 and multiple isomers in 2. Poor solubility of 3 limited its characterization in solution.urn:issn:2056-9890Kraft, B.M.Brennessel, W.W.Andrews, J.W.Viggiani, M.T.Kittrell, N.F.Heckman, M.T.text/htmlThree hexacoordinated bis(aryl)silicon(IV) complexes of 1-oxopyridin-2-one (OPO) are reported, each of which exhibit C/N site disorder in their pyridine rings. In (C6F5)2Si(OPO)2, the equal disorder ratios and solution NMR characterization together indicate the presence of a single totally asymmetric ON-trans-OC isomer. Unequal disorder ratios in p-tolyl2Si(OPO)2 and in mesityl2Si(OPO)2 indicate the presence of up to three isomers.doi:10.1107/S2056989024001543CRYSTAL STRUCTURE; SILICON; PYRIDINONE; PYRIDINE N-OXIDE2024-02-20Synthesis and crystal structures of bis[1-oxopyridin-2-olato(1−)]bis(pentafluorophenyl)silicon(IV)–tetrahydrofuran–pentane (2/1/1), bis[1-oxopyridin-2-olato(1−)]bis(p-tolyl)silicon(IV), and dimesitylbis[1-oxopyridin-2-olato(1−)]silicon(IV)The neutral organosilicon(IV) complex, (C6F5)2Si(OPO)2 (OPO = 1-oxopyridin-2-one, C5H4NO2), was synthesized from (C6F5)2Si(OCH3)2 and 2 equiv. of 1-hydroxypyridin-2-one in tetrahydrofuran (THF). Single crystals grown from the diffusion of n-pentane into a THF solution were identified as a THF hemisolvate and an n-pentane hemisolvate, (C6F5)2Si(OPO)2·0.5THF·0.5C5H12 (1). p-Tolyl2Si(OPO)2 (2) and mesityl2Si(OPO)2 (3) crystallized directly from reaction mixtures of 2 equiv. of Me3Si(OPO) with p-tolyl2SiCl2 and mesityl2SiCl2, respectively, in acetonitrile. The oxygen-bonded carbon and nitrogen atoms of the OPO ligands in 1, 2, and 3 were modeled as disordered indicating co-crystallization of up to three possible diastereomers in each. Solution NMR studies support the presence of exclusively the all-cis isomer in 1 and multiple isomers in 2. Poor solubility of 3 limited its characterization in solution.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98903324med@iucr.org80Acta Crystallographica Section E: Crystallographic CommunicationsMarch 2024research communicationshttps://creativecommons.org/licenses/by/4.0/3182024-02-20Crystal structure and Hirshfeld surface analysis of 3-phenyl-1-{3-[(3-phenylquinoxalin-2-yl)oxy]propyl}-1,2-dihydroquinoxalin-2-one
http://scripts.iucr.org/cgi-bin/paper?vm2295
In the title compound, C31H24N4O2, the quinoxaline units are distinctly non-planar and twisted end-to-end. In the crystal, C—H⋯O and C—H⋯N hydrogen bonds link the molecules into chains extending along the a-axis direction. The chains are linked through π-stacking interactions between inversion-related quinoxaline moieties.urn:issn:2056-9890Abad, N.Mague, J.T.Alsubari, A.Essassi, E.M.Alzahrani, A.Y.A.Ramli, Y.text/htmlIn the title compound, the quinoxaline units are distinctly non-planar and twisted end-to-end. In the crystal, C—H⋯O and C—H⋯N hydrogen bonds link the molecules into chains extending along the a-axis direction. The chains are linked through π-stacking interactions between inversion-related quinoxaline moieties.doi:10.1107/S2056989024001518CRYSTAL STRUCTURE; QUINOXALINE; ALKYLATION; HYDROGEN BOND; [PI]-STACKING; HIRSHFELD SURFACE ANALYSIS2024-02-20Crystal structure and Hirshfeld surface analysis of 3-phenyl-1-{3-[(3-phenylquinoxalin-2-yl)oxy]propyl}-1,2-dihydroquinoxalin-2-oneIn the title compound, C31H24N4O2, the quinoxaline units are distinctly non-planar and twisted end-to-end. In the crystal, C—H⋯O and C—H⋯N hydrogen bonds link the molecules into chains extending along the a-axis direction. The chains are linked through π-stacking interactions between inversion-related quinoxaline moieties.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext80March 2024Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications3002024-02-202056-98902056-98903304med@iucr.orgSynthesis, characterization, and crystal structure of 2-(2-azidophenyl)-3-oxo-3H-indole 1-oxide
http://scripts.iucr.org/cgi-bin/paper?dx2056
An attempt to explore the reactivity of the nitro group in the presence of gold catalysis in comparison to the azide group yielded intriguing results. Surprisingly, only the nitro group exhibited reactivity, ultimately giving rise to the formation of the title isatogen, C14H8N4O2. In the crystal structure, weak C—H⋯O hydrogen bonds and π–π stacking interactions link the molecules. The structure exhibits disorder of the molecule.urn:issn:2056-9890Dhote, P.Tothadi, S.Ramana, C.V.text/htmlAn attempt to explore the reactivity of the nitro group in the presence of gold catalysis in comparison to the azide group yielded intriguing results. Surprisingly, only the nitro group exhibited reactivity, ultimately giving rise to the formation of the title isatogen.doi:10.1107/S2056989024001440CRYSTAL STRUCTURE; ISATOGEN; REACTIVITY; HYDROGEN BONDING2024-02-20Synthesis, characterization, and crystal structure of 2-(2-azidophenyl)-3-oxo-3H-indole 1-oxideAn attempt to explore the reactivity of the nitro group in the presence of gold catalysis in comparison to the azide group yielded intriguing results. Surprisingly, only the nitro group exhibited reactivity, ultimately giving rise to the formation of the title isatogen, C14H8N4O2. In the crystal structure, weak C—H⋯O hydrogen bonds and π–π stacking interactions link the molecules. The structure exhibits disorder of the molecule.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98903313med@iucr.org80https://creativecommons.org/licenses/by/4.0/research communicationsMarch 2024Acta Crystallographica Section E: Crystallographic Communications2024-02-20310Crystal structure of the sodium salt of mesotrione: a triketone herbicide
http://scripts.iucr.org/cgi-bin/paper?oi2003
The crystal structure of the sodium salt of mesotrione, namely, catena-poly[[sodium-μ3-2-[(4-methanesulfonyl-2-nitrophenyl)carbonyl]-3-oxocyclohex-1-en-1-olato] ethanol monosolvate], {[Na(C14H12NO7S)]C2H5OH}n, is described. The X-ray structural analysis results reveal that the coordination sphere is established by two chelating O atoms, the O atom of the coordinated ethanol molecule, and an O atom from the methylsulfonyl group of a neighboring molecule. Simultaneously, an O atom of the cyclohexane fragment serves as a bridge to a neighboring sodium ion, forming a flat Na–O–Na–O quadrangle, thereby forming a mono-periodic polymer. The structure displays O—H⋯O hydrogen bonds and C—H⋯O short contacts. Thermogravimetric analysis (TGA) data indicate that the sodium salt of mesotrione decomposes in four stages.urn:issn:2056-9890Bereziuk, O.Gubina, K.Trush, V.Ovchynnikov, V.text/htmlThe crystal structure of the sodium salt of mesotrione [2-(4-methylsulfonyl-2-nitrobenzoyl)cyclohexane-1,3-dione] is described. A one-dimensional polymer is formed by the coordination of all functional groups except the NO2 group. The coordination number of the sodium atom in the compound is 5.doi:10.1107/S2056989024001439MESOTRIONE; HERBICIDES; SODIUM SALT; CRYSTAL STRUCTURE; TGA ANALYSIS2024-02-16Crystal structure of the sodium salt of mesotrione: a triketone herbicideThe crystal structure of the sodium salt of mesotrione, namely, catena-poly[[sodium-μ3-2-[(4-methanesulfonyl-2-nitrophenyl)carbonyl]-3-oxocyclohex-1-en-1-olato] ethanol monosolvate], {[Na(C14H12NO7S)]C2H5OH}n, is described. The X-ray structural analysis results reveal that the coordination sphere is established by two chelating O atoms, the O atom of the coordinated ethanol molecule, and an O atom from the methylsulfonyl group of a neighboring molecule. Simultaneously, an O atom of the cyclohexane fragment serves as a bridge to a neighboring sodium ion, forming a flat Na–O–Na–O quadrangle, thereby forming a mono-periodic polymer. The structure displays O—H⋯O hydrogen bonds and C—H⋯O short contacts. Thermogravimetric analysis (TGA) data indicate that the sodium salt of mesotrione decomposes in four stages.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext32056-98902056-9890med@iucr.org299802024-02-16296March 2024Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/Omadacycline dihydrate, C29H40N4O7·2H2O, from X-ray powder diffraction data
http://scripts.iucr.org/cgi-bin/paper?hb8082
The crystal structure of the title compound {systematic name: (4S,4aS,5aR,12aR)-4,7-bis(dimethylamino)-9-[(2,2-dimethylpropylamino)methyl]-1,10,11,12a-tetrahydroxy-3,12-dioxo-4a,5,5a,6-tetrahydro-4H-tetracene-2-carboxamide dihydrate, C29H40N4O7·2H2O} has been solved and refined using synchrotron X-ray powder diffraction data: it crystallizes in space group R3 with a = 24.34430 (7), c = 14.55212 (4) Å, V = 7468.81 (2) Å3 and Z = 9. Most of the hydrogen bonds are intramolecular, but two classical N—H⋯O intermolecular hydrogen bonds (along with probable weak C—H⋯O and C—H⋯N hydrogen bonds) link the molecules into a three-dimensional framework. The framework contains voids, which contain disordered water molecules. Keto–enol tautomerism is apparently important in this molecule, and the exact molecular structure is ambiguous.urn:issn:2056-9890Kaduk, J.A.Boaz, N.C.Gates-Rector, S.Gindhart, A.M.Blanton, T.N.text/htmlThe crystal structure of omadacycline dihydrate has been solved and refined using synchrotron X-ray powder diffraction data.doi:10.1107/S2056989024001403POWDER DIFFRACTION; OMADACYCLINE; NUZYRA; RIETVELD REFINEMENT2024-02-16Omadacycline dihydrate, C29H40N4O7·2H2O, from X-ray powder diffraction dataThe crystal structure of the title compound {systematic name: (4S,4aS,5aR,12aR)-4,7-bis(dimethylamino)-9-[(2,2-dimethylpropylamino)methyl]-1,10,11,12a-tetrahydroxy-3,12-dioxo-4a,5,5a,6-tetrahydro-4H-tetracene-2-carboxamide dihydrate, C29H40N4O7·2H2O} has been solved and refined using synchrotron X-ray powder diffraction data: it crystallizes in space group R3 with a = 24.34430 (7), c = 14.55212 (4) Å, V = 7468.81 (2) Å3 and Z = 9. Most of the hydrogen bonds are intramolecular, but two classical N—H⋯O intermolecular hydrogen bonds (along with probable weak C—H⋯O and C—H⋯N hydrogen bonds) link the molecules into a three-dimensional framework. The framework contains voids, which contain disordered water molecules. Keto–enol tautomerism is apparently important in this molecule, and the exact molecular structure is ambiguous.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2024-02-16292research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsMarch 202480med@iucr.org29532056-98902056-9890Crystal structure and characterization of a new one-dimensional copper(II) coordination polymer containing a 4-aminobenzoic acid ligand
http://scripts.iucr.org/cgi-bin/paper?zv2032
A CuII coordination polymer, catena-poly[[[aquacopper(II)]-bis(μ-4-aminobenzoato)-κ2N:O;κ2O:N] monohydrate], {[Cu(pABA)2(H2O)]·H2O}n (pABA = p-aminobenzoate, C7H4NO2−), was synthesized and characterized. It exhibits a one-dimensional chain structure extended into a three-dimensional supramolecular assembly through hydrogen bonds and π–π interactions. While the twinned crystal shows a metrically orthorhombic lattice and an apparent space group Pbcm, the true symmetry is monoclinic (space group P2/c), with disordered Cu atoms and mixed roles of water molecules (aqua ligand/crystallization water). The luminescence spectrum of the complex shows an emission at 345 nm, cf. 349 nm for pABAH.urn:issn:2056-9890Gogia, A.Novikov, E.M.Guzei, I.A.Fonari, M.S.Timofeeva, T.V.text/htmlA new coordination polymer based on CuII and 4-aminobenzoic acid is isolated and characterized using single-crystal X-ray diffraction, FTIR and fluorescence spectroscopy, and thermal analysis.doi:10.1107/S20569890240013364-AMINOBENZOIC ACID; PABAH; ONE-DIMENSIONAL COORDINATION POLYMER; CRYSTAL STRUCTURE2024-02-20Crystal structure and characterization of a new one-dimensional copper(II) coordination polymer containing a 4-aminobenzoic acid ligandA CuII coordination polymer, catena-poly[[[aquacopper(II)]-bis(μ-4-aminobenzoato)-κ2N:O;κ2O:N] monohydrate], {[Cu(pABA)2(H2O)]·H2O}n (pABA = p-aminobenzoate, C7H4NO2−), was synthesized and characterized. It exhibits a one-dimensional chain structure extended into a three-dimensional supramolecular assembly through hydrogen bonds and π–π interactions. While the twinned crystal shows a metrically orthorhombic lattice and an apparent space group Pbcm, the true symmetry is monoclinic (space group P2/c), with disordered Cu atoms and mixed roles of water molecules (aqua ligand/crystallization water). The luminescence spectrum of the complex shows an emission at 345 nm, cf. 349 nm for pABAH.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org33432056-98902056-98903302024-02-20https://creativecommons.org/licenses/by/4.0/research communicationsMarch 2024Acta Crystallographica Section E: Crystallographic Communications80Crystal structure of the tetraethylammonium salt of the non-steroidal anti-inflammatory drug nimesulide (polymorph II)
http://scripts.iucr.org/cgi-bin/paper?dx2059
The crystal structure of the tetraethylammonium salt of the non-steroidal anti-inflammatory drug nimesulide (polymorph II) (systematic name: tetraethylammonium N-methanesulfonyl-4-nitro-2-phenoxyanilinide), C8H20N+·C13H11N2O5S−, was determined using single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group P21/c with one tetraethylammonium cation and one nimesulide anion in the asymmetric unit. In the crystal, the ions are linked by C—H⋯N and C—H⋯O hydrogen bonds and C—H⋯π interactions. There are differences in the geometry of both the nimesulide anion and the tetraethylammonium cation in polymorphs I [Rybczyńska & Sikorski (2023). Sci. Rep. 13, 17268] and II of the title compound.urn:issn:2056-9890Rybczyńska, M.Sikorski, A.text/htmlThe crystal structure of the tetraethylammonium salt of the non-steroidal anti-inflammatory drug nimesulide (polymorph II), C8H20N+·C13H11N2O5S−, was determined using single-crystal X-ray diffraction. There are differences in the geometry of both the nimesulide anion and the tetraethylammonium cation in polymorphs I and II of the title compound.doi:10.1107/S2056989024001300NIMESULIDE; N-(4-NITRO-2-PHENOXYPHENYL)METHANESULFONAMIDE; TETRAETHYLAMMONIUM SALT; API; CRYSTAL STRUCTURE; POLYMORPHISM2024-02-20Crystal structure of the tetraethylammonium salt of the non-steroidal anti-inflammatory drug nimesulide (polymorph II)The crystal structure of the tetraethylammonium salt of the non-steroidal anti-inflammatory drug nimesulide (polymorph II) (systematic name: tetraethylammonium N-methanesulfonyl-4-nitro-2-phenoxyanilinide), C8H20N+·C13H11N2O5S−, was determined using single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group P21/c with one tetraethylammonium cation and one nimesulide anion in the asymmetric unit. In the crystal, the ions are linked by C—H⋯N and C—H⋯O hydrogen bonds and C—H⋯π interactions. There are differences in the geometry of both the nimesulide anion and the tetraethylammonium cation in polymorphs I [Rybczyńska & Sikorski (2023). Sci. Rep. 13, 17268] and II of the title compound.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98903317med@iucr.org80https://creativecommons.org/licenses/by/4.0/research communicationsMarch 2024Acta Crystallographica Section E: Crystallographic Communications2024-02-20314Crystal structure of 4-(benzo[d]thiazol-2-yl)-1,2-dimethyl-1H-pyrazol-3(2H)-one
http://scripts.iucr.org/cgi-bin/paper?yz2050
In the title compound, C12H11N3OS, the interplanar angle between the pyrazole and benzothiazole rings is 3.31 (7)°. In the three-dimensional molecular packing, the carbonyl oxygen acts as acceptor to four C—H donors (with one H⋯O as short as 2.25 Å), while one methyl hydrogen is part of the three-centre system H⋯(S, O). A double layer structure parallel to (\overline{1}01) can be recognized as a subsection of the packing.urn:issn:2056-9890Elboshi, H.A.Azzam, R.A.Elgemeie, G.H.Jones, P.G.text/htmlThe ring systems of 4-(benzo[d]thiazol-2-yl)-1,2-dimethyl-1H-pyrazol-3(2H)-one are almost coplanar. In the three-dimensional packing, the carbonyl oxygen accepts four weak hydrogen bonds.doi:10.1107/S2056989024001257CRYSTAL STRUCTURE; BENZOTHIAZOLE; PYRAZOLONE; WEAK HYDROGEN BONDS2024-02-16Crystal structure of 4-(benzo[d]thiazol-2-yl)-1,2-dimethyl-1H-pyrazol-3(2H)-oneIn the title compound, C12H11N3OS, the interplanar angle between the pyrazole and benzothiazole rings is 3.31 (7)°. In the three-dimensional molecular packing, the carbonyl oxygen acts as acceptor to four C—H donors (with one H⋯O as short as 2.25 Å), while one methyl hydrogen is part of the three-centre system H⋯(S, O). A double layer structure parallel to (\overline{1}01) can be recognized as a subsection of the packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextActa Crystallographica Section E: Crystallographic CommunicationsMarch 2024https://creativecommons.org/licenses/by/4.0/research communications2892024-02-1680291med@iucr.org2056-98902056-98903Syntheses, characterizations, crystal structures and Hirshfeld surface analyses of methyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, isopropyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate and tert-butyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate
http://scripts.iucr.org/cgi-bin/paper?jy2044
The crystal structures and Hirshfeld surface analyses of three similar compounds are reported. Methyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C21H23F2NO4), (I), crystallizes in the monoclinic space group C2/c with Z = 8, while isopropyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C23H27F2NO4), (II) and tert-butyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C24H29F2NO4), (III) crystallize in the orthorhombic space group Pbca with Z = 8. In the crystal structure of (I), molecules are linked by N—H⋯O and C—H⋯O interactions, forming a tri-periodic network, while molecules of (II) and (III) are linked by N—H⋯O, C—H⋯F and C—H⋯π interactions, forming layers parallel to (002). The cohesion of the molecular packing is ensured by van der Waals forces between these layers. In (I), the atoms of the 4-difluoromethoxyphenyl group are disordered over two sets of sites in a 0.647 (3): 0.353 (3) ratio. In (III), the atoms of the dimethyl group attached to the cyclohexane ring, and the two carbon atoms of the cyclohexane ring are disordered over two sets of sites in a 0.646 (3):0.354 (3) ratio.urn:issn:2056-9890Yıldırım, S. Ö.Akkurt, M.Pehlivanlar, E.Çetin, G.Şimşek, R.Butcher, R.J.Bhattarai, A.text/htmlIn the crystal structure of methyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate (I), molecules are linked by N—H⋯O and C—H⋯O interactions, forming a tri-periodic network, while molecules of isopropyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate (II) and tert-butyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate (III) are linked by N—H⋯O, C—H⋯F and C—H⋯π interactions, forming layers parallel to (002).doi:10.1107/S2056989024001233CRYSTAL STRUCTURE; 1,4-DIHYDROPYRIDINE RING; CYCLOHEXENE RING; QUINOLINE RING SYSTEM; DISORDER; VAN DER WAALS INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2024-02-08Syntheses, characterizations, crystal structures and Hirshfeld surface analyses of methyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, isopropyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate and tert-butyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylateThe crystal structures and Hirshfeld surface analyses of three similar compounds are reported. Methyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C21H23F2NO4), (I), crystallizes in the monoclinic space group C2/c with Z = 8, while isopropyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C23H27F2NO4), (II) and tert-butyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C24H29F2NO4), (III) crystallize in the orthorhombic space group Pbca with Z = 8. In the crystal structure of (I), molecules are linked by N—H⋯O and C—H⋯O interactions, forming a tri-periodic network, while molecules of (II) and (III) are linked by N—H⋯O, C—H⋯F and C—H⋯π interactions, forming layers parallel to (002). The cohesion of the molecular packing is ensured by van der Waals forces between these layers. In (I), the atoms of the 4-difluoromethoxyphenyl group are disordered over two sets of sites in a 0.647 (3): 0.353 (3) ratio. In (III), the atoms of the dimethyl group attached to the cyclohexane ring, and the two carbon atoms of the cyclohexane ring are disordered over two sets of sites in a 0.646 (3):0.354 (3) ratio.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext802024-02-08281https://creativecommons.org/licenses/by/4.0/research communicationsMarch 2024Acta Crystallographica Section E: Crystallographic Communications32056-98902056-9890med@iucr.org288Crystal structure of diethylammonium dioxido{Z)-N-[(pyridin-2-yl)carbonylazanidyl]pyridine-2-carboximidato}vanadate(1−) monohydrate
http://scripts.iucr.org/cgi-bin/paper?ev2002
The title compound, (C4H12N)[V(C12H8N4O2)O2]·H2O, was synthesized via aerial oxidation on refluxing picolinohydrazide with ethyl picolinate followed by addition of VIVO(acac)2 and diethylamine in methanol. It crystallizes in the triclinic crystal system in space group P\overline{1}. In the complex anion, the dioxidovanadium(V) moiety exhibits a distorted square-pyramidal geometry. In the crystal, extensive hydrogen bonding links the water molecule to two complex anions and one diethylammonium ion. One of the CH2 groups in the diethylamine is disordered over two sets of sites in a 0.7:0.3 ratio.urn:issn:2056-9890Mondal, B.text/htmlA new ionic dioxidovanadium(V) compound with an O,N,O donor ligand is reported. In the crystal, extensive hydrogen bonding is observed.doi:10.1107/S2056989024001166CRYSTAL STRUCTURE; DIOXIDOVANADIUM(V); O,N,O -DONOR SCHIFF-BASE; HYDROGEN BOND2024-02-08Crystal structure of diethylammonium dioxido{Z)-N-[(pyridin-2-yl)carbonylazanidyl]pyridine-2-carboximidato}vanadate(1−) monohydrateThe title compound, (C4H12N)[V(C12H8N4O2)O2]·H2O, was synthesized via aerial oxidation on refluxing picolinohydrazide with ethyl picolinate followed by addition of VIVO(acac)2 and diethylamine in methanol. It crystallizes in the triclinic crystal system in space group P\overline{1}. In the complex anion, the dioxidovanadium(V) moiety exhibits a distorted square-pyramidal geometry. In the crystal, extensive hydrogen bonding links the water molecule to two complex anions and one diethylammonium ion. One of the CH2 groups in the diethylamine is disordered over two sets of sites in a 0.7:0.3 ratio.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98903280med@iucr.org80https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsMarch 20242772024-02-08Crystal structures of sulfonamide protected bicyclic guanidines: (S)-8-{[(tert-butyldimethylsilyl)oxy]methyl}-1-[(2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran-5-yl)sulfonyl]-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidin-1-ium trifluoromethanesulfonate and (S)-8-(iodomethyl)-1-tosyl-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidin-1-ium iodide
http://scripts.iucr.org/cgi-bin/paper?dj2073
Two compounds, (S)-8-{[(tert-butyldimethylsilyl)oxy]methyl}-1-[(2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran-5-yl)sulfonyl]-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidin-1-ium trifluoromethanesulfonate, C27H46N3O4SSi+·CF3O3S−, (1) and (S)-8-(iodomethyl)-1-tosyl-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidin-1-ium iodide, C15H21IN3O2S+·I−, (2), have been synthesized and characterized. They are bicyclic guanidinium salts and were synthesized from N-(tert-butoxycarbonyl)-l-methionine (Boc-l-Met-OH). The guanidine is protected by a 2,2,4,6,7-pentamethyldihydrobenzofuran-5-sulfonyl (Pbf, 1) or a tosyl (2) group. In the crystals of both compounds, the guanidinium group is almost planar and the N–H forms an intramolecular hydrogen bond in a six-membered ring to the oxygen atom of the sulfonamide protecting group.urn:issn:2056-9890Alaboosh, J.M.H.Hill, S.P.Kariuki, B.M.Redman, J.E.text/htmlThe crystal structures of two sulfonamide-protected bicyclic guanidine salts are reported. The structures feature intramolecular N—H⋯O hydrogen bonding between the guanidinium group and the sulfonamide.doi:10.1107/S2056989024001129CRYSTAL STRUCTURE; BICYCLIC GUANIDINE; PBF; TOSYL2024-02-20Crystal structures of sulfonamide protected bicyclic guanidines: (S)-8-{[(tert-butyldimethylsilyl)oxy]methyl}-1-[(2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran-5-yl)sulfonyl]-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidin-1-ium trifluoromethanesulfonate and (S)-8-(iodomethyl)-1-tosyl-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidin-1-ium iodideTwo compounds, (S)-8-{[(tert-butyldimethylsilyl)oxy]methyl}-1-[(2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran-5-yl)sulfonyl]-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidin-1-ium trifluoromethanesulfonate, C27H46N3O4SSi+·CF3O3S−, (1) and (S)-8-(iodomethyl)-1-tosyl-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidin-1-ium iodide, C15H21IN3O2S+·I−, (2), have been synthesized and characterized. They are bicyclic guanidinium salts and were synthesized from N-(tert-butoxycarbonyl)-l-methionine (Boc-l-Met-OH). The guanidine is protected by a 2,2,4,6,7-pentamethyldihydrobenzofuran-5-sulfonyl (Pbf, 1) or a tosyl (2) group. In the crystals of both compounds, the guanidinium group is almost planar and the N–H forms an intramolecular hydrogen bond in a six-membered ring to the oxygen atom of the sulfonamide protecting group.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org30932056-98902056-98903052024-02-20research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsMarch 202480Structural characterization of a new samarium–sodium heterometallic coordination polymer
http://scripts.iucr.org/cgi-bin/paper?oo2002
Lanthanide-containing materials are of interest in the field of crystal engineering because of their unique properties and distinct structure types. In this context, a new samarium–sodium heterometallic coordination polymer, poly[tetrakis(μ2-2-formyl-6-methoxyphenolato)samarium(III)sodium(I)], {[SmNa(C8H7O3)4]·solvent}n (Sm-1), was synthesized and crystallized via slow evaporation from a mixture of ethanol and acetonitrile. The compound features alternating SmIII and NaI ions, which are linked by ortho-vanillin (o-vanillin) ligands to form a mono-periodic chain-like coordination polymer. The chains propagate along the [001] direction. Residual electron density of disordered solvent molecules in the void space could not be reasonably modeled, thus the SQUEEZE function was applied. The structural, vibrational, and optical properties are reported.urn:issn:2056-9890Hastings, A.M.Williams, A.Surbella III, R.G.Hixon, A.E.Arteaga, A.text/htmlThe crystal structure is reported of a new heterometallic samarium compound comprised of alternating SmIII and NaI metal centers bridged by o-vanillin ligands to create a helical chain.doi:10.1107/S2056989024001051CRYSTAL STRUCTURE; SAMARIUM; O-VANILLIN; COORDINATION POLYMER; LANTHANIDE CHEMISTRY2024-02-06Structural characterization of a new samarium–sodium heterometallic coordination polymerLanthanide-containing materials are of interest in the field of crystal engineering because of their unique properties and distinct structure types. In this context, a new samarium–sodium heterometallic coordination polymer, poly[tetrakis(μ2-2-formyl-6-methoxyphenolato)samarium(III)sodium(I)], {[SmNa(C8H7O3)4]·solvent}n (Sm-1), was synthesized and crystallized via slow evaporation from a mixture of ethanol and acetonitrile. The compound features alternating SmIII and NaI ions, which are linked by ortho-vanillin (o-vanillin) ligands to form a mono-periodic chain-like coordination polymer. The chains propagate along the [001] direction. Residual electron density of disordered solvent molecules in the void space could not be reasonably modeled, thus the SQUEEZE function was applied. The structural, vibrational, and optical properties are reported.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext270med@iucr.org2056-98902056-98903https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsMarch 20242672024-02-0680Crystal structure and Hirshfeld surface analysis of (Z)-N-{chloro[(4-ferrocenylphenyl)imino]methyl}-4-ferrocenylaniline N,N-dimethylformamide monosolvate
http://scripts.iucr.org/cgi-bin/paper?ox2002
The title molecule, [Fe2(C5H5)2(C23H17ClN2)]·C3H7NO, is twisted end to end and the central N/C/N unit is disordered. In the crystal, several C—H⋯π(ring) interactions lead to the formation of layers, which are connected by further C—H⋯π(ring) interactions. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (60.2%) and H⋯C/C⋯H (27.0%) interactions. Hydrogen bonding, C—H⋯π(ring) interactions and van der Waals interactions dominate the crystal packing.urn:issn:2056-9890Sghyar, R.Bentama, A.Haoudi, A.Mazzah, A.Mague, J.T.Hökelek, T.EL Hadrami, E.M.Sebbar, N.K.text/htmlThe molecule of the title compound is twisted end to end so that the ferrocenyl groups are nearly perpendicular to one another. The central N/C/N unit is disordered. In the crystal, several C—H⋯π(ring) interactions lead to the formation of layers parallel to (010), which are connected by further C—H⋯π(ring) interactions.doi:10.1107/S2056989024001002CRYSTAL STRUCTURE; FERROCENE; CARBAMIDIC CHLORIDE; HYDROGEN BOND; C-H...[PI](RING) INTERACTIONS2024-02-02Crystal structure and Hirshfeld surface analysis of (Z)-N-{chloro[(4-ferrocenylphenyl)imino]methyl}-4-ferrocenylaniline N,N-dimethylformamide monosolvateThe title molecule, [Fe2(C5H5)2(C23H17ClN2)]·C3H7NO, is twisted end to end and the central N/C/N unit is disordered. In the crystal, several C—H⋯π(ring) interactions lead to the formation of layers, which are connected by further C—H⋯π(ring) interactions. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (60.2%) and H⋯C/C⋯H (27.0%) interactions. Hydrogen bonding, C—H⋯π(ring) interactions and van der Waals interactions dominate the crystal packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext802024-02-02research communicationshttps://creativecommons.org/licenses/by/4.0/March 2024Acta Crystallographica Section E: Crystallographic Communications32056-98902056-9890med@iucr.org[4-(2-Aminoethyl)morpholine-κ2N,N′]dibromidocadmium(II): synthesis, crystal structure and Hirshfeld surface analysis
http://scripts.iucr.org/cgi-bin/paper?jq2033
The title compound, [CdBr2(C6H14N2O)], was synthesized upon complexation of 4-(2-aminoethyl)morpholine and cadmium(II) bromide tetrahydrate at 303 K. It crystallizes as a centrosymmetric dimer, with one cadmium atom, two bromine atoms and one N,N′-bidentate 4-(2-aminoethyl)morpholine ligand in the asymmetric unit. The metal atom is six-coordinated and has a distorted octahedral geometry. In the crystal, O⋯Cd interactions link the dimers into a polymeric double chain and intermolecular C—H⋯O hydrogen bonds form R22(6) ring motifs. Further C—H⋯Br and N—H⋯Br hydrogen bonds link the components into a three-dimensional network. As the N—H⋯Br hydrogen bonds are shorter than the C—H⋯Br interactions, they have a larger effect on the packing. A Hirshfeld surface analysis reveals that the largest contributions to the packing are from H⋯H (46.1%) and Br⋯H/H⋯Br (38.9%) interactions with smaller contributions from the O⋯H/H⋯O (4.7%), Br⋯Cd/Cd⋯Br (4.4%), O⋯Cd/Cd⋯O (3.5%), Br⋯Br (1.1%), Cd⋯H/H⋯Cd (0.9%), Br⋯O/O⋯Br (0.3%) and O⋯N/N⋯O (0.1%) contacts.urn:issn:2056-9890Chidambaranathan, B.Sivaraj, S.Vijayamathubalan, P.Abraham Rajasekar, S.Selvakumar, S.text/htmlThe title coordination compound was synthesized upon complexation of 4-(2-aminoethyl)morpholine and cadmium(II) bromide tetrahydrate at 303 K. It crystallizes as a centrosymmetric dimer, with one cadmium atom, two bromine atoms and one N,N′-bidentate 4-(2-aminoethyl)morpholine ligand in the asymmetric unit.doi:10.1107/S2056989024000963CRYSTAL STRUCTURE; MORPHOLINE LIGAND; HIRSHFELD SURFACE ANALYSIS; FTIR; NMR2024-02-08[4-(2-Aminoethyl)morpholine-κ2N,N′]dibromidocadmium(II): synthesis, crystal structure and Hirshfeld surface analysisThe title compound, [CdBr2(C6H14N2O)], was synthesized upon complexation of 4-(2-aminoethyl)morpholine and cadmium(II) bromide tetrahydrate at 303 K. It crystallizes as a centrosymmetric dimer, with one cadmium atom, two bromine atoms and one N,N′-bidentate 4-(2-aminoethyl)morpholine ligand in the asymmetric unit. The metal atom is six-coordinated and has a distorted octahedral geometry. In the crystal, O⋯Cd interactions link the dimers into a polymeric double chain and intermolecular C—H⋯O hydrogen bonds form R22(6) ring motifs. Further C—H⋯Br and N—H⋯Br hydrogen bonds link the components into a three-dimensional network. As the N—H⋯Br hydrogen bonds are shorter than the C—H⋯Br interactions, they have a larger effect on the packing. A Hirshfeld surface analysis reveals that the largest contributions to the packing are from H⋯H (46.1%) and Br⋯H/H⋯Br (38.9%) interactions with smaller contributions from the O⋯H/H⋯O (4.7%), Br⋯Cd/Cd⋯Br (4.4%), O⋯Cd/Cd⋯O (3.5%), Br⋯Br (1.1%), Cd⋯H/H⋯Cd (0.9%), Br⋯O/O⋯Br (0.3%) and O⋯N/N⋯O (0.1%) contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2024-02-08271research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsMarch 202480med@iucr.org27632056-98902056-9890Synthesis and crystal structure of the adduct between 2-pyridylselenyl chloride and isobutyronitrile
http://scripts.iucr.org/cgi-bin/paper?ex2079
The reaction between 2-pyridylselenenyl chloride and isobutyronitrile results in the formation of the corresponding cationic pyridinium-fused 1,2,4-selenodiazole, namely, 3-(propan-2-yl)-1,2,4-[1,2,4]selenadiazolo[4,5-a]pyridin-4-ylium chloride, C9H11N2Se+·Cl−, in high yield (89%). The structure of the compound, established by means of single-crystal X-ray analysis at 100 K, has monoclinic (P21/c) symmetry and revealed the presence of bifurcated chalcogen-hydrogen bonding Se⋯Cl−⋯H—Cl, and these non-covalent contacts were analysed by DFT calculations followed by a topological analysis of the electron-density distribution (ωB97XD/6-311++G** level of theory).urn:issn:2056-9890Temesgen, A.W.Sapronov, A.A.Kubasov, A.S.Novikov, A.S.Le, T.A.Tskhovrebov, A.G.text/htmlThe reaction between 2-pyridylselenenyl chloride and isobutyronitrile results in the formation of the corresponding cationic pyridinium-fused 1,2,4-selenodiazole, namely, 3-(propan-2-yl)-1,2,4-[1,2,4]selenadiazolo[4,5-a]pyridin-4-ylium chloride, C9H11N2Se+·Cl−, in high yield (89%). The bifurcated Se⋯Cl−⋯H—Cl chalcogen-hydrogen-bonding interactions were analysed by DFT followed by a topological analysis of the electron-density distribution.doi:10.1107/S2056989024000938CRYSTAL STRUCTURE; CHALCOGEN-HYDROGEN BONDING; 1,2,4-SELENODIAZOLE2024-02-06Synthesis and crystal structure of the adduct between 2-pyridylselenyl chloride and isobutyronitrileThe reaction between 2-pyridylselenenyl chloride and isobutyronitrile results in the formation of the corresponding cationic pyridinium-fused 1,2,4-selenodiazole, namely, 3-(propan-2-yl)-1,2,4-[1,2,4]selenadiazolo[4,5-a]pyridin-4-ylium chloride, C9H11N2Se+·Cl−, in high yield (89%). The structure of the compound, established by means of single-crystal X-ray analysis at 100 K, has monoclinic (P21/c) symmetry and revealed the presence of bifurcated chalcogen-hydrogen bonding Se⋯Cl−⋯H—Cl, and these non-covalent contacts were analysed by DFT calculations followed by a topological analysis of the electron-density distribution (ωB97XD/6-311++G** level of theory).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2472024-02-06March 2024Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/80med@iucr.org25132056-98902056-9890Crystal structure, Hirsfeld surface analysis and DFT study of N-(2-nitrophenyl)maleimide
http://scripts.iucr.org/cgi-bin/paper?vu2003
The title compound [systematic name: 1-(2-nitrophenyl)pyrrole-2,5-dione], C10H6N2O4, crystallizes in the monoclinic system (space group P21/n) with two molecules in the asymmetric unit, which are linked by C—H⋯O hydrogen bonds. Hirshfeld surface analysis showed that the most significant contributions to the crystal packing are from H⋯O/O⋯H, H⋯C/C⋯H and H⋯H interactions, which contribute 54.7%, 15.2% and 15.6%, respectively. A DFT study was conducted using three different levels of theory [(B3LYP/6–311+G(d,p), wB97XD/Def2TZVPP and LC-wpbe/6–311(2 d,2p)] in order to determine the stability, structural and electronic properties of the title molecule with a view to its potential applications and photochemical and copolymer properties.urn:issn:2056-9890Montoya-Garcia, M.Cortes-Hernandez, H.D'Vries, R.Valencia-Sanchez, H.text/htmlThe title compound crystallizes in the monoclinic system (space group P21/n) with two molecules in the asymmetric unit, which are linked by C—H⋯O hydrogen bonds. Hirshfeld surface analysis showed that the most significant contributions to the crystal packing are from H⋯O/O⋯H, H⋯C/C⋯H and H⋯H interactions. A DFT study was conducted using three different levels of theory.doi:10.1107/S2056989024000926CRYSTAL STRUCTURE; NITROPHENYLMALEIMIDE; HIRSFELD SURFACE ANALYSIS; 1-(2-NITROPHENYL)-1H-PYRROLE-2,5-DIONE2024-02-02Crystal structure, Hirsfeld surface analysis and DFT study of N-(2-nitrophenyl)maleimideThe title compound [systematic name: 1-(2-nitrophenyl)pyrrole-2,5-dione], C10H6N2O4, crystallizes in the monoclinic system (space group P21/n) with two molecules in the asymmetric unit, which are linked by C—H⋯O hydrogen bonds. Hirshfeld surface analysis showed that the most significant contributions to the crystal packing are from H⋯O/O⋯H, H⋯C/C⋯H and H⋯H interactions, which contribute 54.7%, 15.2% and 15.6%, respectively. A DFT study was conducted using three different levels of theory [(B3LYP/6–311+G(d,p), wB97XD/Def2TZVPP and LC-wpbe/6–311(2 d,2p)] in order to determine the stability, structural and electronic properties of the title molecule with a view to its potential applications and photochemical and copolymer properties.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext32056-98902056-9890med@iucr.org802024-02-02https://creativecommons.org/licenses/by/4.0/research communicationsMarch 2024Acta Crystallographica Section E: Crystallographic CommunicationsCrystal structure and characterization of a new lanthanide coordination polymer, [Pr2(pydc)(phth)2(H2O)3]·H2O
http://scripts.iucr.org/cgi-bin/paper?jw2002
A new lanthanide coordination polymer, poly[[triaquabis(μ4-phthalato)(μ3-pyridine-2,5-dicarboxylato)dipraseodymium] monohydrate], {[Pr2(C7H3NO4)2(C8H4O4)(H2O)3]·H2O}n or {[Pr2(phth)2(pydc)(H2O)3]·H2O}n, (pydc2− = pyridine-2,5-dicarboxylate and phth2− = phthalate) was synthesized and characterized, revealing the structure to be an assembly of di-periodic {Pr2(pydc)(phth)2(H2O)3}n layers. Each layer is built up by edge-sharing {Pr2N2O14} and {Pr2O16} dimers, which are connected through a new coordination mode of pydc2− and phth2−. These layers are stabilized by internal hydrogen bonds and π–π interactions. In addition, a three-dimensional supramolecular framework is built by interlayer hydrogen-bonding interactions involving the non-coordinated water molecule. Thermogravimetric analysis shows that the title compound is thermally stable up to 400°C.urn:issn:2056-9890Yotnoi, B.Rujiwatra, A.text/htmlThe crystal structure and thermogravimetric stability of [Pr2(pydc)(phth)2(H2O)3]·H2O, a two-dimensional coordination polymer with a novel coordination mode of pyridine-2,5-dicarboxylate (pydc2−), are reported.doi:10.1107/S2056989024000872CRYSTAL STRUCTURE; COORDINATION POLYMER; LANTHANIDE; PYRIDINE-2,5-DICARBOXYLATE; PHTHALATE.2024-01-31Crystal structure and characterization of a new lanthanide coordination polymer, [Pr2(pydc)(phth)2(H2O)3]·H2OA new lanthanide coordination polymer, poly[[triaquabis(μ4-phthalato)(μ3-pyridine-2,5-dicarboxylato)dipraseodymium] monohydrate], {[Pr2(C7H3NO4)2(C8H4O4)(H2O)3]·H2O}n or {[Pr2(phth)2(pydc)(H2O)3]·H2O}n, (pydc2− = pyridine-2,5-dicarboxylate and phth2− = phthalate) was synthesized and characterized, revealing the structure to be an assembly of di-periodic {Pr2(pydc)(phth)2(H2O)3}n layers. Each layer is built up by edge-sharing {Pr2N2O14} and {Pr2O16} dimers, which are connected through a new coordination mode of pydc2− and phth2−. These layers are stabilized by internal hydrogen bonds and π–π interactions. In addition, a three-dimensional supramolecular framework is built by interlayer hydrogen-bonding interactions involving the non-coordinated water molecule. Thermogravimetric analysis shows that the title compound is thermally stable up to 400°C.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext80Acta Crystallographica Section E: Crystallographic CommunicationsFebruary 2024research communicationshttps://creativecommons.org/licenses/by/4.0/2282024-01-312056-98902056-98902231med@iucr.orgCrystal structure and Hirshfeld surface analysis of 4-(2-chloroethyl)-5-methyl-1,2-dihydropyrazol-3-one
http://scripts.iucr.org/cgi-bin/paper?nx2004
In the crystal of the title compound, C6H9ClN2O, molecular pairs form dimers with an R22(8) motif through N—H⋯O hydrogen bonds. These dimers are connect into ribbons parallel to the (100) plane with R44(10) motifs by N—H⋯O hydrogen bonds along the c-axis direction. In addition, π–π [centroid-to-centroid distance = 3.4635 (9) Å] and C—Cl⋯π interactions between the ribbons form layers parallel to the (100) plane. The three-dimensional consolidation of the crystal structure is also ensured by Cl⋯H and Cl⋯Cl interactions between these layers. According to a Hirshfeld surface study, H⋯H (43.3%), Cl⋯H/H⋯Cl (22.1%) and O⋯H/H⋯O (18.7%) interactions are the most significant contributors to the crystal packing.urn:issn:2056-9890Naghiyev, F.N.Khrustalev, V.N.Akkurt, M.Dukhnovsky, E.A.Bhattarai, A.Khalilov, A.N.Mamedov, İ.G.text/htmlIn the crystal, molecular pairs form dimers through N—H⋯O hydrogen bonds. These dimers are linked into ribbons parallel to the (100) plane by further N—H⋯O hydrogen bonds. In addition, π–π and C—Cl⋯π interactions between the ribbons form layers parallel to the (100) plane.doi:10.1107/S2056989024000835CRYSTAL STRUCTURE; HYDROGEN BONDS; DIMERS; PYRAZOLE RING; HIRSHFELD SURFACE ANALYSIS2024-01-31Crystal structure and Hirshfeld surface analysis of 4-(2-chloroethyl)-5-methyl-1,2-dihydropyrazol-3-oneIn the crystal of the title compound, C6H9ClN2O, molecular pairs form dimers with an R22(8) motif through N—H⋯O hydrogen bonds. These dimers are connect into ribbons parallel to the (100) plane with R44(10) motifs by N—H⋯O hydrogen bonds along the c-axis direction. In addition, π–π [centroid-to-centroid distance = 3.4635 (9) Å] and C—Cl⋯π interactions between the ribbons form layers parallel to the (100) plane. The three-dimensional consolidation of the crystal structure is also ensured by Cl⋯H and Cl⋯Cl interactions between these layers. According to a Hirshfeld surface study, H⋯H (43.3%), Cl⋯H/H⋯Cl (22.1%) and O⋯H/H⋯O (18.7%) interactions are the most significant contributors to the crystal packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext22056-98902056-9890med@iucr.org227802024-01-31223February 2024Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/Synthesis, crystal structure and Hirshfeld surface analysis of 2-({5-[(naphthalen-1-yl)methyl]-4-phenyl-4H-1,2,4-triazol-3-yl}sulfanyl)-1-(4-nitrophenyl)ethanone
http://scripts.iucr.org/cgi-bin/paper?zv2033
The title compound, C27H20N4O3S, crystallizes in the monoclinic system, space group P21/n, with Z = 4. The global shape of the molecule is determined by the orientation of the substituents on the central 4H-1,2,4-triazole ring. The nitrophenyl ring, phenyl ring, and naphthalene ring system are oriented at dihedral angles of 82.95 (17), 77.14 (18) and 89.46 (15)°, respectively, with respect to the triazole ring. The crystal packing features chain formation in the b-axis direction by S⋯O interactions. A Hirshfeld surface analysis indicates that the highest contributions to surface contacts arise from contacts in which H atoms are involved.urn:issn:2056-9890Le, T.D.Nguyen, T.C.Hoang, T.K.D.Huynh, M.K.Phan, Q.T.Van Meervelt, L.text/htmlIn the title compound, C27H20N4O3S, the three aromatic rings are oriented almost perpendicular to the plane of the central 1,2,4-triazole ring.doi:10.1107/S2056989024000859CRYSTAL STRUCTURE; 1,2,4-TRIAZOLE; HIRSHFELD SURFACE2024-01-26Synthesis, crystal structure and Hirshfeld surface analysis of 2-({5-[(naphthalen-1-yl)methyl]-4-phenyl-4H-1,2,4-triazol-3-yl}sulfanyl)-1-(4-nitrophenyl)ethanoneThe title compound, C27H20N4O3S, crystallizes in the monoclinic system, space group P21/n, with Z = 4. The global shape of the molecule is determined by the orientation of the substituents on the central 4H-1,2,4-triazole ring. The nitrophenyl ring, phenyl ring, and naphthalene ring system are oriented at dihedral angles of 82.95 (17), 77.14 (18) and 89.46 (15)°, respectively, with respect to the triazole ring. The crystal packing features chain formation in the b-axis direction by S⋯O interactions. A Hirshfeld surface analysis indicates that the highest contributions to surface contacts arise from contacts in which H atoms are involved.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext22056-98902056-9890med@iucr.org222802182024-01-26research communicationshttps://creativecommons.org/licenses/by/4.0/February 2024Acta Crystallographica Section E: Crystallographic CommunicationsCadmium phosphates Cd2(PO4)OH and Cd5(PO4)2(OH)4 crystallizing in mineral structures
http://scripts.iucr.org/cgi-bin/paper?tx2081
Single crystals of two basic cadmium phosphates, dicadmium orthophosphate hydroxide, Cd2(PO4)OH, and pentacadmium bis(orthophosphate) tetrakis(hydroxide), Cd5(PO4)2(OH)4, were obtained under hydrothermal conditions. Cd2(PO4)OH adopts the triplite [(Mn,Fe)2(PO4)F] structure type. Its asymmetric unit comprises two Cd, one P and five O sites, all situated at the general Wyckoff position 8 f of space group I2/a; two of the O atoms are positionally disordered over two sites, and the H atom could not be localized. Disregarding the disorder, distorted [CdO6] polyhedra form a tri-periodic network by edge-sharing with neighbouring [CdO6] units and by vertex-sharing with [PO4] units. The site associated with the OH group is coordinated by four Cd atoms in a distorted tetrahedral manner forming 1∞[(OH)Cd4/2] chains parallel to [001]. The oxygen environment around the OH site suggests multiple acceptor atoms for possible O—H⋯O hydrogen-bonding interactions and is the putative reason for the disorder. Cd5(PO4)2(OH)4 adopts the arsenoclasite [Mn5(AsO4)2(OH)4] structure type. Its asymmetric unit comprises five Cd, two P, and twelve O sites all located at the general Wyckoff position 4 a of space group P212121; the H atoms could not be localized. The crystal structure of Cd5(PO4)2(OH)4 can be subdivided into two main sub-units. One consists of three edge-sharing [CdO6] octahedra, and the other of two edge- and vertex-sharing [CdO6] octahedra. Each sub-unit forms corrugated ribbons extending parallel to [100]. The two types of ribbons are linked into the tri-periodic arrangement through vertex-sharing and through common [PO4] tetrahedra. Quantitative structure comparisons are made with isotypic M5(XO4)2(OH)4 crystal structures (M = Cd, Mn, Co; X = P, As, V).urn:issn:2056-9890Eder, F.Weil, M.text/htmlCd2(PO4)OH and Cd5(PO4)2(OH)4 crystallize in the mineral structures of triplite and arsenoclasite, respectively.doi:10.1107/S2056989024000793CRYSTAL STRUCTURE; CADMIUM PHOSPHATE(V); TRIPLITE; ARSENOCLASITE; ISOTYPISM; STRUCTURE COMPARISON2024-01-26Cadmium phosphates Cd2(PO4)OH and Cd5(PO4)2(OH)4 crystallizing in mineral structuresSingle crystals of two basic cadmium phosphates, dicadmium orthophosphate hydroxide, Cd2(PO4)OH, and pentacadmium bis(orthophosphate) tetrakis(hydroxide), Cd5(PO4)2(OH)4, were obtained under hydrothermal conditions. Cd2(PO4)OH adopts the triplite [(Mn,Fe)2(PO4)F] structure type. Its asymmetric unit comprises two Cd, one P and five O sites, all situated at the general Wyckoff position 8 f of space group I2/a; two of the O atoms are positionally disordered over two sites, and the H atom could not be localized. Disregarding the disorder, distorted [CdO6] polyhedra form a tri-periodic network by edge-sharing with neighbouring [CdO6] units and by vertex-sharing with [PO4] units. The site associated with the OH group is coordinated by four Cd atoms in a distorted tetrahedral manner forming 1∞[(OH)Cd4/2] chains parallel to [001]. The oxygen environment around the OH site suggests multiple acceptor atoms for possible O—H⋯O hydrogen-bonding interactions and is the putative reason for the disorder. Cd5(PO4)2(OH)4 adopts the arsenoclasite [Mn5(AsO4)2(OH)4] structure type. Its asymmetric unit comprises five Cd, two P, and twelve O sites all located at the general Wyckoff position 4 a of space group P212121; the H atoms could not be localized. The crystal structure of Cd5(PO4)2(OH)4 can be subdivided into two main sub-units. One consists of three edge-sharing [CdO6] octahedra, and the other of two edge- and vertex-sharing [CdO6] octahedra. Each sub-unit forms corrugated ribbons extending parallel to [100]. The two types of ribbons are linked into the tri-periodic arrangement through vertex-sharing and through common [PO4] tetrahedra. Quantitative structure comparisons are made with isotypic M5(XO4)2(OH)4 crystal structures (M = Cd, Mn, Co; X = P, As, V).https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextFebruary 2024Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2024-01-2620780212med@iucr.org2056-98902056-98902Crystal structure, Hirshfeld surface analysis, crystal voids, interaction energy calculations and energy frameworks, and DFT calculations of 1-(4-methylbenzyl)indoline-2,3-dione
http://scripts.iucr.org/cgi-bin/paper?jp2002
The indoline portion of the title molecule, C16H13NO2, is planar. In the crystal, a layer structure is generated by C—H⋯O hydrogen bonds and C—H⋯π(ring), π-stacking and C=O⋯π(ring) interactions. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (43.0%), H⋯C/C⋯H (25.0%) and H⋯O/O⋯H (22.8%) interactions. Hydrogen bonding and van der Waals interactions are the dominant interactions in the crystal packing. The volume of the crystal voids and the percentage of free space were calculated to be 120.52 Å3 and 9.64%, respectively, showing that there is no large cavity in the crystal packing. Evaluation of the electrostatic, dispersion and total energy frameworks indicate that the stabilization is dominated by the dispersion energy contributions in the title compound. Moreover, the DFT-optimized structure at the B3LYP/6-311G(d,p) level is compared with the experimentally determined molecular structure in the solid state.urn:issn:2056-9890Rharmili, N.Abdellaoui, O.Ouazzani Chahdi, F.Mague, J.T.Hökelek, T.Mazzah, A.Kandri Rodi, Y.Sebbar, N.K.text/htmlIn the crystal of 1-(4-methylbenzyl)indoline-2,3-dione, a layer structure is generated by C—H⋯O hydrogen bonds and C—H⋯π(ring), π-stacking and C=O⋯π(ring) interactions.doi:10.1107/S2056989024000756HYDROGEN BONDS; C-H...[PI](RING) INTERACTION; [PI]-STACKING; C=O...[PI](RING) INTERACTION; INDOLINE-2,3-DIONE; CRYSTAL STRUCTURE2024-01-31Crystal structure, Hirshfeld surface analysis, crystal voids, interaction energy calculations and energy frameworks, and DFT calculations of 1-(4-methylbenzyl)indoline-2,3-dioneThe indoline portion of the title molecule, C16H13NO2, is planar. In the crystal, a layer structure is generated by C—H⋯O hydrogen bonds and C—H⋯π(ring), π-stacking and C=O⋯π(ring) interactions. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (43.0%), H⋯C/C⋯H (25.0%) and H⋯O/O⋯H (22.8%) interactions. Hydrogen bonding and van der Waals interactions are the dominant interactions in the crystal packing. The volume of the crystal voids and the percentage of free space were calculated to be 120.52 Å3 and 9.64%, respectively, showing that there is no large cavity in the crystal packing. Evaluation of the electrostatic, dispersion and total energy frameworks indicate that the stabilization is dominated by the dispersion energy contributions in the title compound. Moreover, the DFT-optimized structure at the B3LYP/6-311G(d,p) level is compared with the experimentally determined molecular structure in the solid state.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98902239med@iucr.org80February 2024Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2024-01-31232Crystal structure, Hirshfeld surface analysis, crystal voids, interaction energy calculations and energy frameworks and DFT calculations of ethyl 2-cyano-3-(3-hydroxy-5-methyl-1H-pyrazol-4-yl)-3-phenylpropanoate
http://scripts.iucr.org/cgi-bin/paper?ny2002
The title compound, C16H17N3O3, is racemic as it crystallizes in a centrosymmetric space group (P\overline{1}), although the trans disposition of substituents about the central C—C bond is established. The five- and six-membered rings are oriented at a dihedral angle of 75.88 (8)°. In the crystal, N—H⋯N hydrogen bonds form chains of molecules extending along the c-axis direction that are connected by inversion-related pairs of O—H⋯N into ribbons. The ribbons are linked by C—H⋯π(ring) interactions, forming layers parallel to the ab plane. A Hirshfeld surface analysis indicates that the most important contributions for the crystal packing are from H⋯H (45.9%), H⋯N/N⋯H (23.3%), H⋯C/C⋯H (16.2%) and H⋯O/O⋯H (12.3%) interactions. Hydrogen bonding and van der Waals interactions are the dominant interactions in the crystal packing. The volume of the crystal voids and the percentage of free space were calculated to be 100.94 Å3 and 13.20%, showing that there is no large cavity in the crystal packing. Evaluation of the electrostatic, dispersion and total energy frameworks indicates that the stabilization is dominated by the electrostatic energy contributions in the title compound. Moreover, the DFT-optimized structure at the B3LYP/6–311 G(d,p) level is compared with the experimentally determined molecular structure in the solid state. The HOMO–LUMO behaviour was elucidated to determine the energy gap.urn:issn:2056-9890Ait Elmachkouri, Y.Irrou, E.El Monfalouti, H.Mazzah, A.Hökelek, T.Mague, J.T.Taha, M.L.Sebbar, N.K.text/htmlIn the title molecule, the five- and six-membered rings are oriented at a dihedral angle of 75.88 (8)°. In the crystal, N—H⋯N hydrogen bonds form chains of molecules extending along the c-axis direction that are connected by inversion-related pairs of O—H⋯N into ribbons. The ribbons are linked by C—H⋯π(ring) interactions, forming layers parallel to the ab plane.doi:10.1107/S2056989024000744CRYSTAL STRUCTURE; PYRAZOLE; C-H...[PI](RING) INTERACTION; HYDROGEN BOND2024-01-31Crystal structure, Hirshfeld surface analysis, crystal voids, interaction energy calculations and energy frameworks and DFT calculations of ethyl 2-cyano-3-(3-hydroxy-5-methyl-1H-pyrazol-4-yl)-3-phenylpropanoateThe title compound, C16H17N3O3, is racemic as it crystallizes in a centrosymmetric space group (P\overline{1}), although the trans disposition of substituents about the central C—C bond is established. The five- and six-membered rings are oriented at a dihedral angle of 75.88 (8)°. In the crystal, N—H⋯N hydrogen bonds form chains of molecules extending along the c-axis direction that are connected by inversion-related pairs of O—H⋯N into ribbons. The ribbons are linked by C—H⋯π(ring) interactions, forming layers parallel to the ab plane. A Hirshfeld surface analysis indicates that the most important contributions for the crystal packing are from H⋯H (45.9%), H⋯N/N⋯H (23.3%), H⋯C/C⋯H (16.2%) and H⋯O/O⋯H (12.3%) interactions. Hydrogen bonding and van der Waals interactions are the dominant interactions in the crystal packing. The volume of the crystal voids and the percentage of free space were calculated to be 100.94 Å3 and 13.20%, showing that there is no large cavity in the crystal packing. Evaluation of the electrostatic, dispersion and total energy frameworks indicates that the stabilization is dominated by the electrostatic energy contributions in the title compound. Moreover, the DFT-optimized structure at the B3LYP/6–311 G(d,p) level is compared with the experimentally determined molecular structure in the solid state. The HOMO–LUMO behaviour was elucidated to determine the energy gap.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98902246med@iucr.org80research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsFebruary 20242402024-01-31Crystal structures and Hirshfeld surface analyses of methyl 4-{2,2-dichloro-1-[(E)-phenyldiazenyl]ethenyl}benzoate, methyl 4-{2,2-dichloro-1-[(E)-(4-methylphenyl)diazenyl]ethenyl}benzoate and methyl 4-{2,2-dichloro-1-[(E)-(3,4-dimethylphenyl)diazenyl]ethenyl}benzoate
http://scripts.iucr.org/cgi-bin/paper?wm5708
The crystal structures and Hirshfeld surface analyses of three similar azo compounds are reported. Methyl 4-{2,2-dichloro-1-[(E)-phenyldiazenyl]ethenyl}benzoate, C16H12Cl2N2O2, (I), and methyl 4-{2,2-dichloro-1-[(E)-(4-methylphenyl)diazenyl]ethenyl}benzoate, C17H14Cl2N2O2, (II), crystallize in the space group P21/c with Z = 4, and methyl 4-{2,2-dichloro-1-[(E)-(3,4-dimethylphenyl)diazenyl]ethenyl}benzoate, C18H16Cl2N2O2, (III), in the space group P\overline{1} with Z = 2. In the crystal of (I), molecules are linked by C—H⋯N hydrogen bonds, forming chains with C(6) motifs parallel to the b axis. Short intermolecular Cl⋯O contacts of 2.8421 (16) Å and weak van der Waals interactions between these chains stabilize the crystal structure. In (II), molecules are linked by C—H⋯O hydrogen bonds and C—Cl⋯π interactions, forming layers parallel to (010). Weak van der Waals interactions between these layers consolidate the molecular packing. In (III), molecules are linked by C—H⋯π and C—Cl⋯π interactions forming chains parallel to [011]. Furthermore, these chains are connected by C—Cl⋯π interactions parallel to the a axis, forming (0\overline{1}1) layers. The stability of the molecular packing is ensured by van der Waals forces between these layers.urn:issn:2056-9890Shikhaliyev, N.Q.İbrahimova, S.A.Atakishiyeva, G.T.Ahmedova, N.E.Babayeva, G.V.Khrustalev, V.N.Atioğlu, Z.Akkurt, M.Bhattarai, A.text/htmlIn the crystal of methyl 4-{2,2-dichloro-1-[(E)-phenyldiazenyl]ethenyl}benzoate, molecules are linked by C—H⋯N hydrogen bonds, forming chains with C(6) motifs parallel to the b axis. In methyl 4-{2,2-dichloro-1-[(E)-(4-methylphenyl)diazenyl]ethenyl}benzoate, molecules are linked by C—H⋯O hydrogen bonds and C—Cl⋯π interactions, forming layers parallel to (010). In methyl 4-{2,2-dichloro-1-[(E)-(3,4-dimethylphenyl)diazenyl]ethenyl}benzoate, molecules are linked by C—H⋯π and C—Cl⋯π interactions, forming chains parallel to [011].doi:10.1107/S2056989024000732CRYSTAL STRUCTURE; C-H...N HYDROGEN BONDS; C-H...[PI] INTERACTIONS; C-CL...[PI] INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2024-01-26Crystal structures and Hirshfeld surface analyses of methyl 4-{2,2-dichloro-1-[(E)-phenyldiazenyl]ethenyl}benzoate, methyl 4-{2,2-dichloro-1-[(E)-(4-methylphenyl)diazenyl]ethenyl}benzoate and methyl 4-{2,2-dichloro-1-[(E)-(3,4-dimethylphenyl)diazenyl]ethenyl}benzoateThe crystal structures and Hirshfeld surface analyses of three similar azo compounds are reported. Methyl 4-{2,2-dichloro-1-[(E)-phenyldiazenyl]ethenyl}benzoate, C16H12Cl2N2O2, (I), and methyl 4-{2,2-dichloro-1-[(E)-(4-methylphenyl)diazenyl]ethenyl}benzoate, C17H14Cl2N2O2, (II), crystallize in the space group P21/c with Z = 4, and methyl 4-{2,2-dichloro-1-[(E)-(3,4-dimethylphenyl)diazenyl]ethenyl}benzoate, C18H16Cl2N2O2, (III), in the space group P\overline{1} with Z = 2. In the crystal of (I), molecules are linked by C—H⋯N hydrogen bonds, forming chains with C(6) motifs parallel to the b axis. Short intermolecular Cl⋯O contacts of 2.8421 (16) Å and weak van der Waals interactions between these chains stabilize the crystal structure. In (II), molecules are linked by C—H⋯O hydrogen bonds and C—Cl⋯π interactions, forming layers parallel to (010). Weak van der Waals interactions between these layers consolidate the molecular packing. In (III), molecules are linked by C—H⋯π and C—Cl⋯π interactions forming chains parallel to [011]. Furthermore, these chains are connected by C—Cl⋯π interactions parallel to the a axis, forming (0\overline{1}1) layers. The stability of the molecular packing is ensured by van der Waals forces between these layers.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98902190med@iucr.org80February 2024Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2024-01-26184(S)-(+)-1-(4-Bromophenyl)-N-[(4-methoxyphenyl)methylidene]ethylamine and bis{(S)-(+)-1-(4-bromophenyl)-N-[(4-methoxyphenyl)methylidene]ethylamine-κN}dichloridopalladium(II)
http://scripts.iucr.org/cgi-bin/paper?ee2003
The (S)-(+)-1-(4-bromophenyl)-N-[(4-methoxyphenyl)methylidene]ethylamine ligand, C16H16BrNO, (I), was synthesized through the reaction of 4-methoxyanisaldehyde with (S)-(−)-1-(4-bromophenyl)ethylamine. It crystallizes in the orthorhombic space group P212121 belonging to the Sohncke group, featuring a single molecule in the asymmetric unit. The refinement converged successfully, achieving an R factor of 0.0508. The PdII complex bis{(S)-(+)-1-(4-bromophenyl)-N-[(4-methoxyphenyl)methylidene]ethylamine-κN}dichloridopalladium(II), [PdCl2(C16H16BrNO)2], (II), crystallizes in the monoclinic space group P21 belonging to the Sohncke group, with two molecules in the asymmetric unit. The central atom is tetracoordinated by two N atoms and two Cl atoms, resulting in a square-planar configuration. The imine moieties exhibit a trans configuration around the PdII centre, with average Cl—Pd—N angles of approximately 89.95 and 90°. The average distances within the palladium complex for the two molecules are ∼2.031 Å for Pd—N and ∼2.309 Å for Pd—Cl.urn:issn:2056-9890Anzaldo, B.Moreno Morales, G.E.Villamizar C., C.P.Mendoza, Á.Hernández Téllez, G.text/htmlThe synthesis, crystal structure and analysis of a chiral Schiff base (S)-(+)-1-(4-bromophenyl)-N-[(4-methoxyphenyl)methylidene]ethylamine ligand along with its corresponding palladium(II) complex are detailed. The crystal structures exhibit monoclinic P21 and orthorhombic P212121 symmetries, respectively. The structure of the palladium(II) complex reveals C—H⋯O and C—H⋯Br hydrogen-bonding interactions involving two distinct molecules within the asymmetric unit.doi:10.1107/S2056989024000690CRYSTAL STRUCTURE; SCHIFF BASE; PALLADIUM(II) COMPLEX; MONODENTATE2024-01-26(S)-(+)-1-(4-Bromophenyl)-N-[(4-methoxyphenyl)methylidene]ethylamine and bis{(S)-(+)-1-(4-bromophenyl)-N-[(4-methoxyphenyl)methylidene]ethylamine-κN}dichloridopalladium(II)The (S)-(+)-1-(4-bromophenyl)-N-[(4-methoxyphenyl)methylidene]ethylamine ligand, C16H16BrNO, (I), was synthesized through the reaction of 4-methoxyanisaldehyde with (S)-(−)-1-(4-bromophenyl)ethylamine. It crystallizes in the orthorhombic space group P212121 belonging to the Sohncke group, featuring a single molecule in the asymmetric unit. The refinement converged successfully, achieving an R factor of 0.0508. The PdII complex bis{(S)-(+)-1-(4-bromophenyl)-N-[(4-methoxyphenyl)methylidene]ethylamine-κN}dichloridopalladium(II), [PdCl2(C16H16BrNO)2], (II), crystallizes in the monoclinic space group P21 belonging to the Sohncke group, with two molecules in the asymmetric unit. The central atom is tetracoordinated by two N atoms and two Cl atoms, resulting in a square-planar configuration. The imine moieties exhibit a trans configuration around the PdII centre, with average Cl—Pd—N angles of approximately 89.95 and 90°. The average distances within the palladium complex for the two molecules are ∼2.031 Å for Pd—N and ∼2.309 Å for Pd—Cl.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98902217med@iucr.org80research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsFebruary 20242132024-01-26(E)-N,N-Diethyl-4-{[(4-methoxyphenyl)imino]methyl}aniline: crystal structure, Hirshfeld surface analysis and energy framework
http://scripts.iucr.org/cgi-bin/paper?hb8091
In the title benzylideneaniline Schiff base, C18H22N2O, the aromatic rings are inclined to each other by 46.01 (6)°, while the Car—N= C—Car torsion angle is 176.9 (1)°. In the crystal, the only identifiable directional interaction is a weak C—H⋯π hydrogen bond, which generates inversion dimers that stack along the a-axis direction.urn:issn:2056-9890Subashini, A.Kumaravel, R.Tharmalingam, B.Ramamurthi, K.Crochet, A.Stoeckli-Evans, H.text/htmlIn the title compound, a benzylideneaniline Schiff base, the planes of the p-substituted aromatic rings subtend a dihedral angle of 46.01 (6)°.doi:10.1107/S2056989024000574CRYSTAL STRUCTURE; BENZYLIDENEANILINE; SCHIFF BASE; HIRSHFELD SURFACE ANALYSIS; ENERGY FRAMEWORK2024-01-26(E)-N,N-Diethyl-4-{[(4-methoxyphenyl)imino]methyl}aniline: crystal structure, Hirshfeld surface analysis and energy frameworkIn the title benzylideneaniline Schiff base, C18H22N2O, the aromatic rings are inclined to each other by 46.01 (6)°, while the Car—N= C—Car torsion angle is 176.9 (1)°. In the crystal, the only identifiable directional interaction is a weak C—H⋯π hydrogen bond, which generates inversion dimers that stack along the a-axis direction.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext22056-98902056-9890med@iucr.org206802012024-01-26https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsFebruary 2024Synthesis, crystal structure and Hirshfeld surface analysis of sodium bis(malonato)borate monohydrate
http://scripts.iucr.org/cgi-bin/paper?hb8086
In the title salt, poly[aqua[μ4-bis(malonato)borato]sodium], {[Na(C6H4BO8)]·H2O}n or Na+·[B(C3H2O4)2]−·H2O, the sodium cation exhibits fivefold coordination by four carbonyl O atoms of the bis(malonato)borate anions and a water O atom. The tetrahedral B atom at the centre of the anion leads to the formation of a polymeric three-dimensional framework, which is consolidated by C—H⋯O and O—H⋯O hydrogen bonds. A Hirshfeld surface analysis indicates that the most significant contacts in the crystal packing are H⋯O/O⋯H (49.7%), Na⋯O/O⋯Na (16.1%), O⋯O (12.6%), H⋯H (10.7%) and C⋯O/O⋯C (7.3%).urn:issn:2056-9890Selvi, R.Gokila, G.Thiruvalluvar, A.A.Sundararajan, R.S.text/htmlThe asymmetric unit of the title salt, Na+·C6H4BO8−·H2O, comprises a five-coordinate sodium cation, a bis(malonato)borate anion and a water molecule of crystallization.doi:10.1107/S2056989024000537SYNTHESIS; CRYSTAL STRUCTURE; BIS(MALONATO)BORATE ANION; SODIUM; HIRSHFELD SURFACE ANALYSIS.2024-01-26Synthesis, crystal structure and Hirshfeld surface analysis of sodium bis(malonato)borate monohydrateIn the title salt, poly[aqua[μ4-bis(malonato)borato]sodium], {[Na(C6H4BO8)]·H2O}n or Na+·[B(C3H2O4)2]−·H2O, the sodium cation exhibits fivefold coordination by four carbonyl O atoms of the bis(malonato)borate anions and a water O atom. The tetrahedral B atom at the centre of the anion leads to the formation of a polymeric three-dimensional framework, which is consolidated by C—H⋯O and O—H⋯O hydrogen bonds. A Hirshfeld surface analysis indicates that the most significant contacts in the crystal packing are H⋯O/O⋯H (49.7%), Na⋯O/O⋯Na (16.1%), O⋯O (12.6%), H⋯H (10.7%) and C⋯O/O⋯C (7.3%).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext801802024-01-26https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsFebruary 202422056-98902056-9890med@iucr.org183Crystal structures of the alkali aluminoboracites A4B4Al3O12Cl (A = Li, Na)
http://scripts.iucr.org/cgi-bin/paper?wm5704
Single crystals of alkali aluminoboracites, A4B4Al3O12Cl (A = Li, Na), were grown using the self-flux method, and their isotypic cubic crystal structures were determined by single-crystal X-ray diffraction. Na4B4Al3O12Cl is the first reported sodium boracite, and its lattice parameter [13.5904 (1) Å] is the largest among the boracites consisting of a cation–oxygen framework reported so far. For both crystals, structure models refined in the cubic space group F\overline{4}3c, which assume that all cubic octant subcells in the unit cell are equivalent, converged with R1 factors of ∼0.03. However, the presence of weak hhl reflections with odd h and l values indicates that refinements in the space group F23, which presume a checkerboard-like ordering of two types of subcells with slightly different atomic positions, are more appropriate.urn:issn:2056-9890Yoshino, S.Arima, H.Ishijima, M.Kajihara, K.text/htmlSingle crystals of cubic alkali aluminoboracites A4B4Al3O12Cl (A = Li, Na) were grown from a self-flux and their crystal structures were determined and compared in two space group types, F\overline{4}3c and F23. Na4B4Al3O12Cl is the first sodium boracite and its lattice parameter is the largest among boracites with a cation–oxygen framework.doi:10.1107/S2056989024000501ALKALI ALUMINOBORACITE; SELF-FLUX METHOD; WEAK STRUCTURE ORDERING; ISOTYPISM; CRYSTAL STRUCTURE2024-01-26Crystal structures of the alkali aluminoboracites A4B4Al3O12Cl (A = Li, Na)Single crystals of alkali aluminoboracites, A4B4Al3O12Cl (A = Li, Na), were grown using the self-flux method, and their isotypic cubic crystal structures were determined by single-crystal X-ray diffraction. Na4B4Al3O12Cl is the first reported sodium boracite, and its lattice parameter [13.5904 (1) Å] is the largest among the boracites consisting of a cation–oxygen framework reported so far. For both crystals, structure models refined in the cubic space group F\overline{4}3c, which assume that all cubic octant subcells in the unit cell are equivalent, converged with R1 factors of ∼0.03. However, the presence of weak hhl reflections with odd h and l values indicates that refinements in the space group F23, which presume a checkerboard-like ordering of two types of subcells with slightly different atomic positions, are more appropriate.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext801692024-01-26Acta Crystallographica Section E: Crystallographic CommunicationsFebruary 2024research communicationshttps://creativecommons.org/licenses/by/4.0/22056-98902056-9890med@iucr.org173Synthesis and crystal structure of diisothiocyanatotetrakis(4-methylpyridine N-oxide)cobalt(II) and diisothiocyanatotris(4-methylpyridine N-oxide)cobalt(II) showing two different metal coordination polyhedra
http://scripts.iucr.org/cgi-bin/paper?hb8092
The reaction of Co(NCS)2 with 4-methylpyridine N-oxide (C6H7NO) leads to the formation of two compounds, namely, tetrakis(4-methylpyridine N-oxide-κO)bis(thiocyanato-κN)cobalt(II), [Co(NCS)2(C6H7NO)4] (1), and tris(4-methylpyridine N-oxide-κO)bis(thiocyanato-κN)cobalt(II), [Co(NCS)2(C6H7NO)3] (2). The asymmetric unit of 1 consists of one CoII cation located on a centre of inversion, as well as one thiocyanate anion and two 4-methylpyridine N-oxide coligands in general positions. The CoII cations are octahedrally coordinated by two terminal N-bonding thiocyanate anions in trans positions and four 4-methylpyridine N-oxide ligands. In the extended structure, these complexes are linked by C—H⋯O and C—H⋯S interactions. In compound 2, two crystallographically independent complexes are present, which occupy general positions. In each of these complexes, the CoII cations are coordinated in a trigonal–bipyramidal manner by two terminal N-bonding thiocyanate anions in axial positions and by three 4-methylpyridine N-oxide ligands in equatorial positions. In the crystal, these complex molecules are linked by C—H⋯S interactions. For compound 2, a nonmerohedral twin refinement was performed. Powder X-ray diffraction (PXRD) reveals that 2 was nearly obtained as a pure phase, which is not possible for compound 1. Differential thermoanalysis and thermogravimetry data (DTA–TG) show that compound 2 start to decompose at about 518 K.urn:issn:2056-9890Näther, C.Jess, I.text/htmlIn the crystal structure of the title compounds, the CoII cations are either sixfold or fivefold coordinated by two thiocyanate anions and four or three 4-methylpyridine N-oxide coligands within a slightly distorted octahedral or a trigonal–bipyramidal coordination polyhedron.doi:10.1107/S2056989024000471SYNTHESIS; COORDINATION COMPOUND; COBALT THIOCYANATE; 4-METHYLPYRIDINE N-OXIDE; CRYSTAL STRUCTURE2024-01-26Synthesis and crystal structure of diisothiocyanatotetrakis(4-methylpyridine N-oxide)cobalt(II) and diisothiocyanatotris(4-methylpyridine N-oxide)cobalt(II) showing two different metal coordination polyhedraThe reaction of Co(NCS)2 with 4-methylpyridine N-oxide (C6H7NO) leads to the formation of two compounds, namely, tetrakis(4-methylpyridine N-oxide-κO)bis(thiocyanato-κN)cobalt(II), [Co(NCS)2(C6H7NO)4] (1), and tris(4-methylpyridine N-oxide-κO)bis(thiocyanato-κN)cobalt(II), [Co(NCS)2(C6H7NO)3] (2). The asymmetric unit of 1 consists of one CoII cation located on a centre of inversion, as well as one thiocyanate anion and two 4-methylpyridine N-oxide coligands in general positions. The CoII cations are octahedrally coordinated by two terminal N-bonding thiocyanate anions in trans positions and four 4-methylpyridine N-oxide ligands. In the extended structure, these complexes are linked by C—H⋯O and C—H⋯S interactions. In compound 2, two crystallographically independent complexes are present, which occupy general positions. In each of these complexes, the CoII cations are coordinated in a trigonal–bipyramidal manner by two terminal N-bonding thiocyanate anions in axial positions and by three 4-methylpyridine N-oxide ligands in equatorial positions. In the crystal, these complex molecules are linked by C—H⋯S interactions. For compound 2, a nonmerohedral twin refinement was performed. Powder X-ray diffraction (PXRD) reveals that 2 was nearly obtained as a pure phase, which is not possible for compound 1. Differential thermoanalysis and thermogravimetry data (DTA–TG) show that compound 2 start to decompose at about 518 K.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org17922056-98902056-98901742024-01-26https://creativecommons.org/licenses/by/4.0/research communicationsFebruary 2024Acta Crystallographica Section E: Crystallographic Communications80Crystal structure and Hirshfeld surface analysis of (2E)-1-phenyl-3-(1H-pyrrol-2-yl)propen-1-one
http://scripts.iucr.org/cgi-bin/paper?tx2080
The title compound, C13H11NO, adopts an E configuration about the C=C double bond. The pyrrole ring is inclined to the phenyl ring at an angle of 44.94 (8)°. In the crystal, molecules are linked by N—H⋯O hydrogen bonds, forming ribbons parallel to (020) in zigzag C(7) chains along the a axis. These ribbons are connected via C—H⋯π interactions, forming a three-dimensional network. No significant π–π interactions are observed.urn:issn:2056-9890Safarova, A.S.Khalilov, A.N.Akkurt, M.Maharramov, A.M.Bhattarai, A.Naghiyev, F.N.Mamedov, İ.G.text/htmlIn the title crystal, molecules are linked by N—H⋯O hydrogen bonds, forming ribbons parallel to (020) in zigzag C(7) chains along the a axis. These ribbons are connected via C—H⋯π interactions, forming a three-dimensional network.doi:10.1107/S2056989024000495CRYSTAL STRUCTURE; 1H-PYRROLE RING; HYDROGEN BOND; CHALCONE; HIRSHFELD SURFACE ANALYSIS2024-01-26Crystal structure and Hirshfeld surface analysis of (2E)-1-phenyl-3-(1H-pyrrol-2-yl)propen-1-oneThe title compound, C13H11NO, adopts an E configuration about the C=C double bond. The pyrrole ring is inclined to the phenyl ring at an angle of 44.94 (8)°. In the crystal, molecules are linked by N—H⋯O hydrogen bonds, forming ribbons parallel to (020) in zigzag C(7) chains along the a axis. These ribbons are connected via C—H⋯π interactions, forming a three-dimensional network. No significant π–π interactions are observed.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext80Acta Crystallographica Section E: Crystallographic CommunicationsFebruary 2024research communicationshttps://creativecommons.org/licenses/by/4.0/2024-01-261912056-98902056-98902195med@iucr.orgSynthesis and crystal structure of [1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene](isocyanato-κN)gold(I)
http://scripts.iucr.org/cgi-bin/paper?zv2031
The title complex, [Au(NCO)(C27H36N2)], was synthesized by ligand metathesis from [1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene]gold(I) chloride and sodium cyanate in anhydrous tetrahydrofuran and crystallized from toluene at 233 K in the orthorhombic space group P212121, as a neutral complex with the central Au atom di-coordinated by an N-heterocyclic carbene [Au—C = 1.963 (2) Å] and an isocyanate [Au—N 1.999 (2) Å] ligands, with a linear CAuNCO moiety. The crystal packing is consolidated by C—H⋯O hydrogen bonds.urn:issn:2056-9890Bakhoda, A.text/htmlThe title complex was synthesized by ligand metathesis from [1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene]gold(I) chloride and sodium cyanate in anhydrous tetrahydrofuran and crystallized from toluene at 233 K as a neutral complex with the central Au atom di-coordinated by an N-heterocyclic carbene and an isocyanate, with a linear CAuNCO moiety.doi:10.1107/S205698902400046XCRYSTAL STRUCTURE; GOLD(I); ISOCYANATE; N-HETEROCYCLIC CARBENE2024-01-19Synthesis and crystal structure of [1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene](isocyanato-κN)gold(I)The title complex, [Au(NCO)(C27H36N2)], was synthesized by ligand metathesis from [1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene]gold(I) chloride and sodium cyanate in anhydrous tetrahydrofuran and crystallized from toluene at 233 K in the orthorhombic space group P212121, as a neutral complex with the central Au atom di-coordinated by an N-heterocyclic carbene [Au—C = 1.963 (2) Å] and an isocyanate [Au—N 1.999 (2) Å] ligands, with a linear CAuNCO moiety. The crystal packing is consolidated by C—H⋯O hydrogen bonds.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext22056-98902056-9890med@iucr.org802024-01-19research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsFebruary 2024Synthesis and crystal structures of boryl ortho-silylaryl trifluoromethanesulfonates
http://scripts.iucr.org/cgi-bin/paper?dj2074
We report the synthesis and structural characterization of three crystalline borylated ortho-silylaryl trifluoromethanesulfonates: 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-(trimethylsilyl)phenyl trifluoromethanesulfonate, C16H24BF3O5SSi (1a), 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-(trimethylsilyl)phenyl trifluoromethanesulfonate, C16H24BF3O5SSi (1b), and 2-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-6-(trimethylsilyl)phenyl trifluoromethanesulfonate, C17H26BF3O5SSi (2), which are versatile aryne precursors. For all three compounds, the heteroatom substituents are almost coplanar with the central aromatic moiety. C—heteroatom bonding metrics are unexceptional and fall withing the typical range of C—B, C—Si, and C—O single bonds. Despite numerous electronegative sites, only weak intermolecular interactions are observed in the solid state.urn:issn:2056-9890Barnå, F.Hribersek, M.Orthaber, A.Pilarski, L.T.text/htmlThe preparation and solid-state structures of three borylated ortho-silylaryl trifluoromethanesulfonates are reported. All compounds show the expected connectivity and unexceptional metric parameters as well as weak intramolecular interactions.doi:10.1107/S2056989024000264SOLID-STATE STRUCTURE; ARYNE PRECURSOR; PINACOLE BORANE; CRYSTAL STRUCTURE2024-01-12Synthesis and crystal structures of boryl ortho-silylaryl trifluoromethanesulfonatesWe report the synthesis and structural characterization of three crystalline borylated ortho-silylaryl trifluoromethanesulfonates: 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-(trimethylsilyl)phenyl trifluoromethanesulfonate, C16H24BF3O5SSi (1a), 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-(trimethylsilyl)phenyl trifluoromethanesulfonate, C16H24BF3O5SSi (1b), and 2-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-6-(trimethylsilyl)phenyl trifluoromethanesulfonate, C17H26BF3O5SSi (2), which are versatile aryne precursors. For all three compounds, the heteroatom substituents are almost coplanar with the central aromatic moiety. C—heteroatom bonding metrics are unexceptional and fall withing the typical range of C—B, C—Si, and C—O single bonds. Despite numerous electronegative sites, only weak intermolecular interactions are observed in the solid state.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98902med@iucr.org80February 2024Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2024-01-12A triclinic polymorph of miconazole
http://scripts.iucr.org/cgi-bin/paper?jy2040
The crystal structure of the new triclinic polymorph of miconazole {MIC; C18H14Cl4N2O; systematic name: (RS)-1-[2-(2,4-dichlorobenzyloxy)-2-(2,4-dichlorophenyl)ethyl]-1H-imidazole} is reported and compared with the monoclinic form of solvent-free miconazole previously reported [Kaspiaruk & Chęcińska (2022). Acta Cryst. C78, 343–350]. A comparison shows a different orientation of imidazole and one dichlorophenyl ring between polymorphic molecules. In the crystal structure of the title compound, only weak halogen bonds and C—H⋯π(arene) interactions are found. Hirshfeld surface analysis and energy framework calculations complement the comparison of the two polymorphic forms of the miconazole drug.urn:issn:2056-9890Kaspiaruk, H.Chęcińska, L.text/htmlA second polymorphic form of solvent-free miconazole, a triclinic form (MIC-tri), is reported, and compared with the anhydrous monoclinic form of miconazole (MIC-mono).doi:10.1107/S2056989024000276MICONAZOLE; CRYSTAL STRUCTURE; HIRSHFELD SURFACE; ENERGY FRAMEWORKS2024-01-26A triclinic polymorph of miconazoleThe crystal structure of the new triclinic polymorph of miconazole {MIC; C18H14Cl4N2O; systematic name: (RS)-1-[2-(2,4-dichlorobenzyloxy)-2-(2,4-dichlorophenyl)ethyl]-1H-imidazole} is reported and compared with the monoclinic form of solvent-free miconazole previously reported [Kaspiaruk & Chęcińska (2022). Acta Cryst. C78, 343–350]. A comparison shows a different orientation of imidazole and one dichlorophenyl ring between polymorphic molecules. In the crystal structure of the title compound, only weak halogen bonds and C—H⋯π(arene) interactions are found. Hirshfeld surface analysis and energy framework calculations complement the comparison of the two polymorphic forms of the miconazole drug.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98902200med@iucr.org80February 2024Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications1962024-01-26Synthesis, crystal structure and thermal properties of dibromidobis(2-methylpyridine N-oxide-κO)cobalt(II)
http://scripts.iucr.org/cgi-bin/paper?yz2048
Reaction of CoBr2 with 2-methylpyridine N-oxide in n-butanol leads to the formation of the title compound, [CoBr2(C6H7NO)2] or [CoBr2(2-methylpyridine N-oxide)2]. Its asymmetric unit consists of one CoII cation as well as two bromide anions and two 2-methylpyridine N-oxide coligands in general positions. The CoII cations are tetrahedrally coordinated by two bromide anions and two 2-methylpyridine N-oxides, forming discrete complexes. In the crystal structure, these complexes are linked predominantly by weak C–H⋯Br hydrogen bonding into chains that propagate along the crystallographic a-axis. Powder X-ray diffraction (PXRD) measurements indicate that a pure phase was obtained. Thermoanalytical investigations prove that the title compound melts before decomposition; before melting, a further endothermic signal of unknown origin was observed that does not correspond to a phase transition.urn:issn:2056-9890Näther, C.Jess, I.text/htmlThe crystal structure of the title compound consists of discrete tetrahedral complexes that are linked by weak intermolecular hydrogen bonding. Upon heating, melting before decomposition is observed.doi:10.1107/S2056989024000252CRYSTAL STRUCTURE; POWDER X-RAY DIFFRACTION; SYNTHESIS; COBALT BROMIDE; 2-METHYLPYRIDINE N-OXIDE; DIFFERENTIAL THERMOANALYSIS; DIFFERENTIAL SCANNING CALORIMETRY2024-01-12Synthesis, crystal structure and thermal properties of dibromidobis(2-methylpyridine N-oxide-κO)cobalt(II)Reaction of CoBr2 with 2-methylpyridine N-oxide in n-butanol leads to the formation of the title compound, [CoBr2(C6H7NO)2] or [CoBr2(2-methylpyridine N-oxide)2]. Its asymmetric unit consists of one CoII cation as well as two bromide anions and two 2-methylpyridine N-oxide coligands in general positions. The CoII cations are tetrahedrally coordinated by two bromide anions and two 2-methylpyridine N-oxides, forming discrete complexes. In the crystal structure, these complexes are linked predominantly by weak C–H⋯Br hydrogen bonding into chains that propagate along the crystallographic a-axis. Powder X-ray diffraction (PXRD) measurements indicate that a pure phase was obtained. Thermoanalytical investigations prove that the title compound melts before decomposition; before melting, a further endothermic signal of unknown origin was observed that does not correspond to a phase transition.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext22056-98902056-9890med@iucr.org802024-01-12research communicationshttps://creativecommons.org/licenses/by/4.0/February 2024Acta Crystallographica Section E: Crystallographic CommunicationsSynthesis and crystal structure of N1,N2-dimethylethanedihydrazide
http://scripts.iucr.org/cgi-bin/paper?vm2294
The title compound, N1,N2-dimethylethanedihydrazide, C4H10N4O2, was obtained by the methylation of oxalyl dihydrazide protected with phthalimide. The molecule is essentially non-planar with a dihedral angle between the two planar hydrazide fragments of 86.5 (2)°. This geometry contributes to the formation of a multi-contact three-dimensional supramolecular network via C—H⋯O, N—H⋯O and N—H⋯N hydrogen bonds.urn:issn:2056-9890Bibik, Y.S.Khomenko, D.M.Doroshchuk, R.O.Raspertova, I.V.Bargan, A.Lampeka, R.D.text/htmlIn the title compound, the two hydrazide planes make a dihedral angle of 86.5 (2)°. In the crystal, C—H⋯O, N—H⋯O and N—H⋯N hydrogen bonds lead to the formation of a three-dimensional supramolecular network.doi:10.1107/S2056989024000239CRYSTAL STRUCTURE; X-RAY CRYSTALLOGRAPHY; HYDRAZIDE; HYDROGEN BONDS2024-01-12Synthesis and crystal structure of N1,N2-dimethylethanedihydrazideThe title compound, N1,N2-dimethylethanedihydrazide, C4H10N4O2, was obtained by the methylation of oxalyl dihydrazide protected with phthalimide. The molecule is essentially non-planar with a dihedral angle between the two planar hydrazide fragments of 86.5 (2)°. This geometry contributes to the formation of a multi-contact three-dimensional supramolecular network via C—H⋯O, N—H⋯O and N—H⋯N hydrogen bonds.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2024-01-12Acta Crystallographica Section E: Crystallographic CommunicationsFebruary 2024research communicationshttps://creativecommons.org/licenses/by/4.0/80med@iucr.org22056-98902056-9890Crystal structure, Hirshfeld surface analysis and energy frameworks of 1-[(E)-2-(2-fluorophenyl)diazan-1-ylidene]naphthalen-2(1H)-one
http://scripts.iucr.org/cgi-bin/paper?ee2002
The title compound, C16H11N2OF, is a member of the azo dye family. The dihedral angle subtended by the benzene ring and the naphthalene ring system measures 18.75 (7)°, indicating that the compound is not perfectly planar. An intramolecular N—H⋯O hydrogen bond occurs between the imino and carbonyl groups. In the crystal, the molecules are linked into inversion dimers by C—H⋯O interactions. Aromatic π–π stacking between the naphthalene ring systems lead to the formation of chains along [001]. A Hirshfeld surface analysis was undertaken to investigate and quantify the intermolecular interactions. In addition, energy frameworks were used to examine the cooperative effect of these intermolecular interactions across the crystal, showing dispersion energy to be the most influential factor in the crystal organization of the compound.urn:issn:2056-9890Akkache, H.E.M.Hamdouni, N.Boudjada, A.Medjroubi, M. larbiMili, A.Jeannin, O.text/htmlIn the crystal, molecules of the title compound are linked into infinite sinusoidal chains along the [001] direction. The study demonstrated that dispersion energy was the most influential factor in the crystal organization of the compound.doi:10.1107/S2056989024000227AZO COMPOUNDS; 2-NAPHTHOLS; CRYSTAL STRUCTURE; HIRSHFELD SURFACE CALCULATIONS; TWO-DIMENSIONAL FINGERPRINT PLOT; ENERGY FRAMEWORKS2024-01-12Crystal structure, Hirshfeld surface analysis and energy frameworks of 1-[(E)-2-(2-fluorophenyl)diazan-1-ylidene]naphthalen-2(1H)-oneThe title compound, C16H11N2OF, is a member of the azo dye family. The dihedral angle subtended by the benzene ring and the naphthalene ring system measures 18.75 (7)°, indicating that the compound is not perfectly planar. An intramolecular N—H⋯O hydrogen bond occurs between the imino and carbonyl groups. In the crystal, the molecules are linked into inversion dimers by C—H⋯O interactions. Aromatic π–π stacking between the naphthalene ring systems lead to the formation of chains along [001]. A Hirshfeld surface analysis was undertaken to investigate and quantify the intermolecular interactions. In addition, energy frameworks were used to examine the cooperative effect of these intermolecular interactions across the crystal, showing dispersion energy to be the most influential factor in the crystal organization of the compound.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2024-01-12Acta Crystallographica Section E: Crystallographic CommunicationsFebruary 2024research communicationshttps://creativecommons.org/licenses/by/4.0/80med@iucr.org22056-98902056-9890Synthesis and crystal structure of a cadmium(II) coordination polymer based on 4,4′-(1H-1,2,4-triazole-3,5-diyl)dibenzoate
http://scripts.iucr.org/cgi-bin/paper?hb8090
The asymmetric unit of the title compound, catena-poly[[[aquabis(pyridine-κN)cadmium(II)]-μ2-4,4′-(1H-1,2,4-triazole-3,5-diyl)dibenzoato-κ4O,O′:O′′,O′′′] 4.5-hydrate], {[Cd(C16H9N3O4)(C5H5N)2(H2O)]·4.5H2O}n or {[Cd(bct)(py)2(H2O)]·4.5H2O}n (I), consists of a Cd2+ cation coordinated to one bct2– carboxylate dianion, two molecules of pyridine and a water molecule as well as four and a half water molecules of crystallization. The metal ion in I possesses a pentagonal–bipyramidal environment with the four O atoms of the two bidentately coordinated carboxylate groups and the N atom of a pyridine molecule forming the O4N equatorial plane, while the N atom of another pyridine ligand and the O atom of the water molecule occupy the axial positions. The bct2– bridging ligand connects two metal ions via its carboxylic groups, resulting in the formation of a parallel linear polymeric chain running along the [1\overline{1}1] direction. The coordinated water molecule of one chain forms a strong O—H⋯O hydrogen bond with the carboxylate O atom of a neighboring chain, leading to the formation of double chains with a closest distance of 5.425 (7) Å between the cadmium ions belonging to different chains. Aromatic π–π stacking interactions between the benzene fragments of the anions as well as between the coordinated pyridine molecules belonging to different chains results in the formation of sheets oriented parallel to the (\overline{1}01) plane. As a result of hydrogen-bonding interactions involving the water molecules of crystallization, the sheets are joined together in a three-dimensional network.urn:issn:2056-9890Popovych, A.M.Tsymbal, L.V.Khomenko, D.M.Bargan, A.Lampeka, Y.D.Lampeka, R.D.text/htmlThe coordination polyhedron of the Cd2+ ion in the title compound is a CdN2O5 pentagonal bipyramid formed by two bidentately coordinated carboxylic groups of different anions, one water molecule and two pyridine molecules. In the crystal, polymeric chains propagate along the [1\overline{1}1] direction; the chains are linked by hydrogen bonds and π–π stacking interactions into a three-dimensional network.doi:10.1107/S2056989024000185CRYSTAL STRUCTURE; COORDINATION POLYMER; CADMIUM; 4,4'-(1H-1,2,4-TRIAZOLE-3,5-DIYL)DIBENZOATE; [PI]-STACKING; HYDROGEN BONDS2024-01-09Synthesis and crystal structure of a cadmium(II) coordination polymer based on 4,4′-(1H-1,2,4-triazole-3,5-diyl)dibenzoateThe asymmetric unit of the title compound, catena-poly[[[aquabis(pyridine-κN)cadmium(II)]-μ2-4,4′-(1H-1,2,4-triazole-3,5-diyl)dibenzoato-κ4O,O′:O′′,O′′′] 4.5-hydrate], {[Cd(C16H9N3O4)(C5H5N)2(H2O)]·4.5H2O}n or {[Cd(bct)(py)2(H2O)]·4.5H2O}n (I), consists of a Cd2+ cation coordinated to one bct2– carboxylate dianion, two molecules of pyridine and a water molecule as well as four and a half water molecules of crystallization. The metal ion in I possesses a pentagonal–bipyramidal environment with the four O atoms of the two bidentately coordinated carboxylate groups and the N atom of a pyridine molecule forming the O4N equatorial plane, while the N atom of another pyridine ligand and the O atom of the water molecule occupy the axial positions. The bct2– bridging ligand connects two metal ions via its carboxylic groups, resulting in the formation of a parallel linear polymeric chain running along the [1\overline{1}1] direction. The coordinated water molecule of one chain forms a strong O—H⋯O hydrogen bond with the carboxylate O atom of a neighboring chain, leading to the formation of double chains with a closest distance of 5.425 (7) Å between the cadmium ions belonging to different chains. Aromatic π–π stacking interactions between the benzene fragments of the anions as well as between the coordinated pyridine molecules belonging to different chains results in the formation of sheets oriented parallel to the (\overline{1}01) plane. As a result of hydrogen-bonding interactions involving the water molecules of crystallization, the sheets are joined together in a three-dimensional network.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext80Acta Crystallographica Section E: Crystallographic CommunicationsFebruary 2024research communicationshttps://creativecommons.org/licenses/by/4.0/2024-01-092056-98902056-98902med@iucr.org{[(E)-(1,3-Benzodioxol-5-yl)methylidene]amino}thiourea
http://scripts.iucr.org/cgi-bin/paper?nx2003
The synthesis and crystallographic analysis of the title compound, C9H9N3O2S, are reported. The compound crystallizes in the monoclinic space group P21/c, revealing characteristic bond lengths and angles typical of thiosemicarbazone groups. The supramolecular organization primarily arises from hydrogen bonding and π–π stacking interactions, leading to distinctive dimeric formations.urn:issn:2056-9890Mesto, E.Okio, C.K.Y.A.Lemus, M.A.Schingaro, E.text/htmlThe synthesis and crystallographic analysis of [(E)-1,3-benzodioxol-5-ylmethylideneamino]thiourea is reported, offering a comprehensive exploration of its structural features and supramolecular arrangements within the crystal.doi:10.1107/S2056989024000033CRYSTAL STRUCTURE; THIO-SEMICARBAZONE; THREE-DIMENSIONAL NETWORK2024-01-09{[(E)-(1,3-Benzodioxol-5-yl)methylidene]amino}thioureaThe synthesis and crystallographic analysis of the title compound, C9H9N3O2S, are reported. The compound crystallizes in the monoclinic space group P21/c, revealing characteristic bond lengths and angles typical of thiosemicarbazone groups. The supramolecular organization primarily arises from hydrogen bonding and π–π stacking interactions, leading to distinctive dimeric formations.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98902med@iucr.org80https://creativecommons.org/licenses/by/4.0/research communicationsFebruary 2024Acta Crystallographica Section E: Crystallographic Communications2024-01-09Crystal structure and Hirshfeld surface analysis of (E)-2-[2-(2-amino-1-cyano-2-oxoethylidene)hydrazin-1-yl]benzoic acid N,N-dimethylformamide monosolvate
http://scripts.iucr.org/cgi-bin/paper?ej2001
In the title compound, C10H8N4O3·C3H7NO, the asymmetric unit contains two crystallographically independent molecules A and B, each of which has one DMF solvate molecule. Molecules A and B both feature intramolecular N—H⋯O hydrogen bonds, forming S(6) ring motifs and consolidating the molecular configuration. In the crystal, N—H⋯O and O—H⋯O hydrogen bonds connect molecules A and B, forming R22(8) ring motifs. Weak C—H⋯O interactions link the molecules, forming layers parallel to the (\overline{2}12) plane. The DMF solvent molecules are also connected to the main molecules (A and B) by N—H⋯O hydrogen bonds. π–π stacking interactions [centroid-to-centroid distance = 3.8702 (17) Å] between the layers also increase the stability of the molecular structure in the third dimension. According to the Hirshfeld surface study, O⋯H/H⋯O interactions are the most significant contributors to the crystal packing (27.5% for molecule A and 25.1% for molecule B).urn:issn:2056-9890Hajiyeva, S.R.Huseynov, F.E.Atioğlu, Z.Akkurt, M.Bhattarai, A.text/htmlIn the crystal, N—-H⋯O and O—H⋯O hydrogen bonds connect the two independent molecules, forming R_{2}^{2}(8) ring motifs. Weak C—H⋯O interactions link the molecules, forming layers parallel to the (\overline{2}12) plane. The DMF solvent molecules are also connected to the main molecules N—H⋯O hydrogen bonds. π–π stacking interactions between the layers are also observed.doi:10.1107/S2056989023011118CRYSTAL STRUCTURE; HYDROGEN BONDS; RING MOTIFS; [PI]-[PI] STACKING INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2024-01-05Crystal structure and Hirshfeld surface analysis of (E)-2-[2-(2-amino-1-cyano-2-oxoethylidene)hydrazin-1-yl]benzoic acid N,N-dimethylformamide monosolvateIn the title compound, C10H8N4O3·C3H7NO, the asymmetric unit contains two crystallographically independent molecules A and B, each of which has one DMF solvate molecule. Molecules A and B both feature intramolecular N—H⋯O hydrogen bonds, forming S(6) ring motifs and consolidating the molecular configuration. In the crystal, N—H⋯O and O—H⋯O hydrogen bonds connect molecules A and B, forming R22(8) ring motifs. Weak C—H⋯O interactions link the molecules, forming layers parallel to the (\overline{2}12) plane. The DMF solvent molecules are also connected to the main molecules (A and B) by N—H⋯O hydrogen bonds. π–π stacking interactions [centroid-to-centroid distance = 3.8702 (17) Å] between the layers also increase the stability of the molecular structure in the third dimension. According to the Hirshfeld surface study, O⋯H/H⋯O interactions are the most significant contributors to the crystal packing (27.5% for molecule A and 25.1% for molecule B).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext22056-98902056-9890med@iucr.org802024-01-05February 2024Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communicationsCrystal structure of a layered phosphate molybdate K2Gd(PO4)(MoO4)
http://scripts.iucr.org/cgi-bin/paper?oi2002
The title compound dipotassium gadolinium(III) phosphate(V) molybdate(VI), K2Gd(PO4)(MoO4), was synthesized from a high-temperature melt starting from GdF3 as a source of gadolinium. Its structure is isotypic with other MI2MIII(MVIO4)(PO4) compounds, where MI = Na, K or Cs, and MIII = rare-earth cation, MVI = Mo or W. The three-dimensional framework is built up from [Gd(PO4)(MoO4)] anionic sheets, which are organized by adhesion of [GdPO4] layers and [MoO4] tetrahedra stacked above and below these layers. The interstitial space is occupied by K cations having eightfold oxygen coordination. The polyhedron of GdO8 was estimated to be a triangular dodecahedron by the continuous shape measurement method.urn:issn:2056-9890Zozulia, V.Terebilenko, K.Voinalovych, A.Potaskalov, V.Slobodyanik, M.text/htmlDipotassium gadolinium(III) phosphate(V) molybdate(VI), synthesized from a high-temperature melt starting from GdF3 as a source of gadolinium, has a structure that is isotypic with other MI2MIII(MVIO4)(PO4) compounds, where MI = Na, K or Cs, and MIII = rare-earth cation, MVI = Mo or W. The three-dimensional framework is built up from [Gd(PO4)(MoO4)] anionic sheets, which are organized by adhesion of [GdPO4] layers and [MoO4] tetrahedra stacked above and below of these layers, and the interstitial space is occupied by K cations having eightfold oxygen coordination.doi:10.1107/S2056989023011106CRYSTAL STRUCTURE; MOLYBDATE; PHOSPHATE; GADOLINIUM; TRIANGULAR DODECAHEDRON2024-01-05Crystal structure of a layered phosphate molybdate K2Gd(PO4)(MoO4)The title compound dipotassium gadolinium(III) phosphate(V) molybdate(VI), K2Gd(PO4)(MoO4), was synthesized from a high-temperature melt starting from GdF3 as a source of gadolinium. Its structure is isotypic with other MI2MIII(MVIO4)(PO4) compounds, where MI = Na, K or Cs, and MIII = rare-earth cation, MVI = Mo or W. The three-dimensional framework is built up from [Gd(PO4)(MoO4)] anionic sheets, which are organized by adhesion of [GdPO4] layers and [MoO4] tetrahedra stacked above and below these layers. The interstitial space is occupied by K cations having eightfold oxygen coordination. The polyhedron of GdO8 was estimated to be a triangular dodecahedron by the continuous shape measurement method.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98902med@iucr.org80research communicationshttps://creativecommons.org/licenses/by/4.0/February 2024Acta Crystallographica Section E: Crystallographic Communications2024-01-05An unexpected tautomer: synthesis and crystal structure of N-[6-amino-4-(methylsulfanyl)-1,2-dihydro-1,3,5-triazin-2-ylidene]benzenesulfonamide
http://scripts.iucr.org/cgi-bin/paper?yz2047
The title compound, C10H11N5O2S2, consists of an unexpected tautomer with a protonated nitrogen atom in the triazine ring and a formal exocyclic double bond C=N to the sulfonamide moiety. The ring angles at the unsubstituted nitrogen atoms are narrow, at 115.57 (12) and 115.19 (12)°, respectively, whereas the angle at the carbon atom between these N atoms is very wide, 127.97 (13)°. The interplanar angle between the two rings is 79.56 (5)°. The molecules are linked by three classical hydrogen bonds, forming a ribbon structure. There are also unusual linkages involving three short contacts (< 3 Å) from a sulfonamide oxygen atom to the C—NH—C part of a triazine ring.urn:issn:2056-9890Mohamed-Ezzat, R.A.Elgemeie, G.H.Jones, P.G.text/htmlThe title compound, C10H11N5O2S2, consists of an unexpected imino-dihydro-triazine tautomer. Molecules are linked by hydrogen bonds and by Osulfonamide⋯(C—NH—C)triazine contacts.doi:10.1107/S2056989023011076CRYSTAL STRUCTURE; 1,3,5-TRIAZINE; BENZENESULFONAMIDE; HYDROGEN BONDS2024-01-09An unexpected tautomer: synthesis and crystal structure of N-[6-amino-4-(methylsulfanyl)-1,2-dihydro-1,3,5-triazin-2-ylidene]benzenesulfonamideThe title compound, C10H11N5O2S2, consists of an unexpected tautomer with a protonated nitrogen atom in the triazine ring and a formal exocyclic double bond C=N to the sulfonamide moiety. The ring angles at the unsubstituted nitrogen atoms are narrow, at 115.57 (12) and 115.19 (12)°, respectively, whereas the angle at the carbon atom between these N atoms is very wide, 127.97 (13)°. The interplanar angle between the two rings is 79.56 (5)°. The molecules are linked by three classical hydrogen bonds, forming a ribbon structure. There are also unusual linkages involving three short contacts (< 3 Å) from a sulfonamide oxygen atom to the C—NH—C part of a triazine ring.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext802024-01-09research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsFebruary 202422056-98902056-9890med@iucr.orgSynthesis, structure and Hirshfeld surface analysis of 2-oxo-2H-chromen-6-yl 4-tert-butylbenzoate: work carried out as part of the AFRAMED project
http://scripts.iucr.org/cgi-bin/paper?hb8087
In the title compound, C20H18O4, the dihedral angle between the 2H-chromen-2-one ring system and the phenyl ring is 89.12 (5)°. In the crystal, the molecules are connected through C—H⋯O hydrogen bonds to generate [010] double chains that are reinforced by weak aromatic π–π stacking interactions. The unit-cell packing can be described as a tilted herringbone motif. The H⋯H, H⋯O/O⋯H, H⋯C/C⋯H and C⋯C contacts contribute 46.7, 24.2, 16.7 and 7.6%, respectively, to its Hirshfeld surface.urn:issn:2056-9890Kenfack Tsobnang, P.Ziki, E.Siaka, S.Yoda, J.Kamal, S.Bouraima, A.Djifa Hounsi, A.Wenger, E.Bendeif, E.-E.Lecomte, C.text/htmlIn the title coumarin derivative, the dihedral angle between the 2H-chromen-2-one ring system and the phenyl ring is 89.12 (5)°. In the crystal, the molecules are linked by C—H⋯O hydrogen bonds into [010] double chains.doi:10.1107/S2056989023011052COUMARIN DERIVATIVE; HIRSHFELD SURFACE; HERRINGBONE PACKING; CRYSTAL STRUCTURE2024-01-05Synthesis, structure and Hirshfeld surface analysis of 2-oxo-2H-chromen-6-yl 4-tert-butylbenzoate: work carried out as part of the AFRAMED projectIn the title compound, C20H18O4, the dihedral angle between the 2H-chromen-2-one ring system and the phenyl ring is 89.12 (5)°. In the crystal, the molecules are connected through C—H⋯O hydrogen bonds to generate [010] double chains that are reinforced by weak aromatic π–π stacking interactions. The unit-cell packing can be described as a tilted herringbone motif. The H⋯H, H⋯O/O⋯H, H⋯C/C⋯H and C⋯C contacts contribute 46.7, 24.2, 16.7 and 7.6%, respectively, to its Hirshfeld surface.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext22056-98902056-9890med@iucr.org802024-01-05research communicationshttps://creativecommons.org/licenses/by/4.0/February 2024Acta Crystallographica Section E: Crystallographic CommunicationsCrystal structure of poly[hexa-μ-bromido-bis{2-[1-(pyridin-2-yl)ethylideneamino]ethanolato}tetracopper(II)]
http://scripts.iucr.org/cgi-bin/paper?ex2076
The reaction of the Schiff base 2-[1-(pyridin-2-yl)ethylideneamino]ethanol (HL), which is formed by reaction of 2-aminoethanol and 2-acetylpyridine with CuBr2 in ethanol results in the isolation of the new polymeric complex poly[hexa-μ-bromido-bis{2-[1-(pyridin-2-yl)ethylideneamino]ethanolato}tetracopper(II)], [Cu4Br6(C9H11N2O)2]n or [Cu4Br6L2]n. The asymmetric unit of the crystal structure of the polymeric [Cu4Br6L2]n complex is composed by four copper (II) cations, two monodeprotonated molecules of the ligand, and six bromide anions, which act as bridges. The ligand molecules act in a tridentate fashion through their azomethine nitrogen atoms, their pyridine nitrogen atoms, and their alcoholate O atoms. The crystal structure shows two types of geometries in the coordination polyhedrons around Cu2+ ions. Two copper cations are situated in a square-based pyramidal environment, while the two other copper cations adopt a tetrahedral geometry. Bromides anions acting as bridges between two metal ions connect the units, resulting in a tetranuclear polymer compound.urn:issn:2056-9890Traoré, B.Diouf, N.Kébé, M.Guéye-Sylla, R.Thiam, I.E.Diouf, O.Retailleau, P.Gaye, M.text/htmlIn the title Schiff base tetranuclear copper(II) complex, two discrete environments are present in the structure: CuN2OBr2 and CuBr4. Two copper(II) cations are situated in distorted square-based pyramidal environment, while two copper(II) cations are located in distorted tetrahedral geometry.doi:10.1107/S2056989023011040CRYSTAL STRUCTURE; ACETYLPYRIDINE; 2-AMINOETHANOL; 2-(1-((2-HYROXYETHYL)IMINO)ACETYLPYRIDINE); SQUARE PYRAMIDAL; TETRAHEDRAL2024-01-12Crystal structure of poly[hexa-μ-bromido-bis{2-[1-(pyridin-2-yl)ethylideneamino]ethanolato}tetracopper(II)]The reaction of the Schiff base 2-[1-(pyridin-2-yl)ethylideneamino]ethanol (HL), which is formed by reaction of 2-aminoethanol and 2-acetylpyridine with CuBr2 in ethanol results in the isolation of the new polymeric complex poly[hexa-μ-bromido-bis{2-[1-(pyridin-2-yl)ethylideneamino]ethanolato}tetracopper(II)], [Cu4Br6(C9H11N2O)2]n or [Cu4Br6L2]n. The asymmetric unit of the crystal structure of the polymeric [Cu4Br6L2]n complex is composed by four copper (II) cations, two monodeprotonated molecules of the ligand, and six bromide anions, which act as bridges. The ligand molecules act in a tridentate fashion through their azomethine nitrogen atoms, their pyridine nitrogen atoms, and their alcoholate O atoms. The crystal structure shows two types of geometries in the coordination polyhedrons around Cu2+ ions. Two copper cations are situated in a square-based pyramidal environment, while the two other copper cations adopt a tetrahedral geometry. Bromides anions acting as bridges between two metal ions connect the units, resulting in a tetranuclear polymer compound.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-98902https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsFebruary 20242024-01-1280JUAMI, the joint undertaking for an African materials institute: building materials science research collaborations and capabilities between continents
http://scripts.iucr.org/cgi-bin/paper?vz2002
JUAMI, the joint undertaking for an African materials institute, is a project to build collaborations and materials research capabilities between PhD researchers in Africa, the United States, and the world. Focusing on research-active universities in the East African countries of Kenya, Ethiopia, Tanzania and Uganda, the effort has run a series of schools focused on materials for sustainable energy and materials for sustainable development. These bring together early-career researchers from Africa, the US, and beyond, for two weeks in a close-knit environment. The program includes lectures on cutting-edge research from internationally renowned speakers, highly interactive tutorial lectures on the science behind the research, also from internationally known researchers, and hands-on practicals and team-building exercises that culminate in group proposals from self-formed student teams. The schools have benefited more than 300 early-career students and led to proposals that have received funding and have led to research collaborations and educational non-profits. JUAMI continues and has an ongoing community of alumni who share resources and expertise, and is open to like-minded people who want to join and develop contacts and collaborations internationally.urn:issn:2056-9890Billinge, S.J.L.text/htmlJUAMI, the joint undertaking for an African materials institute, is a project to build collaborations and materials research capabilities between PhD researchers in Africa, the United States, and the world. Focusing on research-active universities in the East African countries of Kenya, Ethiopia, Tanzania and Uganda, the effort has run a series of schools focused on materials for sustainable energy and materials for sustainable development.doi:10.1107/S2056989023010915COLLABORATION; CAPABILITY BUILDING; MATERIALS SCIENCE; AFRICA2024-01-26JUAMI, the joint undertaking for an African materials institute: building materials science research collaborations and capabilities between continentsJUAMI, the joint undertaking for an African materials institute, is a project to build collaborations and materials research capabilities between PhD researchers in Africa, the United States, and the world. Focusing on research-active universities in the East African countries of Kenya, Ethiopia, Tanzania and Uganda, the effort has run a series of schools focused on materials for sustainable energy and materials for sustainable development. These bring together early-career researchers from Africa, the US, and beyond, for two weeks in a close-knit environment. The program includes lectures on cutting-edge research from internationally renowned speakers, highly interactive tutorial lectures on the science behind the research, also from internationally known researchers, and hands-on practicals and team-building exercises that culminate in group proposals from self-formed student teams. The schools have benefited more than 300 early-career students and led to proposals that have received funding and have led to research collaborations and educational non-profits. JUAMI continues and has an ongoing community of alumni who share resources and expertise, and is open to like-minded people who want to join and develop contacts and collaborations internationally.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytexthttps://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsFebruary 20242024-01-2610280105med@iucr.org2056-98902056-98902Crystal structure and Hirshfeld surface analysis of 2-picolyllithium·3thf
http://scripts.iucr.org/cgi-bin/paper?hb8083
In the title compound, (2-methylidene-1,2-dihydropyridinium-κN)tris(tetrahydrofuran-κO)lithium, [Li(C6H6N)(C4H8O)3], the lithium ion adopts a distorted LiNO3 tetrahedral coordination geometry and the 2-picolyl anion adopts its enamido form with the lithium ion lying close to the plane of the pyridine ring. A methylene group of one of the thf ligands is disordered over two orientations. In the crystal, a weak C—H⋯O interaction generates inversion dimers. A Hirshfeld surface analysis shows that H⋯H contacts dominate the packing (86%) followed by O⋯H/H⋯O and C⋯H/H⋯C contacts, which contribute 3% and 10.4%, respectively.urn:issn:2056-9890Mairath, T.Schmidt, A.Strohmann, C.text/htmlIn the title compound, the lithium ion adopts a distorted LiNO3 tetrahedral coordination geometry and the 2-picolyl anion adopts its enamido form with the lithium ion lying close to the plane of the pyridine ring. In the crystal, a weak C—H⋯O interaction generates inversion dimers. A Hirshfeld surface analysis shows that H⋯H contacts dominate the packing (86%) followed by O⋯H/H⋯O and C⋯H/H⋯C contacts, which contribute 3% and 10.4%, respectively.doi:10.1107/S2056989023010873CRYSTAL STRUCTURE; 2-PICOLYLLITHIUM; 2-METHYLPYRIDYLLITHIUM; HIRSHFELD SURFACE ANALYSIS2023-12-22Crystal structure and Hirshfeld surface analysis of 2-picolyllithium·3thfIn the title compound, (2-methylidene-1,2-dihydropyridinium-κN)tris(tetrahydrofuran-κO)lithium, [Li(C6H6N)(C4H8O)3], the lithium ion adopts a distorted LiNO3 tetrahedral coordination geometry and the 2-picolyl anion adopts its enamido form with the lithium ion lying close to the plane of the pyridine ring. A methylene group of one of the thf ligands is disordered over two orientations. In the crystal, a weak C—H⋯O interaction generates inversion dimers. A Hirshfeld surface analysis shows that H⋯H contacts dominate the packing (86%) followed by O⋯H/H⋯O and C⋯H/H⋯C contacts, which contribute 3% and 10.4%, respectively.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextJanuary 2024Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-12-22788082med@iucr.org2056-98902056-98901Crystal structures of two formamidinium hexafluoridophosphate salts, one with batch-dependent disorder
http://scripts.iucr.org/cgi-bin/paper?wm5706
Syntheses of the acyclic amidinium salts, morpholinoformamidinium hexafluoridophosphate [OC4H8N—CH=NH2]PF6 or C5H11N2O+·PF6−, 1, and pyrrolidinoformamidinium hexafluoridophosphate [C4H8N—CH= NH2]PF6 or C5H11N2+·PF6−, 2, were carried out by heating either morpholine or pyrrolidine with triethyl orthoformate and ammonium hexafluoridophosphate. Crystals of 1 obtained directly from the reaction mixture contain one cation and one anion in the asymmetric unit. The structure involves cations linked in chains parallel to the b axis by N—H⋯O hydrogen bonds in space group Pbca, with glide-related chains pointing in opposite directions. Crystals of 1 obtained by recrystallization from ethanol, however, showed a similar unit cell and the same basic structure, but unexpectedly, there was positional disorder [occupancy ratio 0.639 (4):0.361 (4)] in one of the cation chains, which lowered the crystal symmetry to the non-centrosymmetric space group Pca21, with two cations and anions in the asymmetric unit. In the pyrrolidino compound, 2, cations and anions are ordered and are stacked separately, with zigzag N—H⋯F hydrogen-bonding between stacks, forming ribbons parallel to (101), extended along the b-axis direction. Slight differences in the delocalized C=N distances between the two cations may reflect the inductive effect of the oxygen atom in the morpholino compound.urn:issn:2056-9890Neary, M.C.Corfield, P.W.R.Parkin, S.R.Saba, S.text/htmlThe crystal structures of two nitrogen heterocycle hexafluoridophosphate salts with terminal animinium groups are described. Unexpectedly, there is cation disorder in crystals of the morpholinoformamidinium compound obtained from ethanol recrystallization, which is not found in the original crystals.doi:10.1107/S2056989023010848CRYSTAL STRUCTURE; FORMAMIDINIUM ION; NITROGEN HETEROCYCLES; HEXAFLUORIDOPHOSPHATE; HYDROGEN BONDING; DISORDER2023-12-22Crystal structures of two formamidinium hexafluoridophosphate salts, one with batch-dependent disorderSyntheses of the acyclic amidinium salts, morpholinoformamidinium hexafluoridophosphate [OC4H8N—CH=NH2]PF6 or C5H11N2O+·PF6−, 1, and pyrrolidinoformamidinium hexafluoridophosphate [C4H8N—CH= NH2]PF6 or C5H11N2+·PF6−, 2, were carried out by heating either morpholine or pyrrolidine with triethyl orthoformate and ammonium hexafluoridophosphate. Crystals of 1 obtained directly from the reaction mixture contain one cation and one anion in the asymmetric unit. The structure involves cations linked in chains parallel to the b axis by N—H⋯O hydrogen bonds in space group Pbca, with glide-related chains pointing in opposite directions. Crystals of 1 obtained by recrystallization from ethanol, however, showed a similar unit cell and the same basic structure, but unexpectedly, there was positional disorder [occupancy ratio 0.639 (4):0.361 (4)] in one of the cation chains, which lowered the crystal symmetry to the non-centrosymmetric space group Pca21, with two cations and anions in the asymmetric unit. In the pyrrolidino compound, 2, cations and anions are ordered and are stacked separately, with zigzag N—H⋯F hydrogen-bonding between stacks, forming ribbons parallel to (101), extended along the b-axis direction. Slight differences in the delocalized C=N distances between the two cations may reflect the inductive effect of the oxygen atom in the morpholino compound.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext882023-12-22research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsJanuary 202480med@iucr.org9312056-98902056-9890Temperature-dependent solid-state phase transition with twinning in the crystal structure of 4-methoxyanilinium chloride
http://scripts.iucr.org/cgi-bin/paper?hb8089
At room temperature, the title salt, C7H10NO+·Cl−, is orthorhombic, space group Pbca with Z′ = 1, as previously reported [Zhao (2009). Acta Cryst. E65, o2378]. Between 250 and 200 K, there is a solid-state phase transition to a twinned monoclinic P21/c structure with Z′ = 2. We report the high temperature structure at 250 K and the low-temperature structure at 100 K. In the low-temperature structure, the –NH3 hydrogen atoms are ordered and this group has a different orientation in each independent molecule, in keeping with optimizing N—H⋯Cl hydrogen bonding, some of which are bifurcated: these hydrogen bonds have N⋯Cl distances in the range 3.1201 (8)–3.4047 (8) Å. In the single cation of the high-temperature structure, the NH hydrogen atoms are disordered into the average of the two low-temperature positions and the N⋯Cl hydrogen bond distances are in the range 3.1570 (15)–3.3323 (18) Å. At both temperatures, the methoxy group is nearly coplanar with the rest of the molecule, with the C—C—O—C torsion angles being −7.0 (2)° at 250 K and −6.94 (12) and −9.35 (12)° at 100 K. In the extended orthorhombic structure, (001) hydrogen-bonded sheets occur; in the monoclinic structure, the sheets propagate in the (010) plane.urn:issn:2056-9890Uppu, R.M.Babu, S.Fronczek, F.R.text/htmlThe room temperature (298 K) structure of the title salt has been redetermined with disordered H atoms for the –NH3 group. Additionally, a twinned monoclinic structure has been identified with lower symmetry at low temperature (100 K) in which the H atoms of the –NH3 groups are ordered to optimize N—H⋯Cl hydrogen bonding.doi:10.1107/S2056989023010812CRYSTAL STRUCTURE; 4-ALKOXYACETANILIDES; 4-ALKOXYANILINIUM SALTS; NONSTEROIDAL ANALGESICS; MECHANISMS OF TOXICITY2023-12-22Temperature-dependent solid-state phase transition with twinning in the crystal structure of 4-methoxyanilinium chlorideAt room temperature, the title salt, C7H10NO+·Cl−, is orthorhombic, space group Pbca with Z′ = 1, as previously reported [Zhao (2009). Acta Cryst. E65, o2378]. Between 250 and 200 K, there is a solid-state phase transition to a twinned monoclinic P21/c structure with Z′ = 2. We report the high temperature structure at 250 K and the low-temperature structure at 100 K. In the low-temperature structure, the –NH3 hydrogen atoms are ordered and this group has a different orientation in each independent molecule, in keeping with optimizing N—H⋯Cl hydrogen bonding, some of which are bifurcated: these hydrogen bonds have N⋯Cl distances in the range 3.1201 (8)–3.4047 (8) Å. In the single cation of the high-temperature structure, the NH hydrogen atoms are disordered into the average of the two low-temperature positions and the N⋯Cl hydrogen bond distances are in the range 3.1570 (15)–3.3323 (18) Å. At both temperatures, the methoxy group is nearly coplanar with the rest of the molecule, with the C—C—O—C torsion angles being −7.0 (2)° at 250 K and −6.94 (12) and −9.35 (12)° at 100 K. In the extended orthorhombic structure, (001) hydrogen-bonded sheets occur; in the monoclinic structure, the sheets propagate in the (010) plane.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org6112056-98902056-9890582023-12-22Acta Crystallographica Section E: Crystallographic CommunicationsJanuary 2024research communicationshttps://creativecommons.org/licenses/by/4.0/80Crystal structure and Hirshfeld surface analysis of diethyl (3aS,3a1R,4S,5S,6R,6aS,7R,9aS)-3a1,5,6,6a-tetrahydro-1H,3H,4H,7H-3a,6:7,9a-diepoxybenzo[de]isochromene-4,5-dicarboxylate
http://scripts.iucr.org/cgi-bin/paper?jy2042
In the title compound, C18H22O7, two hexane rings and an oxane ring are fused together. The two hexane rings tend toward a distorted boat conformation, while the tetrahydrofuran and dihydrofuran rings adopt envelope conformations. The oxane ring is puckered. The crystal structure features C—H⋯O hydrogen bonds, which link the molecules into a three-dimensional network. According to a Hirshfeld surface study, H⋯H (60.3%) and O⋯H/H⋯O (35.3%) interactions are the most significant contributors to the crystal packing.urn:issn:2056-9890Sadikhova, N.D.Atioğlu, Z.Guliyeva, N.A.Podrezova, A.G.Nikitina, E.V.Akkurt, M.Bhattarai, A.text/htmlThe crystal structure of the title compound features C—H⋯O hydrogen bonds, which link the molecules into a three-dimensional network.doi:10.1107/S2056989023010794CRYSTAL STRUCTURE; (1R,4S)-7-OXABICYCLO[2.2.1]HEPT-2-ENE; (1S,4S)-7-OXABICYCLO[2.2.1]HEPTANE; OXANE; WEAK INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-12-22Crystal structure and Hirshfeld surface analysis of diethyl (3aS,3a1R,4S,5S,6R,6aS,7R,9aS)-3a1,5,6,6a-tetrahydro-1H,3H,4H,7H-3a,6:7,9a-diepoxybenzo[de]isochromene-4,5-dicarboxylateIn the title compound, C18H22O7, two hexane rings and an oxane ring are fused together. The two hexane rings tend toward a distorted boat conformation, while the tetrahydrofuran and dihydrofuran rings adopt envelope conformations. The oxane ring is puckered. The crystal structure features C—H⋯O hydrogen bonds, which link the molecules into a three-dimensional network. According to a Hirshfeld surface study, H⋯H (60.3%) and O⋯H/H⋯O (35.3%) interactions are the most significant contributors to the crystal packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext80Acta Crystallographica Section E: Crystallographic CommunicationsJanuary 2024https://creativecommons.org/licenses/by/4.0/research communications832023-12-222056-98902056-9890187med@iucr.orgCrystal structure and Hirshfeld surface analysis of 3-benzyl-2-[bis(1H-pyrrol-2-yl)methyl]thiophene
http://scripts.iucr.org/cgi-bin/paper?jy2043
In the title compound, C20H18N2S, the asymmetric unit comprises two similar molecules (A and B). In molecule A, the central thiophene ring makes dihedral angles of 89.96 (12) and 57.39 (13)° with the 1H-pyrrole rings, which are bent at 83.22 (14)° relative to each other, and makes an angle of 85.98 (11)° with the phenyl ring. In molecule B, the corresponding dihedral angles are 89.49 (13), 54.64 (12)°, 83.62 (14)° and 85.67 (11)°, respectively. In the crystal, molecular pairs are bonded to each other by N—H⋯N interactions. N—H⋯π and C—H⋯π interactions further connect the molecules, forming a three-dimensional network. A Hirshfeld surface analysis indicates that H⋯H (57.1% for molecule A; 57.3% for molecule B), C⋯H/H⋯C (30.7% for molecules A and B) and S⋯H/H⋯S (6.2% for molecule A; 6.4% for molecule B) interactions are the most important contributors to the crystal packing.urn:issn:2056-9890Sadikhova, N.D.Atioğlu, Z.Guliyeva, N.A.Shelukho, E.R.Polyanskaya, D.K.Khrustalev, V.N.Akkurt, M.Bhattarai, A.text/htmlThe asymmetric unit of the title compound contains two similar molecules. In the crystal, molecular pairs are bonded to each other by N—H⋯N interactions. N—H⋯π and C—H⋯π interactions further connect the molecules, forming a three-dimensional network.doi:10.1107/S2056989023010800CRYSTAL STRUCTURE; THIOPHENE RING; 1H-PYRROLE RING; HYDROGEN BONDS; HIRSHFELD SURFACE ANALYSIS2023-12-22Crystal structure and Hirshfeld surface analysis of 3-benzyl-2-[bis(1H-pyrrol-2-yl)methyl]thiopheneIn the title compound, C20H18N2S, the asymmetric unit comprises two similar molecules (A and B). In molecule A, the central thiophene ring makes dihedral angles of 89.96 (12) and 57.39 (13)° with the 1H-pyrrole rings, which are bent at 83.22 (14)° relative to each other, and makes an angle of 85.98 (11)° with the phenyl ring. In molecule B, the corresponding dihedral angles are 89.49 (13), 54.64 (12)°, 83.62 (14)° and 85.67 (11)°, respectively. In the crystal, molecular pairs are bonded to each other by N—H⋯N interactions. N—H⋯π and C—H⋯π interactions further connect the molecules, forming a three-dimensional network. A Hirshfeld surface analysis indicates that H⋯H (57.1% for molecule A; 57.3% for molecule B), C⋯H/H⋯C (30.7% for molecules A and B) and S⋯H/H⋯S (6.2% for molecule A; 6.4% for molecule B) interactions are the most important contributors to the crystal packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext12056-98902056-9890med@iucr.org7780722023-12-22January 2024Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/Crystal structure and Hirshfeld surface analysis of dimethyl 4-hydroxy-5,4′-dimethyl-2′-(toluene-4-sulfonylamino)biphenyl-2,3-dicarboxylate
http://scripts.iucr.org/cgi-bin/paper?jy2041
In the title compound, C25H25NO7S, the molecular conformation is stabilized by intramolecular O—H⋯O and N—H⋯O hydrogen bonds, which form S(6) and S(8) ring motifs, respectively. The molecules are bent at the S atom with a C—SO2—NH—C torsion angle of −70.86 (11)°. In the crystal, molecules are linked by C—H⋯O and N—H⋯O hydrogen bonds, forming molecular layers parallel to the (100) plane. C—H⋯π interactions are observed between these layers.urn:issn:2056-9890Guliyeva, N.A.Burkin, G.M.Annadurdyyeva, S.Khrustalev, V.N.Atioğlu, Z.Akkurt, M.Bhattarai, A.text/htmlIn the crystal, molecules are connected by C—H⋯O and N—H⋯O hydrogen bonds, forming molecular layers parallel to the (100) plane. These layers are connected to each other by C—H⋯π interactions.doi:10.1107/S205698902301071XCRYSTAL STRUCTURE; HYDROGEN BONDS; HIRSHFELD SURFACE ANALYSIS; [4+2] CYCLOADDITION; FURAN; ARYLSULFONAMIDES2023-12-22Crystal structure and Hirshfeld surface analysis of dimethyl 4-hydroxy-5,4′-dimethyl-2′-(toluene-4-sulfonylamino)biphenyl-2,3-dicarboxylateIn the title compound, C25H25NO7S, the molecular conformation is stabilized by intramolecular O—H⋯O and N—H⋯O hydrogen bonds, which form S(6) and S(8) ring motifs, respectively. The molecules are bent at the S atom with a C—SO2—NH—C torsion angle of −70.86 (11)°. In the crystal, molecules are linked by C—H⋯O and N—H⋯O hydrogen bonds, forming molecular layers parallel to the (100) plane. C—H⋯π interactions are observed between these layers.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext66med@iucr.org2056-98902056-98901Acta Crystallographica Section E: Crystallographic CommunicationsJanuary 2024https://creativecommons.org/licenses/by/4.0/research communications622023-12-2280Synthesis, crystal structure and properties of poly[(μ-2-methylpyridine N-oxide-κ2O:O)bis(μ-thiocyanato-κ2N:S)cobalt(II)]
http://scripts.iucr.org/cgi-bin/paper?pk2699
The title compound, [Co(NCS)2(C6H7NO)]n or Co(NCS)2(2-methylpyridine N-oxide), was prepared by the reaction of Co(NCS)2 and 2-methylpyridine N-oxide in methanol. All crystals obtained by this procedure show reticular pseudo-merohedric twinning, but after recrystallization, one crystal was found that had a minor component with only a very few overlapping reflections. The asymmetric unit consists of one CoII cation, two thiocyanate anions and one 2-methylpyridine N-oxide coligand in general positions. The CoII cations are octahedrally coordinated by two O-bonding 2-methylpyridine N-oxide ligands, as well as two S- and two N-bonding thiocyanate anions, and are connected via μ-1,3(N,S)-bridging thiocyanate anions into chains that are linked by μ-1,1(O,O) bridging coligands into layers. No pronounced directional intermolecular interactions are observed between the layers. The 2-methylpyridine coligand is disordered over two orientations and was refined using a split model with restraints. Powder X-ray diffraction (PXRD) indicates that a pure sample was obtained and IR spectroscopy confirms that bridging thiocyanate anions are present. Thermogravimetry and differential thermoanalysis (TG-DTA) shows one poorly resolved mass loss in the TG curve that is accompanied by an exothermic and an endothermic signal in the DTA curve, which indicate the decomposition of the 2-methylpyridine N-oxide coligands.urn:issn:2056-9890Näther, C.Jess, I.text/htmlIn the crystal structure of the title compound, the cobalt cations are octahedrally coordinated by two N- and two S-bonding thiocyanate anions as well as two O-bonding 2-methylpyridine N-oxide coligands. The cations are linked by pairs of anionic ligands into chains that are connected into layers by two μ-1,1-bridging O atoms of the 2-methylpyridine N-oxide coligands.doi:10.1107/S2056989023010721SYNTHESIS; CRYSTAL STRUCTURE; LAYERED STRUCTURE; IR SPECTRUM; THERMAL PROPERTIES2023-12-22Synthesis, crystal structure and properties of poly[(μ-2-methylpyridine N-oxide-κ2O:O)bis(μ-thiocyanato-κ2N:S)cobalt(II)]The title compound, [Co(NCS)2(C6H7NO)]n or Co(NCS)2(2-methylpyridine N-oxide), was prepared by the reaction of Co(NCS)2 and 2-methylpyridine N-oxide in methanol. All crystals obtained by this procedure show reticular pseudo-merohedric twinning, but after recrystallization, one crystal was found that had a minor component with only a very few overlapping reflections. The asymmetric unit consists of one CoII cation, two thiocyanate anions and one 2-methylpyridine N-oxide coligand in general positions. The CoII cations are octahedrally coordinated by two O-bonding 2-methylpyridine N-oxide ligands, as well as two S- and two N-bonding thiocyanate anions, and are connected via μ-1,3(N,S)-bridging thiocyanate anions into chains that are linked by μ-1,1(O,O) bridging coligands into layers. No pronounced directional intermolecular interactions are observed between the layers. The 2-methylpyridine coligand is disordered over two orientations and was refined using a split model with restraints. Powder X-ray diffraction (PXRD) indicates that a pure sample was obtained and IR spectroscopy confirms that bridging thiocyanate anions are present. Thermogravimetry and differential thermoanalysis (TG-DTA) shows one poorly resolved mass loss in the TG curve that is accompanied by an exothermic and an endothermic signal in the DTA curve, which indicate the decomposition of the 2-methylpyridine N-oxide coligands.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext80https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsJanuary 20242023-12-22672056-98902056-9890171med@iucr.orgCrystal structure and Hirshfeld-surface analysis of diaquabis(5-methyl-1H-1,2,4-triazole-3-carboxylato)copper(II)
http://scripts.iucr.org/cgi-bin/paper?pk2702
The title compound, [Cu(HL)2(H2O)2] or [Cu(C4H4N3O2)2(H2O)2], is a mononuclear octahedral CuII complex based on 5-methyl-1H-1,2,4-triazole-3-carboxylic acid (H2L). [Cu(HL)2(H2O)2] was synthesized by reaction of H2L with copper(II) nitrate hexahydrate (2:1 stoichiometric ratio) in water under ambient conditions to produce clear light-blue crystals. The central Cu atom exhibits an N2O4 coordination environment in an elongated octahedral geometry provided by two bidentate HL− anions in the equatorial plane and two water molecules in the axial positions. Hirshfeld surface analysis revealed that the most important contributions to the surface contacts are from H⋯O/O⋯H (33.1%), H⋯H (29.5%) and H⋯N/N⋯H (19.3%) interactions.urn:issn:2056-9890Petrenko, Y.P.Vynohradov, O.S.Khomenko, D.M.Doroshchuk, R.O.Raspertova, I.V.Shova, S.Lampeka, R.D.text/htmlHerein, the synthesis and structure of the title compound, diaquabis(5-methyl-1H-1,2,4-triazole-3-carboxylato)copper(II), which is a mononuclear complex based on 5-methyl-1H-1,2,4-triazole-3-carboxylic acid, are reported. A Hirshfeld surface analysis was also performed.doi:10.1107/S2056989023010770COPPER; COPPER COMPLEXES; CRYSTAL STRUCTURE; 1,2,4-TRIAZOLE; X-RAY CRYSTALLOGRAPHY; HIRSHFELD SURFACE ANALYSIS2023-12-22Crystal structure and Hirshfeld-surface analysis of diaquabis(5-methyl-1H-1,2,4-triazole-3-carboxylato)copper(II)The title compound, [Cu(HL)2(H2O)2] or [Cu(C4H4N3O2)2(H2O)2], is a mononuclear octahedral CuII complex based on 5-methyl-1H-1,2,4-triazole-3-carboxylic acid (H2L). [Cu(HL)2(H2O)2] was synthesized by reaction of H2L with copper(II) nitrate hexahydrate (2:1 stoichiometric ratio) in water under ambient conditions to produce clear light-blue crystals. The central Cu atom exhibits an N2O4 coordination environment in an elongated octahedral geometry provided by two bidentate HL− anions in the equatorial plane and two water molecules in the axial positions. Hirshfeld surface analysis revealed that the most important contributions to the surface contacts are from H⋯O/O⋯H (33.1%), H⋯H (29.5%) and H⋯N/N⋯H (19.3%) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-9890157med@iucr.org80January 2024Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/2023-12-2254When a dream comes true: birth of the African Crystallographic Association (AfCA)
http://scripts.iucr.org/cgi-bin/paper?vz2001
This paper summarizes brief perspectives on the historic process of establishing an African Crystallographic Association (AfCA) and includes representative references. It covers activities within four arbitrarily selected, approximate time slots, i.e., 1890s–1999, 2000–2013, 2014–2019 and 2020–2023. A genuine attempt is made to include appropriate role players, organizations and accompanying events within these periods. It concludes with the official admission of AfCA as the fifth Regional Associate of the IUCr at the 26th Congress and General Assembly of the IUCr in Melbourne, Australia in 2023.urn:issn:2056-9890Roodt, A.text/htmlThis paper summarizes brief perspectives on the historic process of establishing an African Crystallographic Association (AfCA), including appropriate role players, organizations and accompanying events. It concludes with the official admission of AfCA as the fifth Regional Associate of the IUCr at the 26th Congress and General Assembly of the IUCr in Melbourne, Australia in 2023.doi:10.1107/S2056989023010757AFRICAN CRYSTALLOGRAPHIC ASSOCIATION (AFCA); HISTORICAL NOTES; OUTREACH; PEOPLE AND EVENTS.2024-01-05When a dream comes true: birth of the African Crystallographic Association (AfCA)This paper summarizes brief perspectives on the historic process of establishing an African Crystallographic Association (AfCA) and includes representative references. It covers activities within four arbitrarily selected, approximate time slots, i.e., 1890s–1999, 2000–2013, 2014–2019 and 2020–2023. A genuine attempt is made to include appropriate role players, organizations and accompanying events within these periods. It concludes with the official admission of AfCA as the fifth Regional Associate of the IUCr at the 26th Congress and General Assembly of the IUCr in Melbourne, Australia in 2023.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext802024-01-05research communicationshttps://creativecommons.org/licenses/by/4.0/February 2024Acta Crystallographica Section E: Crystallographic Communications22056-98902056-9890med@iucr.orgCrystal structure of 2-[(5-amino-1-tosyl-1H-pyrazol-3-yl)oxy]-1-(4-methoxyphenyl)ethan-1-one 1,4-dioxane monosolvate
http://scripts.iucr.org/cgi-bin/paper?yz2045
In the structure of the title compound, C19H19N3O5S·C4H8O2, the two independent dioxane molecules each display inversion symmetry. The pyrazole ring is approximately parallel to the aromatic ring of the oxy-ethanone group and approximately perpendicular to the tolyl ring of the sulfonyl substituent. An extensive system of classical and `weak' hydrogen bonds connects the residues to form a layer structure parallel to (201), within which dimeric subunits are conspicuous; neighbouring layers are connected by classical hydrogen bonds to dioxanes and by `weak' hydrogen bonds from Htolyl donors.urn:issn:2056-9890Metwally, N.H.Elgemeie, G.H.Jones, P.G.text/htmlIn the molecular structure of the title compound, the pyrazole and its oxy-ethanone substituent lie parallel to each other, whereas the sulfonyl ring is roughly perpendicular to the pyrazole. The residues form a layer structure by hydrogen bonding.doi:10.1107/S205698902301054XCRYSTAL STRUCTURE; PYRAZOLE; TOSYL; HYDROGEN BOND2023-12-19Crystal structure of 2-[(5-amino-1-tosyl-1H-pyrazol-3-yl)oxy]-1-(4-methoxyphenyl)ethan-1-one 1,4-dioxane monosolvateIn the structure of the title compound, C19H19N3O5S·C4H8O2, the two independent dioxane molecules each display inversion symmetry. The pyrazole ring is approximately parallel to the aromatic ring of the oxy-ethanone group and approximately perpendicular to the tolyl ring of the sulfonyl substituent. An extensive system of classical and `weak' hydrogen bonds connects the residues to form a layer structure parallel to (201), within which dimeric subunits are conspicuous; neighbouring layers are connected by classical hydrogen bonds to dioxanes and by `weak' hydrogen bonds from Htolyl donors.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytexthttps://creativecommons.org/licenses/by/4.0/research communicationsJanuary 2024Acta Crystallographica Section E: Crystallographic Communications292023-12-198033med@iucr.org2056-98902056-98901Crystal structure of a water oxidation catalyst solvate with composition (NH4)2[FeIV(L-6H)]·3CH3COOH (L = clathrochelate ligand)
http://scripts.iucr.org/cgi-bin/paper?wm5703
The synthetic availability of molecular water oxidation catalysts containing high-valent ions of 3d metals in the active site is a prerequisite to enabling photo- and electrochemical water splitting on a large scale. Herein, the synthesis and crystal structure of diammonium {μ-1,3,4,7,8,10,12,13,16,17,19,22-dodecaazatetracyclo[8.8.4.13,17.18,12]tetracosane-5,6,14,15,20,21-hexaonato}ferrate(IV) acetic acid trisolvate, (NH4)2[FeIV(C12H12N12O6)]·3CH3COOH or (NH4)2[FeIV(L–6H)]·3CH3COOH is reported. The FeIV ion is encapsulated by the macropolycyclic ligand, which can be described as a dodeca-aza-quadricyclic cage with two capping triazacyclohexane fragments making three five- and six six-membered alternating chelate rings with the central FeIV ion. The local coordination environment of FeIV is formed by six deprotonated hydrazide nitrogen atoms, which stabilize the unusual oxidation state. The FeIV ion lies on a twofold rotation axis (multiplicity 4, Wyckoff letter e) of the space group C2/c. Its coordination geometry is intermediate between a trigonal prism (distortion angle φ = 0°) and an antiprism (φ = 60°) with φ = 31.1°. The Fe—N bond lengths lie in the range 1.9376 (13)–1.9617 (13) Å, as expected for tetravalent iron. Structure analysis revealed that three acetic acid molecules additionally co-crystallize per one iron(IV) complex, and one of them is positionally disordered over four positions. In the crystal structure, the ammonium cations, complex dianions and acetic acid molecules are interconnected by an intricate system of hydrogen bonds, mainly via the oxamide oxygen atoms acting as acceptors.urn:issn:2056-9890Plutenko, M.O.Shylin, S.I.Shova, S.Blinder, A.V.Fritsky, I.O.text/htmlThe coordination polyhedron of the complex [FeIV(C12H12N12O6)]2− or [FeIV(L–6H)]2− anions exhibits a shape intermediate between trigonal-prismatic and antiprismatic.doi:10.1107/S2056989023010514CLATHROCHELATE; CAGE COMPLEX; HIGH-VALENT IRON; TEMPLATE SYNTHESIS; CRYSTAL STRUCTURE2023-12-19Crystal structure of a water oxidation catalyst solvate with composition (NH4)2[FeIV(L-6H)]·3CH3COOH (L = clathrochelate ligand)The synthetic availability of molecular water oxidation catalysts containing high-valent ions of 3d metals in the active site is a prerequisite to enabling photo- and electrochemical water splitting on a large scale. Herein, the synthesis and crystal structure of diammonium {μ-1,3,4,7,8,10,12,13,16,17,19,22-dodecaazatetracyclo[8.8.4.13,17.18,12]tetracosane-5,6,14,15,20,21-hexaonato}ferrate(IV) acetic acid trisolvate, (NH4)2[FeIV(C12H12N12O6)]·3CH3COOH or (NH4)2[FeIV(L–6H)]·3CH3COOH is reported. The FeIV ion is encapsulated by the macropolycyclic ligand, which can be described as a dodeca-aza-quadricyclic cage with two capping triazacyclohexane fragments making three five- and six six-membered alternating chelate rings with the central FeIV ion. The local coordination environment of FeIV is formed by six deprotonated hydrazide nitrogen atoms, which stabilize the unusual oxidation state. The FeIV ion lies on a twofold rotation axis (multiplicity 4, Wyckoff letter e) of the space group C2/c. Its coordination geometry is intermediate between a trigonal prism (distortion angle φ = 0°) and an antiprism (φ = 60°) with φ = 31.1°. The Fe—N bond lengths lie in the range 1.9376 (13)–1.9617 (13) Å, as expected for tetravalent iron. Structure analysis revealed that three acetic acid molecules additionally co-crystallize per one iron(IV) complex, and one of them is positionally disordered over four positions. In the crystal structure, the ammonium cations, complex dianions and acetic acid molecules are interconnected by an intricate system of hydrogen bonds, mainly via the oxamide oxygen atoms acting as acceptors.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-9890128med@iucr.org80research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsJanuary 20242023-12-1925Crystal structures of sixteen phosphane chalcogenide complexes of gold(I) chloride, bromide and iodide
http://scripts.iucr.org/cgi-bin/paper?yz2044
The structures of 16 phosphane chalcogenide complexes of gold(I) halides, with the general formula R13-nR2nPEAuX (R1 = t-butyl; R2 = isopropyl; n = 0 to 3; E = S or Se; X = Cl, Br or I), are presented. The eight possible chlorido derivatives are: 1a, n = 3, E = S; 2a, n = 2, E = S; 3a, n = 1, E = S; 4a, n = 0, E = S; 5a, n = 3, E = Se; 6a, n = 2, E = Se; 7a, n = 1, E = Se; and 8a, n = 0, E = Se, and the corresponding bromido derivatives are 1b–8b in the same order. However, 2a and 2b were badly disordered and 8a was not obtained. The iodido derivatives are 2c, 6c and 7c (numbered as for the series a and b). All structures are solvent-free and all have Z′ = 1 except for 6b and 6c (Z′ = 2). All molecules show the expected linear geometry at gold and approximately tetrahedral angles P—E—Au. The presence of bulky ligands forces some short intramolecular contacts, in particular H⋯Au and H⋯E. The Au—E bond lengths have a slight but consistent tendency to be longer when trans to a softer X ligand, and vice versa. The five compounds 1a, 5a, 6a, 1b and 5b form an isotypic set, despite the different alkyl groups in 6a. Compounds 3a/3b, 4b/8b and 6b/6c form isotypic pairs. The crystal packing can be analysed in terms of various types of secondary interactions, of which the most frequent are `weak' hydrogen bonds from methine hydrogen atoms to the halogenido ligands. For the structure type 1a, H⋯X and H⋯E contacts combine to form a layer structure. For 3a/3b, the packing is almost featureless, but can be described in terms of a double-layer structure involving borderline H⋯Cl/Br and H⋯S contacts. In 4a and 4b/8b, which lack methine groups, Cmethyl—H⋯X contacts combine to form layer structures. In 7a/7b, short C—H⋯X interactions form chains of molecules that are further linked by association of short Au⋯Se contacts to form a layer structure. The packing of compound 6b/6c can conveniently be analysed for each independent molecule separately, because they occupy different regions of the cell. Molecule 1 forms chains in which the molecules are linked by a Cmethine⋯Au contact. The molecules 2 associate via a short Se⋯Se contact and a short H⋯X contact to form a layer structure. The packing of compound 2c can be described in terms of two short Cmethine—H⋯I contacts, which combine to form a corrugated ribbon structure. Compound 7c is the only compound in this paper to feature Au⋯Au contacts, which lead to twofold-symmetric dimers. Apart from this, the packing is almost featureless, consisting of layers with only translation symmetry except for two very borderline Au⋯H contacts.urn:issn:2056-9890Upmann, D.Jones, P.G.Bockfeld, D.Târcoveanu, E.text/htmlThe structures of sixteen phosphane chalcogenide complexes of gold(I) halides are presented and compared.doi:10.1107/S2056989023010459CRYSTAL STRUCTURE; GOLD(I) HALIDES; PHOSPHANE CHALCOGENIDES; SECONDARY INTERACTIONS2023-12-19Crystal structures of sixteen phosphane chalcogenide complexes of gold(I) chloride, bromide and iodideThe structures of 16 phosphane chalcogenide complexes of gold(I) halides, with the general formula R13-nR2nPEAuX (R1 = t-butyl; R2 = isopropyl; n = 0 to 3; E = S or Se; X = Cl, Br or I), are presented. The eight possible chlorido derivatives are: 1a, n = 3, E = S; 2a, n = 2, E = S; 3a, n = 1, E = S; 4a, n = 0, E = S; 5a, n = 3, E = Se; 6a, n = 2, E = Se; 7a, n = 1, E = Se; and 8a, n = 0, E = Se, and the corresponding bromido derivatives are 1b–8b in the same order. However, 2a and 2b were badly disordered and 8a was not obtained. The iodido derivatives are 2c, 6c and 7c (numbered as for the series a and b). All structures are solvent-free and all have Z′ = 1 except for 6b and 6c (Z′ = 2). All molecules show the expected linear geometry at gold and approximately tetrahedral angles P—E—Au. The presence of bulky ligands forces some short intramolecular contacts, in particular H⋯Au and H⋯E. The Au—E bond lengths have a slight but consistent tendency to be longer when trans to a softer X ligand, and vice versa. The five compounds 1a, 5a, 6a, 1b and 5b form an isotypic set, despite the different alkyl groups in 6a. Compounds 3a/3b, 4b/8b and 6b/6c form isotypic pairs. The crystal packing can be analysed in terms of various types of secondary interactions, of which the most frequent are `weak' hydrogen bonds from methine hydrogen atoms to the halogenido ligands. For the structure type 1a, H⋯X and H⋯E contacts combine to form a layer structure. For 3a/3b, the packing is almost featureless, but can be described in terms of a double-layer structure involving borderline H⋯Cl/Br and H⋯S contacts. In 4a and 4b/8b, which lack methine groups, Cmethyl—H⋯X contacts combine to form layer structures. In 7a/7b, short C—H⋯X interactions form chains of molecules that are further linked by association of short Au⋯Se contacts to form a layer structure. The packing of compound 6b/6c can conveniently be analysed for each independent molecule separately, because they occupy different regions of the cell. Molecule 1 forms chains in which the molecules are linked by a Cmethine⋯Au contact. The molecules 2 associate via a short Se⋯Se contact and a short H⋯X contact to form a layer structure. The packing of compound 2c can be described in terms of two short Cmethine—H⋯I contacts, which combine to form a corrugated ribbon structure. Compound 7c is the only compound in this paper to feature Au⋯Au contacts, which lead to twofold-symmetric dimers. Apart from this, the packing is almost featureless, consisting of layers with only translation symmetry except for two very borderline Au⋯H contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2023-12-1934Acta Crystallographica Section E: Crystallographic CommunicationsJanuary 2024research communicationshttps://creativecommons.org/licenses/by/4.0/80med@iucr.org4912056-98902056-9890Crystal structure of dilithium biphenyl-4,4′-disulfonate dihydrate
http://scripts.iucr.org/cgi-bin/paper?jp2001
The asymmetric unit of the title compound, μ-biphenyl-4,4′-disulfonato-bis(aqualithium), [Li2(C12H8O6S2)(H2O)2] or Li2[Bph(SO3)2](H2O)2, consists of an Li ion, half of the diphenyl-4,4′-disulfonate [Bph(SO3−)2] ligand, and a water molecule. The Li ion exhibits a four-coordinate tetrahedral geometry with three oxygen atoms of the Bph(SO3−)2 ligands and a water molecule. The tetrahedral LiO4 units, which are interconnected by biphenyl moieties, form a layer structure parallel to (100). These layers are further connected by hydrogen-bonding interactions to yield a three-dimensional network.urn:issn:2056-9890Kumagai, H.Kawata, S.Ogihara, N.text/htmlThe asymmetric unit of the title compound consists of an Li ion, half of the diphenyl-4,4-disulfonate ligand, and a water molecule. The Li ion exhibits a four-coordinate tetrahedral geometry with three oxygen atoms of the Bph(SO3−)2 ligands and a water molecule. The tetrahedral LiO4 units, which are interconnected by biphenyl moieties, form a layer structure parallel to (100). These layers are further connected by hydrogen-bonding interactions to yield a three-dimensional network.doi:10.1107/S2056989023010411CRYSTAL STRUCTURE; HYDROGEN BONDING; LI ION2023-12-12Crystal structure of dilithium biphenyl-4,4′-disulfonate dihydrateThe asymmetric unit of the title compound, μ-biphenyl-4,4′-disulfonato-bis(aqualithium), [Li2(C12H8O6S2)(H2O)2] or Li2[Bph(SO3)2](H2O)2, consists of an Li ion, half of the diphenyl-4,4′-disulfonate [Bph(SO3−)2] ligand, and a water molecule. The Li ion exhibits a four-coordinate tetrahedral geometry with three oxygen atoms of the Bph(SO3−)2 ligands and a water molecule. The tetrahedral LiO4 units, which are interconnected by biphenyl moieties, form a layer structure parallel to (100). These layers are further connected by hydrogen-bonding interactions to yield a three-dimensional network.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2412056-98902056-9890222023-12-12https://creativecommons.org/licenses/by/4.0/research communicationsJanuary 2024Acta Crystallographica Section E: Crystallographic Communications80The synthesis and structural properties of a chloridobis{N-[(4-methoxyphenyl)imino]pyrrolidine-1-carboxamide}zinc(II) (acetonitrile)trichloridozincate coordination complex
http://scripts.iucr.org/cgi-bin/paper?yy2008
The title complex, [ZnCl(C12H15N3O2)2][ZnCl3(CH3CN)], was synthesized and its structure was fully characterized through single-crystal X-ray diffraction analysis. The complex crystallizes in the orthorhombic system, space group Pbca (61), with a central zinc atom coordinating one chlorine atom and two pyrrolidinyl-4-methoxyphenyl azoformamide ligands in a bidentate manner, utilizing both the nitrogen and oxygen atoms in a 1,3-heterodiene (N=N—C=O) motif for coordinative bonding, yielding an overall positively (+1) charged complex. The complex is accompanied by a [(CH3CN)ZnCl3]− counter-ion. The crystal data show that the harder oxygen atoms in the heterodiene zinc chelate form bonding interactions with distances of 2.002 (3) and 2.012 (3) Å, while nitrogen atoms are coordinated by the central zinc cation with bond lengths of 2.207 (3) and 2.211 (3) Å. To gain further insight into the intermolecular interactions within the crystal, Hirshfeld surface analysis was performed, along with the calculation of two-dimensional fingerprint plots. This analysis revealed that H⋯H (39.9%), Cl⋯H/H⋯Cl (28.2%) and C⋯H/H⋯C (7.2%) interactions are dominant. This unique crystal structure sheds light on arrangement and bonding interactions with azoformamide ligands, and their unique qualities over similar semicarbazone and azothioformamide structures.urn:issn:2056-9890Tiwari, L.Waynant, K.V.text/htmlThe title compound was formed from the reaction of zinc(II) chloride and pyrrolidine-4-methoxyphenyl azoformamide ligands. The ligands associated in a bidentate manner and the recrystallized complex indicated that the central zinc(II) gave a chloride to a second zinc(II) chloride compound and associated with an acetonitrile solvent to give a acetonitriletrichloridozincate counter-ion.doi:10.1107/S2056989023010447CRYSTAL STRUCTURE; COORDINATION COMPLEX; ZINC(II); ARYLAZOFORMAMIDE2023-12-07The synthesis and structural properties of a chloridobis{N-[(4-methoxyphenyl)imino]pyrrolidine-1-carboxamide}zinc(II) (acetonitrile)trichloridozincate coordination complexThe title complex, [ZnCl(C12H15N3O2)2][ZnCl3(CH3CN)], was synthesized and its structure was fully characterized through single-crystal X-ray diffraction analysis. The complex crystallizes in the orthorhombic system, space group Pbca (61), with a central zinc atom coordinating one chlorine atom and two pyrrolidinyl-4-methoxyphenyl azoformamide ligands in a bidentate manner, utilizing both the nitrogen and oxygen atoms in a 1,3-heterodiene (N=N—C=O) motif for coordinative bonding, yielding an overall positively (+1) charged complex. The complex is accompanied by a [(CH3CN)ZnCl3]− counter-ion. The crystal data show that the harder oxygen atoms in the heterodiene zinc chelate form bonding interactions with distances of 2.002 (3) and 2.012 (3) Å, while nitrogen atoms are coordinated by the central zinc cation with bond lengths of 2.207 (3) and 2.211 (3) Å. To gain further insight into the intermolecular interactions within the crystal, Hirshfeld surface analysis was performed, along with the calculation of two-dimensional fingerprint plots. This analysis revealed that H⋯H (39.9%), Cl⋯H/H⋯Cl (28.2%) and C⋯H/H⋯C (7.2%) interactions are dominant. This unique crystal structure sheds light on arrangement and bonding interactions with azoformamide ligands, and their unique qualities over similar semicarbazone and azothioformamide structures.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext17med@iucr.org2056-98902056-98901research communicationshttps://creativecommons.org/licenses/by/4.0/January 2024Acta Crystallographica Section E: Crystallographic Communications142023-12-0780Crystal structure of [1,3-bis(2,4,6-trimethylphenyl)imidazolidin-2-ylidene]dichlorido(2-{[(2-methoxyethyl)(methyl)amino]methyl}benzylidene)ruthenium
http://scripts.iucr.org/cgi-bin/paper?tx2079
The title compound, [RuCl2(C33H43N3O)], is an example of a new generation of N,N-dialkyl ruthenium catalysts with an N—Ru coordination bond as part of a six-membered chelate ring. The Ru atom has an Addison τ parameter of 0.244, which indicates a geometry intermediate between square-based pyramidal and trigonal–bipyramidal. The complex shows the usual trans arrangement of the two chlorides, with Ru—Cl bond lengths of 2.3515 (8) and 2.379 (7) Å, and a Cl—Ru—Cl angle of 158.02 (3)°. One of the chlorine atoms and the atoms of the 2-methoxy-N-methyl-N-[(2-methylphenyl)methyl]ethane-1-amine group of the title complex display disorder over two positions in a 0.889 (2): 0.111 (2) ratio.urn:issn:2056-9890Mammadova, G.Z.Atioğlu, Z.Akkurt, M.Grigoriev, M.S.Volchkov, N.S.Azizova, A.N.Bhattarai, A.Antonova, A.S.text/htmlThe title compound [RuCl2(C33H44N3O)] is an example of a new generation of N,N-dialkyl metallocomplex ruthenium catalysts with an N→Ru coordination bond in a six-membered chelate ring.doi:10.1107/S2056989023010381CRYSTAL STRUCTURE; RUTHENIUM CATALYST; HOVEYDA-GRUBBS CATALYST; OLEFIN METATHESIS2023-12-19Crystal structure of [1,3-bis(2,4,6-trimethylphenyl)imidazolidin-2-ylidene]dichlorido(2-{[(2-methoxyethyl)(methyl)amino]methyl}benzylidene)rutheniumThe title compound, [RuCl2(C33H43N3O)], is an example of a new generation of N,N-dialkyl ruthenium catalysts with an N—Ru coordination bond as part of a six-membered chelate ring. The Ru atom has an Addison τ parameter of 0.244, which indicates a geometry intermediate between square-based pyramidal and trigonal–bipyramidal. The complex shows the usual trans arrangement of the two chlorides, with Ru—Cl bond lengths of 2.3515 (8) and 2.379 (7) Å, and a Cl—Ru—Cl angle of 158.02 (3)°. One of the chlorine atoms and the atoms of the 2-methoxy-N-methyl-N-[(2-methylphenyl)methyl]ethane-1-amine group of the title complex display disorder over two positions in a 0.889 (2): 0.111 (2) ratio.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext502023-12-19January 2024Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications80med@iucr.org5312056-98902056-9890Crystal structure and Hirshfeld surface analysis of a new benzimidazole compound, 3-{1-[(2-hydroxyphenyl)methyl]-1H-1,3-benzodiazol-2-yl}phenol
http://scripts.iucr.org/cgi-bin/paper?zn2033
The title compound, C20H16N2O2, is composed of two monosubstituted benzene rings and one benzimidazole unit. The benzimidazole moiety subtends dihedral angles of 46.16 (7) and 77.45 (8)° with the benzene rings, which themselves form a dihedral angle of 54.34 (9)°. The crystal structure features O—H⋯N and O—H⋯O hydrogen-bonding interactions, which together lead to the formation of two-dimensional hydrogen-bonded layers parallel to the (101) plane. In addition, π–π interactions also contribute to the crystal cohesion. Hirshfeld surface analysis indicates that the most significant contacts in the crystal packing are: H⋯H (47.5%), O⋯H/H⋯O (12.4%), N⋯H/H⋯N (6.1%), C⋯H/H⋯C (27.6%) and C⋯C (4.6%).urn:issn:2056-9890Bouhidel, Z.Sahli, K.Cherouana, A.text/htmlIn the title compound, the benzimidazole moiety subtends dihedral angles of 46.16 (7) and 77.45 (8)° with the benzene rings, which themselves form a dihedral angle of 54.34 (9)°. The crystal structure features O—H⋯N and O—H⋯O hydrogen-bonding interactions, which together lead to the formation of two-dimensional hydrogen-bonded layers parallel to the (101) plane, as well as π–π interactionsdoi:10.1107/S2056989023010368BENZIMIDAZOLE; SINGLE CRYSTAL; X-RAY DIFFRACTION; HYDROGEN BONDING; INTERMOLECULAR INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-12-12Crystal structure and Hirshfeld surface analysis of a new benzimidazole compound, 3-{1-[(2-hydroxyphenyl)methyl]-1H-1,3-benzodiazol-2-yl}phenolThe title compound, C20H16N2O2, is composed of two monosubstituted benzene rings and one benzimidazole unit. The benzimidazole moiety subtends dihedral angles of 46.16 (7) and 77.45 (8)° with the benzene rings, which themselves form a dihedral angle of 54.34 (9)°. The crystal structure features O—H⋯N and O—H⋯O hydrogen-bonding interactions, which together lead to the formation of two-dimensional hydrogen-bonded layers parallel to the (101) plane. In addition, π–π interactions also contribute to the crystal cohesion. Hirshfeld surface analysis indicates that the most significant contacts in the crystal packing are: H⋯H (47.5%), O⋯H/H⋯O (12.4%), N⋯H/H⋯N (6.1%), C⋯H/H⋯C (27.6%) and C⋯C (4.6%).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytexthttps://creativecommons.org/licenses/by/4.0/research communicationsJanuary 2024Acta Crystallographica Section E: Crystallographic Communications182023-12-128021med@iucr.org2056-98902056-98901New copper carboxylate pyrene dimers: synthesis, crystal structure, Hirshfeld surface analysis and electrochemical characterization
http://scripts.iucr.org/cgi-bin/paper?ny2001
Two new copper dimers, namely, bis(dimethyl sulfoxide)tetrakis(μ-pyrene-1-carboxylato)dicopper(Cu—Cu), [Cu2(C17H9O2)4(C2H6OS)2] or [Cu2(pyr-COO−)4(DMSO)2] (1), and bis(dimethylformamide)tetrakis(μ-pyrene-1-carboxylato)dicopper(Cu—Cu), [Cu2(C17H9O2)4(C3H7NO)2] or [Cu2(pyr-COO−)4(DMF)2] (2) (pyr = pyrene), were synthesized from the reaction of pyrene-1-carboxylic acid, copper(II) nitrate and triethylamine from solvents DMSO and DMF, respectively. While 1 crystallized in the space group P\overline{1}, the crystal structure of 2 is in space group P21/n. The Cu atoms have octahedral geometries, with four oxygen atoms from carboxylate pyrene ligands occupying the equatorial positions, a solvent molecule coordinating at one of the axial positions, and a Cu⋯Cu contact in the opposite position. The packing in the crystal structures exhibits π–π stacking interactions and short contacts through the solvent molecules. The Hirshfeld surfaces and two-dimensional fingerprint plots were generated for both compounds to better understand the intermolecular interactions and the contribution of heteroatoms from the solvent ligands to the crystal packing. In addition, a Cu2+/Cu1+ quasi-reversible redox process was identified for compound 2 using cyclic voltammetry that accounts for a diffusion-controlled electron-donation process to the Cu dimer.urn:issn:2056-9890Nogué-Guzmán, V.C.Burgos-Suazo, A.Rivera-Reyes, J.O.Montes Quiñones, V.P.Ramis-Aybar, P.C.Burgos-Jiménez, A.C.González-Nieves, K.Piñero-Cruz, D.M.text/htmlTwo new copper dimers, [Cu2(pyr-COO–)4(DMSO)2] (1) and [Cu2(pyr-COO–)4(DMF)2] (2) (pyr = pyrene) were synthesized from the reaction of pyrene-1-carboxylic acid, copper(II) nitrate and triethylamine from solvents DMSO and DMF, respectively. Electrochemical characterization and Hirshfeld surface analysis was carried out.doi:10.1107/S2056989023010277DICOPPER; CARBOXYLATE; PYRENE; [PI]-[PI] STACKING; CRYSTAL STRUCTURE2023-12-05New copper carboxylate pyrene dimers: synthesis, crystal structure, Hirshfeld surface analysis and electrochemical characterizationTwo new copper dimers, namely, bis(dimethyl sulfoxide)tetrakis(μ-pyrene-1-carboxylato)dicopper(Cu—Cu), [Cu2(C17H9O2)4(C2H6OS)2] or [Cu2(pyr-COO−)4(DMSO)2] (1), and bis(dimethylformamide)tetrakis(μ-pyrene-1-carboxylato)dicopper(Cu—Cu), [Cu2(C17H9O2)4(C3H7NO)2] or [Cu2(pyr-COO−)4(DMF)2] (2) (pyr = pyrene), were synthesized from the reaction of pyrene-1-carboxylic acid, copper(II) nitrate and triethylamine from solvents DMSO and DMF, respectively. While 1 crystallized in the space group P\overline{1}, the crystal structure of 2 is in space group P21/n. The Cu atoms have octahedral geometries, with four oxygen atoms from carboxylate pyrene ligands occupying the equatorial positions, a solvent molecule coordinating at one of the axial positions, and a Cu⋯Cu contact in the opposite position. The packing in the crystal structures exhibits π–π stacking interactions and short contacts through the solvent molecules. The Hirshfeld surfaces and two-dimensional fingerprint plots were generated for both compounds to better understand the intermolecular interactions and the contribution of heteroatoms from the solvent ligands to the crystal packing. In addition, a Cu2+/Cu1+ quasi-reversible redox process was identified for compound 2 using cyclic voltammetry that accounts for a diffusion-controlled electron-donation process to the Cu dimer.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2023-12-05Acta Crystallographica Section E: Crystallographic CommunicationsJanuary 2024research communicationshttps://creativecommons.org/licenses/by/4.0/80med@iucr.org12056-98902056-9890Dimorphism of [Bi2O2(OH)](NO3) – the ordered Pna21 structure at 100 K
http://scripts.iucr.org/cgi-bin/paper?hb8084
The re-investigation of [Bi2O2(OH)](NO3), dioxidodibismuth(III) hydroxide nitrate, on the basis of single-crystal X-ray diffraction data revealed an apparent structural phase transition of a crystal structure determined previously (space group Cmc21 at 173 K) to a crystal structure with lower symmetry (space group Pna21 at 100 K). The Cmc21 → Pna21 group–subgroup relationship between the two crystal structures is klassengleiche with index 2. In contrast to the crystal structure in Cmc21 with orientational disorder of the nitrate anion, disorder does not occur in the Pna21 structure. Apart from the disorder of the nitrate anion, the general structural set-up in the two crystal structures is very similar: [Bi2O2]2+ layers extend parallel to (001) and alternate with layers of (OH)− anions above and (NO3)− anions below the cationic layer. Whereas the (OH)− anion shows strong bonds to the BiIII cations, the (NO3)− anion weakly binds to the BiIII cations of the cationic layer. A rather weak O—H⋯O hydrogen-bonding interaction between the (OH)− anion and the (NO3)− anion links adjacent sheets along [001].urn:issn:2056-9890Weil, M.Missen, O.P.Mills, S.J.text/htmlA structural phase transition occurs for [Bi2O2(OH)](NO3) between 173 K (space group Cmc21; previous single-crystal X-ray data) and 100 K (space group Pna21; current single-crystal X-ray data).doi:10.1107/S205698902301023XCRYSTAL STRUCTURE; PHASE TRANSITION; ORDERED STRUCTURE; [BI2O2]2+; NITRATE GROUP; GROUP-SUBGROUP RELATIONSHIP; BARNIGHAUSEN TREE2023-11-30Dimorphism of [Bi2O2(OH)](NO3) – the ordered Pna21 structure at 100 KThe re-investigation of [Bi2O2(OH)](NO3), dioxidodibismuth(III) hydroxide nitrate, on the basis of single-crystal X-ray diffraction data revealed an apparent structural phase transition of a crystal structure determined previously (space group Cmc21 at 173 K) to a crystal structure with lower symmetry (space group Pna21 at 100 K). The Cmc21 → Pna21 group–subgroup relationship between the two crystal structures is klassengleiche with index 2. In contrast to the crystal structure in Cmc21 with orientational disorder of the nitrate anion, disorder does not occur in the Pna21 structure. Apart from the disorder of the nitrate anion, the general structural set-up in the two crystal structures is very similar: [Bi2O2]2+ layers extend parallel to (001) and alternate with layers of (OH)− anions above and (NO3)− anions below the cationic layer. Whereas the (OH)− anion shows strong bonds to the BiIII cations, the (NO3)− anion weakly binds to the BiIII cations of the cationic layer. A rather weak O—H⋯O hydrogen-bonding interaction between the (OH)− anion and the (NO3)− anion links adjacent sheets along [001].https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79Acta Crystallographica Section E: Crystallographic CommunicationsDecember 2023https://creativecommons.org/licenses/by/4.0/research communications2023-11-3012232056-98902056-9890121227med@iucr.orgSynthesis, crystal structure and computational analysis of 2,7-bis(4-chlorophenyl)-3,3-dimethyl-1,4-diazepan-5-one
http://scripts.iucr.org/cgi-bin/paper?jw2001
In the title compound, C19H20Cl2N2O, the seven-membered 1,4-diazepane ring adopts a chair conformation while the 4-chlorophenyl substituents adopt equatorial orientations. The chlorophenyl ring at position 7 is disordered over two positions [site occupancies 0.480 (16):0.520 (16)]. The dihedral angle between the two benzene rings is 63.0 (4)°. The methyl groups at position 3 have an axial and an equatorial orientation. The compound exists as a dimer exhibiting intermolecular N—H⋯O hydrogen bonding with R22(8) graph-set motifs. The crystal structure is further stabilized by C—H⋯O hydrogen bonds together with two C—Cl⋯π (ring) interactions. The geometry was optimized by DFT using the B3LYP/6–31 G(d,p) level basis set. In addition, the HOMO and LUMO energies, chemical reactivity parameters and molecular electrostatic potential were calculated at the same level of theory. Hirshfeld surface analysis indicated that the most important contributions to the crystal packing are from H⋯H (45.6%), Cl⋯H/H⋯Cl (23.8%), H⋯C/C⋯H (12.6%), H⋯O/O⋯H (8.7%) and C⋯Cl/Cl⋯C (7.1%) interactions. Analysis of the interaction energies showed that the dispersion energy is greater than the electrostatic energy. A crystal void volume of 237.16 Å3 is observed. A molecular docking study with the human oestrogen receptor 3ERT protein revealed good docking with a score of −8.9 kcal mol−1.urn:issn:2056-9890Akila, S.Vidhyasagar, T.Winfred Jebaraj, J.P.Thiruvalluvar, A.A.Rajeswari, K.text/htmlThe seven-membered 1,4-diazepane ring adopts a chair conformation with the 4-chlorophenyl groups in equatorial orientations. The title compound possesses a docking score of −8.9 kcal mol−1 with the human oestrogen receptor 3ERT protein.doi:10.1107/S2056989023010162SYNTHESIS; X-RAY CRYSTAL STRUCTURE; C-H...O AND N-H...O HYDROGEN BONDS; C-CL...[PI] (RING) INTERACTIONS; 1,4-DIAZEPANE DERIVATIVE; CHAIR CONFORMATION; DFT; HIRSHFELD SURFACE ANALYSIS; 3ERT PROTEIN; MOLECULAR DOCKING2023-11-30Synthesis, crystal structure and computational analysis of 2,7-bis(4-chlorophenyl)-3,3-dimethyl-1,4-diazepan-5-oneIn the title compound, C19H20Cl2N2O, the seven-membered 1,4-diazepane ring adopts a chair conformation while the 4-chlorophenyl substituents adopt equatorial orientations. The chlorophenyl ring at position 7 is disordered over two positions [site occupancies 0.480 (16):0.520 (16)]. The dihedral angle between the two benzene rings is 63.0 (4)°. The methyl groups at position 3 have an axial and an equatorial orientation. The compound exists as a dimer exhibiting intermolecular N—H⋯O hydrogen bonding with R22(8) graph-set motifs. The crystal structure is further stabilized by C—H⋯O hydrogen bonds together with two C—Cl⋯π (ring) interactions. The geometry was optimized by DFT using the B3LYP/6–31 G(d,p) level basis set. In addition, the HOMO and LUMO energies, chemical reactivity parameters and molecular electrostatic potential were calculated at the same level of theory. Hirshfeld surface analysis indicated that the most important contributions to the crystal packing are from H⋯H (45.6%), Cl⋯H/H⋯Cl (23.8%), H⋯C/C⋯H (12.6%), H⋯O/O⋯H (8.7%) and C⋯Cl/Cl⋯C (7.1%) interactions. Analysis of the interaction energies showed that the dispersion energy is greater than the electrostatic energy. A crystal void volume of 237.16 Å3 is observed. A molecular docking study with the human oestrogen receptor 3ERT protein revealed good docking with a score of −8.9 kcal mol−1.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-11-301212December 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/122056-98902056-9890med@iucr.org1217Synthesis and redetermination of the crystal structure of NbF5
http://scripts.iucr.org/cgi-bin/paper?ox2001
Single crystals of NbF5, niobium(V) fluoride, have been obtained by the reaction of niobium metal in a stream of dilute elemental fluorine at 473 K and subsequent sublimation. The as-obtained bulk phase compound was shown to be pure by powder X-ray diffraction at 293 K and by IR and Raman spectroscopy. A single-crystal X-ray analysis was conducted at 100 K. In comparison to the previously reported structure model [Edwards (1964). J. Chem. Soc. pp. 3714–3718], the lattice parameters and fractional atom coordinates were determined to much higher precision and individual, anisotropic displacement parameters were refined for all atoms.urn:issn:2056-9890Möbs, M.Kraus, F.text/htmlNbF5 was synthesized in high purity by direct fluorination. IR and Raman spectroscopy confirms the high purity. The crystal structure was redetermined at 100 K with higher precision.doi:10.1107/S2056989023010150CRYSTAL STRUCTURE; REDETERMINATION; NIOBIUM(V) FLUORIDE; SYNTHESIS; POWDER X-RAY DIFFRACTION2023-11-30Synthesis and redetermination of the crystal structure of NbF5Single crystals of NbF5, niobium(V) fluoride, have been obtained by the reaction of niobium metal in a stream of dilute elemental fluorine at 473 K and subsequent sublimation. The as-obtained bulk phase compound was shown to be pure by powder X-ray diffraction at 293 K and by IR and Raman spectroscopy. A single-crystal X-ray analysis was conducted at 100 K. In comparison to the previously reported structure model [Edwards (1964). J. Chem. Soc. pp. 3714–3718], the lattice parameters and fractional atom coordinates were determined to much higher precision and individual, anisotropic displacement parameters were refined for all atoms.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext12072023-11-30https://creativecommons.org/licenses/by/4.0/research communicationsDecember 2023Acta Crystallographica Section E: Crystallographic Communications79med@iucr.org1211122056-98902056-9890Synthesis, crystal structure and Hirshfeld surface analysis of a cadmium complex of naphthalene-1,5-disulfonate and o-phenylenediamine
http://scripts.iucr.org/cgi-bin/paper?dj2067
A novel o-phenylenediamine (opda)-based cadmium complex, bis(benzene-1,2-diamine-κ2N,N′)bis(benzene-1,2-diamine-κN)cadmium(II) naphthalene-1,5-disulfonate, [Cd(C6H8N2)4](C10H6O6S2), was synthesized. The complex salt crystallizes in the monoclinic space group C2/c. The Cd atom occupies a special position and coordinates six nitrogen atoms from four o-phenylenediamine molecules, two as chelating ligands and two as monodentate ligands. The amino H atoms of opda interact with two O atoms of the naphthalene-1,5-disulfonate anions. The anions act as bridges between [Cd(opda)4]2+ cations, forming a two-dimensional network in the [010] and [001] directions. The Hirshfeld surface analysis shows that the primary factors contributing to the supramolecular interactions are short contacts, particularly van der Waals forces of the type H⋯H, O⋯H and C⋯H.urn:issn:2056-9890Suyunov, J.Torambetov, B.Turaev, K.Kadirova, S.Alimnazarov, B.Ashurov, J.text/htmlThe molecular and crystal structure of a cadmium complex of naphthalene-1,5-disulfonate and o-phenylenediamine was studied and Hirshfeld surfaces and fingerprint plots were generated to investigate the various intermolecular interactions.doi:10.1107/S2056989023010125CRYSTAL STRUCTURE; CADMIUM COMPLEX; O-PHENYLENEDIAMINE; NAPHTHALENE-1,5-DISULFONATE; HIRSHFELD SURFACE ANALYSIS2023-11-30Synthesis, crystal structure and Hirshfeld surface analysis of a cadmium complex of naphthalene-1,5-disulfonate and o-phenylenediamineA novel o-phenylenediamine (opda)-based cadmium complex, bis(benzene-1,2-diamine-κ2N,N′)bis(benzene-1,2-diamine-κN)cadmium(II) naphthalene-1,5-disulfonate, [Cd(C6H8N2)4](C10H6O6S2), was synthesized. The complex salt crystallizes in the monoclinic space group C2/c. The Cd atom occupies a special position and coordinates six nitrogen atoms from four o-phenylenediamine molecules, two as chelating ligands and two as monodentate ligands. The amino H atoms of opda interact with two O atoms of the naphthalene-1,5-disulfonate anions. The anions act as bridges between [Cd(opda)4]2+ cations, forming a two-dimensional network in the [010] and [001] directions. The Hirshfeld surface analysis shows that the primary factors contributing to the supramolecular interactions are short contacts, particularly van der Waals forces of the type H⋯H, O⋯H and C⋯H.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext7911902023-11-30Acta Crystallographica Section E: Crystallographic CommunicationsDecember 2023research communicationshttps://creativecommons.org/licenses/by/4.0/122056-98902056-9890med@iucr.org1193Crystal structure and antimycobacterial evaluation of 2-(cyclohexylmethyl)-7-nitro-5-(trifluoromethyl)benzo[d]isothiazol-3(2H)-one
http://scripts.iucr.org/cgi-bin/paper?vm2292
The title compound, C15H15F3N2O3S, crystallizes in the monoclinic system, space group I2/a, with Z = 8. As expected, the nine-membered heterobicyclic system is virtually planar and the cyclohexyl group adopts a chair conformation. There is structural evidence for intramolecular N—S⋯O chalcogen bonding between the benzisothiazolinone S atom and one O atom of the nitro group, approximately aligned along the extension of the covalent N—S bond [N—S⋯O = 162.7 (1)°]. In the crystal, the molecules form centrosymmetric dimers through C—H⋯O weak hydrogen bonding between a C—H group of the electron-deficient benzene ring and the benzothiazolinone carbonyl O atom with an R22(10) motif. In contrast to the previously described N-acyl 7-nitro-5-(trifluoromethyl)benzo[d]isothiazol-3(2H)-ones, the title N-cyclohexylmethyl analogue does not inhibit growth of Mycobacterium aurum and Mycobacterium smegmatis in vitro.urn:issn:2056-9890Richter, A.Goddard, R.Imming, P.Seidel, R.W.text/htmlThe crystal structure of the title compound features centrosymmetric dimers formed through C—H⋯O weak hydrogen bonds between a C—H group of the electron-deficient benzene ring and the benzothiazolinone carbonyl O atom with an R_{2}^{2}(10) motif.doi:10.1107/S2056989023010137BENZISOTHIAZOLINONE; BENZOTHIAZINONE; MYCOBACTERIA; HYDROGEN BONDING; CRYSTAL STRUCTURE2023-11-30Crystal structure and antimycobacterial evaluation of 2-(cyclohexylmethyl)-7-nitro-5-(trifluoromethyl)benzo[d]isothiazol-3(2H)-oneThe title compound, C15H15F3N2O3S, crystallizes in the monoclinic system, space group I2/a, with Z = 8. As expected, the nine-membered heterobicyclic system is virtually planar and the cyclohexyl group adopts a chair conformation. There is structural evidence for intramolecular N—S⋯O chalcogen bonding between the benzisothiazolinone S atom and one O atom of the nitro group, approximately aligned along the extension of the covalent N—S bond [N—S⋯O = 162.7 (1)°]. In the crystal, the molecules form centrosymmetric dimers through C—H⋯O weak hydrogen bonding between a C—H group of the electron-deficient benzene ring and the benzothiazolinone carbonyl O atom with an R22(10) motif. In contrast to the previously described N-acyl 7-nitro-5-(trifluoromethyl)benzo[d]isothiazol-3(2H)-ones, the title N-cyclohexylmethyl analogue does not inhibit growth of Mycobacterium aurum and Mycobacterium smegmatis in vitro.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext11942023-11-30https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsDecember 202379med@iucr.org1198122056-98902056-9890An octanuclear nickel(II) pyrazolate cluster with a cubic Ni8 core and its methyl- and n-octyl-functionalized derivatives
http://scripts.iucr.org/cgi-bin/paper?xi2028
The molecular and crystal structure of a discrete [Ni8(μ4-OH)6(μ-4-Rpz)12]2− (R = H; pz = pyrazolate anion, C3H3N2−) cluster with an unprecedented, perfectly cubic arrangement of its eight Ni centers is reported, along with its lower-symmetry alkyl-functionalized (R = methyl and n-octyl) derivatives. Crystals of the latter two were obtained with two identical counter-ions (Bu4N+), whereas the crystal of the complex with the parent pyrazole ligand has one Me4N+ and one Bu4N+ counter-ion. The methyl derivative incorporates 1,2-dichloroethane solvent molecules in its crystal structure, whereas the other two are solvent-free. The compounds are tetrabutylazanium tetramethylazanium hexa-μ4-hydroxido-dodeca-μ2-pyrazolato-hexahedro-octanickel, (C16H36N)(C4H12N)[Ni8(C3H3N2)12(OH)6] or (Bu4N)(Me4N)[Ni8(μ4-OH)6(μ-pz)12] (1), bis(tetrabutylazanium) hexa-μ4-hydroxido-dodeca-μ2-(4-methylpyrazolato)-hexahedro-octanickel 1,2-dichloroethane 7.196-solvate, (C16H36N)2[Ni8(C4H5N2)12(OH)6]·7.196C2H4Cl2 or (Bu4N)2[Ni8(μ4-OH)6(μ-4-Mepz)12]·7.196(ClCH2CH2Cl) (2), and bis(tetrabutylazanium) hexa-μ4-hydroxido-dodeca-μ2-(4-octylpyrazolato)-hexahedro-octanickel, (C16H36N)2[Ni8(C11H19N2)12(OH)6] or (Bu4N)2[Ni8(μ4-OH)6(μ-4-nOctpz)12] (3). All counter-ions are disordered (with the exception of one Bu4N+ in 3). Some of the octyl chains of 3 (the crystal is twinned by non-merohedry) are also disordered. Various structural features are discussed and contrasted with those of other known [Ni8(μ4-OH)6(μ-4-Rpz)12]2− complexes, including extended three-dimensional metal–organic frameworks. In all three structures, the Ni8 units are lined up in columns.urn:issn:2056-9890Al Isawi, W.A.Zeller, M.Mezei, G.text/htmlThe molecular and crystal structure of a discrete [Ni8(μ4-OH)6(μ-4-Rpz)12]2− (R = H; pz = pyrazolato anion) cluster with an unprecedented, perfectly cubic arrangement of its eight Ni centers is reported, along with its lower-symmetry alkyl-functionalized (R = methyl and n-octyl) derivatives.doi:10.1107/S2056989023010101CRYSTAL STRUCTURE; NICKEL; PYRAZOLATE COMPLEX; OCTANUCLEAR CORE2023-11-30An octanuclear nickel(II) pyrazolate cluster with a cubic Ni8 core and its methyl- and n-octyl-functionalized derivativesThe molecular and crystal structure of a discrete [Ni8(μ4-OH)6(μ-4-Rpz)12]2− (R = H; pz = pyrazolate anion, C3H3N2−) cluster with an unprecedented, perfectly cubic arrangement of its eight Ni centers is reported, along with its lower-symmetry alkyl-functionalized (R = methyl and n-octyl) derivatives. Crystals of the latter two were obtained with two identical counter-ions (Bu4N+), whereas the crystal of the complex with the parent pyrazole ligand has one Me4N+ and one Bu4N+ counter-ion. The methyl derivative incorporates 1,2-dichloroethane solvent molecules in its crystal structure, whereas the other two are solvent-free. The compounds are tetrabutylazanium tetramethylazanium hexa-μ4-hydroxido-dodeca-μ2-pyrazolato-hexahedro-octanickel, (C16H36N)(C4H12N)[Ni8(C3H3N2)12(OH)6] or (Bu4N)(Me4N)[Ni8(μ4-OH)6(μ-pz)12] (1), bis(tetrabutylazanium) hexa-μ4-hydroxido-dodeca-μ2-(4-methylpyrazolato)-hexahedro-octanickel 1,2-dichloroethane 7.196-solvate, (C16H36N)2[Ni8(C4H5N2)12(OH)6]·7.196C2H4Cl2 or (Bu4N)2[Ni8(μ4-OH)6(μ-4-Mepz)12]·7.196(ClCH2CH2Cl) (2), and bis(tetrabutylazanium) hexa-μ4-hydroxido-dodeca-μ2-(4-octylpyrazolato)-hexahedro-octanickel, (C16H36N)2[Ni8(C11H19N2)12(OH)6] or (Bu4N)2[Ni8(μ4-OH)6(μ-4-nOctpz)12] (3). All counter-ions are disordered (with the exception of one Bu4N+ in 3). Some of the octyl chains of 3 (the crystal is twinned by non-merohedry) are also disordered. Various structural features are discussed and contrasted with those of other known [Ni8(μ4-OH)6(μ-4-Rpz)12]2− complexes, including extended three-dimensional metal–organic frameworks. In all three structures, the Ni8 units are lined up in columns.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextresearch communicationshttps://creativecommons.org/licenses/by/4.0/December 2023Acta Crystallographica Section E: Crystallographic Communications2023-11-301199791206med@iucr.org2056-98902056-989012Synthesis, crystal structure and Hirshfeld surface analysis of the tetrakis complex NaNdPyr4(i-PrOH)2·i-PrOH with a carbacylamidophosphate of the amide type
http://scripts.iucr.org/cgi-bin/paper?mw2199
The tetrakis complex of neodymium(III), tetrakis{μ-N-[bis(pyrrolidin-1-yl)phosphoryl]acetamidato}bis(propan-2-ol)neodymiumsodium propan-2-ol monosolvate, [NaNd(C10H16Cl3N3O2)4(C3H8O)2]·C3H8O or NaNdPyr4(i-PrOH)2·i-PrOH, with the amide type CAPh ligand bis(N,N-tetramethylene)(trichloroacetyl)phosphoric acid triamide (HPyr), has been synthesized, crystallized and characterized by X-ray diffraction. The complex does not have the tetrakis(CAPh)lanthanide anion, which is typical for ester-type CAPh-based coordination compounds. Instead, the NdO8 polyhedron is formed by one oxygen atom of a 2-propanol molecule and seven oxygen atoms of CAPh ligands in the title compound. Three CAPh ligands are coordinated in a bidentate chelating manner to the NdIII ion and simultaneously binding the sodium cation by μ2-bridging PO and CO groups while the fourth CAPh ligand is coordinated to the sodium cation in a bidentate chelating manner and, due to the μ2-bridging function of the PO group, also binds the neodymium ion.urn:issn:2056-9890Kariaka, N.S.Dyakonenko, V.V.Znovjyak, K.O.Shishkina, S.V.Amirkhanov, V.M.text/htmlThe crystal structure of neodymium tetrakis complex based on bis(N,N-tetramethylene)(trichloroacetyl)phosphoric acid triamide is reported and discussed.doi:10.1107/S2056989023010071CRYSTAL STRUCTURE; CARBACYLAMIDOPHOSPHATE; NEODYMIUM; TETRAKIS-COMPLEX2023-11-30Synthesis, crystal structure and Hirshfeld surface analysis of the tetrakis complex NaNdPyr4(i-PrOH)2·i-PrOH with a carbacylamidophosphate of the amide typeThe tetrakis complex of neodymium(III), tetrakis{μ-N-[bis(pyrrolidin-1-yl)phosphoryl]acetamidato}bis(propan-2-ol)neodymiumsodium propan-2-ol monosolvate, [NaNd(C10H16Cl3N3O2)4(C3H8O)2]·C3H8O or NaNdPyr4(i-PrOH)2·i-PrOH, with the amide type CAPh ligand bis(N,N-tetramethylene)(trichloroacetyl)phosphoric acid triamide (HPyr), has been synthesized, crystallized and characterized by X-ray diffraction. The complex does not have the tetrakis(CAPh)lanthanide anion, which is typical for ester-type CAPh-based coordination compounds. Instead, the NdO8 polyhedron is formed by one oxygen atom of a 2-propanol molecule and seven oxygen atoms of CAPh ligands in the title compound. Three CAPh ligands are coordinated in a bidentate chelating manner to the NdIII ion and simultaneously binding the sodium cation by μ2-bridging PO and CO groups while the fourth CAPh ligand is coordinated to the sodium cation in a bidentate chelating manner and, due to the μ2-bridging function of the PO group, also binds the neodymium ion.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext7912182023-11-30December 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications122056-98902056-9890med@iucr.org1222Synthesis, crystal structure and hydrogenation properties of MgxLi3 − xB48 − y (x = 1.11, y = 0.40)
http://scripts.iucr.org/cgi-bin/paper?nu2001
The ternary magnesium/lithium boride, MgxLi3 − xB48 − y (x = 1.11, y = 0.40, idealized formula MgLi2B48), crystallizes as its own structure type in P43212, which is closely related to the structural family comprising α-AlB12, Be0.7Al1.1B22 and tetragonal β-boron. The asymmetric unit of title structure contains two statistical mixtures Mg/Li in Wyckoff sites 8b with relative occupancies Mg:Li = 0.495 (9):0.505 (9) and 4a with Mg:Li = 0.097 (8):0.903 (8). The boron atoms occupy 23 8b sites and two 4a sites. One of the latter sites has a partial occupancy factor of 0.61 (2). Both unique Mg/Li atoms adopt a twelvefold coordination environment in the form of truncated tetrahedra (Laves polyhedra). These polyhedra are connected by triangular faces to four [B12] icosahedra. The boron atoms exhibit four kinds of polyhedra, namely pentagonal pyramid (coordination number CN = 6), distorted tetragonal pyramid (CN = 5), bicapped hexagon (CN = 8) and gyrobifastigium (CN = 8). At the gas hydrogenation of MgLi2B48 alloy, formation of the eutectic composite hydride LiBH4+Mg(BH4)2 and amorphous boron is observed. In the temperature range 543–623 K, the hydride eutectics decompose, forming MgH2, LiH, MgB4, B and H2.urn:issn:2056-9890Pavlyuk, N.Milashius, V.Kordan, V.Pavlyuk, V.text/htmlThe crystal structure of the new tetragonal boride MgxLi3 - xB48 - y (x = 1.11, x = 0.40) has been determined by the single-crystal method. This new structure type is closely related to the structural family comprising tetragonal β-boron, α-AlB12 and Be0.7Al1.1B22.doi:10.1107/S2056989023009969CRYSTAL STRUCTURE; INTERMETALLIC COMPOUNDS; HYDRIDES2023-12-05Synthesis, crystal structure and hydrogenation properties of MgxLi3 − xB48 − y (x = 1.11, y = 0.40)The ternary magnesium/lithium boride, MgxLi3 − xB48 − y (x = 1.11, y = 0.40, idealized formula MgLi2B48), crystallizes as its own structure type in P43212, which is closely related to the structural family comprising α-AlB12, Be0.7Al1.1B22 and tetragonal β-boron. The asymmetric unit of title structure contains two statistical mixtures Mg/Li in Wyckoff sites 8b with relative occupancies Mg:Li = 0.495 (9):0.505 (9) and 4a with Mg:Li = 0.097 (8):0.903 (8). The boron atoms occupy 23 8b sites and two 4a sites. One of the latter sites has a partial occupancy factor of 0.61 (2). Both unique Mg/Li atoms adopt a twelvefold coordination environment in the form of truncated tetrahedra (Laves polyhedra). These polyhedra are connected by triangular faces to four [B12] icosahedra. The boron atoms exhibit four kinds of polyhedra, namely pentagonal pyramid (coordination number CN = 6), distorted tetragonal pyramid (CN = 5), bicapped hexagon (CN = 8) and gyrobifastigium (CN = 8). At the gas hydrogenation of MgLi2B48 alloy, formation of the eutectic composite hydride LiBH4+Mg(BH4)2 and amorphous boron is observed. In the temperature range 543–623 K, the hydride eutectics decompose, forming MgH2, LiH, MgB4, B and H2.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-98901https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsJanuary 20242023-12-0580Crystal structure, Hirshfeld surface analysis, intermolecular interaction energies, energy frameworks and DFT calculations of 4-amino-1-(prop-2-yn-1-yl)pyrimidin-2(1H)-one
http://scripts.iucr.org/cgi-bin/paper?wm5702
In the title molecule, C7H7N3O, the pyrimidine ring is essentially planar, with the propynyl group rotated out of this plane by 15.31 (4)°. In the crystal, a tri-periodic network is formed by N—H⋯O, N—H⋯N and C—H⋯O hydrogen-bonding and slipped π–π stacking interactions, leading to narrow channels extending parallel to the c axis. Hirshfeld surface analysis of the crystal structure reveals that the most important contributions for the crystal packing are from H⋯H (36.2%), H⋯C/C⋯H (20.9%), H⋯O/O⋯H (17.8%) and H⋯N/N⋯H (12.2%) interactions, showing that hydrogen-bonding and van der Waals interactions are the dominant interactions in the crystal packing. Evaluation of the electrostatic, dispersion and total energy frameworks indicates that the stabilization is dominated by the electrostatic energy contributions. The molecular structure optimized by density functional theory (DFT) calculations at the B3LYP/6–311 G(d,p) level is compared with the experimentally determined structure in the solid state. The HOMO–LUMO behaviour was also elucidated to determine the energy gap.urn:issn:2056-9890Lahyaoui, M.Haoudi, A.Kartah, B.E.Mazzah, A.Hökelek, T.Mague, J.T.Kandri Rodi, Y.Sebbar, N.K.text/htmlThe molecular structure of the title compound comprises an essentially planar pyrimidine ring from which the propynyl group is rotated by 15.31 (4)°. In the crystal, a tri-periodic network is formed by N—H⋯O, N—H⋯N and C—H⋯O hydrogen-bonding and slipped π–π stacking interactions, leading to narrow channels extending parallel to the c axis.doi:10.1107/S2056989023009933CRYSTAL STRUCTURE; AMINO GROUP; HYDROGEN BONDING; HETEROCYCLIC COMPOUND2023-11-21Crystal structure, Hirshfeld surface analysis, intermolecular interaction energies, energy frameworks and DFT calculations of 4-amino-1-(prop-2-yn-1-yl)pyrimidin-2(1H)-oneIn the title molecule, C7H7N3O, the pyrimidine ring is essentially planar, with the propynyl group rotated out of this plane by 15.31 (4)°. In the crystal, a tri-periodic network is formed by N—H⋯O, N—H⋯N and C—H⋯O hydrogen-bonding and slipped π–π stacking interactions, leading to narrow channels extending parallel to the c axis. Hirshfeld surface analysis of the crystal structure reveals that the most important contributions for the crystal packing are from H⋯H (36.2%), H⋯C/C⋯H (20.9%), H⋯O/O⋯H (17.8%) and H⋯N/N⋯H (12.2%) interactions, showing that hydrogen-bonding and van der Waals interactions are the dominant interactions in the crystal packing. Evaluation of the electrostatic, dispersion and total energy frameworks indicates that the stabilization is dominated by the electrostatic energy contributions. The molecular structure optimized by density functional theory (DFT) calculations at the B3LYP/6–311 G(d,p) level is compared with the experimentally determined structure in the solid state. The HOMO–LUMO behaviour was also elucidated to determine the energy gap.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-11-211183research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsDecember 2023122056-98902056-9890med@iucr.org1189Synthesis, crystal structure and Hirshfeld analysis of trans-bis(2-{1-[(6R,S)-3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl]ethylidene}-N-methylhydrazinecarbothioamidato-κ2N2,S)palladium(II) ethanol monosolvate
http://scripts.iucr.org/cgi-bin/paper?zn2034
The reaction between the (R,S)-fixolide 4-methylthiosemicarbazone and PdII chloride yielded the title compound, [Pd(C20H30N3S)2]·C2H6O {common name: trans-bis[(R,S)-fixolide 4-methylthiosemicarbazonato-κ2N2S]palladium(II) ethanol monosolvate}. The asymmetric unit of the title compound consists of one bis-thiosemicarbazonato PdII complex and one ethanol solvent molecule. The thiosemicarbazononato ligands act as metal chelators with a trans configuration in a distorted square-planar geometry. A C—H⋯S intramolecular interaction, with graph-set motif S(6), is observed and the coordination sphere resembles a hydrogen-bonded macrocyclic environment. Additionally, one C—H⋯Pd anagostic interaction can be suggested. Each ligand is disordered over the aliphatic ring, which adopts a half-chair conformation, and two methyl groups [s.o.f. = 0.624 (2):0.376 (2)]. The disorder includes the chiral carbon atoms and, remarkably, one ligand has the (R)-isomer with the highest s.o.f. value atoms, while the other one shows the opposite, the atoms with the highest s.o.f. value are associated with the (S)-isomer. The N—N—C(=S)—N fragments of the ligands are approximately planar, with the maximum deviations from the mean plane through the selected atoms being 0.0567 (1) and −0.0307 (8) Å (r.m.s.d. = 0.0403 and 0.0269 Å) and the dihedral angle with the respective aromatic rings amount to 46.68 (5) and 50.66 (4)°. In the crystal, the complexes are linked via pairs of N—H⋯S interactions, with graph-set motif R22(8), into centrosymmetric dimers. The dimers are further connected by centrosymmetric pairs of ethanol molecules, building mono-periodic hydrogen-bonded ribbons along [011]. The Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are [atoms with highest/lowest s.o.f.s considered separately]: H⋯H (81.6/82.0%), H⋯C/C⋯H (6.5/6.4%), H⋯N/N⋯H (5.2/5.0%) and H⋯S/S⋯H (5.0/4.9%).urn:issn:2056-9890Melo, A.P.L. deBresolin, L.Tirloni, B.Farias, R.L. deOliveira, A.B. detext/htmlThe synthesis, crystal structure and Hirshfeld analysis of the first complex with the (R,S)-fixolide 4-methylthiosemicarbazonato ligand is reported. A hydrogen-bonded macrocyclic environment type is observed for the PdII homoleptic complex. In the crystal, the complexes and the ethanol solvate molecules are linked by H⋯S and H⋯O interactions, forming mono-periodic hydrogen-bonded ribbons along [011].doi:10.1107/S2056989023009908PALLADIUM(II) THIOSEMICARBAZONE-COMPLEX; FIXOLIDE 4-METHYLTHIOSEMICARBAZONE; HIRSHFELD SURFACE ANALYSIS; ANAGOSTIC INTERACTION; HYDROGEN-BONDED MACROCYCLIC ENVIRONMENT; HYDROGEN-BONDED RIBBONS; CRYSTAL STRUCTURE2023-11-16Synthesis, crystal structure and Hirshfeld analysis of trans-bis(2-{1-[(6R,S)-3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl]ethylidene}-N-methylhydrazinecarbothioamidato-κ2N2,S)palladium(II) ethanol monosolvateThe reaction between the (R,S)-fixolide 4-methylthiosemicarbazone and PdII chloride yielded the title compound, [Pd(C20H30N3S)2]·C2H6O {common name: trans-bis[(R,S)-fixolide 4-methylthiosemicarbazonato-κ2N2S]palladium(II) ethanol monosolvate}. The asymmetric unit of the title compound consists of one bis-thiosemicarbazonato PdII complex and one ethanol solvent molecule. The thiosemicarbazononato ligands act as metal chelators with a trans configuration in a distorted square-planar geometry. A C—H⋯S intramolecular interaction, with graph-set motif S(6), is observed and the coordination sphere resembles a hydrogen-bonded macrocyclic environment. Additionally, one C—H⋯Pd anagostic interaction can be suggested. Each ligand is disordered over the aliphatic ring, which adopts a half-chair conformation, and two methyl groups [s.o.f. = 0.624 (2):0.376 (2)]. The disorder includes the chiral carbon atoms and, remarkably, one ligand has the (R)-isomer with the highest s.o.f. value atoms, while the other one shows the opposite, the atoms with the highest s.o.f. value are associated with the (S)-isomer. The N—N—C(=S)—N fragments of the ligands are approximately planar, with the maximum deviations from the mean plane through the selected atoms being 0.0567 (1) and −0.0307 (8) Å (r.m.s.d. = 0.0403 and 0.0269 Å) and the dihedral angle with the respective aromatic rings amount to 46.68 (5) and 50.66 (4)°. In the crystal, the complexes are linked via pairs of N—H⋯S interactions, with graph-set motif R22(8), into centrosymmetric dimers. The dimers are further connected by centrosymmetric pairs of ethanol molecules, building mono-periodic hydrogen-bonded ribbons along [011]. The Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are [atoms with highest/lowest s.o.f.s considered separately]: H⋯H (81.6/82.0%), H⋯C/C⋯H (6.5/6.4%), H⋯N/N⋯H (5.2/5.0%) and H⋯S/S⋯H (5.0/4.9%).https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextDecember 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-11-161166791172med@iucr.org2056-98902056-989012Synthesis, structure and Hirshfeld surface analysis of 1,3-bis[(1-octyl-1H-1,2,3-triazol-4-yl)methyl]-1H-benzo[d]imidazol-2(3H)-one
http://scripts.iucr.org/cgi-bin/paper?hb8081
The title molecule, C29H44N8O, adopts a conformation resembling a two-bladed fan with the octyl chains largely in fully extended conformations. In the crystal, C—H⋯O hydrogen bonds form chains of molecules extending along the b-axis direction, which are linked by weak C—H⋯N hydrogen bonds and C—H⋯π interactions to generate a three-dimensional network. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (68.3%), H⋯N/N⋯H (15.7%) and H⋯C/C⋯H (10.4%) interactions.urn:issn:2056-9890Zouhair, M.El Ghayati, L.El Monfalouti, H.Abchihi, H.Hökelek, T.Ahmed, M.Mague, J.T.Sebbar, N.K.text/htmlThe title molecule adopts a conformation resembling a two-bladed fan with the octyl chains in fully extended conformations. In the crystal, the molecules are linked by C—H⋯O and C—H⋯N hydrogen bonds and C—H⋯π interactions.doi:10.1107/S2056989023009891CRYSTAL STRUCTURE; BENZIMIDAZOLONE; TRIAZOLE; C-H...[PI](RING) INTERACTION; HYDROGEN BOND2023-11-21Synthesis, structure and Hirshfeld surface analysis of 1,3-bis[(1-octyl-1H-1,2,3-triazol-4-yl)methyl]-1H-benzo[d]imidazol-2(3H)-oneThe title molecule, C29H44N8O, adopts a conformation resembling a two-bladed fan with the octyl chains largely in fully extended conformations. In the crystal, C—H⋯O hydrogen bonds form chains of molecules extending along the b-axis direction, which are linked by weak C—H⋯N hydrogen bonds and C—H⋯π interactions to generate a three-dimensional network. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (68.3%), H⋯N/N⋯H (15.7%) and H⋯C/C⋯H (10.4%) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextActa Crystallographica Section E: Crystallographic CommunicationsDecember 2023https://creativecommons.org/licenses/by/4.0/research communications2023-11-211179791182med@iucr.org2056-98902056-989012Synthesis, crystal structure and properties of chloridotetrakis(pyridine-3-carbonitrile)thiocyanatoiron(II)
http://scripts.iucr.org/cgi-bin/paper?nx2002
Reaction of FeCl2·4H2O with KSCN and 3-cyanopyridine (pyridine-3-carbonitrile) in ethanol accidentally leads to the formation of single crystals of Fe(NCS)(Cl)(3-cyanopyridine)4 or [FeCl(NCS)(C6H4N2)4]. The asymmetric unit of this compound consists of one FeII cation, one chloride and one thiocyanate anion that are located on a fourfold rotation axis as well as of one 3-cyanopyridine coligand in a general position. The FeII cations are sixfold coordinated by one chloride anion and one terminally N-bonding thiocyanate anion in trans-positions and four 3-cyanopyridine coligands that coordinate via the pyridine N atom to the FeII cations. The complexes are arranged in columns with the chloride anions, with the thiocyanate anions always oriented in the same direction, which shows the non-centrosymmetry of this structure. No pronounced intermolecular interactions are observed between the complexes. Initially, FeCl2 and KSCN were reacted in a 1:2 ratio, which lead to a sample that contains the title compound as the major phase together with a small amount of an unknown crystalline phase, as proven by powder X-ray diffraction (PXRD). If FeCl2 and KSCN is reacted in a 1:1 ratio, the title compound is obtained as a nearly pure phase. IR investigations reveal that the CN stretching vibration for the thiocyanate anion is observed at 2074 cm−1, and that of the cyano group at 2238 cm−1, which also proves that the anionic ligands are only terminally bonded and that the cyano group is not involved in the metal coordination. Measurements with thermogravimetry and differential thermoanalysis reveal that the title compound decomposes at 169°C when heated at a rate of 4°C min−1 and that the 3-cyanopyridine ligands are emitted in two separate poorly resolved steps. After the first step, an intermediate compound with the composition Fe(NCS)(Cl)(3-cyanopyridine)2 of unknown structure is formed, for which the CN stretching vibration of the thiocyanate anion is observed at 2025 cm−1, whereas the CN stretching vibration of the cyano group remain constant. This strongly indicates that the FeII cations are linked by μ-1,3-bridging thiocyanate anions into chains or layers.urn:issn:2056-9890Müller-Meinhard, A.Jess, I.Näther, C.text/htmlIn the crystal structure of the title compound, Fe(NCS)(Cl)(3-cyanopyridine)4 (3-cyanopyridine = pyridine-3-carbonitrile) the FeII cations are octahedrally coordinated by one terminal N-bonding thiocyanate anion, one chloride anion and four 3-cyanopyridine coligands that coordinate with the pyridine N atom to the iron centers. Upon heating the 3-cyanopyridine coligands are emitted in two separate steps, leading to the formation of an intermediate compound with the composition Fe(NCS)(Cl)(3-cyanopyridine)2.doi:10.1107/S205698902300988XSYNTHESIS; CRYSTAL STRUCTURE; MIXED IRON THIOCYANATE CHLORIDE COMPLEX; POWDER DIFFRACTION; THERMAL PROPERTIES2023-11-21Synthesis, crystal structure and properties of chloridotetrakis(pyridine-3-carbonitrile)thiocyanatoiron(II)Reaction of FeCl2·4H2O with KSCN and 3-cyanopyridine (pyridine-3-carbonitrile) in ethanol accidentally leads to the formation of single crystals of Fe(NCS)(Cl)(3-cyanopyridine)4 or [FeCl(NCS)(C6H4N2)4]. The asymmetric unit of this compound consists of one FeII cation, one chloride and one thiocyanate anion that are located on a fourfold rotation axis as well as of one 3-cyanopyridine coligand in a general position. The FeII cations are sixfold coordinated by one chloride anion and one terminally N-bonding thiocyanate anion in trans-positions and four 3-cyanopyridine coligands that coordinate via the pyridine N atom to the FeII cations. The complexes are arranged in columns with the chloride anions, with the thiocyanate anions always oriented in the same direction, which shows the non-centrosymmetry of this structure. No pronounced intermolecular interactions are observed between the complexes. Initially, FeCl2 and KSCN were reacted in a 1:2 ratio, which lead to a sample that contains the title compound as the major phase together with a small amount of an unknown crystalline phase, as proven by powder X-ray diffraction (PXRD). If FeCl2 and KSCN is reacted in a 1:1 ratio, the title compound is obtained as a nearly pure phase. IR investigations reveal that the CN stretching vibration for the thiocyanate anion is observed at 2074 cm−1, and that of the cyano group at 2238 cm−1, which also proves that the anionic ligands are only terminally bonded and that the cyano group is not involved in the metal coordination. Measurements with thermogravimetry and differential thermoanalysis reveal that the title compound decomposes at 169°C when heated at a rate of 4°C min−1 and that the 3-cyanopyridine ligands are emitted in two separate poorly resolved steps. After the first step, an intermediate compound with the composition Fe(NCS)(Cl)(3-cyanopyridine)2 of unknown structure is formed, for which the CN stretching vibration of the thiocyanate anion is observed at 2025 cm−1, whereas the CN stretching vibration of the cyano group remain constant. This strongly indicates that the FeII cations are linked by μ-1,3-bridging thiocyanate anions into chains or layers.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextActa Crystallographica Section E: Crystallographic CommunicationsDecember 2023https://creativecommons.org/licenses/by/4.0/research communications2023-11-211173791178med@iucr.org2056-98902056-989012Synthesis and crystal structures of two related Co and Mn complexes: a celebration of collaboration between the universities of Dakar and Southampton
http://scripts.iucr.org/cgi-bin/paper?ex2078
We report the synthesis and structures of two transition-metal complexes involving 2-(2-hydroxyphenyl)benzimidazole (2hpbi – a ligand of interest for its photoluminescent applications), with cobalt, namely, bis[μ-2-(1H-1,3-benzodiazol-2-yl)phenolato]bis[ethanol(thiocyanato)cobalt(II)], [Co2(C13H9N2O)2(NCS)2(C2H6O)2], (1), and manganese, namely, bis[μ-2-(1H-1,3-benzodiazol-2-yl)phenolato]bis{[2-(1H-1,3-benzodiazol-2-yl)phenolato](thiocyanato)manganese(III)} dihydrate, [Mn2(C13H9N2O)4(NCS)2]·2H2O, (2). These structures are two recent examples of a fruitful collaboration between researchers at the Laboratoire de Chimie de Coordination Organique/Organic Coordination Chemistry Laboratory (LCCO), University of Dakar, Senegal and the National Crystallography Service (NCS), School of Chemistry, University Southampton, UK. This productive partnership was forged through meeting at Pan-African Conferences on Crystallography and quickly grew as the plans for the AfCA (African Crystallographic Association) developed. This article therefore also showcases this productive partnership, in celebration of the IUCr's 75 year anniversary and the recent inclusion of AfCA as a Regional Associate of the IUCr.urn:issn:2056-9890Orton, J.B.Diouf, N.Gueye, R.S.Gaye, M.Thiam, I.E.Coles, S.J.text/htmlThe synthesis and structures are reported of two transition-metal complexes involving 2-(2-hydroxyphenyl)benzimidazole with cobalt and manganese, arising from a UK–Africa collaboration.doi:10.1107/S2056989023009805AFRICA-UK COLLABORATION; AFCA-IUCR VIRTUAL COLLECTION; MANGANESE COMPLEX; COBALT COMPLEX; STRUCTURAL CHEMISTRY; CRYSTAL STRUCTURE2023-11-16Synthesis and crystal structures of two related Co and Mn complexes: a celebration of collaboration between the universities of Dakar and SouthamptonWe report the synthesis and structures of two transition-metal complexes involving 2-(2-hydroxyphenyl)benzimidazole (2hpbi – a ligand of interest for its photoluminescent applications), with cobalt, namely, bis[μ-2-(1H-1,3-benzodiazol-2-yl)phenolato]bis[ethanol(thiocyanato)cobalt(II)], [Co2(C13H9N2O)2(NCS)2(C2H6O)2], (1), and manganese, namely, bis[μ-2-(1H-1,3-benzodiazol-2-yl)phenolato]bis{[2-(1H-1,3-benzodiazol-2-yl)phenolato](thiocyanato)manganese(III)} dihydrate, [Mn2(C13H9N2O)4(NCS)2]·2H2O, (2). These structures are two recent examples of a fruitful collaboration between researchers at the Laboratoire de Chimie de Coordination Organique/Organic Coordination Chemistry Laboratory (LCCO), University of Dakar, Senegal and the National Crystallography Service (NCS), School of Chemistry, University Southampton, UK. This productive partnership was forged through meeting at Pan-African Conferences on Crystallography and quickly grew as the plans for the AfCA (African Crystallographic Association) developed. This article therefore also showcases this productive partnership, in celebration of the IUCr's 75 year anniversary and the recent inclusion of AfCA as a Regional Associate of the IUCr.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext1114med@iucr.org2056-98902056-989012research communicationshttps://creativecommons.org/licenses/by/4.0/December 2023Acta Crystallographica Section E: Crystallographic Communications2023-11-16110979Crystal structure and Hirshfeld surface analysis of (2Z)-3-oxo-N-phenyl-2-[(1H-pyrrol-2-yl)methylidene]butanamide monohydrate
http://scripts.iucr.org/cgi-bin/paper?vm2291
In the title compound, C15H14N2O2·H2O, the 1H-pyrrole ring makes a dihedral angle of 59.95 (13)° with the phenyl ring. In the crystal, the molecules are connected by C—H⋯O hydrogen bonds into layers parallel to the (020) plane, while two molecules are connected to the water molecule by two N—H⋯O hydrogen bonds and one molecule by an O—H⋯O hydrogen bond. C—H⋯π and π–π interactions further link the molecules into chains extending in the [\overline{1}01] direction and stabilize the molecular packing. According to a Hirshfeld surface study, H⋯H (49.4%), C⋯H/H⋯C (23.2%) and O⋯H/H⋯O (20.0%) interactions are the most significant contributors to the crystal packing.urn:issn:2056-9890Safarova, A.S.Khalilov, A.N.Akkurt, M.Brito, I.Bhattarai, A.Naghiyev, F.N.Mamedov, I.G.text/htmlIn the title compound, the molecules are connected by C—H⋯O hydrogen bonds in layers parallel to the (020) plane. C—H⋯π and π–π interactions further link the molecules into chains extending in the [\overline{1}01] direction.doi:10.1107/S2056989023009799CRYSTAL STRUCTURE; 1H-PYRROLE RING; HYDROGEN BONDS; HIRSHFELD SURFACE ANALYSIS2023-11-14Crystal structure and Hirshfeld surface analysis of (2Z)-3-oxo-N-phenyl-2-[(1H-pyrrol-2-yl)methylidene]butanamide monohydrateIn the title compound, C15H14N2O2·H2O, the 1H-pyrrole ring makes a dihedral angle of 59.95 (13)° with the phenyl ring. In the crystal, the molecules are connected by C—H⋯O hydrogen bonds into layers parallel to the (020) plane, while two molecules are connected to the water molecule by two N—H⋯O hydrogen bonds and one molecule by an O—H⋯O hydrogen bond. C—H⋯π and π–π interactions further link the molecules into chains extending in the [\overline{1}01] direction and stabilize the molecular packing. According to a Hirshfeld surface study, H⋯H (49.4%), C⋯H/H⋯C (23.2%) and O⋯H/H⋯O (20.0%) interactions are the most significant contributors to the crystal packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytexthttps://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsDecember 202311422023-11-14791146med@iucr.org2056-98902056-989012Crystal structure reinvestigation and spectroscopic analysis of tricadmium orthophosphate
http://scripts.iucr.org/cgi-bin/paper?oo2001
Single crystals of tricadmium orthophosphate, Cd3(PO4)2, have been synthesized successfully by the hydrothermal route, while its powder form was obtained by a solid-solid process. The corresponding crystal structure was determined using X-ray diffraction data in the monoclinic space group P21/n. The crystal structure consists of Cd2O8 or Cd2O10 dimers linked together by PO4 tetrahedra through sharing vertices or edges. Scanning electron microscopy (SEM) was used to investigate the morphology and to confirm the chemical composition of the synthesized powder. Infrared analysis corroborates the presence of isolated phosphate tetrahedrons in the structure. UV–Visible studies showed an absorbance peak at 289 nm and a band gap energy of 3.85 eV, as determined by the Kubelka–Munk model.urn:issn:2056-9890Cherif, F.-Z.Taibi, M.Boukhari, A.Assani, A.Saadi, M.El Ammari, L.text/htmlThe transition-metal orthophosphate, β-Cd3(PO4)2, was synthesized by a solid-state reaction and characterized by single-crystal X-ray diffraction and EDS spectroscopy. It crystallizes in the monoclinic system, space group P21/n.doi:10.1107/S2056989023009775CRYSTAL STRUCTURE; CADMIUM PHOSPHATE; ORTHOPHOSPHATES; INFRARED SPECTROSCOPY2023-11-14Crystal structure reinvestigation and spectroscopic analysis of tricadmium orthophosphateSingle crystals of tricadmium orthophosphate, Cd3(PO4)2, have been synthesized successfully by the hydrothermal route, while its powder form was obtained by a solid-solid process. The corresponding crystal structure was determined using X-ray diffraction data in the monoclinic space group P21/n. The crystal structure consists of Cd2O8 or Cd2O10 dimers linked together by PO4 tetrahedra through sharing vertices or edges. Scanning electron microscopy (SEM) was used to investigate the morphology and to confirm the chemical composition of the synthesized powder. Infrared analysis corroborates the presence of isolated phosphate tetrahedrons in the structure. UV–Visible studies showed an absorbance peak at 289 nm and a band gap energy of 3.85 eV, as determined by the Kubelka–Munk model.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-9890121160med@iucr.org79December 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/2023-11-141155Crystal structure of polymeric bis(3-amino-1H-pyrazole)cadmium dibromide
http://scripts.iucr.org/cgi-bin/paper?tx2078
The reaction of cadmium bromide tetrahydrate with 3-aminopyrazole (3-apz) in ethanolic solution leads to tautomerization of the ligand and the formation of crystals of the title compound, catena-poly[[dibromidocadmium(II)]-bis(μ-3-amino-1H-pyrazole)-κ2N3:N2;κ2N2:N3], [CdBr2(C3H5N3)2]n or [CdBr2(3-apz)2]n. Its asymmetric unit consists of a half of a Cd2+ cation, a bromide anion and a 3-apz molecule. The Cd2+ cations are coordinated by two bromide anions and two 3-apz ligands, generating trans-CdN4Br2 octahedra, which are linked into chains by pairs of the bridging ligands. In the crystal, the ligand molecules and bromide anions of neighboring chains are linked through interchain hydrogen bonds into a two-dimensional network. The intermolecular contacts were quantified using Hirshfeld surface analysis and two-dimensional fingerprint plots, revealing the relative quantitative contributions of the weak intermolecular contacts.urn:issn:2056-9890Kuzevanova, I.S.Vynohradov, O.S.Pavlenko, V.A.Malinkin, S.O.Shova, S.Fritsky, I.O.Seredyuk, M.text/htmlThe title compound {[CdBr2(3-apz)2]}n consists of a Cd2+ cation, bromide anions balancing the charge and bridging 3-aminopyrazole (3-apz) molecules. The Cd2+ cations are coordinated by two bromide anions and two 3-apz ligands, generating trans-CdN4Br2 octahedra, and are linked into chains by pairs of the bridging ligands. In the crystal, the 3-apz ligands and bromide anions of neighboring chains are linked through interchain hydrogen bonding into a two-dimensional supramolecular network.doi:10.1107/S2056989023009751CRYSTAL STRUCTURE; CADMIUM COMPLEX; COORDINATION POLYMER; HYDROGEN BONDING2023-11-14Crystal structure of polymeric bis(3-amino-1H-pyrazole)cadmium dibromideThe reaction of cadmium bromide tetrahydrate with 3-aminopyrazole (3-apz) in ethanolic solution leads to tautomerization of the ligand and the formation of crystals of the title compound, catena-poly[[dibromidocadmium(II)]-bis(μ-3-amino-1H-pyrazole)-κ2N3:N2;κ2N2:N3], [CdBr2(C3H5N3)2]n or [CdBr2(3-apz)2]n. Its asymmetric unit consists of a half of a Cd2+ cation, a bromide anion and a 3-apz molecule. The Cd2+ cations are coordinated by two bromide anions and two 3-apz ligands, generating trans-CdN4Br2 octahedra, which are linked into chains by pairs of the bridging ligands. In the crystal, the ligand molecules and bromide anions of neighboring chains are linked through interchain hydrogen bonds into a two-dimensional network. The intermolecular contacts were quantified using Hirshfeld surface analysis and two-dimensional fingerprint plots, revealing the relative quantitative contributions of the weak intermolecular contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext122056-98902056-9890med@iucr.org1154792023-11-141151research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsDecember 2023Synthesis and crystallographic characterization of 6-hydroxy-1,2-dihydropyridin-2-one
http://scripts.iucr.org/cgi-bin/paper?jy2036
The title compound, C5H5NO2, is a hydroxylated pyridine ring that has been studied for its involvement in microbial degradation of nicotinic acid. Here we describe its synthesis as a formic acid salt, rather than the standard hydrochloride salt that is commercially available, and its spectroscopic and crystallographic characterization.urn:issn:2056-9890Phillips, S.K.Brancato, S.G.MacMillan, S.N.Snider, M.J.Roering, A.J.Hicks, K.A.text/htmlThe synthesis of the title compound as a formic acid salt, rather than the standard hydrochloride salt that is commercially available, and its spectroscopic and crystallographic characterization are described.doi:10.1107/S205698902300974XCRYSTAL STRUCTURE; HYDROGEN BONDING; NICOTINIC ACID DERIVATIVE2023-11-14Synthesis and crystallographic characterization of 6-hydroxy-1,2-dihydropyridin-2-oneThe title compound, C5H5NO2, is a hydroxylated pyridine ring that has been studied for its involvement in microbial degradation of nicotinic acid. Here we describe its synthesis as a formic acid salt, rather than the standard hydrochloride salt that is commercially available, and its spectroscopic and crystallographic characterization.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2023-11-141147research communicationshttps://creativecommons.org/licenses/by/4.0/December 2023Acta Crystallographica Section E: Crystallographic Communications79med@iucr.org1150122056-98902056-9890Crystal structures of the isotypic complexes bis(morpholine)gold(I) chloride and bis(morpholine)gold(I) bromide
http://scripts.iucr.org/cgi-bin/paper?yz2043
The compounds bis(morpholine-κN)gold(I) chloride, [Au(C4H9NO)2]Cl, 1, and bis(morpholine-κN)gold(I) bromide, [Au(C4H9NO)2]Br, 2, crystallize isotypically in space group C2/c with Z = 4. The gold atoms, which are axially positioned at the morpholine rings, lie on inversion centres (so that the N—Au—N coordination is exactly linear) and the halide anions on twofold axes. The residues are connected by a classical hydrogen bond N—H⋯halide and by a short gold⋯halide contact to form a layer structure parallel to the bc plane. The morpholine oxygen atom is not involved in classical hydrogen bonding.urn:issn:2056-9890Döring, C.Jones, P.G.text/htmlIn the title compounds, the gold atoms lie on inversion centres and are linearly coordinated by two morpholine ligands. The halide anions lie on twofold axes. Hydrogen bonds and Au⋯halide contacts lead to a layer structure.doi:10.1107/S2056989023009702CRYSTAL STRUCTURE; GOLD; MORPHOLINE; SECONDARY INTERACTIONS2023-11-16Crystal structures of the isotypic complexes bis(morpholine)gold(I) chloride and bis(morpholine)gold(I) bromideThe compounds bis(morpholine-κN)gold(I) chloride, [Au(C4H9NO)2]Cl, 1, and bis(morpholine-κN)gold(I) bromide, [Au(C4H9NO)2]Br, 2, crystallize isotypically in space group C2/c with Z = 4. The gold atoms, which are axially positioned at the morpholine rings, lie on inversion centres (so that the N—Au—N coordination is exactly linear) and the halide anions on twofold axes. The residues are connected by a classical hydrogen bond N—H⋯halide and by a short gold⋯halide contact to form a layer structure parallel to the bc plane. The morpholine oxygen atom is not involved in classical hydrogen bonding.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext1165med@iucr.org2056-98902056-989012Acta Crystallographica Section E: Crystallographic CommunicationsDecember 2023https://creativecommons.org/licenses/by/4.0/research communications11612023-11-1679Crystal structure of S-n-octyl 3-(1-phenylethylidene)dithiocarbazate and of its bis-chelated nickel(II) complex
http://scripts.iucr.org/cgi-bin/paper?zv2030
The nitrogen–sulfur Schiff base proligand S-n-octyl 3-(1-phenylethylidene)dithiocarbazate, C17H26N2S2 (HL), was prepared by reaction of S-octyl dithiocarbamate with acetophenone. Treatment of HL with nickel acetate yielded the complex bis[S-n-octyl 3-(1-phenylethylidene)dithiocarbazato]nickel(II), [Ni(C17H25N2S2)2] (NiL2), which was shown to adopt a tetrahedrally distorted cis-square-planar coordination geometry, with the NiSN planes of the two ligands forming a dihedral angle of 21.66 (6)°. Changes in the geometry of the L ligand upon chelation of Ni2+ are described, involving a ca 180° rotation around the N(azomethine)—C(thiolate) bond.urn:issn:2056-9890Khan, S.S.Howlader, M.B.H.Sheikh, M.C.Miyatake, R.Zangrando, E.Ansary, M.R.H.text/htmlA bis-chelated mononuclear nickel(II) complex with a dithiocarbazate ligand bearing a long saturated alkyl chain exhibits a distorted cis square planar coordination of the metal with two ligands conformationally different from the proligand.doi:10.1107/S2056989023009726CRYSTAL STRUCTURE; DITHIOCARBAZATE LIGAND; NIII COMPLEX; CIS CONFIGURATION COMPLEX; OCTYL ALKYL CHAIN2023-11-14Crystal structure of S-n-octyl 3-(1-phenylethylidene)dithiocarbazate and of its bis-chelated nickel(II) complexThe nitrogen–sulfur Schiff base proligand S-n-octyl 3-(1-phenylethylidene)dithiocarbazate, C17H26N2S2 (HL), was prepared by reaction of S-octyl dithiocarbamate with acetophenone. Treatment of HL with nickel acetate yielded the complex bis[S-n-octyl 3-(1-phenylethylidene)dithiocarbazato]nickel(II), [Ni(C17H25N2S2)2] (NiL2), which was shown to adopt a tetrahedrally distorted cis-square-planar coordination geometry, with the NiSN planes of the two ligands forming a dihedral angle of 21.66 (6)°. Changes in the geometry of the L ligand upon chelation of Ni2+ are described, involving a ca 180° rotation around the N(azomethine)—C(thiolate) bond.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextActa Crystallographica Section E: Crystallographic CommunicationsDecember 2023https://creativecommons.org/licenses/by/4.0/research communications2023-11-141137791141med@iucr.org2056-98902056-989012Synthesis, characterization, crystal structure and Hirshfeld surface analysis of isobutyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate
http://scripts.iucr.org/cgi-bin/paper?ev2001
In the title compound, C24H29F2NO4, which crystallizes in the orthorhombic Pca21 space group with Z = 4, the 1,4-dihydropyridine ring adopts a distorted boat conformation, while the cyclohexene ring is in a distorted half-chair conformation. In the crystal, the molecules are linked by N—H⋯O and C—H⋯O interactions, forming supramolecular chains parallel to the a axis. These chains pack with C—H⋯π interactions between them, forming layers parallel to the (010) plane. The cohesion of the crystal structure is ensured by van der Waals interactions between these layers. Hirshfeld surface analysis shows the major contributions to the crystal packing are from H⋯H (56.9%), F⋯H/H⋯F (15.7%), O⋯H/H⋯O (13.7%) and C⋯H/H⋯C (9.5%) contacts.urn:issn:2056-9890Yıldırım, S. Ö.Akkurt, M.Çetin, G.Şimşek, R.Butcher, R.J.Bhattarai, A.text/htmlIn the crystal, the molecules are linked by N—H⋯O and C—H⋯O interactions, forming supramolecular chains parallel to the a axis. These chains pack with C—H⋯π interactions between them, forming layers parallel to the (010) plane.doi:10.1107/S2056989023009623CRYSTAL STRUCTURE; 1,4-DIHYDROPYRIDINE RING; CYCLOHEXENE RING; QUINOLINE RING SYSTEM; VAN DER WAALS INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-11-10Synthesis, characterization, crystal structure and Hirshfeld surface analysis of isobutyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylateIn the title compound, C24H29F2NO4, which crystallizes in the orthorhombic Pca21 space group with Z = 4, the 1,4-dihydropyridine ring adopts a distorted boat conformation, while the cyclohexene ring is in a distorted half-chair conformation. In the crystal, the molecules are linked by N—H⋯O and C—H⋯O interactions, forming supramolecular chains parallel to the a axis. These chains pack with C—H⋯π interactions between them, forming layers parallel to the (010) plane. The cohesion of the crystal structure is ensured by van der Waals interactions between these layers. Hirshfeld surface analysis shows the major contributions to the crystal packing are from H⋯H (56.9%), F⋯H/H⋯F (15.7%), O⋯H/H⋯O (13.7%) and C⋯H/H⋯C (9.5%) contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext11322023-11-10research communicationshttps://creativecommons.org/licenses/by/4.0/December 2023Acta Crystallographica Section E: Crystallographic Communications79med@iucr.org1136122056-98902056-9890Crystal structure and Hirshfeld surface analysis of 10-hydroxy-2-(4-methoxyphenyl)-3-oxo-2,3,3a,4,10,10a-hexahydro-1H-9-thia-2-azacyclopenta[b]fluorene-4-carboxylic acid dimethyl sulfoxide-d6 monosolvate
http://scripts.iucr.org/cgi-bin/paper?tx2077
In the title compound, C22H19NO5S·C2D6OS, the central six-membered ring has a slightly distorted boat conformation, while the fused pyrrolidine ring adopts an envelope conformation. These conformations are stabilized by O—H⋯O hydrogen bonds between the main compound and solvent molecules. In addition, intramolecular C—H⋯O hydrogen bonds in the main molecule form two S(6) rings. Molecules are connected by pairs of intermolecular C—H⋯O hydrogen bonds, forming dimers with a R22(8) motif. These dimers form a three-dimensional network through O—H⋯O, O—H⋯S and C—H⋯O hydrogen bonds with each other directly and through solvent molecules. In addition, weak π–π stacking interactions [centroid-to-centroid distances = 3.9937 (10) and 3.9936 (10) Å, slippages of 2.034 and 1.681 Å] are observed. The intermolecular contacts were quantified using Hirshfeld surface analysis and two-dimensional fingerprint plots, revealing the relative contributions of the contacts to the crystal packing to be H⋯H 41.7%, O⋯H/H⋯O 27.7%, C⋯H/H⋯C 17.0%, and S⋯H/H⋯S 7.5%.urn:issn:2056-9890Mammadova, G.Z.Yakovleva, E.D.Erokhin, P.P.Grigoriev, M.S.Atioğlu, Z.Azizova, A.N.Akkurt, M.Bhattarai, A.text/htmlIn the crystal, molecules are connected by pairs of intermolecular C—H⋯O hydrogen bonds, forming dimers with R_{2}^{2}(8) motifs. These dimers form a three-dimensional network through O—H⋯O, O—H⋯S and C—H⋯O hydrogen bonds with each other directly and through solvent molecules.doi:10.1107/S2056989023009635CRYSTAL STRUCTURE; DISORDER; DIMER; HYDROGEN BONDS; HIRSHFELD SURFACE ANALYSIS2023-11-10Crystal structure and Hirshfeld surface analysis of 10-hydroxy-2-(4-methoxyphenyl)-3-oxo-2,3,3a,4,10,10a-hexahydro-1H-9-thia-2-azacyclopenta[b]fluorene-4-carboxylic acid dimethyl sulfoxide-d6 monosolvateIn the title compound, C22H19NO5S·C2D6OS, the central six-membered ring has a slightly distorted boat conformation, while the fused pyrrolidine ring adopts an envelope conformation. These conformations are stabilized by O—H⋯O hydrogen bonds between the main compound and solvent molecules. In addition, intramolecular C—H⋯O hydrogen bonds in the main molecule form two S(6) rings. Molecules are connected by pairs of intermolecular C—H⋯O hydrogen bonds, forming dimers with a R22(8) motif. These dimers form a three-dimensional network through O—H⋯O, O—H⋯S and C—H⋯O hydrogen bonds with each other directly and through solvent molecules. In addition, weak π–π stacking interactions [centroid-to-centroid distances = 3.9937 (10) and 3.9936 (10) Å, slippages of 2.034 and 1.681 Å] are observed. The intermolecular contacts were quantified using Hirshfeld surface analysis and two-dimensional fingerprint plots, revealing the relative contributions of the contacts to the crystal packing to be H⋯H 41.7%, O⋯H/H⋯O 27.7%, C⋯H/H⋯C 17.0%, and S⋯H/H⋯S 7.5%.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext7911272023-11-10Acta Crystallographica Section E: Crystallographic CommunicationsDecember 2023https://creativecommons.org/licenses/by/4.0/research communications122056-98902056-9890med@iucr.org1131Synthesis, crystal structure and Hirshfeld surface analysis of diaquabis(o-phenylenediamine-κ2N,N′)nickel(II) naphthalene-1,5-disulfonate
http://scripts.iucr.org/cgi-bin/paper?wm5701
The reaction of o-phenylenediamine (OPD), sodium naphthalene1,5-disulfonate (Na2NDS) and nickel sulfate in an ethanol–water mixture yielded the title compound, [Ni(OPD)2(H2O)2]·NDS or [Ni(C6H8N2)2(H2O)2](C10H6O6S2). This salt consists of a complex [Ni(OPD)2(H2O)2]2+ cation with two bidentate OPD ligands and trans aqua ligands, and a non-coordinating NDS2– anion, which is the double-deprotonated form of H2NDS. The NiII atom is situated at a center of inversion and exhibits a slightly tetragonally distorted {O2N4} octahedral coordination environment, with four shorter equatorial Ni—N bonds [2.0775 (17) and 2.0924 (18) Å] and a longer axial Ni—O bond [2.1381 (17) Å]. The OPD ligand is located about an inversion center and is nearly coplanar with the NiN4 plane [dihedral angle 0.95 (9)°]. In the crystal, the cations and anions are connected by charge-assisted intermolecular N—H⋯O and O—H⋯O hydrogen-bonding interactions into the tri-periodic network structure. Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from H⋯H (44.1%), O⋯H/H⋯O (34.3%), C⋯H/H⋯C (14.8%) C⋯C (6.5%) (involving the cations) and O⋯H/H⋯O (50%), H⋯H (25%), C⋯H/H⋯C (15.3%), C⋯C (8.2%) (involving the anions) interactions.urn:issn:2056-9890Suyunov, J.R.Turaev, K.K.Alimnazarov, B.K.Nazarov, Y.E.Mengnorov, I.J.Ibragimov, B.T.Ashurov, J.M.text/htmlIn the title salt, [Ni(C6H8N2)2(H2O)2]·(C10H6O6S2), the NiII atom exhibits a slightly tetragonally distorted {O2N4} octahedral coordination environment, with two pairs of equatorial Ni—N bonds and a pair of longer axial Ni—O bonds.doi:10.1107/S2056989023009350O-PHENYLENEDIAMINE; 1,5-NAPHTHALENEDISULFONIC ACID; CRYSTAL STRUCTURE; INTERMOLECULAR INTERACTIONS; HYDROGEN BONDING; HIRSHFELD SURFACE2023-10-26Synthesis, crystal structure and Hirshfeld surface analysis of diaquabis(o-phenylenediamine-κ2N,N′)nickel(II) naphthalene-1,5-disulfonateThe reaction of o-phenylenediamine (OPD), sodium naphthalene1,5-disulfonate (Na2NDS) and nickel sulfate in an ethanol–water mixture yielded the title compound, [Ni(OPD)2(H2O)2]·NDS or [Ni(C6H8N2)2(H2O)2](C10H6O6S2). This salt consists of a complex [Ni(OPD)2(H2O)2]2+ cation with two bidentate OPD ligands and trans aqua ligands, and a non-coordinating NDS2– anion, which is the double-deprotonated form of H2NDS. The NiII atom is situated at a center of inversion and exhibits a slightly tetragonally distorted {O2N4} octahedral coordination environment, with four shorter equatorial Ni—N bonds [2.0775 (17) and 2.0924 (18) Å] and a longer axial Ni—O bond [2.1381 (17) Å]. The OPD ligand is located about an inversion center and is nearly coplanar with the NiN4 plane [dihedral angle 0.95 (9)°]. In the crystal, the cations and anions are connected by charge-assisted intermolecular N—H⋯O and O—H⋯O hydrogen-bonding interactions into the tri-periodic network structure. Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from H⋯H (44.1%), O⋯H/H⋯O (34.3%), C⋯H/H⋯C (14.8%) C⋯C (6.5%) (involving the cations) and O⋯H/H⋯O (50%), H⋯H (25%), C⋯H/H⋯C (15.3%), C⋯C (8.2%) (involving the anions) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-10-261081November 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications112056-98902056-9890med@iucr.org1085Crystal structure of CaSiF6·2H2O(mP2) and reevaluation of the SiIV–F bond-valence parameter R0
http://scripts.iucr.org/cgi-bin/paper?hb8080
The structure of a second polymorph of CaSiF6·2H2O [calcium hexafluoridosilicate dihydrate; space group P2/c (No. 13), Pearson symbol mP2] was elucidated by single-crystal X-ray diffraction. It arose as an unexpected product when soda-lime glass was attacked by HF. Its crystal structure consists of infinite ∞2[Ca(H2O)2/1(SiF6)4/4] layers oriented parallel to the bc-crystallographic plane, a unique motif among structurally characterized hydrated hexafluoridosilicates. The crystal structure also exhibits inter- and intralayer hydrogen bonds, with the interlayer O—H⋯O hydrogen bonds involving a disordered hydrogen atom. The large deviation between the calculated bond-valence sum for Si and the expected value prompted a redetermination of the empirical SiIV–F bond-valence parameter R0. Based on a data set of 42 high-quality crystal structures containing 49 independent SiIV coordination environments, a revised value of 1.534 Å was derived for R0.urn:issn:2056-9890Motaln, K.Lozinšek, M.text/htmlThe crystal structure of a second polymorph of CaSiF6·2H2O featuring a layered structure connected by hydrogen bonds is presented.doi:10.1107/S2056989023009349CALCIUM HEXAFLUORIDOSILICATE; BOND-VALENCE PARAMETER; CRYSTAL STRUCTURE; DISORDER; HYDROGEN BONDING2023-11-02Crystal structure of CaSiF6·2H2O(mP2) and reevaluation of the SiIV–F bond-valence parameter R0The structure of a second polymorph of CaSiF6·2H2O [calcium hexafluoridosilicate dihydrate; space group P2/c (No. 13), Pearson symbol mP2] was elucidated by single-crystal X-ray diffraction. It arose as an unexpected product when soda-lime glass was attacked by HF. Its crystal structure consists of infinite ∞2[Ca(H2O)2/1(SiF6)4/4] layers oriented parallel to the bc-crystallographic plane, a unique motif among structurally characterized hydrated hexafluoridosilicates. The crystal structure also exhibits inter- and intralayer hydrogen bonds, with the interlayer O—H⋯O hydrogen bonds involving a disordered hydrogen atom. The large deviation between the calculated bond-valence sum for Si and the expected value prompted a redetermination of the empirical SiIV–F bond-valence parameter R0. Based on a data set of 42 high-quality crystal structures containing 49 independent SiIV coordination environments, a revised value of 1.534 Å was derived for R0.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2023-11-02December 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/79med@iucr.org122056-98902056-9890Crystal structure and Hirshfeld surface analysis of triazatriborinotris[1,3,2]benzodiazaborole acetone disolvate
http://scripts.iucr.org/cgi-bin/paper?ex2077
The title compound, alternatively known as benzodiazaborole trimer, C18H15B3N6·2C3H6O, at 100 K crystallizes in the triclinic system, space group P\overline{1}. The structure displays N—H⋯O hydrogen bonding connecting the main molecule with the crystallization solvent. Disorder of the main molecule is observed with occupancy factors refined to 0.8922 (14):0.1078 (14). The packing of the crystal shows a parallel-displaced atom-centered orientation with 3.30 (2) Å between the planes of the rings. In the solid state, the title compound is linked with weak C—H⋯π interactions, which is supported by Hirshfeld surface analysis.urn:issn:2056-9890Streeter, C.Wheeler, K.A.Lamm, A.N.text/htmlThe title compound, alternatively known as benzodiazaborole trimer, C18H15B3N6·2C3H6O, at 100 K crystallizes in the triclinic system, space group P\overline{1}. The structure displays N—H⋯O hydrogen bonding connecting the main molecule with the crystallization solvent.doi:10.1107/S2056989023009337CRYSTAL STRUCTURE; HIRSHFELD SURFACE ANALYSIS; BORAZINE; BENZODIAZABOROLE2023-10-31Crystal structure and Hirshfeld surface analysis of triazatriborinotris[1,3,2]benzodiazaborole acetone disolvateThe title compound, alternatively known as benzodiazaborole trimer, C18H15B3N6·2C3H6O, at 100 K crystallizes in the triclinic system, space group P\overline{1}. The structure displays N—H⋯O hydrogen bonding connecting the main molecule with the crystallization solvent. Disorder of the main molecule is observed with occupancy factors refined to 0.8922 (14):0.1078 (14). The packing of the crystal shows a parallel-displaced atom-centered orientation with 3.30 (2) Å between the planes of the rings. In the solid state, the title compound is linked with weak C—H⋯π interactions, which is supported by Hirshfeld surface analysis.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextresearch communicationshttps://creativecommons.org/licenses/by/4.0/November 2023Acta Crystallographica Section E: Crystallographic Communications2023-10-311102791106med@iucr.org2056-98902056-989011Crystal structure and Hirshfeld surface analysis of bis(3-aminopyrazole-κN1)bis(3-aminopyrazole-κN2)bis(nitrato-κO)copper(II)
http://scripts.iucr.org/cgi-bin/paper?wm5699
In the crystal structure of the title compound, [Cu(NO3)2(C3H5N3)4], the CuII atom is situated on an inversion center (Wyckoff position 2c of space group P21/n) and shows an octahedral [N4O2] coordination environment. The axial positions are occupied by O atoms of nitrate anions, while the equatorial positions are taken up by the N atoms of four 3-aminopyrazole ligands. As a result of the tautomerism of the latter, two coordinate with the N1-atom of 3-aminopyrazole while the other two with the N2-atom. The presence of pyrrole-like N—H groups and amine substituents as donor groups leads to numerous intra- and intermolecular hydrogen-bonding interactions, which were quantified by Hirshfeld surface analysis.urn:issn:2056-9890Kucheriv, O.I.Golenya, I.A.Prysiazhna, O.Partsevska, S.V.Gural'skiy, I.A.text/htmlThe title molecular coordination compound exhibits a central CuII atom with a distorted octahedral [N4O2] coordination environment. The axial positions are occupied by two O atoms from nitrate anions and equatorial positions occupied by pyridine-like N atoms from four 3-aminopyrazole ligands.doi:10.1107/S2056989023009295CRYSTAL STRUCTURE; PYRAZOLE COMPLEX; COPPER(II); JAHN-TELLER DISTORTION2023-10-31Crystal structure and Hirshfeld surface analysis of bis(3-aminopyrazole-κN1)bis(3-aminopyrazole-κN2)bis(nitrato-κO)copper(II)In the crystal structure of the title compound, [Cu(NO3)2(C3H5N3)4], the CuII atom is situated on an inversion center (Wyckoff position 2c of space group P21/n) and shows an octahedral [N4O2] coordination environment. The axial positions are occupied by O atoms of nitrate anions, while the equatorial positions are taken up by the N atoms of four 3-aminopyrazole ligands. As a result of the tautomerism of the latter, two coordinate with the N1-atom of 3-aminopyrazole while the other two with the N2-atom. The presence of pyrrole-like N—H groups and amine substituents as donor groups leads to numerous intra- and intermolecular hydrogen-bonding interactions, which were quantified by Hirshfeld surface analysis.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org1101112056-98902056-98902023-10-311098Acta Crystallographica Section E: Crystallographic CommunicationsNovember 2023research communicationshttps://creativecommons.org/licenses/by/4.0/79Crystal structure and Hirshfeld surface analysis of a new mononuclear copper(II) complex: [bis(pyridin-2-yl-κN)amine](formato-κO)(m-hydroxybenzoato-κ2O,O′)copper(II)
http://scripts.iucr.org/cgi-bin/paper?wm5700
A new mononuclear copper(II) complex, [Cu(C7H5O3)(HCO2)(C10H9N3)], containing mixed N- and O-donor ligands, 2,2′-dipyridylamine (dpyam) and m-hydroxybenzoate (m-OHbenz), has been obtained from a solvent mixture. The coordination environment of the CuII ion is distorted square-pyramidal with a [N2O3] coordination set originating from the chelating dpyam and m-OHbenz ligands in the basal plane and the O atom of a formato ligand at the apical position. The crystal structure of the title complex is stabilized by N—H⋯O, O—H⋯O, C—H⋯O hydrogen-bonding, π–π and C—H⋯π intermolecular interactions, which were quantified by Hirshfeld surface analysis.urn:issn:2056-9890Chaisuriya, W.Chainok, K.Wannarit, N.text/htmlThe molecular structure of the ternary mononuclear copper(II) title complex shows a slightly distorted square-pyramidal coordination environment of the CuII atom with an [N2O3] coordination set.doi:10.1107/S2056989023009234COPPER(II); TERNARY COMPLEX; M-HYDROXYBENZOATE; 2,2'-DIPYRIDYLAMINE; CRYSTAL STRUCTURE; HIRSHFELD SURFACE ANALYSIS2023-11-02Crystal structure and Hirshfeld surface analysis of a new mononuclear copper(II) complex: [bis(pyridin-2-yl-κN)amine](formato-κO)(m-hydroxybenzoato-κ2O,O′)copper(II)A new mononuclear copper(II) complex, [Cu(C7H5O3)(HCO2)(C10H9N3)], containing mixed N- and O-donor ligands, 2,2′-dipyridylamine (dpyam) and m-hydroxybenzoate (m-OHbenz), has been obtained from a solvent mixture. The coordination environment of the CuII ion is distorted square-pyramidal with a [N2O3] coordination set originating from the chelating dpyam and m-OHbenz ligands in the basal plane and the O atom of a formato ligand at the apical position. The crystal structure of the title complex is stabilized by N—H⋯O, O—H⋯O, C—H⋯O hydrogen-bonding, π–π and C—H⋯π intermolecular interactions, which were quantified by Hirshfeld surface analysis.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytexthttps://creativecommons.org/licenses/by/4.0/research communicationsDecember 2023Acta Crystallographica Section E: Crystallographic Communications2023-11-0279med@iucr.org2056-98902056-989012Crystal structure of 4-(naphthalen-2-yl)-2-oxo-6-phenyl-1,2-dihydropyridine-3-carbonitrile
http://scripts.iucr.org/cgi-bin/paper?dj2070
The synthesis and crystal structure of the title compound, C22H14N2O, are described. The title compound was synthesized by a three-component one-pot reaction in DMSO involving chalcone, cyanoacetamide and elemental sulfur as catalyst. The compound was characterized by spectroscopic methods and single-crystal X-ray diffraction. The structure consists of inversion-related dimers produced by N—H⋯O hydrogen bonding, which further interact through π–π contacts.urn:issn:2056-9890Bui, T.T.T.Mac, D.H.Quang Trung, P.Pham, C.T.text/htmlThe structure of 4-(naphthalen-2-yl)-2-oxo-6-phenyl-1,2-dihydropyridine-3-carbonitrile, prepared by a three-component one-pot reaction, is based on dimers connected by N—H⋯O hydrogen bonds, which also interact through π–π contacts.doi:10.1107/S2056989023009180PYRIDONE; ELEMENTAL SULFUR; THREE-COMPONENT ONE-POT REACTION; CRYSTAL STRUCTURE2023-10-26Crystal structure of 4-(naphthalen-2-yl)-2-oxo-6-phenyl-1,2-dihydropyridine-3-carbonitrileThe synthesis and crystal structure of the title compound, C22H14N2O, are described. The title compound was synthesized by a three-component one-pot reaction in DMSO involving chalcone, cyanoacetamide and elemental sulfur as catalyst. The compound was characterized by spectroscopic methods and single-crystal X-ray diffraction. The structure consists of inversion-related dimers produced by N—H⋯O hydrogen bonding, which further interact through π–π contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-9890111076med@iucr.org79https://creativecommons.org/licenses/by/4.0/research communicationsNovember 2023Acta Crystallographica Section E: Crystallographic Communications2023-10-261074Synthesis and crystal structure of bis(9-mesityl-9,10-dihydro-10-aza-9-borabenzo[h]quinolinato-κ2N1,N10)zinc(II)
http://scripts.iucr.org/cgi-bin/paper?dj2071
The title compound, [Zn(C20H18BN2)2] (ZnL2), is an overall uncharged chelate that consists of two units of an NH-deprotonated 10-aza-9-borabenzo[h]quinoline ligand (L) per ZnII center. It was synthesized in two steps by treating the protonated ligand HL with lithium bis(trimethylsilyl)amide and further conversion with diethylzinc. Its asymmetric unit comprises one ZnL fragment; the molecule is completed by application of inversion symmetry at Zn. Due to the fourfold coordination with nitrogen atoms, the zinc(II) ion is located in a distorted tetrahedral environment. Besides the relatively short N—Zn bonds, ZnL2 is characterized by the significant protrusion of the central ion from the plane of the ligand backbone. The crystal structure is consolidated by intra- and intermolecular π–π stacking interactions, while the polarized B—N bond is barely involved in any close atom contacts.urn:issn:2056-9890Appiarius, Y.Puylaert, P.Staubitz, A.text/htmlThe NH-deprotonation of a 10-aza-9-borabenzo[h]quinoline yields a bidentate ligand that was used for the synthesis of a 2:1 coordination complex with zinc. Its crystal packing is dominated by intense intra- and intermolecular π–π stacking interactions.doi:10.1107/S2056989023009192CRYSTAL STRUCTURE; 1,2-AZABORININE; BORON-NITROGEN; ZINC; BIDENTATE LIGAND; HIRSHFELD ANALYSIS2023-10-24Synthesis and crystal structure of bis(9-mesityl-9,10-dihydro-10-aza-9-borabenzo[h]quinolinato-κ2N1,N10)zinc(II)The title compound, [Zn(C20H18BN2)2] (ZnL2), is an overall uncharged chelate that consists of two units of an NH-deprotonated 10-aza-9-borabenzo[h]quinoline ligand (L) per ZnII center. It was synthesized in two steps by treating the protonated ligand HL with lithium bis(trimethylsilyl)amide and further conversion with diethylzinc. Its asymmetric unit comprises one ZnL fragment; the molecule is completed by application of inversion symmetry at Zn. Due to the fourfold coordination with nitrogen atoms, the zinc(II) ion is located in a distorted tetrahedral environment. Besides the relatively short N—Zn bonds, ZnL2 is characterized by the significant protrusion of the central ion from the plane of the ligand backbone. The crystal structure is consolidated by intra- and intermolecular π–π stacking interactions, while the polarized B—N bond is barely involved in any close atom contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org1064112056-98902056-989010612023-10-24https://creativecommons.org/licenses/by/4.0/research communicationsNovember 2023Acta Crystallographica Section E: Crystallographic Communications79Crystal structure of 2-methyl-1H-imidazol-3-ium 3,5-dicarboxybenzoate
http://scripts.iucr.org/cgi-bin/paper?jq2031
The structure of the title salt, C4H7N2+·C9H5O6− (1), is reported. The compound is built from a protonated 2-methylimidazole and a singly deprotonated trimesic acid. Detailed analysis of bond distances and angles for both ions reveals subtle differences compared with their neutral molecule counterpart. Analysis of the crystal packing in compound 1 reveals the formation of undulating chains by the ions through hydrogen bonding. The chains stack along the b axis through π–π interactions and interconnect with other chains in an out-of-phase arrangement along the ac plane through further hydrogen-bonding interactions.urn:issn:2056-9890Baletska, S.Techert, S.Velazquez-Garcia, J. de J.text/htmlThe structure of a 2-methyl-1H-imidazol-3-ium trimesate compound was determined by single-crystal X-ray diffraction. The compound is composed of protonated 2-methylimidazole and singly deprotonated trimesic acid molecules.doi:10.1107/S2056989023009209CRYSTAL STRUCTURE; 2-METHYLIMIDAZOLE; TRIMESIC ACID2023-10-31Crystal structure of 2-methyl-1H-imidazol-3-ium 3,5-dicarboxybenzoateThe structure of the title salt, C4H7N2+·C9H5O6− (1), is reported. The compound is built from a protonated 2-methylimidazole and a singly deprotonated trimesic acid. Detailed analysis of bond distances and angles for both ions reveals subtle differences compared with their neutral molecule counterpart. Analysis of the crystal packing in compound 1 reveals the formation of undulating chains by the ions through hydrogen bonding. The chains stack along the b axis through π–π interactions and interconnect with other chains in an out-of-phase arrangement along the ac plane through further hydrogen-bonding interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2023-10-311086Acta Crystallographica Section E: Crystallographic CommunicationsNovember 2023https://creativecommons.org/licenses/by/4.0/research communications79med@iucr.org1090112056-98902056-9890Synthesis and crystal structures of two solvates of 1-{[2,6-bis(hydroxymethyl)-4-methylphenoxy]methyl}-3,5-bis{[(4,6-dimethylpyridin-2-yl)amino]methyl}-2,4,6-triethylbenzene
http://scripts.iucr.org/cgi-bin/paper?ex2075
In the crystal structures of the formamide monosolvate (1a) and the n-propanol/H2O solvate/hydrate (1b) of the title compound, C38H50N4O3 (1), the tripodal host molecule adopts a conformation in which the substituents attached to the central benzene ring are arranged in an alternating order above and below the ring plane. As a result of the different nature of the involved guest species, the crystal components in 1a create a three-dimensional supramolecular architecture, while the crystal structure of 1b consists of two-dimensional supramolecular aggregates extending parallel to the crystallographic ab plane.urn:issn:2056-9890Stapf, M.Schmidt, U.Seichter, W.Mazik, M.text/htmlIn the crystal structures of the formamide monosolvate (1a) and the n-propanol/water solvate/hydrate (1b), the host molecules adopt similar geometries with an alternating arrangement of the substituents above and below the plane of the central arene ring.doi:10.1107/S2056989023009155CRYSTAL STRUCTURES; TRIPODAL MOLECULE; HYDROGEN BONDING; C-H...[PI] AND [PI]-[PI] INTERACTIONS2023-10-24Synthesis and crystal structures of two solvates of 1-{[2,6-bis(hydroxymethyl)-4-methylphenoxy]methyl}-3,5-bis{[(4,6-dimethylpyridin-2-yl)amino]methyl}-2,4,6-triethylbenzeneIn the crystal structures of the formamide monosolvate (1a) and the n-propanol/H2O solvate/hydrate (1b) of the title compound, C38H50N4O3 (1), the tripodal host molecule adopts a conformation in which the substituents attached to the central benzene ring are arranged in an alternating order above and below the ring plane. As a result of the different nature of the involved guest species, the crystal components in 1a create a three-dimensional supramolecular architecture, while the crystal structure of 1b consists of two-dimensional supramolecular aggregates extending parallel to the crystallographic ab plane.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-10-241065research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsNovember 2023112056-98902056-9890med@iucr.org1069Crystal structure of 1-(2,6-diisopropylphenyl)-1H-imidazole
http://scripts.iucr.org/cgi-bin/paper?oi2001
The crystal structure of the title compound, C15H20N2 or DippIm, is reported. At 106 (2) K, the molecule has monoclinic P21/c symmetry with four molecules in the unit cell. The imidazole ring is rotated 80.7 (1)° relative to the phenyl ring. Intermolecular stabilization primarily results from close contacts between the N atom at the 3-position on the imidazole ring and the C—H bond at the 4-position on the neighboring DippIm, with aryl–aryl distances outside of the accepted distance of 5 Å for π-stacking.urn:issn:2056-9890Dudeja, N.Arreaga, B.C.Brannon, J.P.Stieber, S.C.E.text/htmlAt 106 (2) K, the title molecule has monoclinic P21/c symmetry with four molecules in the unit cell. The imidazole ring is rotated 80.7 (1)° relative to the phenyl ring. Intermolecular stabilization primarily results from close contacts between the N-atom at the 3-position on the imidazole ring and the C—H bond at the 4-position on the neighboring DippIm.doi:10.1107/S2056989023009179CRYSTAL STRUCTURE; DIPPIM; IMIDAZOLE; ARYL IMIDAZOLE2023-10-26Crystal structure of 1-(2,6-diisopropylphenyl)-1H-imidazoleThe crystal structure of the title compound, C15H20N2 or DippIm, is reported. At 106 (2) K, the molecule has monoclinic P21/c symmetry with four molecules in the unit cell. The imidazole ring is rotated 80.7 (1)° relative to the phenyl ring. Intermolecular stabilization primarily results from close contacts between the N atom at the 3-position on the imidazole ring and the C—H bond at the 4-position on the neighboring DippIm, with aryl–aryl distances outside of the accepted distance of 5 Å for π-stacking.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-9890111080med@iucr.org79Acta Crystallographica Section E: Crystallographic CommunicationsNovember 2023https://creativecommons.org/licenses/by/4.0/research communications2023-10-261077Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquadithiocyanatobis(pyridine-3-carbonitrile)iron(II) pyridine-3-carbonitrile monosolvate
http://scripts.iucr.org/cgi-bin/paper?hb8079
The reaction of iron thiocyanate with 3-cyanopyridine (C6H4N2) leads to the formation of two compounds with the composition [Fe(NCS)2(C6H4N2)4] (1) and [Fe(NCS)2(C6H4N2)2(H2O)2]·2C6H4N2 (2). The asymmetric unit of 1 consists of one iron cation, two thiocyanate anions and four 3-cyanopyridine ligands in general positions. The iron cation is octahedrally coordinated by two N-bonded thiocyanate anions and four 3-cyanopyridine ligands. The complexes are arranged in columns along the crystallographic c-axis direction and are linked by weak C—H⋯N interactions. In 2, the asymmetric unit consists of one iron cation on a center of inversion as well as one thiocyanate anion, one 3-cyanopyridine ligand, one water ligand and one 3-cyanopyridine solvate molecule in general positions. The iron cation is octahedrally coordinated by two N-bonded thiocyanate anions, two cyanopyridine ligands and two water ligands. O—H⋯N and C—H⋯S hydrogen bonding is observed between the water ligands and the solvent 3-cyanopyridine molecules. In the crystal structure, alternating layers of the iron complexes and the solvated 3-cyanopyridine molecules are observed. Powder X-ray (PXRD) investigations reveal that both compounds were obtained as pure phases and from IR spectroscopic measurements conclusions on the coordination mode of the thiocanate anions and the cyanogroup were made. Thermogravimetric (TG) and differential thermoanalysis (DTA) of 1 indicate the formation of a compound with the composition {[Fe(NCS)2]3(C6H4N2)4}n that is isotypic to the corresponding Cd compound already reported in the literature. TG/DTA of 2 show several mass losses. The first mass loss corresponds to the removal of the two water ligands leading to the formation of 1, which transforms into {[Fe(NCS)2]3(C6H4N2)4}n, upon further heating.urn:issn:2056-9890Näther, C.Müller-Meinhard, A.Jess, I.text/htmlTwo complexes, 1 and 2, based on Fe(NCS)2 and 3-cyanopyridine as coligand were synthesized, structurally characterized and investigated for their thermal behavior. In both compounds the FeII cations are octahedrally coordinated by two N-bonded thiocyanate anions in trans-position as well as four 3-cyanopyridine coligands for compound 1 and two 3-cyanopyridine ligands and two water molecules for compound 2. Upon heating, both complexes transform into an intermediate with bridging anionic ligands that is isotypic to its Cd(NCS)2 and Mn(NCS)2 analogs.doi:10.1107/S205698902300909XCRYSTAL STRUCTURE; IRON THIOCYANATE; 3-CYANOPYRIDINE; THERMAL PROPERTIES; IR SPECTRUM2023-10-31Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquadithiocyanatobis(pyridine-3-carbonitrile)iron(II) pyridine-3-carbonitrile monosolvateThe reaction of iron thiocyanate with 3-cyanopyridine (C6H4N2) leads to the formation of two compounds with the composition [Fe(NCS)2(C6H4N2)4] (1) and [Fe(NCS)2(C6H4N2)2(H2O)2]·2C6H4N2 (2). The asymmetric unit of 1 consists of one iron cation, two thiocyanate anions and four 3-cyanopyridine ligands in general positions. The iron cation is octahedrally coordinated by two N-bonded thiocyanate anions and four 3-cyanopyridine ligands. The complexes are arranged in columns along the crystallographic c-axis direction and are linked by weak C—H⋯N interactions. In 2, the asymmetric unit consists of one iron cation on a center of inversion as well as one thiocyanate anion, one 3-cyanopyridine ligand, one water ligand and one 3-cyanopyridine solvate molecule in general positions. The iron cation is octahedrally coordinated by two N-bonded thiocyanate anions, two cyanopyridine ligands and two water ligands. O—H⋯N and C—H⋯S hydrogen bonding is observed between the water ligands and the solvent 3-cyanopyridine molecules. In the crystal structure, alternating layers of the iron complexes and the solvated 3-cyanopyridine molecules are observed. Powder X-ray (PXRD) investigations reveal that both compounds were obtained as pure phases and from IR spectroscopic measurements conclusions on the coordination mode of the thiocanate anions and the cyanogroup were made. Thermogravimetric (TG) and differential thermoanalysis (DTA) of 1 indicate the formation of a compound with the composition {[Fe(NCS)2]3(C6H4N2)4}n that is isotypic to the corresponding Cd compound already reported in the literature. TG/DTA of 2 show several mass losses. The first mass loss corresponds to the removal of the two water ligands leading to the formation of 1, which transforms into {[Fe(NCS)2]3(C6H4N2)4}n, upon further heating.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext1097med@iucr.org2056-98902056-989011Acta Crystallographica Section E: Crystallographic CommunicationsNovember 2023research communicationshttps://creativecommons.org/licenses/by/4.0/2023-10-31109179Synthesis, crystal structure and Hirshfeld surface analysis of 1-(12-bromododecyl)indoline-2,3-dione
http://scripts.iucr.org/cgi-bin/paper?hb8077
In the title compound, C20H28BrNO2, the indoline portion is almost planar and the 12-bromododecyl chain adopts an all-trans conformation apart from the gauche terminal C—C—C—Br fragment. A micellar-like structure is generated in the crystal by C—H⋯O hydrogen bonds and π-stacking interactions between indolinedione head groups and intercalation of the 12-bromododecyl tails. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (58.9%), H⋯O/O⋯H (17.9%) and H⋯Br/Br⋯H (9.5%) contacts. A density functional theory (DFT) optimized structure at the B3LYP/ 6–311 G(d,p) level shows good agreement with the experimentally determined molecular structure in the solid state.urn:issn:2056-9890Rharmili, N.Abdellaoui, O.Haoudi, A.Mague, J.T.Hökelek, T.Ouazzani Chahdi, F.Kandri Rodi, Y.Mazzah, A.Sebbar, N.K.text/htmlThe pendant dodecyl chain in the title compound adopts an all-trans conformation apart from the gauche terminal C—C—C—Br moiety.doi:10.1107/S2056989023009052CRYSTAL STRUCTURE; INDOLINE-2,3-DIONE; HYDROGEN BOND; DODECYL; [PI] STACKING; INTERCALATION2023-10-19Synthesis, crystal structure and Hirshfeld surface analysis of 1-(12-bromododecyl)indoline-2,3-dioneIn the title compound, C20H28BrNO2, the indoline portion is almost planar and the 12-bromododecyl chain adopts an all-trans conformation apart from the gauche terminal C—C—C—Br fragment. A micellar-like structure is generated in the crystal by C—H⋯O hydrogen bonds and π-stacking interactions between indolinedione head groups and intercalation of the 12-bromododecyl tails. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (58.9%), H⋯O/O⋯H (17.9%) and H⋯Br/Br⋯H (9.5%) contacts. A density functional theory (DFT) optimized structure at the B3LYP/ 6–311 G(d,p) level shows good agreement with the experimentally determined molecular structure in the solid state.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org1036112056-98902056-98902023-10-191033Acta Crystallographica Section E: Crystallographic CommunicationsNovember 2023https://creativecommons.org/licenses/by/4.0/research communications79Crystal structure of (μ-hydrogen disulfato)-μ-oxido-bis[(4,4′-di-tert-butyl-2,2′-bipyridine)oxidovanadium(IV/V)] acetonitrile monosolvate
http://scripts.iucr.org/cgi-bin/paper?nx2001
The dinuclear oxidovanadium(IV/V) complex, [V2(HS2O8)O3(C18H24N2)2]·CH3CN or [V2O2(μ-O)(μ-H(SO4)2)(4,4′-tBubpy)2]·CH3CN (4,4′-tBubpy = 4,4′-di-tert-butyl-2,2′-bipyridine), has crystallographic C2 symmetry and exhibits a distorted octahedral geometry around the vanadium center, where the two 4,4′-tBubpy ligands are nearly orthogonal to each other. The two vanadium ions are linked by an oxo anion and a unique protonated sulfate anion [H(SO4)23−]. In the crystal, intermolecular C—H⋯π and π–π interactions between the 4,4′-tBubpy ligands are present, leading to a three-dimensional network.urn:issn:2056-9890Kodama, S.Hashiguchi, T.Nomoto, A.text/htmlThe crystal structure of a dinuclear oxidovanadium(IV/V) complex [V2O2(μ-O)(μ-H(SO4)2)(4,4′-tBubpy)2] acetonitrile monosolvate has been determined.doi:10.1107/S2056989023009040CRYSTAL STRUCTURE; VANADIUM; BIPYRIDINE; SULFATE2023-10-19Crystal structure of (μ-hydrogen disulfato)-μ-oxido-bis[(4,4′-di-tert-butyl-2,2′-bipyridine)oxidovanadium(IV/V)] acetonitrile monosolvateThe dinuclear oxidovanadium(IV/V) complex, [V2(HS2O8)O3(C18H24N2)2]·CH3CN or [V2O2(μ-O)(μ-H(SO4)2)(4,4′-tBubpy)2]·CH3CN (4,4′-tBubpy = 4,4′-di-tert-butyl-2,2′-bipyridine), has crystallographic C2 symmetry and exhibits a distorted octahedral geometry around the vanadium center, where the two 4,4′-tBubpy ligands are nearly orthogonal to each other. The two vanadium ions are linked by an oxo anion and a unique protonated sulfate anion [H(SO4)23−]. In the crystal, intermolecular C—H⋯π and π–π interactions between the 4,4′-tBubpy ligands are present, leading to a three-dimensional network.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsNovember 202310532023-10-192056-98902056-9890111056med@iucr.orgCrystal structure and supramolecular features of a bis-urea-functionalized pillar[5]arene
http://scripts.iucr.org/cgi-bin/paper?jq2032
The crystal structure of a bis-urea derivative based on A1/A2-functionalized pillar[5]arene (DUP) that encapsulates dimethyl formamide (DMF) inside the macrocyclic cavity is reported. The crystal structure of DUP·DMF, C63H70N4O12·C3H7NO, reveals that out of two urea functionalized spacers, one arm is oriented above the macrocyclic cavity with strong hydrogen-bonding interactions between the urea H atoms and DMF guest, whereas, the other arm is positioned away from the macrocycle, leading to intermolecular hydrogen-bonding interactions between the urea H atoms of two adjacent pillar[5]arene macrocycles, resulting in the formation of a supramolecular dimer.urn:issn:2056-9890Vinodh, M.Alipour, F.H.Al-Azemi, T.F.text/htmlThe crystal structure and supramolecular features are reported of a dimeric bis-urea-functionalized pillar[5]arene macrocycle, which functions as a receptor system to the DMF guest molecule.doi:10.1107/S2056989023009003PILLARARENE; UREA SUBSTITUTION; RECEPTOR; CRYSTAL STRUCTURE; DIMER2023-10-19Crystal structure and supramolecular features of a bis-urea-functionalized pillar[5]areneThe crystal structure of a bis-urea derivative based on A1/A2-functionalized pillar[5]arene (DUP) that encapsulates dimethyl formamide (DMF) inside the macrocyclic cavity is reported. The crystal structure of DUP·DMF, C63H70N4O12·C3H7NO, reveals that out of two urea functionalized spacers, one arm is oriented above the macrocyclic cavity with strong hydrogen-bonding interactions between the urea H atoms and DMF guest, whereas, the other arm is positioned away from the macrocycle, leading to intermolecular hydrogen-bonding interactions between the urea H atoms of two adjacent pillar[5]arene macrocycles, resulting in the formation of a supramolecular dimer.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org1048112056-98902056-989010442023-10-19https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsNovember 202379Redetermination of the crystal structure of yttrium chromium tetraboride, YCrB4, from single-crystal X-ray diffraction data
http://scripts.iucr.org/cgi-bin/paper?pk2696
The structural parameters of yttrium chromium tetraboride YCrB4 were refined based on single-crystal X-ray diffraction data. YCrB4 is orthorhombic, having a space group of type Pbam (No. 55) and with lattice parameters of a = 5.9425 (2), b = 11.4831 (4), c = 3.4643 (1) Å. The Y and Cr atoms are located at Wyckoff 4h sites (x, y, 0) and B atoms at the Wyckoff 4g sites (x, y, 1/2). The first structural investigation of YCrB4 was performed using a single crystalline sample [Kuz'ma, (1970). Kristallografiya. 15, 372–374]. The present study successfully refined all the positional and atomic displacement parameters of the Y, Cr, and B atoms.urn:issn:2056-9890Tokuda, M.Yubuta, K.Shishido, T.Sugiyama, K.text/htmlThe structural parameters of yttrium chromium tetraboride YCrB4 were refined based on single-crystal X-ray diffraction data. The present study successfully refined all the positional and atomic displacement parameters of the Y, Cr, and B atoms.doi:10.1107/S2056989023008952SINGLE-CRYSTAL DIFFRACTION; CRYSTAL STRUCTURE; BORIDE2023-10-26Redetermination of the crystal structure of yttrium chromium tetraboride, YCrB4, from single-crystal X-ray diffraction dataThe structural parameters of yttrium chromium tetraboride YCrB4 were refined based on single-crystal X-ray diffraction data. YCrB4 is orthorhombic, having a space group of type Pbam (No. 55) and with lattice parameters of a = 5.9425 (2), b = 11.4831 (4), c = 3.4643 (1) Å. The Y and Cr atoms are located at Wyckoff 4h sites (x, y, 0) and B atoms at the Wyckoff 4g sites (x, y, 1/2). The first structural investigation of YCrB4 was performed using a single crystalline sample [Kuz'ma, (1970). Kristallografiya. 15, 372–374]. The present study successfully refined all the positional and atomic displacement parameters of the Y, Cr, and B atoms.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext1073med@iucr.org2056-98902056-989011Acta Crystallographica Section E: Crystallographic CommunicationsNovember 2023research communicationshttps://creativecommons.org/licenses/by/4.0/2023-10-26107079Synthesis, crystal structure and thermal properties of poly[[μ-1,2-bis(pyridin-4-yl)ethene-κ2N:N′-μ-bromido-copper(I)] 1,2-bis(pyridin-4-yl)ethene 0.25-solvate]
http://scripts.iucr.org/cgi-bin/paper?hb8078
The reaction of copper(I) bromide with 1,2-bis(pyridin-4-yl)ethene in acetonitrile leads to the formation of the title compound, {[CuBr(C12H10N2)]·0.25C12H10N2}n or CuBr(4-bpe)·0.25(4-bpe) [4-bpe = 1,2-bis(pyridin-4-yl)ethene]. The asymmetric unit consists of one copper(I) cation and one bromide anion in general positions as well as two crystallographically independent half 4-bpe ligands and a quarter of a disordered 4-bpe solvate molecule that are completed by centers of inversion. The copper(I) cations are tetrahededrally coordinated as CuBr2N2 and linked by pairs of μ-1,1-bridging bromide anions into centrosymmetric dinuclear units that are further connected into layers by the 4-bpe coligands. Between the layers, interlayer C—H⋯Br hydrogen bonding is observed. The layers are arranged in such a way that cavities are formed in which the disordered 4-bpe solvate molecules are located. Powder X-ray (PXRD) investigations reveal that a pure sample has been obtained. Thermogravimetric (TG) and differential thermoanalysis (DTA) measurements show two mass losses that are accompanied by endothermic events in the DTA curve. The first mass loss correspond to the removal of 0.75 4-bpe molecules, leading to the formation of (CuBr)2(4-bpe), already reported in the literature as proven by PXRD.urn:issn:2056-9890Näther, C.Müller-Meinhard, A.Jess, I.text/htmlIn the crystal structure of the title compound, the copper(I) cations are tetrahededrally coordinated and linked by pairs of bromide anions into dinuclear units that are further connected into layers by the 1,2-bis(pyridin-4-yl)ethene (4-bpe) coligands. The layers are stacked so that cavities are formed in which disordered 4-bpe molecules are embedded.doi:10.1107/S205698902300885XCRYSTAL STRUCTURE; SYNTHESIS; THERMAL PROPERTIES; COPPER(I); 1,2-BIS(PYRIDIN-4-YL)ETHENE2023-10-19Synthesis, crystal structure and thermal properties of poly[[μ-1,2-bis(pyridin-4-yl)ethene-κ2N:N′-μ-bromido-copper(I)] 1,2-bis(pyridin-4-yl)ethene 0.25-solvate]The reaction of copper(I) bromide with 1,2-bis(pyridin-4-yl)ethene in acetonitrile leads to the formation of the title compound, {[CuBr(C12H10N2)]·0.25C12H10N2}n or CuBr(4-bpe)·0.25(4-bpe) [4-bpe = 1,2-bis(pyridin-4-yl)ethene]. The asymmetric unit consists of one copper(I) cation and one bromide anion in general positions as well as two crystallographically independent half 4-bpe ligands and a quarter of a disordered 4-bpe solvate molecule that are completed by centers of inversion. The copper(I) cations are tetrahededrally coordinated as CuBr2N2 and linked by pairs of μ-1,1-bridging bromide anions into centrosymmetric dinuclear units that are further connected into layers by the 4-bpe coligands. Between the layers, interlayer C—H⋯Br hydrogen bonding is observed. The layers are arranged in such a way that cavities are formed in which the disordered 4-bpe solvate molecules are located. Powder X-ray (PXRD) investigations reveal that a pure sample has been obtained. Thermogravimetric (TG) and differential thermoanalysis (DTA) measurements show two mass losses that are accompanied by endothermic events in the DTA curve. The first mass loss correspond to the removal of 0.75 4-bpe molecules, leading to the formation of (CuBr)2(4-bpe), already reported in the literature as proven by PXRD.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79research communicationshttps://creativecommons.org/licenses/by/4.0/November 2023Acta Crystallographica Section E: Crystallographic Communications10282023-10-192056-98902056-9890111032med@iucr.orgSynthesis, crystal structure and Hirshfeld surface analysis of diacetatobis[4-(2-aminoethyl)morpholine]cadmium tetrahydrate
http://scripts.iucr.org/cgi-bin/paper?jq2030
The title coordination compound, [Cd(C2H3O2)2(C6H14N2O)2]·4H2O, was synthesized by mixing 2 moles of 4-(2-aminoethyl)morpholine and 1 mole of cadmium acetate in double-distilled water. The Cd atom is octahedrally coordinated by two N,N′-bidentate ligands [4-(2-aminoethyl)morpholine] and two trans-located acetate molecules. The Cd atom is located on a center of inversion, whereas the 4-(2-aminoethyl)morpholine and four water molecules are adjacent to the acetate molecules. The chair conformation of the morpholine molecules is confirmed. In the crystal, adjacent metal complexes and uncoordinated water molecules are linked via N—H⋯O and O—H⋯O hydrogen-bonding interactions, generating R22(6), R66(16), R66(20) and S11(6) motifs and forming a three-dimensional network. A Hirshfeld surface analysis indicated the contributions of various contacts: H⋯H (71.8%), O⋯H/H⋯O (27.1%), and C⋯H/H⋯C (1.0%).urn:issn:2056-9890Chidambaranathan, B.Sivaraj, S.Vijayamathubalan, P.Selvakumar, S.text/htmlIn the title coordination compound, the Cd atom is octahedrally coordinated by two N,N′-bidentate ligands [4-(2-aminoethyl)morpholine] and two trans-located acetate molecules. The Cd atom is located on a centre of inversion, whereas the morpholine and four water molecules are adjacent to the acetate moieties. In the crystal, neighboring metal complexes and uncoordinated water molecules are linked via N—H⋯O and O—H⋯O hydrogen-bonding interactions.doi:10.1107/S2056989023008782CRYSTAL STRUCTURE; COORDINATION COMPOUND; MORPHOLINE LIGAND; CRYSTAL STRUCTURE2023-10-19Synthesis, crystal structure and Hirshfeld surface analysis of diacetatobis[4-(2-aminoethyl)morpholine]cadmium tetrahydrateThe title coordination compound, [Cd(C2H3O2)2(C6H14N2O)2]·4H2O, was synthesized by mixing 2 moles of 4-(2-aminoethyl)morpholine and 1 mole of cadmium acetate in double-distilled water. The Cd atom is octahedrally coordinated by two N,N′-bidentate ligands [4-(2-aminoethyl)morpholine] and two trans-located acetate molecules. The Cd atom is located on a center of inversion, whereas the 4-(2-aminoethyl)morpholine and four water molecules are adjacent to the acetate molecules. The chair conformation of the morpholine molecules is confirmed. In the crystal, adjacent metal complexes and uncoordinated water molecules are linked via N—H⋯O and O—H⋯O hydrogen-bonding interactions, generating R22(6), R66(16), R66(20) and S11(6) motifs and forming a three-dimensional network. A Hirshfeld surface analysis indicated the contributions of various contacts: H⋯H (71.8%), O⋯H/H⋯O (27.1%), and C⋯H/H⋯C (1.0%).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext1052med@iucr.org2056-98902056-989011research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsNovember 20232023-10-19104979Crystal structure of Cs2GdNb6Cl15O3 in the structural evolution of niobium oxychlorides with octahedral Nb6-cluster units
http://scripts.iucr.org/cgi-bin/paper?wm5695
Cs2GdNb6Cl15O3, dicaesium gadolinium hexaniobium pentadecachloride trioxide, was synthesized by solid-state reactions starting from a stoichiometric mixture of CsCl, Gd2O3, Nb, NbCl5, and Nb2O5. The crystal structure is based on octahedral Nb6 cluster units (point group symmetry 3.2) with composition [(Nb6Cli9Oi3)Cla6]5– where i and a denote inner and outer ligands. Cs2GdNb6Cl15O3 exhibits 14 valence electrons per cluster unit. The cluster units are linked to each other by CsI and GdIII atoms, whereby CsI (site symmetry 3..) is 12-coordinated by six Cli and six Cla ligands belonging to six neighboring cluster units and GdIII (site symmetry 3.2) is 9-coordinated by three Oi and six Cli ligands belonging to three adjacent cluster units. The arrangement of cluster units corresponds to a stacking of …AA′A… layers along [001]. Cs2GdNb6Cl15O3 is isotypic with Cs2UNb6Cl15O3.urn:issn:2056-9890Silaban, S.Haryani, M.E.Gulo, F.Perrin, C.text/htmlCs2GdNb6Cl15O3 is an octahedral Nb-cluster compound containing three inner ligands of oxygen atoms. Individual Nb6 clusters are linked to each other via GdIII and CsI atoms, which exhibit a coordination number of 9 (three O and six Cl ligands) and 12 (twelve Cl ligands).doi:10.1107/S205698902300871XCLUSTER COMPOUND; CRYSTAL STRUCTURE; VALENCE ELECTRON COUNT2023-10-10Crystal structure of Cs2GdNb6Cl15O3 in the structural evolution of niobium oxychlorides with octahedral Nb6-cluster unitsCs2GdNb6Cl15O3, dicaesium gadolinium hexaniobium pentadecachloride trioxide, was synthesized by solid-state reactions starting from a stoichiometric mixture of CsCl, Gd2O3, Nb, NbCl5, and Nb2O5. The crystal structure is based on octahedral Nb6 cluster units (point group symmetry 3.2) with composition [(Nb6Cli9Oi3)Cla6]5– where i and a denote inner and outer ligands. Cs2GdNb6Cl15O3 exhibits 14 valence electrons per cluster unit. The cluster units are linked to each other by CsI and GdIII atoms, whereby CsI (site symmetry 3..) is 12-coordinated by six Cli and six Cla ligands belonging to six neighboring cluster units and GdIII (site symmetry 3.2) is 9-coordinated by three Oi and six Cli ligands belonging to three adjacent cluster units. The arrangement of cluster units corresponds to a stacking of …AA′A… layers along [001]. Cs2GdNb6Cl15O3 is isotypic with Cs2UNb6Cl15O3.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextActa Crystallographica Section E: Crystallographic CommunicationsNovember 2023https://creativecommons.org/licenses/by/4.0/research communications2023-10-101008791011med@iucr.org2056-98902056-989011Crystal structure, Hirshfeld surface and crystal void analysis, intermolecular interaction energies, DFT calculations and energy frameworks of 2H-benzo[b][1,4]thiazin-3(4H)-one 1,1-dioxide
http://scripts.iucr.org/cgi-bin/paper?wm5698
In the title molecule, C8H7NO3S, the nitrogen atom has a planar environment, and the thiazine ring exhibits a screw-boat conformation. In the crystal, corrugated layers of molecules parallel to the ab plane are formed by N—H⋯O and C—H⋯O hydrogen bonds together with C—H⋯π(ring) and S=O⋯π(ring) interactions. The layers are connected by additional C—H⋯O hydrogen bonds and π-stacking interactions. Hirshfeld surface analysis indicates that the most important contributions for the crystal packing are from H⋯O/O⋯H (49.4%), H⋯H (23.0%) and H⋯C/C⋯H (14.1%) interactions. The volume of the crystal voids and the percentage of free space were calculated as 75.4 Å3 and 9.3%. Density functional theory (DFT) computations revealed N—H⋯O and C—H⋯O hydrogen-bonding energies of 43.3, 34.7 and 34.4 kJ mol−1, respectively. Evaluation of the electrostatic, dispersion and total energy frameworks indicate that the stabilization is dominated via the electrostatic energy contribution. Moreover, the DFT-optimized structure at the B3LYP/ 6–311 G(d,p) level is compared with the experimentally determined molecular structure in the solid state. The HOMO–LUMO behaviour was elucidated to determine the energy gap.urn:issn:2056-9890Irrou, E.Ait Elmachkouri, Y.Mazzah, A.Hökelek, T.Haoudi, A.Mague, J.T.Taha, M.L.Sebbar, N.K.text/htmlIn the title compound, the thiazine ring exhibits a screw-boat conformation. In the crystal, corrugated layers of molecules parallel to the ab plane are formed by N—H⋯O and C—H⋯O hydrogen bonds together with C—H⋯π(ring) and S=O⋯π(ring) interactions. The layers are connected by additional C—H⋯O hydrogen bonds and π-stacking interactions.doi:10.1107/S205698902300868XCRYSTAL STRUCTURE; HYDROGEN BOND; C-H...[PI](RING) INTERACTION; [PI]-STACKING; SULFONE; CRYSTAL STRUCTURE2023-10-19Crystal structure, Hirshfeld surface and crystal void analysis, intermolecular interaction energies, DFT calculations and energy frameworks of 2H-benzo[b][1,4]thiazin-3(4H)-one 1,1-dioxideIn the title molecule, C8H7NO3S, the nitrogen atom has a planar environment, and the thiazine ring exhibits a screw-boat conformation. In the crystal, corrugated layers of molecules parallel to the ab plane are formed by N—H⋯O and C—H⋯O hydrogen bonds together with C—H⋯π(ring) and S=O⋯π(ring) interactions. The layers are connected by additional C—H⋯O hydrogen bonds and π-stacking interactions. Hirshfeld surface analysis indicates that the most important contributions for the crystal packing are from H⋯O/O⋯H (49.4%), H⋯H (23.0%) and H⋯C/C⋯H (14.1%) interactions. The volume of the crystal voids and the percentage of free space were calculated as 75.4 Å3 and 9.3%. Density functional theory (DFT) computations revealed N—H⋯O and C—H⋯O hydrogen-bonding energies of 43.3, 34.7 and 34.4 kJ mol−1, respectively. Evaluation of the electrostatic, dispersion and total energy frameworks indicate that the stabilization is dominated via the electrostatic energy contribution. Moreover, the DFT-optimized structure at the B3LYP/ 6–311 G(d,p) level is compared with the experimentally determined molecular structure in the solid state. The HOMO–LUMO behaviour was elucidated to determine the energy gap.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-10-191037November 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/112056-98902056-9890med@iucr.org1043Synthesis, crystal structure and Hirshfeld analysis of trans-bis{(2E)-N-phenyl-2-[(2E)-3-phenyl-2-propen-1-ylidene]hydrazinecarbothioamidato-κ2N1,S}palladium(II)
http://scripts.iucr.org/cgi-bin/paper?zn2032
The reaction of (2E)-N-phenyl-2-[(2E)-3-phenyl-2-propen-1-ylidene]hydrazinecarbothioamide (common name: cinnamaldehyde-4-phenylthiosemicarbazone) deprotonated with NaOH in ethanol with an ethanolic suspension of PdII chloride in a 2:1 molar ratio yielded the title compound, [Pd(C16H14N3S)2]. The anionic ligands act as metal chelators, κ2N1S-donors, forming five-membered rings with a trans-configuration. The PdII ion is fourfold coordinated in a slightly distorted square-planar geometry. For each ligand, one H⋯S and one H⋯N intramolecular interactions are observed, with S(5) and S(6) graph-set motifs. Concerning the H⋯S interactions, the coordination sphere resembles a hydrogen-bonded macrocyclic environment-type. In the crystal, the complexes are linked via pairs of H⋯S interactions, with graph-set motif R22(8), and building a mono-periodic hydrogen-bonded ribbon along [001]. The Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are: H⋯H (45.3%), H⋯C/C⋯H (28.0%), H⋯S/S⋯H (8.0%) and H⋯N/N⋯H (7.4%).urn:issn:2056-9890Melo, A.P.L. deMartins, B.B.Bresolin, L.Tirloni, B.Oliveira, A.B. detext/htmlThe synthesis, crystal structure and Hirshfeld surface analysis of a new PdII cinnamaldehyde 4-thiosemicarbazone homoleptic complex is reported. As a result of H⋯S intramolecular interactions, graph-set motif S(5), the coordination sphere resembles a hydrogen-bonded macrocyclic environment-type. In the crystal, the molecules are linked by H⋯S interactions, with graph-set motifs R_{2}^{2}(8), forming a mono-periodic hydrogen-bonded polymer along [001].doi:10.1107/S2056989023008654PALLADIUM(II) THIOSEMICARBAZONE COMPLEX; CINNAMALDEHYDE 4-PHENYLTHIOSEMICARBAZONE; HIRSHFELD SURFACE ANALYSIS; CRYSTAL STRUCTURE2023-10-05Synthesis, crystal structure and Hirshfeld analysis of trans-bis{(2E)-N-phenyl-2-[(2E)-3-phenyl-2-propen-1-ylidene]hydrazinecarbothioamidato-κ2N1,S}palladium(II)The reaction of (2E)-N-phenyl-2-[(2E)-3-phenyl-2-propen-1-ylidene]hydrazinecarbothioamide (common name: cinnamaldehyde-4-phenylthiosemicarbazone) deprotonated with NaOH in ethanol with an ethanolic suspension of PdII chloride in a 2:1 molar ratio yielded the title compound, [Pd(C16H14N3S)2]. The anionic ligands act as metal chelators, κ2N1S-donors, forming five-membered rings with a trans-configuration. The PdII ion is fourfold coordinated in a slightly distorted square-planar geometry. For each ligand, one H⋯S and one H⋯N intramolecular interactions are observed, with S(5) and S(6) graph-set motifs. Concerning the H⋯S interactions, the coordination sphere resembles a hydrogen-bonded macrocyclic environment-type. In the crystal, the complexes are linked via pairs of H⋯S interactions, with graph-set motif R22(8), and building a mono-periodic hydrogen-bonded ribbon along [001]. The Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are: H⋯H (45.3%), H⋯C/C⋯H (28.0%), H⋯S/S⋯H (8.0%) and H⋯N/N⋯H (7.4%).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79Acta Crystallographica Section E: Crystallographic CommunicationsNovember 2023https://creativecommons.org/licenses/by/4.0/research communications2023-10-052056-98902056-989011med@iucr.orgCrystal structure and Hirshfeld surface analysis of poly[[tetraaqua(μ-1,3,4,7,8,10,12,13,16,17,19,22-dodecaazatetracyclo[8.8.4.13,17.18,12]tetracosane-5,6,14,15,20,21-hexaonato)iron(IV)dilithium] tetrahydrate]
http://scripts.iucr.org/cgi-bin/paper?tx2074
The title compound, [FeLi2(C12H12N12O6)(H2O)4]·4H2O, consists of iron complex anions, lithium cations and water molecules. The complex anion shows a clathrochelate topology. The coordination geometry of the FeIV centre is intermediate between a trigonal prism and a trigonal antiprism. In the crystal, the complex anions are connected through two Li cations into dimers, which are connected by Li—O bonds, forming infinite chains along the b-axis direction.urn:issn:2056-9890Plutenko, M.O.Shova, S.Pavlenko, V.A.Golenya, I.A.Fritsky, I.O.text/htmlThe title compound was obtained as a result of a template reaction between oxalohydrazide, formaldehyde and iron(III) chloride in the presence of atmospheric O2. The complex anion of the title compound reveals clathrochelate topology and includes an FeIV metal centre. In the crystal, the complex anions are connected through two Li cations into dimers, which are connected by Li—O bonds, forming infinite chains along the b-axis direction.doi:10.1107/S2056989023008587CRYSTAL STRUCTURE; IRON(IV) COMPLEX; CLATHROCHELATE; TEMPLATE REACTION; MACROCYCLIC LIGAND; HYDRAZIDE-BASED LIGAND; HIRSHFELD SURFACE ANALYSIS2023-10-19Crystal structure and Hirshfeld surface analysis of poly[[tetraaqua(μ-1,3,4,7,8,10,12,13,16,17,19,22-dodecaazatetracyclo[8.8.4.13,17.18,12]tetracosane-5,6,14,15,20,21-hexaonato)iron(IV)dilithium] tetrahydrate]The title compound, [FeLi2(C12H12N12O6)(H2O)4]·4H2O, consists of iron complex anions, lithium cations and water molecules. The complex anion shows a clathrochelate topology. The coordination geometry of the FeIV centre is intermediate between a trigonal prism and a trigonal antiprism. In the crystal, the complex anions are connected through two Li cations into dimers, which are connected by Li—O bonds, forming infinite chains along the b-axis direction.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext1060med@iucr.org2056-98902056-989011November 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/2023-10-19105779Carbon dioxide capture from air leading to bis[N-(5-methyl-1H-pyrazol-3-yl-κN2)carbamato-κO]copper(II) tetrahydrate
http://scripts.iucr.org/cgi-bin/paper?tx2076
A mononuclear square-planar CuII complex of (5-methyl-1H-pyrazol-3-yl)carbamate, [Cu(C5H6N3O2)2]·4H2O, was synthesized using a one-pot reaction from 5-methyl-3-pyrazolamine and copper(II) acetate in water under ambient conditions. The adsorption of carbon dioxide from air was facilitated by the addition of diethanolamine to the reaction mixture. While diethanolamine is not a component of the final product, it plays a pivotal role in the reaction by creating an alkaline environment, thereby enabling the adsorption of atmospheric carbon dioxide. The central copper(II) atom is in an (N2O2) square-planar coordination environment formed by two N atoms and two O atoms of two equivalent (5-methyl-1H-pyrazol-3-yl)carbamate ligands. Additionally, there are co-crystallized water molecules within the crystal structure of this compound. These co-crystallized water molecules are linked to the CuII mononuclear complex by O—H⋯O hydrogen bonds. According to Hirshfeld surface analysis, the most frequently observed weak intermolecular interactions are H⋯O/O⋯H (33.6%), H⋯C/C⋯H (11.3%) and H⋯N/N⋯H (9.0%) contacts.urn:issn:2056-9890Sirenko, V.Y.Kuzevanova, I.S.Vynohradov, O.S.Naumova, D.D.Shova, S.text/htmlA mononuclear square-planar CuII complex was synthesized by reacting 5-methyl-3-pyrazolamine and copper(II) acetate in water under ambient conditions. Diethanolamine was added to facilitate carbon dioxide adsorption, creating an alkaline environment. Structural analysis revealed that the complex crystallizes in the P21/c space group of the monoclinic crystal system, with the central copper(II) atom in a square-planar coordination environment N2O2. Co-crystallized water molecules are present, forming O—H⋯O hydrogen bonds with the CuII mononuclear complex. Hirshfeld surface analysis highlighted the importance of various interactions, including H⋯O/O⋯H, H⋯C/C⋯H, and H⋯N/N⋯H, in providing crystal structure packing.doi:10.1107/S20569890230085755-METHYL-3-PYRAZOLAMINE; COPPER(II) ACETATE; DIETHANOLAMINE; HIRSHFELD SURFACE ANALYSIS; CRYSTAL STRUCTURE; COPPER(II) COMPLEXES2023-10-05Carbon dioxide capture from air leading to bis[N-(5-methyl-1H-pyrazol-3-yl-κN2)carbamato-κO]copper(II) tetrahydrateA mononuclear square-planar CuII complex of (5-methyl-1H-pyrazol-3-yl)carbamate, [Cu(C5H6N3O2)2]·4H2O, was synthesized using a one-pot reaction from 5-methyl-3-pyrazolamine and copper(II) acetate in water under ambient conditions. The adsorption of carbon dioxide from air was facilitated by the addition of diethanolamine to the reaction mixture. While diethanolamine is not a component of the final product, it plays a pivotal role in the reaction by creating an alkaline environment, thereby enabling the adsorption of atmospheric carbon dioxide. The central copper(II) atom is in an (N2O2) square-planar coordination environment formed by two N atoms and two O atoms of two equivalent (5-methyl-1H-pyrazol-3-yl)carbamate ligands. Additionally, there are co-crystallized water molecules within the crystal structure of this compound. These co-crystallized water molecules are linked to the CuII mononuclear complex by O—H⋯O hydrogen bonds. According to Hirshfeld surface analysis, the most frequently observed weak intermolecular interactions are H⋯O/O⋯H (33.6%), H⋯C/C⋯H (11.3%) and H⋯N/N⋯H (9.0%) contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org112056-98902056-98902023-10-05Acta Crystallographica Section E: Crystallographic CommunicationsNovember 2023research communicationshttps://creativecommons.org/licenses/by/4.0/79Synthesis, crystal structure, stereochemical and Hirshfeld surface analysis of trans-diaquabis(1-phenylpropane-1,2-diamine-κ2N,N′)nickel(II) dichloride dihydrate
http://scripts.iucr.org/cgi-bin/paper?wm5696
In the hydrated complex salt, [Ni(C9H14N2)2(H2O)2]Cl2·2H2O, the asymmetric unit comprises of half of the complex cation along with one chloride anion and one non-coordinating water molecule. The central nickel(II) atom is located on an inversion center and is coordinated in a trans octahedral fashion by four N atoms from two bidentate 1,2-diamino-1-phenylpropane ligands in the equatorial plane, and by two oxygen atoms from two water molecules occupying the axial sites. The five-membered chelate ring is in a slightly twisted envelope conformation. The crystal packing features O—H⋯Cl, N—H⋯O and N—H⋯Cl hydrogen bonds. Hirshfeld surface analysis revealed that the most important contributions to the crystal packing are from H⋯H (56.4%), O⋯H/H⋯O (16.4%) and H⋯Cl (13.3%) interactions. The crystal void volume was calculated to be 15.17%.urn:issn:2056-9890Akila, S.Vidhyasagar, T.Thiruvalluvar, A.A.Rajeswari, K.text/htmlThe cation of the title compound exhibits point group symmetry \overline{1}, with the central NiII atom in a trans [N4O2] coordination environment.doi:10.1107/S2056989023008538SYNTHESIS; X-RAY CRYSTAL STRUCTURE; NIII COMPLEX; ETHYLENEDIAMINE METAL COMPLEX; VICINAL DIAMINE DERIVATIVE; DFT; HIRSHFELD SURFACE ANALYSIS; DISTORTED OCTAHEDRAL COMPLEX; TRANS-NI COMPLEX.2023-09-29Synthesis, crystal structure, stereochemical and Hirshfeld surface analysis of trans-diaquabis(1-phenylpropane-1,2-diamine-κ2N,N′)nickel(II) dichloride dihydrateIn the hydrated complex salt, [Ni(C9H14N2)2(H2O)2]Cl2·2H2O, the asymmetric unit comprises of half of the complex cation along with one chloride anion and one non-coordinating water molecule. The central nickel(II) atom is located on an inversion center and is coordinated in a trans octahedral fashion by four N atoms from two bidentate 1,2-diamino-1-phenylpropane ligands in the equatorial plane, and by two oxygen atoms from two water molecules occupying the axial sites. The five-membered chelate ring is in a slightly twisted envelope conformation. The crystal packing features O—H⋯Cl, N—H⋯O and N—H⋯Cl hydrogen bonds. Hirshfeld surface analysis revealed that the most important contributions to the crystal packing are from H⋯H (56.4%), O⋯H/H⋯O (16.4%) and H⋯Cl (13.3%) interactions. The crystal void volume was calculated to be 15.17%.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytexthttps://creativecommons.org/licenses/by/4.0/research communicationsOctober 2023Acta Crystallographica Section E: Crystallographic Communications2023-09-2996779971med@iucr.org2056-98902056-989010Synthesis, crystal structure and in vitro anti-proliferative activity of 2-[(4-acetylphenyl)carbamoyl]phenyl acetate
http://scripts.iucr.org/cgi-bin/paper?dj2060
2-[(4-Acetylphenyl)carbamoyl]phenyl acetate, C17H15NO4, has been synthesized and structurally characterized. In the structure, N—H⋯O hydrogen-bonding interactions form chains of molecules aligned along the [101] direction. The chains are linked by π–π and C—H⋯π interactions, forming a three dimensional network. The compound has been screened for in vitro anti-proliferative activity revealing considerable activity.urn:issn:2056-9890Mohamed-Ezzat, R.A.Kariuki, B.M.Srour, A.M.text/html2-[(4-Acetylphenyl)carbamoyl]phenyl acetate, a derivative of aspirin, has been structurally characterized revealing a structure based on intermolecular N—H⋯O hydrogen bonds and π–π interactions.doi:10.1107/S2056989023008526CRYSTAL STRUCTURE; ASPIRIN DERIVATIVE; NCI 60 CELL LINE; ANTI-PROLIFERATIVE ACTIVITY2023-10-05Synthesis, crystal structure and in vitro anti-proliferative activity of 2-[(4-acetylphenyl)carbamoyl]phenyl acetate2-[(4-Acetylphenyl)carbamoyl]phenyl acetate, C17H15NO4, has been synthesized and structurally characterized. In the structure, N—H⋯O hydrogen-bonding interactions form chains of molecules aligned along the [101] direction. The chains are linked by π–π and C—H⋯π interactions, forming a three dimensional network. The compound has been screened for in vitro anti-proliferative activity revealing considerable activity.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-989011med@iucr.org79November 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/2023-10-05Unusual reaction of (E)-2-[(benzo[d]thiazol-2-ylimino)methyl]-5-(diethylamino)phenol with triphenylborane: crystal structures and optical properties
http://scripts.iucr.org/cgi-bin/paper?pk2698
The molecular and crystal structure of (E)-2-[(benzo[d]thiazol-2-ylimino)methyl]-5-(diethylamino)phenol (C18H19N3O2S, Et2N-Bz) and its unexpected reaction product with triphenylborane, 2,2-diphenyl-1,3-dioxa-2-borata-1,2-dihydronaphthalene [systematic name: N,N-diethyl-2,2-diphenyl-2H-1,3λ3,2λ4-benzodioxaborinin-7-amine, C23H24BNO2, (I)] are described. For Et2N-Bz, the hydroxyl group is involved in an intramolecular hydrogen bond with the imino nitrogen atom and the C=N bond displays an E configuration. The crystal packing is characterized by layers of inversion dimers parallel to the (10\overline{1}) plane and chains of molecule in the a-axis direction formed through C—H⋯O interactions. Complex (I) crystallizes with two molecules (A and B) in the asymmetric unit, which differ in the orientation of the ethyl groups. The 1,3-dioxa-2-borata-1,2,3,4-tetrahydronaphthalene ring displays a slight envelope conformation with the boron atom as the flap. In the crystal packing, chains of alternating A and B molecules formed by C—H⋯O hydrogen bonds run in the b-axis direction. The UV–vis absorption and emission properties of the compounds are discussed and their aggregation-induced emission properties are further investigated.urn:issn:2056-9890Le Thi Hong, H.Le Phuong, T.Van Pham, T.Minh Thi Nguyen, H.Van Meervelt, L.text/htmlThe molecular and crystal structure of (E)-2-[(benzo[d]thiazol-2-ylimino)methyl]-5-(diethylamino)phenol and its reaction product with triphenylborane are described. In compound Et2N-Bz, one of the ethyl groups and the benzothiazole ring are disordered over two sets of atomic sites with major occupancy components of 0.822 (5) and 0.843 (2), respectively.doi:10.1107/S2056989023008514CRYSTAL STRUCTURE; BENZOTHIAZOLE; BORANILS; FLUORESCENCE; AGGREGATION-INDUCED EMISSION2023-10-03Unusual reaction of (E)-2-[(benzo[d]thiazol-2-ylimino)methyl]-5-(diethylamino)phenol with triphenylborane: crystal structures and optical propertiesThe molecular and crystal structure of (E)-2-[(benzo[d]thiazol-2-ylimino)methyl]-5-(diethylamino)phenol (C18H19N3O2S, Et2N-Bz) and its unexpected reaction product with triphenylborane, 2,2-diphenyl-1,3-dioxa-2-borata-1,2-dihydronaphthalene [systematic name: N,N-diethyl-2,2-diphenyl-2H-1,3λ3,2λ4-benzodioxaborinin-7-amine, C23H24BNO2, (I)] are described. For Et2N-Bz, the hydroxyl group is involved in an intramolecular hydrogen bond with the imino nitrogen atom and the C=N bond displays an E configuration. The crystal packing is characterized by layers of inversion dimers parallel to the (10\overline{1}) plane and chains of molecule in the a-axis direction formed through C—H⋯O interactions. Complex (I) crystallizes with two molecules (A and B) in the asymmetric unit, which differ in the orientation of the ethyl groups. The 1,3-dioxa-2-borata-1,2,3,4-tetrahydronaphthalene ring displays a slight envelope conformation with the boron atom as the flap. In the crystal packing, chains of alternating A and B molecules formed by C—H⋯O hydrogen bonds run in the b-axis direction. The UV–vis absorption and emission properties of the compounds are discussed and their aggregation-induced emission properties are further investigated.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-989011https://creativecommons.org/licenses/by/4.0/research communicationsNovember 2023Acta Crystallographica Section E: Crystallographic Communications2023-10-0379Crystal structures of five halido gold complexes involving piperidine or pyrrolidine as ligands or (protonated) as cations
http://scripts.iucr.org/cgi-bin/paper?yz2040
In bromido(pyrrolidine-κN)gold(I) bis(pyrrolidine-κN)gold(I) bromide, [AuBr(pyr)]·[Au(pyr)2]Br (pyr = pyrrolidine, C4H9N), 2, alternating [AuBr(pyr)] molecules and [Au(pyr)2]+ cations are connected by aurophilic contacts to form infinite chains of residues parallel to the b axis. The chains are cross-linked by three N—H⋯Br− hydrogen bonds and an Au⋯Br contact to form a layer structure parallel to the ab plane. Trichlorido(piperidine-κN)gold(III), [AuCl3(pip)] (pip = piperidine, C5H11N), 3, consists of molecules with the expected square-planar coordination at the gold atom, which are connected by an N—H⋯Cl hydrogen bond and an Au⋯Cl contact to form a layer structure parallel to the ac plane. The structures of bis(piperidinium) tetrachloridoaurate(III) chloride, (pipH)2[AuCl4]Cl, 4, and bis(pyrrolidinium) tetrabromidoaurate(III) bromide, (pyrH)2[AuBr4]Br, 6, are closely related but not isotypic. Compound 6 crystallizes in space group Ibam; the Au and two Br atoms of the anion lie in the mirror plane x, y, 0, whereas the bromide ions occupy special positions 0, 0.5, 0 and 0, 0.5, 0.25, with site symmetry 2/m. The NH2 group forms a hydrogen bond to one bromide ion, and also a three-centre hydrogen bond to the other bromide atom and to a metal-bonded Br atom. The packing involves chains of hydrogen-bonded pyrrolidinium and bromide ions parallel to the c axis, combined with a layer structure of [AuBr4]− and bromide anions, parallel to the ab plane and involving Au⋯Br and Br⋯Br contacts. Compound 4, however, crystallizes pseudosymmetrically in space group Iba2; two chlorine atoms of the anion lie on the twofold axis 0.5, 0.5, z, and there are two independent cations. The packing is closely similar to that of 6, but there are no N—H⋯Cl hydrogen bonds to metal-bonded chlorines. The contact distances Au⋯Cl are appreciably longer than their Au⋯Br counterparts in 6, whereas the Cl⋯Cl contact is much shorter than Br⋯Br in 6. Tribromido(piperidine-κN)gold(III) crystallizes as its dichloromethane solvate, [AuBr3(pip)]·CH2Cl2, 7. It too displays a square-planar coordination at the gold atom. The packing involves hydrogen bonds N—H⋯Br, stacking of neighbouring AuBr3 units by Au⋯Br contacts, and a short Br⋯Br contact; these combine to form a layer structure parallel to the ac plane.urn:issn:2056-9890Döring, C.Jones, P.G.text/htmlThe structures of five gold complexes involving piperidine or pyrrolidine, either as neutral ligands or protonated counter-cations, are presented.doi:10.1107/S205698902300854XCRYSTAL STRUCTURE; GOLD; PIPERIDINE; PYRROLIDINE; SECONDARY INTERACTIONS2023-10-10Crystal structures of five halido gold complexes involving piperidine or pyrrolidine as ligands or (protonated) as cationsIn bromido(pyrrolidine-κN)gold(I) bis(pyrrolidine-κN)gold(I) bromide, [AuBr(pyr)]·[Au(pyr)2]Br (pyr = pyrrolidine, C4H9N), 2, alternating [AuBr(pyr)] molecules and [Au(pyr)2]+ cations are connected by aurophilic contacts to form infinite chains of residues parallel to the b axis. The chains are cross-linked by three N—H⋯Br− hydrogen bonds and an Au⋯Br contact to form a layer structure parallel to the ab plane. Trichlorido(piperidine-κN)gold(III), [AuCl3(pip)] (pip = piperidine, C5H11N), 3, consists of molecules with the expected square-planar coordination at the gold atom, which are connected by an N—H⋯Cl hydrogen bond and an Au⋯Cl contact to form a layer structure parallel to the ac plane. The structures of bis(piperidinium) tetrachloridoaurate(III) chloride, (pipH)2[AuCl4]Cl, 4, and bis(pyrrolidinium) tetrabromidoaurate(III) bromide, (pyrH)2[AuBr4]Br, 6, are closely related but not isotypic. Compound 6 crystallizes in space group Ibam; the Au and two Br atoms of the anion lie in the mirror plane x, y, 0, whereas the bromide ions occupy special positions 0, 0.5, 0 and 0, 0.5, 0.25, with site symmetry 2/m. The NH2 group forms a hydrogen bond to one bromide ion, and also a three-centre hydrogen bond to the other bromide atom and to a metal-bonded Br atom. The packing involves chains of hydrogen-bonded pyrrolidinium and bromide ions parallel to the c axis, combined with a layer structure of [AuBr4]− and bromide anions, parallel to the ab plane and involving Au⋯Br and Br⋯Br contacts. Compound 4, however, crystallizes pseudosymmetrically in space group Iba2; two chlorine atoms of the anion lie on the twofold axis 0.5, 0.5, z, and there are two independent cations. The packing is closely similar to that of 6, but there are no N—H⋯Cl hydrogen bonds to metal-bonded chlorines. The contact distances Au⋯Cl are appreciably longer than their Au⋯Br counterparts in 6, whereas the Cl⋯Cl contact is much shorter than Br⋯Br in 6. Tribromido(piperidine-κN)gold(III) crystallizes as its dichloromethane solvate, [AuBr3(pip)]·CH2Cl2, 7. It too displays a square-planar coordination at the gold atom. The packing involves hydrogen bonds N—H⋯Br, stacking of neighbouring AuBr3 units by Au⋯Br contacts, and a short Br⋯Br contact; these combine to form a layer structure parallel to the ac plane.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext112056-98902056-9890med@iucr.org10277910172023-10-10https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsNovember 2023Crystal structure of bis{3-(3,4-dimethoxyphenyl)-5-[6-(pyrazol-1-yl)pyridin-2-yl]-1,2,4-triazol-3-ato}iron(II)–methanol–dichloroform (1/2/2)
http://scripts.iucr.org/cgi-bin/paper?tx2075
The unit cell of the title compound, [Fe(C18H15N6O2)2]·2CH3OH·2CHCl3, consists of a charge-neutral complex molecule, two methanol and two chloroform molecules. In the complex, the two tridentate 2-(5-(3,4-dimethoxyphenyl)-1,2,4-triazol-3-yl)-6-(pyrazol-1-yl)pyridine ligands coordinate to the central FeII ion through the N atoms of the pyrazole, pyridine and triazole groups, forming a pseudo-octahedral coordination sphere. Neighbouring tapered molecules are linked through weak C—H(pz)⋯π(ph) interactions into one-dimensional chains, which are joined into two-dimensional layers through weak C—H⋯N/C/O interactions. Furthermore, the layers stack in a three-dimensional network linked by weak interlayer C—H⋯π interactions of the methoxy and phenyl groups. The intermolecular contacts were quantified using Hirshfeld surface analysis and two-dimensional fingerprint plots, revealing the relative contributions of the contacts to the crystal packing to be H⋯H 32.0%, H⋯C/C⋯H 26.3%, H⋯N/N⋯H 13.8%, and H⋯O/O⋯H 7.5%. The average Fe—N bond distance is 2.185 Å, indicating the high-spin state of the FeII ion. Energy framework analysis at the HF/3–21 G theory level was performed to quantify the interaction energies in the crystal structure.urn:issn:2056-9890Znovjyak, K.Fritsky, I.O.Sliva, T.Y.Amirkhanov, V.M.Malinkin, S.O.Shova, S.Seredyuk, M.text/htmlThe title compound, a charge-neutral bis{5-(3,4-dimethoxyphenyl)-1,2,4-triazol-3-ato)-6-(pyrazol-1-yl)pyridine} iron(II) dimethanol dichloroform solvate, is a high-spin complex with a distorted pseudooctahedral coordination environment of the metal ion. Due to the tapered shape and polar nature, the molecules stack in one-dimensional columns that are bound by weak hydrogen bonds into layers, which, in turn, are arranged in a three-dimensional network without interlayer interactions below van der Waals radii.doi:10.1107/S2056989023008423CRYSTAL STRUCTURE; IRON(II) COMPLEXES; NEUTRAL COMPLEXES2023-09-29Crystal structure of bis{3-(3,4-dimethoxyphenyl)-5-[6-(pyrazol-1-yl)pyridin-2-yl]-1,2,4-triazol-3-ato}iron(II)–methanol–dichloroform (1/2/2)The unit cell of the title compound, [Fe(C18H15N6O2)2]·2CH3OH·2CHCl3, consists of a charge-neutral complex molecule, two methanol and two chloroform molecules. In the complex, the two tridentate 2-(5-(3,4-dimethoxyphenyl)-1,2,4-triazol-3-yl)-6-(pyrazol-1-yl)pyridine ligands coordinate to the central FeII ion through the N atoms of the pyrazole, pyridine and triazole groups, forming a pseudo-octahedral coordination sphere. Neighbouring tapered molecules are linked through weak C—H(pz)⋯π(ph) interactions into one-dimensional chains, which are joined into two-dimensional layers through weak C—H⋯N/C/O interactions. Furthermore, the layers stack in a three-dimensional network linked by weak interlayer C—H⋯π interactions of the methoxy and phenyl groups. The intermolecular contacts were quantified using Hirshfeld surface analysis and two-dimensional fingerprint plots, revealing the relative contributions of the contacts to the crystal packing to be H⋯H 32.0%, H⋯C/C⋯H 26.3%, H⋯N/N⋯H 13.8%, and H⋯O/O⋯H 7.5%. The average Fe—N bond distance is 2.185 Å, indicating the high-spin state of the FeII ion. Energy framework analysis at the HF/3–21 G theory level was performed to quantify the interaction energies in the crystal structure.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79Acta Crystallographica Section E: Crystallographic CommunicationsOctober 2023https://creativecommons.org/licenses/by/4.0/research communications9622023-09-292056-98902056-989010966med@iucr.orgCrystal structure of bis(3-carboxy-1-methylpyridinium) octabromide
http://scripts.iucr.org/cgi-bin/paper?wm5697
The crystal structure of the title salt, bis(3-carboxy-1-methylpyridinium) octabromide, 2C7H8NO2+·Br82−, consists of 3-carboxy-1-methylpyridinium (N-methylnicotinic acid) cations, which are stacked between relatively rare [Br8]2– anions. The polybromide [Br8]2– anion has point group symmetry \overline{1} and can be described as being composed of two [Br3]− anions connected with a Br2 molecule in a Z-shaped manner. Contacts between neighboring octabromide anions ensure the creation of pseudo-polymeric chains propagating along [111]. The organic cations are located between anionic chains and are connected to each other through O—H⋯O hydrogen bonds and to the [Br8]2– anions through π⋯Br interactions that induce the creation of a supramolecular tri-periodic network. In addition, the presence of weak C—H⋯Br contacts leads to the creation of layers, which align parallel to (11\overline{2}).urn:issn:2056-9890Sirenko, V.Y.Naumova, D.D.Golenya, I.A.Shova, S.Gural'skiy, I.A.text/htmlThe structure of the title compound is composed of rare Z-shaped octabromide anions embedded within N-methylnicotinic acid cations.doi:10.1107/S2056989023008460CRYSTAL STRUCTURE; OCTABROMIDE ANION; POLYHALOGEN IONS; N-METHYLNICOTINIC ACID2023-10-03Crystal structure of bis(3-carboxy-1-methylpyridinium) octabromideThe crystal structure of the title salt, bis(3-carboxy-1-methylpyridinium) octabromide, 2C7H8NO2+·Br82−, consists of 3-carboxy-1-methylpyridinium (N-methylnicotinic acid) cations, which are stacked between relatively rare [Br8]2– anions. The polybromide [Br8]2– anion has point group symmetry \overline{1} and can be described as being composed of two [Br3]− anions connected with a Br2 molecule in a Z-shaped manner. Contacts between neighboring octabromide anions ensure the creation of pseudo-polymeric chains propagating along [111]. The organic cations are located between anionic chains and are connected to each other through O—H⋯O hydrogen bonds and to the [Br8]2– anions through π⋯Br interactions that induce the creation of a supramolecular tri-periodic network. In addition, the presence of weak C—H⋯Br contacts leads to the creation of layers, which align parallel to (11\overline{2}).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext112056-98902056-9890med@iucr.org792023-10-03November 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communicationsCrystal structures of five compounds in the aluminium–ruthenium–silicon system
http://scripts.iucr.org/cgi-bin/paper?wm5690
Single crystals of five compounds with approximate compositions ∼Ru16(Al0.78Si0.22)47, (I), ∼Ru9(Al0.70Si0.30)32, (II), ∼Ru10(Al0.67Si0.33)41, (III), ∼Ru(Al0.57Si0.43)5, (IV), and ∼Ru2(Al0.46Si0.54)9, (V), were obtained from polycrystalline lumps mainly composed of the target compounds, and their crystal structures were determined by means of single-crystal X-ray diffraction. The crystal structure of (I) can be related to that of a cubic rational crystalline approximant to an icosahedral quasicrystal through crystallographic shear and then unit-cell twinning. The crystal structure of (II) is isotypic with that of a phase with composition ∼Fe9(Al,Si)32. The crystal structure of (III) is comprised of edge-sharing Ru(Al,Si)9–11 polyhedra with disordered chains along edges of polyhedra. The crystal structure of (IV) is of the LiIrSn4 type. The crystal structure of (V) can be viewed as a crystallographic shear structure derived from that of (IV).urn:issn:2056-9890Kitahara, K.Takakura, H.Iwasaki, Y.Kimura, K.text/htmlThe crystal structures of five compounds in the Al–Ru–Si system with approximate compositions ∼Ru16(Al0.78Si0.22)47 (I), ∼Ru9(Al0.70Si0.30)32 (II), ∼Ru10(Al0.67Si0.33)41 (III), ∼Ru(Al0.57Si0.43)5 (IV) and ∼Ru2(Al0.46Si0.54)9 (V) are presented. Notably, the crystal structure of (I) can be related to that of a cubic rational crystalline approximant to an icosahedral quasicrystal through crystallographic shear and then unit-cell twinning.doi:10.1107/S2056989023008393CRYSTAL STRUCTURE; ALUMINIUM-RUTHENIUM-SILICON SYSTEM; SINGLE-CRYSTAL X-RAY DIFFRACTION; ISOTYPISM; STRUCTURAL SIMILARITY; CRYSTALLOGRAPHIC SHEAR; UNIT-CELL TWINNING; QUASICRYSTAL APPROXIMANT2023-09-29Crystal structures of five compounds in the aluminium–ruthenium–silicon systemSingle crystals of five compounds with approximate compositions ∼Ru16(Al0.78Si0.22)47, (I), ∼Ru9(Al0.70Si0.30)32, (II), ∼Ru10(Al0.67Si0.33)41, (III), ∼Ru(Al0.57Si0.43)5, (IV), and ∼Ru2(Al0.46Si0.54)9, (V), were obtained from polycrystalline lumps mainly composed of the target compounds, and their crystal structures were determined by means of single-crystal X-ray diffraction. The crystal structure of (I) can be related to that of a cubic rational crystalline approximant to an icosahedral quasicrystal through crystallographic shear and then unit-cell twinning. The crystal structure of (II) is isotypic with that of a phase with composition ∼Fe9(Al,Si)32. The crystal structure of (III) is comprised of edge-sharing Ru(Al,Si)9–11 polyhedra with disordered chains along edges of polyhedra. The crystal structure of (IV) is of the LiIrSn4 type. The crystal structure of (V) can be viewed as a crystallographic shear structure derived from that of (IV).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextresearch communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsOctober 20239462023-09-2979951med@iucr.org2056-98902056-989010Synthesis and crystal structure of 2-(anthracen-9-yl)-1-(tert-butyldimethylsilyl)-3,6-dihydro-1λ4,2λ4-azaborinine
http://scripts.iucr.org/cgi-bin/paper?vm2290
The title compound, C24H30BNSi (I), is an asymmetric 1,2,3,6-tetrahydro-1,2-azaborinine consisting of a BN-substituted cyclohexadiene analog with a B-anthracenyl substituent. A ring-closing metathesis with subsequent substitution of the obtained BCl 1,2-azaborinine using anthracenyl lithium yielded the title compound I. The asymmetric unit (Z = 8) belongs to the orthorhombic space group Pbca and shows an elongated N—C bond compared to previously reported BN-1,4-cyclohexadiene [Abbey et al. (2008) J. Am. Chem. Soc. 130, 7250–7252]. The primarily contributing surface interactions are H⋯H and C⋯H/H⋯C (as elucidated by Hirshfeld surface analysis) which are dominated by van der Waals forces. Moreover, the non-aromatic BN heterocycle and the protecting group exhibit intra- and intermolecular C—H⋯π interactions, respectively, with the anthracenyl substituent.urn:issn:2056-9890Gliese, P.J.Appiarius, Y.Scheele, T.Lork, E.Neudecker, T.Staubitz, A.text/htmlA modification of a B—Cl 1,2–azaborinine precursor with anthracenyl lithium generates an air-stable analog of cyclohexadiene. In the crystal packing, van der Waals interactions are dominant.doi:10.1107/S2056989023008381CRYSTAL STRUCTURE; 1,2-AZABORININE; BORON-NITROGEN BOND; BORON-NITROGEN HETEROCYCLE; RING-CLOSING METATHESIS; BN CYCLOHEXENE2023-10-10Synthesis and crystal structure of 2-(anthracen-9-yl)-1-(tert-butyldimethylsilyl)-3,6-dihydro-1λ4,2λ4-azaborinineThe title compound, C24H30BNSi (I), is an asymmetric 1,2,3,6-tetrahydro-1,2-azaborinine consisting of a BN-substituted cyclohexadiene analog with a B-anthracenyl substituent. A ring-closing metathesis with subsequent substitution of the obtained BCl 1,2-azaborinine using anthracenyl lithium yielded the title compound I. The asymmetric unit (Z = 8) belongs to the orthorhombic space group Pbca and shows an elongated N—C bond compared to previously reported BN-1,4-cyclohexadiene [Abbey et al. (2008) J. Am. Chem. Soc. 130, 7250–7252]. The primarily contributing surface interactions are H⋯H and C⋯H/H⋯C (as elucidated by Hirshfeld surface analysis) which are dominated by van der Waals forces. Moreover, the non-aromatic BN heterocycle and the protecting group exhibit intra- and intermolecular C—H⋯π interactions, respectively, with the anthracenyl substituent.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79research communicationshttps://creativecommons.org/licenses/by/4.0/November 2023Acta Crystallographica Section E: Crystallographic Communications10122023-10-102056-98902056-9890111016med@iucr.orgCo-crystal sustained by π-type halogen-bonding interactions between 1,4-diiodoperchlorobenzene and naphthalene
http://scripts.iucr.org/cgi-bin/paper?jy2037
The formation and crystal structure of a co-crystal based upon 1,4-diiodoperchlorobenzene (C6I2Cl4) as the halogen-bond donor along with naphthalene (nap) as the acceptor is reported. The co-crystal [systematic name: 1,2,4,5-tetrachloro-3,6-diiodobenzene–naphthalene, (C6I2Cl4)·(nap)] generates a chevron-like structure that is held together primarily by π-type halogen bonds (i.e. C—I⋯π contacts) between the components. In addition, C6I2Cl4 also interacts with the acceptor via C—Cl⋯π contacts that help stabilize the co-crystal. Within the solid, both aromatic components are found to engage in offset and homogeneous face-to-face π–π stacking interactions. Lastly, the halogen-bond donor C6I2Cl4 is found to engage with neighboring donors by both Type I chlorine–chlorine and Type II iodine–chlorine contacts, which generates an extended structure.urn:issn:2056-9890Bosch, E.Reinheimer, E.W.Unruh, D.K.Groeneman, R.H.text/htmlThe formation of a co-crystal sustained by π-type halogen bonds involving 1,4-diiodoperchlorobenzene and naphthalene is reported.doi:10.1107/S2056989023008356HALOGEN BONDING; CO-CRYSTAL; TYPE I CHLORINE-CHLORINE CONTACTS; TYPE II IODINE-CHLORINE CONTACTS2023-09-29Co-crystal sustained by π-type halogen-bonding interactions between 1,4-diiodoperchlorobenzene and naphthaleneThe formation and crystal structure of a co-crystal based upon 1,4-diiodoperchlorobenzene (C6I2Cl4) as the halogen-bond donor along with naphthalene (nap) as the acceptor is reported. The co-crystal [systematic name: 1,2,4,5-tetrachloro-3,6-diiodobenzene–naphthalene, (C6I2Cl4)·(nap)] generates a chevron-like structure that is held together primarily by π-type halogen bonds (i.e. C—I⋯π contacts) between the components. In addition, C6I2Cl4 also interacts with the acceptor via C—Cl⋯π contacts that help stabilize the co-crystal. Within the solid, both aromatic components are found to engage in offset and homogeneous face-to-face π–π stacking interactions. Lastly, the halogen-bond donor C6I2Cl4 is found to engage with neighboring donors by both Type I chlorine–chlorine and Type II iodine–chlorine contacts, which generates an extended structure.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext102056-98902056-9890med@iucr.org961799582023-09-29October 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communicationsCrystal structure of dibenzylammonium hydrogen (4-aminophenyl)arsonate monohydrate
http://scripts.iucr.org/cgi-bin/paper?dj2065
The title salt, C14H16N+·C6H7AsNO3−·H2O or [(C6H5CH2)2NH2][H2NC6H4As(OH)O2]·H2O, (I), was synthesized by mixing an aqueous solution of (4-aminophenyl)arsonic acid with an ethanolic solution of dibenzylamine at room temperature. Compound I crystallizes in the monoclinic P21/c space group. The three components forming I are linked via N—H⋯O and O—H⋯O intermolecular hydrogen bonds, resulting in the propagation of an infinite zigzag chain. Additional weak interactions between neighbouring chains, such as π–π and N—H⋯O contacts, involving phenyl rings, –NH2 and –As(OH)O3 functions, and H2O, respectively, lead to a three-dimensional network.urn:issn:2056-9890Traoré, B.Diallo, W.Sidibé, M.Diop, L.Plasseraud, L.Cattey, H.text/htmlThe title salt consists of three components, comprising one dibenzylammonium cation, [(C6H5CH2)2NH2]+, one hydrogen (4-aminophenyl)arsonate anion, [H2NC6H4As(OH)O2]−, and one molecule of water. In the crystal, these components are organized in infinite zigzag chains via intermolecular hydrogen bonds. Weak interactions between the chains lead to a three-dimensional network.doi:10.1107/S205698902300837XCRYSTAL STRUCTURE; GROUP 15 - PNICTOGEN ELEMENTS; ORGANIC SALT; PHENYLARSONIC DERIVATIVES; HYDROGEN BONDS; INFINITE CHAIN2023-10-05Crystal structure of dibenzylammonium hydrogen (4-aminophenyl)arsonate monohydrateThe title salt, C14H16N+·C6H7AsNO3−·H2O or [(C6H5CH2)2NH2][H2NC6H4As(OH)O2]·H2O, (I), was synthesized by mixing an aqueous solution of (4-aminophenyl)arsonic acid with an ethanolic solution of dibenzylamine at room temperature. Compound I crystallizes in the monoclinic P21/c space group. The three components forming I are linked via N—H⋯O and O—H⋯O intermolecular hydrogen bonds, resulting in the propagation of an infinite zigzag chain. Additional weak interactions between neighbouring chains, such as π–π and N—H⋯O contacts, involving phenyl rings, –NH2 and –As(OH)O3 functions, and H2O, respectively, lead to a three-dimensional network.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-10-05November 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications112056-98902056-9890med@iucr.orgCrystal structure and Hirshfeld surface analysis of cyclo-tetrabromido-1κ2Br,3κ2Br-tetrakis(μ2-2-{[(pyridin-2-yl)methyl]amino}ethane-1-thiolato-κ3N,S:S)tetramercury(II)
http://scripts.iucr.org/cgi-bin/paper?yz2039
The macrometallacyclic title compound, [Hg4Br4(C8H11N2S)4] or [((HgL2)(HgBr2))2] (1) where HL = 2-{[(pyridin-2-yl)methyl]amino}ethane-1-thiol, was prepared and structurally characterized. The Hg2+ complex crystallizes in the P21/c space group. The centrosymmetric Hg4S4 metallacycle is constructed from metal ions with alternating distorted tetrahedral Br2S2 and distorted seesaw N2S2 primary coordination environments with pendant pyridyl groups. The backfolded extended chair metallacycle conformation suggests interactions between each of the bis-chelated mercury atoms and Br atoms lying above and below the central Hg2S4 plane. Supramolecular interactions in 1 include a fourfold aryl embrace and potential hydrogen bonds with bromine as the acceptor. Hirshfeld surface analysis indicates that H⋯H (51.7%), Br⋯H/H⋯Br (23.0%) and C⋯H/H⋯C (9.5%) interactions are dominant.urn:issn:2056-9890Thomas, I.D.Kocher, K.R.Viehweg, J.A.Pike, R.D.Bebout, D.C.text/htmlA macrometallacyclic mercury(II) complex [((HgL2)(HgBr2))2], where HL = 2-{[(pyridin-2-yl)methyl]amino}ethane-1-thiol, was synthesized and characterized by single-crystal X-ray diffraction and Hirshfeld analysis.doi:10.1107/S205698902300823XCRYSTAL STRUCTURE; HIRSHFELD SURFACE ANALYSIS; METALLACYCLE; CHELATING N,S-LIGANDS; HG2+ COMPLEX2023-09-29Crystal structure and Hirshfeld surface analysis of cyclo-tetrabromido-1κ2Br,3κ2Br-tetrakis(μ2-2-{[(pyridin-2-yl)methyl]amino}ethane-1-thiolato-κ3N,S:S)tetramercury(II)The macrometallacyclic title compound, [Hg4Br4(C8H11N2S)4] or [((HgL2)(HgBr2))2] (1) where HL = 2-{[(pyridin-2-yl)methyl]amino}ethane-1-thiol, was prepared and structurally characterized. The Hg2+ complex crystallizes in the P21/c space group. The centrosymmetric Hg4S4 metallacycle is constructed from metal ions with alternating distorted tetrahedral Br2S2 and distorted seesaw N2S2 primary coordination environments with pendant pyridyl groups. The backfolded extended chair metallacycle conformation suggests interactions between each of the bis-chelated mercury atoms and Br atoms lying above and below the central Hg2S4 plane. Supramolecular interactions in 1 include a fourfold aryl embrace and potential hydrogen bonds with bromine as the acceptor. Hirshfeld surface analysis indicates that H⋯H (51.7%), Br⋯H/H⋯Br (23.0%) and C⋯H/H⋯C (9.5%) interactions are dominant.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextOctober 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/9522023-09-2979957med@iucr.org2056-98902056-989010Synthesis, crystal structure and reactivity of bis(μ-2-methylpyridine N-oxide-κ2O:O)bis[dibromido(2-methylpyridine N-oxide-κO)cobalt(II)] butanol monosolvate
http://scripts.iucr.org/cgi-bin/paper?pk2697
Reaction of CoBr2 with 2-methylpyridine N-oxide in n-butanol leads to the formation of the title compound, [CoBr2]2(2-methylpyridine N-oxide)4·n-butanol or [Co2Br4(C6H7NO)4]·C4H10O. The asymmetric unit of the title compound consists of one CoII cation as well as two bromide anions and two 2-methylpyridine N-oxide coligands in general positions and one n-butanol molecule that is disordered around a center of inversion. The CoII cations are fivefold coordinated by two bromide anions and one terminal as well as two bridging 2-methylpyridine N-oxide and linked by two symmetry-related μ-1,1(O,O) 2-methylpyridine N-oxide coligands into dinuclear units that are located on centers of inversion. In the crystal structure, the dinuclear units are also connected via pairs of C—H⋯Br hydrogen bonds into chains that elongate in the b-axis direction. The n-butanol molecules are located between the chains and are linked via O—H⋯Br hydrogen bonds each to one chain. Powder X-ray diffraction (PXRD) measurements reveal that a pure phase has been obtained. Measurements using thermogravimetry and differential thermoanalysis shows one mass loss up to 523 K, in which the n-butanol molecules are removed. PXRD measurements of the residue obtained after n-butanol removal shows that a completely different crystalline phase has been obtained and IR investigations indicate significant structural changes in the Co coordination.urn:issn:2056-9890Näther, C.Jess, I.text/htmlThe crystal structure of the title compound consists of dinuclear complexes, in which the CoII cations are fivefold coordinated and linked by centrosymmetric pairs of μ-1,1(O,O)-bridging 2-methylpyridine N-oxide coligands.doi:10.1107/S2056989023008228CRYSTAL STRUCTURE; SYNTHESIS; THERMOANALYTICAL INVESTIGATIONS; COBALT THIOCYANATE; 2-METHYLPYRIDINE N-OXIDE2023-10-03Synthesis, crystal structure and reactivity of bis(μ-2-methylpyridine N-oxide-κ2O:O)bis[dibromido(2-methylpyridine N-oxide-κO)cobalt(II)] butanol monosolvateReaction of CoBr2 with 2-methylpyridine N-oxide in n-butanol leads to the formation of the title compound, [CoBr2]2(2-methylpyridine N-oxide)4·n-butanol or [Co2Br4(C6H7NO)4]·C4H10O. The asymmetric unit of the title compound consists of one CoII cation as well as two bromide anions and two 2-methylpyridine N-oxide coligands in general positions and one n-butanol molecule that is disordered around a center of inversion. The CoII cations are fivefold coordinated by two bromide anions and one terminal as well as two bridging 2-methylpyridine N-oxide and linked by two symmetry-related μ-1,1(O,O) 2-methylpyridine N-oxide coligands into dinuclear units that are located on centers of inversion. In the crystal structure, the dinuclear units are also connected via pairs of C—H⋯Br hydrogen bonds into chains that elongate in the b-axis direction. The n-butanol molecules are located between the chains and are linked via O—H⋯Br hydrogen bonds each to one chain. Powder X-ray diffraction (PXRD) measurements reveal that a pure phase has been obtained. Measurements using thermogravimetry and differential thermoanalysis shows one mass loss up to 523 K, in which the n-butanol molecules are removed. PXRD measurements of the residue obtained after n-butanol removal shows that a completely different crystalline phase has been obtained and IR investigations indicate significant structural changes in the Co coordination.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-989011med@iucr.org79November 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-10-03Racemic cis-bis[bis(pyrimidin-2-yl)amine-κN]bis(dicyanamido-κN1)iron(II) dihydrate: synthesis, crystal structure and Hirshfeld surface analysis
http://scripts.iucr.org/cgi-bin/paper?hb8076
The title compound, [Fe(C2N3)2(C8H7N5)2]·2H2O, has been synthesized solvothermally and characterized by single-crystal X-ray diffraction. The octahedral iron coordination polyhedron contains two di(pyrimidin-2-yl)amine ligands coordinated in a bidentate fashion, and two monodentate dicyanimido ligands, each coordinated via a terminal N atom, with the latter in a cis orientation. The ligand configuration about the iron atom is chiral, although the compound crystallizes as a racemic mixture: the Fe—N distances (> 2.07 Å) are characteristic of high-spin iron(II). In the crystal, an extensive series of N—H⋯N, O—H⋯N and O—H⋯O hydrogen bonds links the independent molecular components into a three-dimensional framework. The H atoms of both water molecules are disordered. The structure also features some π–π and anion–π interactions. The intermolecular interactions were investigated by Hirshfeld surface analysis and two-dimensional fingerprint plots. Comparisons are made with some related compounds.urn:issn:2056-9890Saadallah, Y.Setifi, Z.Jelsch, C.Setifi, F.Al-Douh, M.H.Satour, A.Glidewell, C.text/htmlThe solvothermal synthesis, crystal structure and Hirshfeld surface analysis of a new iron(II) complex containing dicyanamido and di(pyrimidin-2-yl)amine ligands are reporteddoi:10.1107/S2056989023008186SOLVOTHERMAL SYNTHESIS; IRON COMPLEX; DICYANAMIDO LIGANDS; HYDROGEN BONDING; HIRSHFELD SURFACE ANALYSIS; CRYSTAL STRUCTURE2023-09-26Racemic cis-bis[bis(pyrimidin-2-yl)amine-κN]bis(dicyanamido-κN1)iron(II) dihydrate: synthesis, crystal structure and Hirshfeld surface analysisThe title compound, [Fe(C2N3)2(C8H7N5)2]·2H2O, has been synthesized solvothermally and characterized by single-crystal X-ray diffraction. The octahedral iron coordination polyhedron contains two di(pyrimidin-2-yl)amine ligands coordinated in a bidentate fashion, and two monodentate dicyanimido ligands, each coordinated via a terminal N atom, with the latter in a cis orientation. The ligand configuration about the iron atom is chiral, although the compound crystallizes as a racemic mixture: the Fe—N distances (> 2.07 Å) are characteristic of high-spin iron(II). In the crystal, an extensive series of N—H⋯N, O—H⋯N and O—H⋯O hydrogen bonds links the independent molecular components into a three-dimensional framework. The H atoms of both water molecules are disordered. The structure also features some π–π and anion–π interactions. The intermolecular interactions were investigated by Hirshfeld surface analysis and two-dimensional fingerprint plots. Comparisons are made with some related compounds.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext941med@iucr.org2056-98902056-989010https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsOctober 20232023-09-2693679Synthesis and crystal structure of bis(tert-butyl isocyanide-κC)[5,10,15,20-tetrakis(4-chlorophenyl)porphyrinato-κ4N]iron(II)
http://scripts.iucr.org/cgi-bin/paper?hb8075
In the title compound, [FeII(C44H24Cl4N4)(C5H9N)2] or [FeII(TClPP)(t-BuNC)2] [where TClPP and t-BuNC are 5,10,15,20-tetrakis(4-chlorophenyl)porphyrinate and tert-butyl isocyanide ligands, respectively], the metal ion lies on an inversion center and is octahedrally coordinated by the N atoms of the porphyrin ring in the equatorial plane and by carbon atoms of the trans t-BuNC ligands in the axial sites. The Fe—N bond length of 2.0074 (14) Å suggests a low-spin complex (S = 0). The crystal packing of the title compound is sustained by C—H⋯Cl, C—H⋯N and C__H⋯Cg (Cg = the centroid of a pyrrole ring of the TClPP porphyrinate) interactions, leading to a three-dimensional network. The Hirshfeld surface (HS) analysis indicates that 61.4% of the intermolecular interactions are from H⋯H contacts while other contributions are from C⋯H/H⋯C, O⋯H/H⋯O and N⋯H/H⋯N interactions, which comprise 21.3%, 13.3% and 3.6% of the HS, respectively.urn:issn:2056-9890Nasri, S.text/htmlMolecules of the title complex are centrosymmetric and the Fe—N bond lengths to the N atoms of the porphyrin ring indicate that the FeII atom is in the low-spin state.doi:10.1107/S2056989023008083CRYSTAL STRUCTURE; HIRSHFELD SURFACE ANALYSIS; IRON(II) PORPHYRIN COMPLEX; TERT BUTYL ISOCYANIDE2023-09-26Synthesis and crystal structure of bis(tert-butyl isocyanide-κC)[5,10,15,20-tetrakis(4-chlorophenyl)porphyrinato-κ4N]iron(II)In the title compound, [FeII(C44H24Cl4N4)(C5H9N)2] or [FeII(TClPP)(t-BuNC)2] [where TClPP and t-BuNC are 5,10,15,20-tetrakis(4-chlorophenyl)porphyrinate and tert-butyl isocyanide ligands, respectively], the metal ion lies on an inversion center and is octahedrally coordinated by the N atoms of the porphyrin ring in the equatorial plane and by carbon atoms of the trans t-BuNC ligands in the axial sites. The Fe—N bond length of 2.0074 (14) Å suggests a low-spin complex (S = 0). The crystal packing of the title compound is sustained by C—H⋯Cl, C—H⋯N and C__H⋯Cg (Cg = the centroid of a pyrrole ring of the TClPP porphyrinate) interactions, leading to a three-dimensional network. The Hirshfeld surface (HS) analysis indicates that 61.4% of the intermolecular interactions are from H⋯H contacts while other contributions are from C⋯H/H⋯C, O⋯H/H⋯O and N⋯H/H⋯N interactions, which comprise 21.3%, 13.3% and 3.6% of the HS, respectively.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-989010935med@iucr.org79October 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/9312023-09-26Synthesis, crystal structure, and Hirshfeld surface analysis of 3-ferrocenyl-1-(pyridin-2-yl)-1H-pyrazol-5-amine
http://scripts.iucr.org/cgi-bin/paper?wm5693
A key step towards utilizing polynuclear metal-based systems in magnetic device applications involves the careful design of ligands. This strategic planning aims to produce metal assemblies that exhibit some kind of `switch' mechanism. Towards this end, a ligand that incorporates a redox-active functional group (ferrocene) is reported. This communication presents the multi-step synthesis, characterization (1H and 13C NMR), and structural analysis (single-crystal X-ray diffraction and Hirshfeld surface analysis) of 3-ferrocenyl-1-(pyridin-2-yl)-1H-pyrazol-5-amine, [Fe(C5H5)(C13H11N4)]. Supramolecular features, including π–π stacking and hydrogen bonding are quantified, while a database search reveals the unique combination of molecular moieties, which offer future opportunities for studies to involve simultaneous Lewis acid and base coordination.urn:issn:2056-9890Joekar, D.Hiscock, L.K.Dawe, L.N.text/htmlThe multi-step synthesis, characterization, and structural examination (single-crystal X-ray diffraction and Hirshfeld surface analysis) of 3-ferrocenyl-1-(pyridin-2-yl)-1H-pyrazol-5-amine (C18H16FeN4), are reported. The supramolecular characteristics, including π–π stacking and hydrogen bonding, are discussed, and a database exploration highlights the distinctive combination of molecular components.doi:10.1107/S2056989023008101CRYSTAL STRUCTURE; AMINOPYRAZOLE; FERROCENE; HIRSHFELD SURFACE ANALYSIS2023-09-19Synthesis, crystal structure, and Hirshfeld surface analysis of 3-ferrocenyl-1-(pyridin-2-yl)-1H-pyrazol-5-amineA key step towards utilizing polynuclear metal-based systems in magnetic device applications involves the careful design of ligands. This strategic planning aims to produce metal assemblies that exhibit some kind of `switch' mechanism. Towards this end, a ligand that incorporates a redox-active functional group (ferrocene) is reported. This communication presents the multi-step synthesis, characterization (1H and 13C NMR), and structural analysis (single-crystal X-ray diffraction and Hirshfeld surface analysis) of 3-ferrocenyl-1-(pyridin-2-yl)-1H-pyrazol-5-amine, [Fe(C5H5)(C13H11N4)]. Supramolecular features, including π–π stacking and hydrogen bonding are quantified, while a database search reveals the unique combination of molecular moieties, which offer future opportunities for studies to involve simultaneous Lewis acid and base coordination.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextOctober 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-09-1979med@iucr.org2056-98902056-989010Synthesis and crystal structure of silicon pernitride SiN2 at 140 GPa
http://scripts.iucr.org/cgi-bin/paper?wm5694
Silicon pernitride, SiN2, was synthesized from the elements at 140 GPa in a laser-heated diamond anvil cell. Its crystal structure was solved and refined by means of synchrotron-based single-crystal X-ray diffraction data. The title compound crystallizes in the pyrite structure type (space group Pa\overline{3}, No. 205). The Si atom occupies a site with multiplicity 4 (Wyckoff letter b, site symmetry .\overline{3}.), while the N atom is located on a site with multiplicity 8 (Wyckoff letter c, site symmetry .3.). The crystal structure of SiN2 is comprised of slightly distorted [SiN6] octahedra interconnected with each other by sharing vertices. Crystal chemical analysis of bond lengths suggests that Si has a formal oxidation state of +IV, while nitrogen forms pernitride anions (N—N)4–.urn:issn:2056-9890Jurzick, P.L.Krach, G.Brüning, L.Schnick, W.Bykov, M.text/htmlSiN2 was synthesized from the elements at 140 GPa in a laser-heated diamond anvil cell. Crystal-structure determination (single-crystal synchrotron X-ray data) revealed that the title compound crystallizes in the pyrite structure type (space group Pa\overline{3}).doi:10.1107/S2056989023008058NITRIDES; PERNITRIDES; SILICON NITRIDES; HIGH PRESSURE; CRYSTAL STRUCTURE2023-09-19Synthesis and crystal structure of silicon pernitride SiN2 at 140 GPaSilicon pernitride, SiN2, was synthesized from the elements at 140 GPa in a laser-heated diamond anvil cell. Its crystal structure was solved and refined by means of synchrotron-based single-crystal X-ray diffraction data. The title compound crystallizes in the pyrite structure type (space group Pa\overline{3}, No. 205). The Si atom occupies a site with multiplicity 4 (Wyckoff letter b, site symmetry .\overline{3}.), while the N atom is located on a site with multiplicity 8 (Wyckoff letter c, site symmetry .3.). The crystal structure of SiN2 is comprised of slightly distorted [SiN6] octahedra interconnected with each other by sharing vertices. Crystal chemical analysis of bond lengths suggests that Si has a formal oxidation state of +IV, while nitrogen forms pernitride anions (N—N)4–.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext102056-98902056-9890med@iucr.org792023-09-19October 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communicationsSynthesis, crystal structure and Hirshfeld surface analysis of (2Z,2′E)-2,2′-(3-methoxy-3-phenylpropane-1,2-diylidene)bis(hydrazine-1-carbothioamide) dimethylformamide monosolvate
http://scripts.iucr.org/cgi-bin/paper?yz2041
The overall molecular configuration of the title compound, C12H16N6OS2·C3H7NO, is stabilized in the solid state by intramolecular C—H⋯N, C—H⋯O, N—H⋯N and N—H⋯O interactions, forming S(5) ring motifs. In the crystal, molecules are linked to each other and solvent dimethylformamide molecules by N—H⋯S, N—H⋯O, C—H⋯O and C—H⋯S hydrogen bonds, forming a three dimensional network. The phenyl ring of the title compound is disordered over two sites with an occupancy ratio of 0.57 (4):0.43 (4). A Hirshfeld surface analysis was performed to quantify the contributions of the different intermolecular interactions, indicating that the most important contributions to the crystal packing are from H⋯H (38.7%), S⋯H / H⋯S (24.0%), C⋯H / H⋯C (18.5%) and N⋯H / H⋯N (9.8%) interactions.urn:issn:2056-9890Guseinov, F.I.Knyazev, A.V.Shuvalova, E.V.Kobrakov, K.I.Samigullina, A.I.Atioğlu, Z.Akkurt, M.Bhattarai, A.text/htmlIn the crystal of the title compound, molecules are linked to each other and solvent dimethylformamide molecules by N—H⋯S, N—H⋯O, C—H⋯O and C—H⋯S hydrogen bonds, forming a three dimensional network.doi:10.1107/S2056989023007946CRYSTAL STRUCTURE; DISORDER; HYDROGEN BONDS; HIRSHFELD SURFACE ANALYSIS; [ALPHA]-CHLOROKETONE; CHLOROOXIRANE; BISTHIOSEMICARBAZONE2023-09-14Synthesis, crystal structure and Hirshfeld surface analysis of (2Z,2′E)-2,2′-(3-methoxy-3-phenylpropane-1,2-diylidene)bis(hydrazine-1-carbothioamide) dimethylformamide monosolvateThe overall molecular configuration of the title compound, C12H16N6OS2·C3H7NO, is stabilized in the solid state by intramolecular C—H⋯N, C—H⋯O, N—H⋯N and N—H⋯O interactions, forming S(5) ring motifs. In the crystal, molecules are linked to each other and solvent dimethylformamide molecules by N—H⋯S, N—H⋯O, C—H⋯O and C—H⋯S hydrogen bonds, forming a three dimensional network. The phenyl ring of the title compound is disordered over two sites with an occupancy ratio of 0.57 (4):0.43 (4). A Hirshfeld surface analysis was performed to quantify the contributions of the different intermolecular interactions, indicating that the most important contributions to the crystal packing are from H⋯H (38.7%), S⋯H / H⋯S (24.0%), C⋯H / H⋯C (18.5%) and N⋯H / H⋯N (9.8%) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-989010https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsOctober 20232023-09-1479Growth and characterization of a new inorganic metal–halide crystal structure, InPb2Cl5
http://scripts.iucr.org/cgi-bin/paper?pk2694
A new solid-state inorganic compound, indium dilead pentachloride, InPb2Cl5, was synthesized by melting InCl and PbCl2 in a vacuum-sealed quartz ampoule. The ampoule was heated to 793 K and then slowly cooled to room temperature to induce crystallization of InPb2Cl5. InPb2Cl5 crystallizes in the monoclinic crystal system adopting a space group of type P21/c, which is isostructural with other metal halides such as RbPb2Cl5, KPb2Cl5 and TlPb2Cl5. The bulk InPb2Cl5 exhibits a metallic black/grey colour, allowing it to be separated from white/yellow PbCl2 crystals. Due to the incongruent nature of the compound, the pure bulk InPb2Cl5 was not obtained. The black/grey InPb2Cl5 crystals were characterized by powder and single-crystal X-ray diffraction. InPbCl3 was also explored, however the growth was unsuccessful.urn:issn:2056-9890Lewis, M.P.Kandel, R.Schatte, G.Wang, P.L.text/htmlA new solid-state inorganic compound, InPb2Cl5, was synthesized by melting InCl and PbCl2 in a vacuum-sealed quartz ampoule. Bulk InPb2Cl5 was separated from PbCl2 and characterized by single-crystal X-ray diffraction.doi:10.1107/S2056989023007892CRYSTAL STRUCTURE; INORGANIC; INPB2CL5; SOLID-STATE2023-09-26Growth and characterization of a new inorganic metal–halide crystal structure, InPb2Cl5A new solid-state inorganic compound, indium dilead pentachloride, InPb2Cl5, was synthesized by melting InCl and PbCl2 in a vacuum-sealed quartz ampoule. The ampoule was heated to 793 K and then slowly cooled to room temperature to induce crystallization of InPb2Cl5. InPb2Cl5 crystallizes in the monoclinic crystal system adopting a space group of type P21/c, which is isostructural with other metal halides such as RbPb2Cl5, KPb2Cl5 and TlPb2Cl5. The bulk InPb2Cl5 exhibits a metallic black/grey colour, allowing it to be separated from white/yellow PbCl2 crystals. Due to the incongruent nature of the compound, the pure bulk InPb2Cl5 was not obtained. The black/grey InPb2Cl5 crystals were characterized by powder and single-crystal X-ray diffraction. InPbCl3 was also explored, however the growth was unsuccessful.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext102056-98902056-9890med@iucr.org945792023-09-26942https://creativecommons.org/licenses/by/4.0/research communicationsOctober 2023Acta Crystallographica Section E: Crystallographic CommunicationsCrystal structure and Hirshfeld surface analysis of 4-azido-2-(3,5-dimethylphenyl)-5-(4-nitrophenyl)-2H-1,2,3-triazole
http://scripts.iucr.org/cgi-bin/paper?zn2031
In the title compound, C16H13N7O2, the 3,5-dimethylphenyl and 4-nitrophenyl rings are inclined to the central 2H-1,2,3-triazole ring by 1.80 (7) and 1.79 (7)°, respectively, and to one another by 2.16 (7)°. In the crystal, the molecules are linked by C—H⋯N hydrogen bonds and π–π stacking interactions [centroid-to-centroid distances = 3.7295 (9) and 3.7971 (9) Å], forming ribbons along the b-axis direction. These ribbons are connected to each other by weak van der Waals interactions and the stability of the crystal structure is ensured. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions to the crystal packing are from H⋯H (31.5%), N⋯H/H⋯N (19.2%), O⋯H/H⋯O (14.5%), N⋯C/C⋯C (10.9%) and C⋯H/H⋯C (10.2%) contacts.urn:issn:2056-9890Maharramov, A.Shikhaliyev, N.Q.Abdullayeva, A.Atakishiyeva, G.T.Niyazova, A.Khrustalev, V.N.Gahramanova, S.I.Atioğlu, Z.Akkurt, M.Bhattarai, A.text/htmlIn the crystal, the molecules are connected by C—H⋯N hydrogen bonds and π–π stacking interactions, forming ribbons along the b-axis direction. Weak van der Waals interactions link these ribbons together, consolidating the crystal structure.doi:10.1107/S2056989023007855CRYSTAL STRUCTURE; HYDROGEN BONDS; AZIDO GROUP; 2H-1,2,3-TRIAZOLE; HIRSHFELD SURFACE ANALYSIS2023-09-14Crystal structure and Hirshfeld surface analysis of 4-azido-2-(3,5-dimethylphenyl)-5-(4-nitrophenyl)-2H-1,2,3-triazoleIn the title compound, C16H13N7O2, the 3,5-dimethylphenyl and 4-nitrophenyl rings are inclined to the central 2H-1,2,3-triazole ring by 1.80 (7) and 1.79 (7)°, respectively, and to one another by 2.16 (7)°. In the crystal, the molecules are linked by C—H⋯N hydrogen bonds and π–π stacking interactions [centroid-to-centroid distances = 3.7295 (9) and 3.7971 (9) Å], forming ribbons along the b-axis direction. These ribbons are connected to each other by weak van der Waals interactions and the stability of the crystal structure is ensured. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions to the crystal packing are from H⋯H (31.5%), N⋯H/H⋯N (19.2%), O⋯H/H⋯O (14.5%), N⋯C/C⋯C (10.9%) and C⋯H/H⋯C (10.2%) contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextOctober 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/2023-09-1479med@iucr.org2056-98902056-9890102,6-Dibromo-3,4,5-trimethoxybenzoic acid
http://scripts.iucr.org/cgi-bin/paper?jy2033
The title compound, 2,6-dibromo-3,4,5-trimethoxybenzoic acid (DBrTMBA), C10H10Br2O5, was obtained by bromination and transhalogenation of 2-iodo-3,4,5-trimethoxybenzoic acid with KBrO3. Like the previously reported 2,6-diiodo-3,4,5-trimethoxybenzoic acid (DITMBA), the structure of the title compound features a catemeric arrangement of DBrTMBA molecules along an endless chain of carboxylic H–carbonyl interactions. A short carbonyl–phenyl contact hints at a possible lone pair(O)–π-hole interaction further stabilizing the chain-like structure over a dimeric arrangement of the carboxylic acid.urn:issn:2056-9890Meurer, F.Dimova, T.Bodensteiner, M.Kolev, I.text/htmlThe previously unknown crystal structure of 2,6-dibromo-3,4,5-trimethoxybenzoic acid was determined employing state-of-the-art Hirshfeld atom refinement and the crystal packing was analysed using Hirshfeld surface analysis.doi:10.1107/S2056989023007831CRYSTAL STRUCTURE; HIRSHFELD ATOM REFINEMENT (HAR); NOSPHERA2; SUBSTITUTED TRIMETHOXYBENZOIC ACID2023-09-142,6-Dibromo-3,4,5-trimethoxybenzoic acidThe title compound, 2,6-dibromo-3,4,5-trimethoxybenzoic acid (DBrTMBA), C10H10Br2O5, was obtained by bromination and transhalogenation of 2-iodo-3,4,5-trimethoxybenzoic acid with KBrO3. Like the previously reported 2,6-diiodo-3,4,5-trimethoxybenzoic acid (DITMBA), the structure of the title compound features a catemeric arrangement of DBrTMBA molecules along an endless chain of carboxylic H–carbonyl interactions. A short carbonyl–phenyl contact hints at a possible lone pair(O)–π-hole interaction further stabilizing the chain-like structure over a dimeric arrangement of the carboxylic acid.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext102056-98902056-9890med@iucr.org792023-09-14Acta Crystallographica Section E: Crystallographic CommunicationsOctober 2023https://creativecommons.org/licenses/by/4.0/research communicationsCrystal structure and Hirshfeld surface analysis of 3-ethoxy-1-ethyl-6-nitroquinoxalin-2(1H)-one
http://scripts.iucr.org/cgi-bin/paper?hb8072
The asymmetric unit of the title compound, C12H13N3O4, consists of two molecules differing to a small degree in their conformations. In the crystal, layers of molecules are connected by weak C—H⋯O hydrogen bonds and slipped π-stacking interactions. These layers lie parallel to (10\overline{1}) and are stacked along the normal to that plane. Hirshfeld surface analysis indicates that the most important contributions for the crystal packing arise from H⋯H (43.5%) and H⋯O/O⋯H (30.8%) contacts. The density functional theory (DFT) optimized structure of the title compound at the B3LYP/ 6–311 G(d,p) level agrees well with the experimentally determined molecular structure in the solid state.urn:issn:2056-9890Yousra, S.El Ghayati, L.Hökelek, T.Ouazzani Chahdi, F.Mague, J.T.Kandri Rodi, Y.Sebbar, N.K.text/htmlThe asymmetric unit of the title compound consists of two molecules differing to a small degree in their conformations. In the crystal, layers of molecules are connected by weak C—H⋯O hydrogen bonds and slipped π-stacking interactions.doi:10.1107/S2056989023007624CRYSTAL STRUCTURE; HYDROGEN BOND; [PI]-STACKING; QUINOXALINE2023-09-08Crystal structure and Hirshfeld surface analysis of 3-ethoxy-1-ethyl-6-nitroquinoxalin-2(1H)-oneThe asymmetric unit of the title compound, C12H13N3O4, consists of two molecules differing to a small degree in their conformations. In the crystal, layers of molecules are connected by weak C—H⋯O hydrogen bonds and slipped π-stacking interactions. These layers lie parallel to (10\overline{1}) and are stacked along the normal to that plane. Hirshfeld surface analysis indicates that the most important contributions for the crystal packing arise from H⋯H (43.5%) and H⋯O/O⋯H (30.8%) contacts. The density functional theory (DFT) optimized structure of the title compound at the B3LYP/ 6–311 G(d,p) level agrees well with the experimentally determined molecular structure in the solid state.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2023-09-08Acta Crystallographica Section E: Crystallographic CommunicationsOctober 2023https://creativecommons.org/licenses/by/4.0/research communications79med@iucr.org102056-98902056-9890Crystal structure, Hirshfeld surface analysis, interaction energy and energy framework calculations, as well as density functional theory (DFT) computation, of methyl 2-oxo-1-(prop-2-ynyl)-1,2-dihydroquinoline-4-carboxylate
http://scripts.iucr.org/cgi-bin/paper?wm5688
In the title molecule, C14H11NO3, the dihydroquinoline core deviates slightly from planarity, indicated by the dihedral angle of 1.07 (3)° between the two six-membered rings. In the crystal, layers of molecules almost parallel to the bc plane are formed by C—H⋯O hydrogen bonds. These are joined by π–π stacking interactions. A Hirshfeld surface analysis revealed that the most important contributions to the crystal packing are from H⋯H (36.0%), H⋯C/C⋯H (28.9%) and H⋯O/O⋯H (23.5%) interactions. The evaluation of the electrostatic, dispersion and total energy frameworks indicates that the stabilization is dominated by the dispersion energy contribution. Moreover, the molecular structure optimized by density functional theory (DFT) at the B3LYP/6-311G(d,p) level is compared with the experimentally determined molecular structure in the solid state. The HOMO–LUMO behaviour was elucidated to determine the energy gap.urn:issn:2056-9890El-Mrabet, A.Haoudi, A.Dalbouha, S.Skalli, M.K.Hökelek, T.Capet, F.Kandri Rodi, Y.Mazzah, A.Sebbar, N.K.text/htmlIn the crystal of the title compound, C—H⋯O hydrogen bonds link the molecules, enclosing R_{2}^{2}(10) and R_{2}^{2}(16) ring motifs, into layers almost parallel to the bc plane. The layers are further connected by π–π stacking interactions.doi:10.1107/S2056989023007557CRYSTAL STRUCTURE; [PI]-STACKING; C-H...O HYDROGEN BONDS; DIHYDROQUINOLINE2023-09-08Crystal structure, Hirshfeld surface analysis, interaction energy and energy framework calculations, as well as density functional theory (DFT) computation, of methyl 2-oxo-1-(prop-2-ynyl)-1,2-dihydroquinoline-4-carboxylateIn the title molecule, C14H11NO3, the dihydroquinoline core deviates slightly from planarity, indicated by the dihedral angle of 1.07 (3)° between the two six-membered rings. In the crystal, layers of molecules almost parallel to the bc plane are formed by C—H⋯O hydrogen bonds. These are joined by π–π stacking interactions. A Hirshfeld surface analysis revealed that the most important contributions to the crystal packing are from H⋯H (36.0%), H⋯C/C⋯H (28.9%) and H⋯O/O⋯H (23.5%) interactions. The evaluation of the electrostatic, dispersion and total energy frameworks indicates that the stabilization is dominated by the dispersion energy contribution. Moreover, the molecular structure optimized by density functional theory (DFT) at the B3LYP/6-311G(d,p) level is compared with the experimentally determined molecular structure in the solid state. The HOMO–LUMO behaviour was elucidated to determine the energy gap.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-989010med@iucr.org79Acta Crystallographica Section E: Crystallographic CommunicationsOctober 2023research communicationshttps://creativecommons.org/licenses/by/4.0/2023-09-08Synthesis, crystal structure, Hirshfeld surface analysis, DFT and NBO study of ethyl 1-(4-fluorophenyl)-4-[(4-fluorophenyl)amino]-2,6-diphenyl-1,2,5,6-tetrahydropyridine-3-carboxylate
http://scripts.iucr.org/cgi-bin/paper?hb8074
The title compound, C32H28F2N2O2, a highly functionalized tetrahydropyridine, was synthesized by a one-pot multi-component reaction of 4-fluoroaniline, ethyl acetoacetate and benzaldehyde at room temperature using sodium lauryl sulfate as a catalyst. The compound crystallizes with two molecules in the asymmetric unit. The tetrahydropyridine ring adopts a distorted boat conformation in both molecules and the dihedral angles between the planes of the fluoro-substituted rings are 77.1 (6) and 77.3 (6)°. The amino group and carbonyl O atom are involved in an intramolecular N—H⋯O hydrogen bond, thereby generating an S(6) ring motif. In the crystal, molecules are linked by C—H⋯F hydrogen bonds forming a three-dimensional network and C—H⋯π interactions. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions to the crystal packing are from H⋯H (47.9%), C⋯H/H⋯C (30.7%) and F⋯H/H⋯F (12.4%) contacts. The optimized structure calculated using density functional theory (DFT) at the B3LYP/6-311+G(2d,p) level is compared with the experimentally determined molecular structure in the solid state. The HOMO–LUMO behaviour was used to determine the energy gap and the Natural Bond Orbital (NBO) analysis was done to study donor–acceptor interconnections.urn:issn:2056-9890Bansal, R.Butcher, R.J.Gupta, S.K.text/htmlThe one-pot synthesis, crystal structure, Hirshfeld surface analysis, DFT and NBO study of a highly functionalized tetrahydropyridine are reported.doi:10.1107/S205698902300748XFUNCTIONALIZED TETRAHYDROPYRIDINE; CRYSTAL STRUCTURE; HIRSHFELD SURFACE ANALYSIS; TWO-DIMENSIONAL FINGERPRINT PLOT; DFT; NBO2023-09-08Synthesis, crystal structure, Hirshfeld surface analysis, DFT and NBO study of ethyl 1-(4-fluorophenyl)-4-[(4-fluorophenyl)amino]-2,6-diphenyl-1,2,5,6-tetrahydropyridine-3-carboxylateThe title compound, C32H28F2N2O2, a highly functionalized tetrahydropyridine, was synthesized by a one-pot multi-component reaction of 4-fluoroaniline, ethyl acetoacetate and benzaldehyde at room temperature using sodium lauryl sulfate as a catalyst. The compound crystallizes with two molecules in the asymmetric unit. The tetrahydropyridine ring adopts a distorted boat conformation in both molecules and the dihedral angles between the planes of the fluoro-substituted rings are 77.1 (6) and 77.3 (6)°. The amino group and carbonyl O atom are involved in an intramolecular N—H⋯O hydrogen bond, thereby generating an S(6) ring motif. In the crystal, molecules are linked by C—H⋯F hydrogen bonds forming a three-dimensional network and C—H⋯π interactions. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions to the crystal packing are from H⋯H (47.9%), C⋯H/H⋯C (30.7%) and F⋯H/H⋯F (12.4%) contacts. The optimized structure calculated using density functional theory (DFT) at the B3LYP/6-311+G(2d,p) level is compared with the experimentally determined molecular structure in the solid state. The HOMO–LUMO behaviour was used to determine the energy gap and the Natural Bond Orbital (NBO) analysis was done to study donor–acceptor interconnections.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsOctober 20232023-09-082056-98902056-989010med@iucr.orgCrystal structure and Hirshfeld surface analysis of 8-azaniumylquinolinium tetrachloridozincate(II)
http://scripts.iucr.org/cgi-bin/paper?wm5692
The reaction of 8-aminoquinoline, zinc chloride and hydrochloric acid in ethanol yielded the title salt, (C9H10N2)[ZnCl4], which consists of a planar 8-azaniumylquinolinium dication and a tetrahedral tetrachlorozincate dianion. The 8-aminoquinoline moiety is protonated at both the amino and the ring N atoms. In the crystal, the cations and anions are connected by intermolecular N—H⋯Cl and C—H⋯Cl hydrogen bonds, forming sheets parallel to (001). Adjacent sheets are linked through π–π interactions involving the pyridine and arene rings of the 8-azaniumylquinolinium dication. Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from H⋯Cl (48.1%), H⋯H (19.9%), H⋯C/C⋯H (14.3%) (involving the cations) and H⋯Cl (82.6%) (involving the anions) interactions.urn:issn:2056-9890Umirova, G.A.Turaev, K.K.Alimnazarov, B.K.Kasimov, S.A.Djalilov, A.T.Ibragimov, B.T.Ashurov, J.M.text/htmlThe organic–inorganic hybride salt (C9H10N2)[ZnCl4] consists of a planar 8-azaniumylquinolinium dication and a tetrahedral tetrachloridozincate(II) dianion, held together by N—H⋯Cl and C—H⋯Cl hydrogen bonds, and π—π interactions.doi:10.1107/S20569890230074668-AMINOQUINOLINE; INTERMOLECULAR INTERACTIONS; CRYSTAL STRUCTURE; HYDROGEN BONDING; [PI]-[PI] STACKING; HIRSHFELD SURFACE2023-08-30Crystal structure and Hirshfeld surface analysis of 8-azaniumylquinolinium tetrachloridozincate(II)The reaction of 8-aminoquinoline, zinc chloride and hydrochloric acid in ethanol yielded the title salt, (C9H10N2)[ZnCl4], which consists of a planar 8-azaniumylquinolinium dication and a tetrahedral tetrachlorozincate dianion. The 8-aminoquinoline moiety is protonated at both the amino and the ring N atoms. In the crystal, the cations and anions are connected by intermolecular N—H⋯Cl and C—H⋯Cl hydrogen bonds, forming sheets parallel to (001). Adjacent sheets are linked through π–π interactions involving the pyridine and arene rings of the 8-azaniumylquinolinium dication. Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from H⋯Cl (48.1%), H⋯H (19.9%), H⋯C/C⋯H (14.3%) (involving the cations) and H⋯Cl (82.6%) (involving the anions) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org92056-98902056-98902023-08-30research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsAugust 202379Synthesis, structure and Hirshfeld surface analysis of a coordination compound of cadmium acetate with 2-aminobenzoxazole
http://scripts.iucr.org/cgi-bin/paper?jy2035
A first coordination compound of 2-aminobenzoxazole (2AB), namely, bis(2-aminobenzoxazole-κN3)bis(acetato-κ2O,O′)cadmium(II), [Cd(CH3COO)2(2AB)2], has been synthesized from ethanol solutions of Cd(CH3(COO)2 and 2AB. In the monoclinic crystals with the space group C21/c, the cadmium ions coordinate two neutral 2AB molecules in a monodentate fashion through the oxazole N atom, while two acetate ligands are coordinated through the O atoms in a bidentate manner. The coordination polyhedron of the central ion is substantially distorted octahedral. There are two relatively strong intramolecular hydrogen bonds in the complex molecule. Additionally, two intermolecular hydrogen bonds associate complex molecules into columns running in the [1\overline{1}0] and [110] directions. The Hirshfeld surface analysis shows that 45.7% of the intermolecular interactions are from H⋯H contacts, 24.7% are from O⋯H/H⋯O contacts and 18.8% are from C⋯H/H⋯C contacts, while other contributions are from N⋯H/H⋯N and O⋯O contacts.urn:issn:2056-9890Razzoqova, S.Ibragimov, A.Torambetov, B.Kadirova, S.Holczbauer, T.Ashurov, J.Ibragimov, B.text/htmlThe molecular and crystal structures of a cadmium acetate coordination compound with 2-aminobenzoxazole were studied, and the Hirshfeld surfaces and fingerprint plots were generated to investigate various intermolecular interactions.doi:10.1107/S2056989023007399CRYSTAL STRUCTURE; MOLECULAR STRUCTURE; CADMIUM COMPLEX; 2-AMINOBENZOXAZOLE; HIRSHFELD SURFACE ANALYSIS2023-08-30Synthesis, structure and Hirshfeld surface analysis of a coordination compound of cadmium acetate with 2-aminobenzoxazoleA first coordination compound of 2-aminobenzoxazole (2AB), namely, bis(2-aminobenzoxazole-κN3)bis(acetato-κ2O,O′)cadmium(II), [Cd(CH3COO)2(2AB)2], has been synthesized from ethanol solutions of Cd(CH3(COO)2 and 2AB. In the monoclinic crystals with the space group C21/c, the cadmium ions coordinate two neutral 2AB molecules in a monodentate fashion through the oxazole N atom, while two acetate ligands are coordinated through the O atoms in a bidentate manner. The coordination polyhedron of the central ion is substantially distorted octahedral. There are two relatively strong intramolecular hydrogen bonds in the complex molecule. Additionally, two intermolecular hydrogen bonds associate complex molecules into columns running in the [1\overline{1}0] and [110] directions. The Hirshfeld surface analysis shows that 45.7% of the intermolecular interactions are from H⋯H contacts, 24.7% are from O⋯H/H⋯O contacts and 18.8% are from C⋯H/H⋯C contacts, while other contributions are from N⋯H/H⋯N and O⋯O contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98909med@iucr.org79https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsAugust 20232023-08-30Crystal structure and Hirshfeld surface analysis of (2E)-1-(4-bromophenyl)-3-(2-methylphenyl)prop-2-en-1-one
http://scripts.iucr.org/cgi-bin/paper?tx2073
In the title compound, C16H13BrO, the planes of the aromatic rings are inclined at an angle of 23.49 (15)°, and the configuration about the C=C bond is E. In the crystal, the molecules are linked into chains by weak C—H⋯O interactions along the b axis. Successive chains form a zigzag structure along the c axis, and these chains are connected to each other by face-to-face π–π stacking interactions along the a axis. These layers, parallel to the (001) plane, are linked by van der Waals interactions, thus consolidating the crystal structure. Hirshfeld surface analysis showed that the most significant contacts in the structure are H⋯H (43.1%), C⋯H/H⋯C (17.4%), Br⋯H/H⋯Br (14.9%), C⋯C (11.9%) and O⋯H/H⋯O (9.8%).urn:issn:2056-9890Akkurt, M.Naghiyev, F.N.Khrustalev, V.N.Asadov, K.A.Khalilov, A.N.Bhattarai, A.Mamedov, İ.G.text/htmlIn the crystal of (2E)-1-(4-bromophenyl)-3-(2-methylphenyl)prop-2-en-1-one, the molecules are linked into chains by weak C—H⋯O interactions along the b axis. Successive chains form a zigzag structure along the c axis, and these chains are connected to each other by face-to-face π–π stacking interactions along the a axis, forming layers parallel to the (001) plane. The crystal structure maintains its stability via van der Waals interactions between the layers.doi:10.1107/S2056989023007387CRYSTAL STRUCTURE; E CONFIGURATION; WEAK C-H...O INTERACTIONS; FACE-TO-FACE [PI]-[PI] STACKING INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-08-30Crystal structure and Hirshfeld surface analysis of (2E)-1-(4-bromophenyl)-3-(2-methylphenyl)prop-2-en-1-oneIn the title compound, C16H13BrO, the planes of the aromatic rings are inclined at an angle of 23.49 (15)°, and the configuration about the C=C bond is E. In the crystal, the molecules are linked into chains by weak C—H⋯O interactions along the b axis. Successive chains form a zigzag structure along the c axis, and these chains are connected to each other by face-to-face π–π stacking interactions along the a axis. These layers, parallel to the (001) plane, are linked by van der Waals interactions, thus consolidating the crystal structure. Hirshfeld surface analysis showed that the most significant contacts in the structure are H⋯H (43.1%), C⋯H/H⋯C (17.4%), Br⋯H/H⋯Br (14.9%), C⋯C (11.9%) and O⋯H/H⋯O (9.8%).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org92056-98902056-98902023-08-30Acta Crystallographica Section E: Crystallographic CommunicationsAugust 2023https://creativecommons.org/licenses/by/4.0/research communications79Crystal structure of the nucleoside 2′-deoxyguanosine dimethyl sulfoxide disolvate
http://scripts.iucr.org/cgi-bin/paper?zv2028
The title compound, C10H13N5O4·2C2H6OS, which is of interest with respect to its biological activity, at 183 K has orthorhombic (P212121) crystal symmetry. The structure displays a network of intermolecular N—H⋯N, N—H⋯O and O—H⋯O hydrogen bonds. 2′-Deoxyguanosine molecules are linked to each other and to the two dimethyl sulfoxide solvent molecules by hydrogen bonding.urn:issn:2056-9890Spingler, B.text/htmlThe first high-quality crystal structure of unmodified 2′-deoxyguanosine is reported. The isolated crystals are the dimethyl sulfoxide disolvate.doi:10.1107/S2056989023007405CRYSTAL STRUCTURE; NUCLEOSIDE; GUANINE; GUANOSINE; PURINE2023-08-30Crystal structure of the nucleoside 2′-deoxyguanosine dimethyl sulfoxide disolvateThe title compound, C10H13N5O4·2C2H6OS, which is of interest with respect to its biological activity, at 183 K has orthorhombic (P212121) crystal symmetry. The structure displays a network of intermolecular N—H⋯N, N—H⋯O and O—H⋯O hydrogen bonds. 2′-Deoxyguanosine molecules are linked to each other and to the two dimethyl sulfoxide solvent molecules by hydrogen bonding.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-98909research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsAugust 20232023-08-3079Synthesis, characterization and crystal structure of methyl 2-(2-oxo-2H-chromen-4-ylamino)benzoate
http://scripts.iucr.org/cgi-bin/paper?mw2198
Methyl 2-(2-oxo-2H-chromen-4-ylamino)benzoate, C17H13NO4 (1), was prepared by condensation between 4-hydroxycoumarin and methyl 2-aminobenzoate. It crystallizes in the orthorhombic space group Pca21 at 300 K. The molecule of compound 1 consists of the 2H-chromen-2-one part connected by an amine moiety (–NH–) to the methyl benzoate ring. The supramolecular array is formed by hydrogen bonds between the aromatic ring and the O atoms of the lactone and ester portions. The structural details match the spectroscopic data acquired from NMR and IR spectroscopy.urn:issn:2056-9890Hollauer, H.V.P.Vilas Novas, R.C.Guedes, G.P.Buarque, C.D.Escobar, L.B.L.text/htmlA new coumarin derivative, methyl 2-(2-oxo-2H-chromen-4-ylamino)benzoate, has been synthesized and characterized.doi:10.1107/S2056989023007351CRYSTAL STRUCTURE; COUMARIN; BENZOATE; ESTER2023-08-29Synthesis, characterization and crystal structure of methyl 2-(2-oxo-2H-chromen-4-ylamino)benzoateMethyl 2-(2-oxo-2H-chromen-4-ylamino)benzoate, C17H13NO4 (1), was prepared by condensation between 4-hydroxycoumarin and methyl 2-aminobenzoate. It crystallizes in the orthorhombic space group Pca21 at 300 K. The molecule of compound 1 consists of the 2H-chromen-2-one part connected by an amine moiety (–NH–) to the methyl benzoate ring. The supramolecular array is formed by hydrogen bonds between the aromatic ring and the O atoms of the lactone and ester portions. The structural details match the spectroscopic data acquired from NMR and IR spectroscopy.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext92056-98902056-9890med@iucr.org792023-08-29Acta Crystallographica Section E: Crystallographic CommunicationsAugust 2023https://creativecommons.org/licenses/by/4.0/research communicationsSynthesis, crystal structure and Hirshfeld surface analysis of 3-(4-fluorophenyl)-2-formyl-7-methylimidazo[1,2-a]pyridin-1-ium chloride monohydrate
http://scripts.iucr.org/cgi-bin/paper?jy2034
In the title salt, C15H12FN2O+·Cl−·H2O, the imidazo[1,2-a]pyridin-1-ium ring system of the cation is almostly planar [maximum deviaition = −0.047 (2) Å for the ring C atom with the attached arene ring] and forms a dihedral angle of 61.81 (6)° with the plane of the fluorophenyl ring. In the crystal, water molecules form an R24(8) motif parallel to the (100) plane by bonding with the chloride ions via O—H⋯Cl hydrogen bonds. The cations are connected along the b axis via N—H⋯O hydrogen bonds involving the O atoms of water molecules, and C—H⋯O, C—H⋯Cl and π–π interactions [centroid-to-centroid distance = 3.6195 (8) Å] form layers parallel to the (100) plane. Furthermore, these layers are connected via π–π interactions [centroid-to-centroid distance = 3.8051 (9) Å] that further consolidate the crystal structure.urn:issn:2056-9890Guseinov, F.I.Ovsyannikov, V.O.Sokolovskiy, P.V.Sebyakin, Y.L.Samigullina, A.I.Akkurt, M.Çelikesir, S.T.Bhattarai, A.text/htmlIn the salt 3-(4-fluorophenyl)-2-formyl-7-methylimidazo[1,2-a]pyridin-1-ium chloride monohydrate, water molecules form an R_{2}^{4}(8) motif parallel to the (100) plane by bonding with the chloride ions via O—H⋯Cl hydrogen bonds. The cations are connected along the b axis via N—H⋯O hydrogen bonds involving the O atoms of water molecules.doi:10.1107/S2056989023007272CRYSTAL STRUCTURE; IMIDAZO[1,2-A]PYRIDIN-1-IUM; HYDROGEN BONDS; [PI]-[PI] INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-09-12Synthesis, crystal structure and Hirshfeld surface analysis of 3-(4-fluorophenyl)-2-formyl-7-methylimidazo[1,2-a]pyridin-1-ium chloride monohydrateIn the title salt, C15H12FN2O+·Cl−·H2O, the imidazo[1,2-a]pyridin-1-ium ring system of the cation is almostly planar [maximum deviaition = −0.047 (2) Å for the ring C atom with the attached arene ring] and forms a dihedral angle of 61.81 (6)° with the plane of the fluorophenyl ring. In the crystal, water molecules form an R24(8) motif parallel to the (100) plane by bonding with the chloride ions via O—H⋯Cl hydrogen bonds. The cations are connected along the b axis via N—H⋯O hydrogen bonds involving the O atoms of water molecules, and C—H⋯O, C—H⋯Cl and π–π interactions [centroid-to-centroid distance = 3.6195 (8) Å] form layers parallel to the (100) plane. Furthermore, these layers are connected via π–π interactions [centroid-to-centroid distance = 3.8051 (9) Å] that further consolidate the crystal structure.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-09-12https://creativecommons.org/licenses/by/4.0/research communicationsOctober 2023Acta Crystallographica Section E: Crystallographic Communications102056-98902056-9890med@iucr.orgSpectroscopic, crystallographic, and Hirshfeld surface characterization of nine-membered-ring-containing 9-methoxy-3,4,5,6-tetrahydro-1H-benzo[b]azonine-2,7-dione and its parent tetrahydrocarbazole
http://scripts.iucr.org/cgi-bin/paper?dx2054
9-Methoxy-3,4,5,6-tetrahydro-1H-benzo[b]azonine-2,7-dione, C13H15NO3, (I), and 6-methoxy-1,2,3,4-tetrahydrocarbazole, C13H15NO, (II), represent the structures of a benzoazonine that contains a nine-membered ring and its parent tetrahydrocarbazole. The molecules of (I) pack together via strong amide N—H⋯O hydrogen bonding and weak C—H⋯O interactions, whereas the parent tetrahydrocarbazole (II) packs with C/N—H⋯π interactions, as visualized by Hirshfeld surface characterization.urn:issn:2056-9890Flores, M.J.Mai, B.Tanski, J.M.text/html9-Methoxy-3,4,5,6-tetrahydro-1H-benzo[b]azonine-2,7-dione and 6-methoxy-1,2,3,4-tetrahydrocarbazole represent the structures of a benzoazonine that contains a nine-membered ring and its parent tetrahydrocarbazole. The molecules of the former pack together via strong amide N—H⋯O hydrogen bonding and weak C—H⋯O interactions, whereas the parent tetrahydrocarbazole packs with C/N—H⋯π interactions, as visualized by Hirshfeld surface characterization.doi:10.1107/S2056989023007259CRYSTAL STRUCTURE; TETRAHYDROCARBAZOLE; BENZO[B]AZONINE; NINE-MEMBERED RING; HYDROGEN BOND2023-08-23Spectroscopic, crystallographic, and Hirshfeld surface characterization of nine-membered-ring-containing 9-methoxy-3,4,5,6-tetrahydro-1H-benzo[b]azonine-2,7-dione and its parent tetrahydrocarbazole9-Methoxy-3,4,5,6-tetrahydro-1H-benzo[b]azonine-2,7-dione, C13H15NO3, (I), and 6-methoxy-1,2,3,4-tetrahydrocarbazole, C13H15NO, (II), represent the structures of a benzoazonine that contains a nine-membered ring and its parent tetrahydrocarbazole. The molecules of (I) pack together via strong amide N—H⋯O hydrogen bonding and weak C—H⋯O interactions, whereas the parent tetrahydrocarbazole (II) packs with C/N—H⋯π interactions, as visualized by Hirshfeld surface characterization.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-98909Acta Crystallographica Section E: Crystallographic CommunicationsAugust 2023https://creativecommons.org/licenses/by/4.0/research communications2023-08-2379Crystal structure and Hirshfeld surface analysis of 1-(2-amino-4-methyl-1,3-thiazol-5-yl)ethan-1-one
http://scripts.iucr.org/cgi-bin/paper?vm2288
In the title compound, C6H8N2OS, all atoms except for the methyl H atoms are coplanar, with a maximum deviation of 0.026 (4) Å. In the crystal, pairs of molecules are linked by N—H⋯N hydrogen bonds, forming R22(8) ring motifs. Dimers are connected by N—H⋯O hydrogen bonds, forming layers parallel to the (102) plane. Consolidating the molecular packing, these layers are connected by C—H⋯π interactions between the center of the 1,3-thiazole ring and the H atom of the methyl group attached to it, as well as C=O⋯π interactions between the center of the 1,3-thiazole ring and the O atom of the carboxyl group. According to a Hirshfeld surface study, H⋯H (37.6%), O⋯H/H⋯O (16.8%), S⋯H/H⋯S (15.4%), N⋯H/H⋯N (13.0%) and C⋯H/H⋯C (7.6%) interactions are the most significant contributors to the crystal packing.urn:issn:2056-9890Huseynov, E.Z.Akkurt, M.Brito, I.Bhattarai, A.Rzayev, R.M.Asadov, K.A.Maharramov, A.M.text/htmlIn the crystal, pairs of molecules are linked by N—H⋯N hydrogen bonds, forming R_{2}^{2}(8) ring motifs. Dimers are connected by N—H⋯O hydrogen bonds, forming layers parallel to the (102) plane. These layers are connected by C—H⋯π and C=O⋯π interactions, consolidating the molecular packing.doi:10.1107/S2056989023007181CRYSTAL STRUCTURE; THIAZOLE DERIVATIVES; HYDROGEN BONDS; DIMERS; HIRSHFELD SURFACE ANALYSIS2023-09-08Crystal structure and Hirshfeld surface analysis of 1-(2-amino-4-methyl-1,3-thiazol-5-yl)ethan-1-oneIn the title compound, C6H8N2OS, all atoms except for the methyl H atoms are coplanar, with a maximum deviation of 0.026 (4) Å. In the crystal, pairs of molecules are linked by N—H⋯N hydrogen bonds, forming R22(8) ring motifs. Dimers are connected by N—H⋯O hydrogen bonds, forming layers parallel to the (102) plane. Consolidating the molecular packing, these layers are connected by C—H⋯π interactions between the center of the 1,3-thiazole ring and the H atom of the methyl group attached to it, as well as C=O⋯π interactions between the center of the 1,3-thiazole ring and the O atom of the carboxyl group. According to a Hirshfeld surface study, H⋯H (37.6%), O⋯H/H⋯O (16.8%), S⋯H/H⋯S (15.4%), N⋯H/H⋯N (13.0%) and C⋯H/H⋯C (7.6%) interactions are the most significant contributors to the crystal packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-989010med@iucr.org79October 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-09-08Crystal structure studies and Hirshfeld surface analysis of 4-(dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate at 90 K
http://scripts.iucr.org/cgi-bin/paper?vm2289
The crystal structure and a Hirshfeld surface analysis of the substituted anilinium salt 4-(dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate, C8H14N2O+·2Cl−·H2O, at low temperature (90 K) are presented. The organic cation is essentially planar: the r.m.s. deviation of its non-hydrogen atoms (aside from the two methyl groups) is 0.0045 Å. The methyl carbons are 1.3125 (12) Å and 1.1278 (12) Å either side of the mean plane. The crystal packing involves extensive hydrogen bonding of types O—H⋯Cl, N—H⋯Cl, N—H⋯OW, and OW—HW⋯Cl (where W = water), which arrange into chains of R24(12) motifs that combine to form corrugated layers parallel to (10\overline{1}). Atom–atom contacts for the cation primarily involve hydrogen, leading to the most abundant coverage percentages being 51.3% (H⋯H), 23.0% (H⋯Cl), 12.9% (H⋯O), and 9.7% (C⋯H).urn:issn:2056-9890Anil Kumar, H.G.Mohan Kumar, T.M.Divakara, T.R.Geetha, D.Yathirajan, H.S.Parkin, S.text/htmlThe low-temperature (90 K) crystal structure of 4-(dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate is presented along with a Hirshfeld surface analysis of the organic cation.doi:10.1107/S2056989023007223CRYSTAL STRUCTURE; ANILINE DERIVATIVE; ANILINIUM SALT; HYDROGEN BONDING2023-08-23Crystal structure studies and Hirshfeld surface analysis of 4-(dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate at 90 KThe crystal structure and a Hirshfeld surface analysis of the substituted anilinium salt 4-(dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate, C8H14N2O+·2Cl−·H2O, at low temperature (90 K) are presented. The organic cation is essentially planar: the r.m.s. deviation of its non-hydrogen atoms (aside from the two methyl groups) is 0.0045 Å. The methyl carbons are 1.3125 (12) Å and 1.1278 (12) Å either side of the mean plane. The crystal packing involves extensive hydrogen bonding of types O—H⋯Cl, N—H⋯Cl, N—H⋯OW, and OW—HW⋯Cl (where W = water), which arrange into chains of R24(12) motifs that combine to form corrugated layers parallel to (10\overline{1}). Atom–atom contacts for the cation primarily involve hydrogen, leading to the most abundant coverage percentages being 51.3% (H⋯H), 23.0% (H⋯Cl), 12.9% (H⋯O), and 9.7% (C⋯H).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98909med@iucr.org79https://creativecommons.org/licenses/by/4.0/research communicationsAugust 2023Acta Crystallographica Section E: Crystallographic Communications2023-08-23Crystal structure and Hirshfeld surface analysis of 3-(bromomethyl)-2-[1,2-dibromo-2-(6-nitrobenzo[d][1,3]dioxol-5-yl)ethyl]-1-(phenylsulfonyl)-1H-indole chloroform 0.585-solvate
http://scripts.iucr.org/cgi-bin/paper?hb8071
The title indole derivative, C24H17Br3N2O6S, crystallizes with a partial occupancy [0.585 (4)] CHCl3 solvent molecule. The dihedral angles between the indole ring system and pendant nitrobenzodioxolane rings system and phenylsulfonyl ring are 4.81 (14) and 72.24 (19)°, respectively. In the crystal, the indole molecules are linked to each other and to the chloroform molecule by weak C—H⋯O, C—H⋯Cl, C—H⋯π, C—Br⋯π and C—Cl⋯π and aromatic π–π stacking interactions. A Hirshfeld surface analysis was carried out and the intermolecular contacts with the most significant contributions are H⋯O/O⋯H (24.3%), H⋯H (18.4%), Br⋯H/H⋯Br (16.8%) and C⋯H/H⋯C (8.4%).urn:issn:2056-9890Achyuta, N.Kanagasabai, S.Vinayagam, P.Mohanakrishnan, A.K.Gautham, N.Gunasekaran, K.text/htmlThe title indole derivative crystallizes with a partial occupancy [0.585 (4)] CHCl3 solvent molecule. The dihedral angles between the indole ring system and pendant nitrobenzodioxolane rings system and phenylsulfonyl ring are 4.81 (14) and 72.24 (19)°, respectively. In the crystal, the indole molecules are linked to each other and to the chloroform molecule by weak C—H⋯O, C—H⋯Cl, C—H⋯π, C—Br⋯π and C—Cl⋯π and aromatic π–π stacking interactions.doi:10.1107/S2056989023007120CRYSTAL STRUCTURE; SYNTHESIS; 1-(PHENYLSULFONYL)-1H-INDOLE; Y-X...[PI] INTERACTIONS; HYDROGEN BONDING; HIRSHFELD SURFACE ANALYSIS2023-08-17Crystal structure and Hirshfeld surface analysis of 3-(bromomethyl)-2-[1,2-dibromo-2-(6-nitrobenzo[d][1,3]dioxol-5-yl)ethyl]-1-(phenylsulfonyl)-1H-indole chloroform 0.585-solvateThe title indole derivative, C24H17Br3N2O6S, crystallizes with a partial occupancy [0.585 (4)] CHCl3 solvent molecule. The dihedral angles between the indole ring system and pendant nitrobenzodioxolane rings system and phenylsulfonyl ring are 4.81 (14) and 72.24 (19)°, respectively. In the crystal, the indole molecules are linked to each other and to the chloroform molecule by weak C—H⋯O, C—H⋯Cl, C—H⋯π, C—Br⋯π and C—Cl⋯π and aromatic π–π stacking interactions. A Hirshfeld surface analysis was carried out and the intermolecular contacts with the most significant contributions are H⋯O/O⋯H (24.3%), H⋯H (18.4%), Br⋯H/H⋯Br (16.8%) and C⋯H/H⋯C (8.4%).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsAugust 20232023-08-172056-98902056-98909med@iucr.orgCrystal structure and Hirshfeld surface analysis of 2-amino-5-{(1E)-1-[(carbamothioylamino)imino]ethyl}-4-methyl-1,3-thiazol-3-ium chloride monohydrate
http://scripts.iucr.org/cgi-bin/paper?wm5691
In the hydrated title salt, C7H12N5S2+·Cl−·H2O, the asymmetric unit comprises one 2-amino-5-{(1E)-1-[(carbamothioylamino)imino]ethyl}-4-methyl-1,3-thiazol-3-ium cation, one chloride anion and one water molecule of crystallization. The cation is nearly flat (r.m.s. deviation of non-H atoms is 0.0814 Å), with the largest deviation of 0.1484 (14) Å observed for one of the methyl C atoms. In the crystal, the cations are linked by O—H⋯Cl, N—H⋯Cl, N—H⋯O, N—H⋯S and C—H⋯S hydrogen bonds, forming a tri-periodic network. The most important contributions to the crystal packing are from H⋯H (35.4%), S⋯H/H⋯S (24.4%), N⋯H/H⋯N (8.7%), Cl⋯H/H⋯Cl (8.2%) and C⋯H/H⋯C (7.7%) interactions.urn:issn:2056-9890Huseynov, E.Z.Akkurt, M.Brito, I.Bhattarai, A.Naghiyev, F.N.Asadov, K.A.Maharramov, A.M.text/htmlIn the crystal, the 2-amino-5-{(1E)-1-[(carbamothioylamino)imino]ethyl}-4-methyl-1,3-thiazol-3-ium cations are linked by O—H⋯Cl, N—H⋯Cl, N—H⋯O, N—H⋯S and C—H⋯S hydrogen bonds, forming a tri-periodic network.doi:10.1107/S2056989023007090CRYSTAL STRUCTURE; 1,3-THIAZOL-3-IUM; HYDROGEN BONDS; HYDROGEN-BONDED NETWORK; HIRSHFELD SURFACE ANALYSIS2023-08-17Crystal structure and Hirshfeld surface analysis of 2-amino-5-{(1E)-1-[(carbamothioylamino)imino]ethyl}-4-methyl-1,3-thiazol-3-ium chloride monohydrateIn the hydrated title salt, C7H12N5S2+·Cl−·H2O, the asymmetric unit comprises one 2-amino-5-{(1E)-1-[(carbamothioylamino)imino]ethyl}-4-methyl-1,3-thiazol-3-ium cation, one chloride anion and one water molecule of crystallization. The cation is nearly flat (r.m.s. deviation of non-H atoms is 0.0814 Å), with the largest deviation of 0.1484 (14) Å observed for one of the methyl C atoms. In the crystal, the cations are linked by O—H⋯Cl, N—H⋯Cl, N—H⋯O, N—H⋯S and C—H⋯S hydrogen bonds, forming a tri-periodic network. The most important contributions to the crystal packing are from H⋯H (35.4%), S⋯H/H⋯S (24.4%), N⋯H/H⋯N (8.7%), Cl⋯H/H⋯Cl (8.2%) and C⋯H/H⋯C (7.7%) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-98909Acta Crystallographica Section E: Crystallographic CommunicationsAugust 2023research communicationshttps://creativecommons.org/licenses/by/4.0/2023-08-1779Synthesis and crystal structure of catena-poly[cobalt(II)-di-μ-chlorido-μ-pyridazine-κ2N1:N2]
http://scripts.iucr.org/cgi-bin/paper?hb8073
The reaction of cobalt dichloride hexahydrate with pyridazine leads to the formation of crystals of the title compound, [CoCl2(C4H4N2)]n. This compound is isotypic to a number of compounds with other divalent metal ions. Its asymmetric unit consists of a Co2+ atom (site symmetry 2/m), a chloride ion (site symmetry m) and a pyridazine molecule (all atoms with site symmetry m). The Co2+ cations are coordinated by four chloride anions and two pyridazine ligands, generating trans-CoN4Cl2 octahedra, and are linked into [010] chains by pairs of μ-1,1-bridging chloride anions and bridging pyridazine ligands. In the crystal structure, the pyridazine ligands of neighboring chains are stacked onto each other, indicating π–π interactions. Powder X-ray diffraction proves that a pure crystalline phase was obtained. Differential thermonalysis coupled to thermogravimetry (DTA–TG) reveal that decomposition is observed at about 710 K. Magnetic measurements indicate low-temperature metamagnetic behavior as already observed in a related compound.urn:issn:2056-9890Näther, C.Jess, I.text/htmlIn the crystal structure of the title compound, the cobalt cations are octahedrally coordinated by pairs of μ-1,1-bridging chloride anions and bridging pyridazine ligands and linked into chains propagating along the crystallographic b-axis direction.doi:10.1107/S2056989023007065SYNTHESIS; CRYSTAL STRUCTURE; ONE-DIMENSIONAL COORDINATION COMPOUND2023-09-08Synthesis and crystal structure of catena-poly[cobalt(II)-di-μ-chlorido-μ-pyridazine-κ2N1:N2]The reaction of cobalt dichloride hexahydrate with pyridazine leads to the formation of crystals of the title compound, [CoCl2(C4H4N2)]n. This compound is isotypic to a number of compounds with other divalent metal ions. Its asymmetric unit consists of a Co2+ atom (site symmetry 2/m), a chloride ion (site symmetry m) and a pyridazine molecule (all atoms with site symmetry m). The Co2+ cations are coordinated by four chloride anions and two pyridazine ligands, generating trans-CoN4Cl2 octahedra, and are linked into [010] chains by pairs of μ-1,1-bridging chloride anions and bridging pyridazine ligands. In the crystal structure, the pyridazine ligands of neighboring chains are stacked onto each other, indicating π–π interactions. Powder X-ray diffraction proves that a pure crystalline phase was obtained. Differential thermonalysis coupled to thermogravimetry (DTA–TG) reveal that decomposition is observed at about 710 K. Magnetic measurements indicate low-temperature metamagnetic behavior as already observed in a related compound.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2023-09-08https://creativecommons.org/licenses/by/4.0/research communicationsOctober 2023Acta Crystallographica Section E: Crystallographic Communications79med@iucr.org102056-98902056-9890Crystal structure of 2-{[5-(methylsulfanyl)-4-phenyl-4H-1,2,4-triazol-3-yl]methyl}benzo[d]thiazole
http://scripts.iucr.org/cgi-bin/paper?yz2038
In the structure of the title compound, C17H14N4O2, the triazole ring exhibits interplanar angles of 63.86 (2) and 76.96 (2)° with the phenyl and benzothiazole planes, respectively. The C—C—C angle at the methylene group is rather wide at 114.28 (4)°. The packing involves three borderline C—H⋯N contacts, two of which combine to form layers parallel to ac, and a pairing of the triazole rings across an inversion centre [interplanar distance of 3.1852 (2) Å].urn:issn:2056-9890Azzam, R.A.Elgemeie, G.H.Elboshi, H.A.Jones, P.G.text/htmlIn the crystal structure of the title compound, the triazole ring exhibits interplanar angles of ca 64 and 77° with the phenyl and benzothiazole planes, respectively. The packing involves three borderline C—H⋯N contacts and a pairing of the triazole rings across an inversion centre.doi:10.1107/S2056989023007041CRYSTAL STRUCTURE; TRIAZOLE; BENZOTHIAZOLE; THIOETHER2023-08-23Crystal structure of 2-{[5-(methylsulfanyl)-4-phenyl-4H-1,2,4-triazol-3-yl]methyl}benzo[d]thiazoleIn the structure of the title compound, C17H14N4O2, the triazole ring exhibits interplanar angles of 63.86 (2) and 76.96 (2)° with the phenyl and benzothiazole planes, respectively. The C—C—C angle at the methylene group is rather wide at 114.28 (4)°. The packing involves three borderline C—H⋯N contacts, two of which combine to form layers parallel to ac, and a pairing of the triazole rings across an inversion centre [interplanar distance of 3.1852 (2) Å].https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org92056-98902056-98902023-08-23https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsAugust 202379Crystal structures of the complexes containing macrocyclic cations [M(cyclam)]2+ (M = Ni, Zn) and tetraiodidocadmate(2–) anion
http://scripts.iucr.org/cgi-bin/paper?ex2074
The asymmetric units of the isostructural compounds (1,4,8,11-tetraazacyclotetradecane-κ4N)nickel(II) tetraiodidocadmate(II), [Ni(C10H24N4)][CdI4] (I), and triiodido-1κ3I-μ-iodido-(1,4,8,11-tetraazacyclotetradecane-2κ4N)cadmium(II)zinc(II), [CdZnI4(C10H24N4)] (II) (C10H24N4 = 1,4,8,11-tetraazacyclotetradecane, cyclam, L), consist of the centrosymmetric macrocyclic cation [M(L)]2+ [M = NiII or ZnII] with the metal ion lying on a twofold screw axis, and the tetraiodocadmate anion [CdI4]2− located on the mirror plane. In I, the anion acts as an uncoordinated counter-ion while in II it is bound to the ZnII atom via one of the iodide atoms, thus forming an electroneutral heterobimetallic complex [Zn(L)(CdI4)]. The NiII and ZnII ions are coordinated in a square-planar manner by the four secondary N atoms of the macrocyclic ligand L, which adopts the most energetically stable trans-III conformation. The [CdI4]2− anions in I and II are structurally very similar and represent slightly deformed tetrahedrons with average Cd—I bond lengths and I—Cd—I angles of ca 2.79 Å and 109.6°, respectively. The supramolecular organization of the complexes under consideration in the crystals is very similar and is determined by the hydrogen-bonding interactions between the secondary amino groups of the ligand L in the [M(L)]2+ cations and iodide atoms of the [CdI4]2− anion. In particular, the alternating cations and anions form chains running along the b-axis direction that are arranged into di-periodic sheets oriented parallel to the (101) and (\overline{1}01) planes. Because both kinds of sheets are built from the same cations and anions, this feature provides the three-dimensional coherence of the crystals of I and II.urn:issn:2056-9890Andriichuk, I.L.Shova, S.Lampeka, Y.D.text/htmlThe isostructural compounds I and II are composed of planar macrocyclic cations [M(cyclam)]2+ and the tetrahedral anion [CdI4]2−, which plays a purely charge-compensation function in the NiII complex I and is axially coordinated via the iodide atom in the ZnII complex II. In both complexes, as a result of N–H⋯I hydrogen bonding, the alternating cations and anions form chains running along the b-axis direction that are arranged into di-periodic sheets oriented parallel to the (101) and (\overline{1}01) planes.doi:10.1107/S2056989023007004CRYSTAL STRUCTURE; NICKEL; ZINC; CYCLAM; TETRAIODOCADMATE2023-08-23Crystal structures of the complexes containing macrocyclic cations [M(cyclam)]2+ (M = Ni, Zn) and tetraiodidocadmate(2–) anionThe asymmetric units of the isostructural compounds (1,4,8,11-tetraazacyclotetradecane-κ4N)nickel(II) tetraiodidocadmate(II), [Ni(C10H24N4)][CdI4] (I), and triiodido-1κ3I-μ-iodido-(1,4,8,11-tetraazacyclotetradecane-2κ4N)cadmium(II)zinc(II), [CdZnI4(C10H24N4)] (II) (C10H24N4 = 1,4,8,11-tetraazacyclotetradecane, cyclam, L), consist of the centrosymmetric macrocyclic cation [M(L)]2+ [M = NiII or ZnII] with the metal ion lying on a twofold screw axis, and the tetraiodocadmate anion [CdI4]2− located on the mirror plane. In I, the anion acts as an uncoordinated counter-ion while in II it is bound to the ZnII atom via one of the iodide atoms, thus forming an electroneutral heterobimetallic complex [Zn(L)(CdI4)]. The NiII and ZnII ions are coordinated in a square-planar manner by the four secondary N atoms of the macrocyclic ligand L, which adopts the most energetically stable trans-III conformation. The [CdI4]2− anions in I and II are structurally very similar and represent slightly deformed tetrahedrons with average Cd—I bond lengths and I—Cd—I angles of ca 2.79 Å and 109.6°, respectively. The supramolecular organization of the complexes under consideration in the crystals is very similar and is determined by the hydrogen-bonding interactions between the secondary amino groups of the ligand L in the [M(L)]2+ cations and iodide atoms of the [CdI4]2− anion. In particular, the alternating cations and anions form chains running along the b-axis direction that are arranged into di-periodic sheets oriented parallel to the (101) and (\overline{1}01) planes. Because both kinds of sheets are built from the same cations and anions, this feature provides the three-dimensional coherence of the crystals of I and II.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextAugust 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/2023-08-2379med@iucr.org2056-98902056-98909Synthesis, crystal structure and Hirshfeld surface analysis of a copper(II) complex involving 3-methylbenzoate and 2,2′-bipyridine ligands
http://scripts.iucr.org/cgi-bin/paper?dj2063
3-Methylbenzoic acid (3-mbH) and 2,2′-bipyridine (bipy) reacted with a copper(II) salt forming a new mixed ligand complex, aqua(2,2′-bipyridine-κ2N,N′)bis(3-methylbenzoato)-κ2O,O′;κO-copper(II) 0.68-hydrate, [Cu(C8H7O2)2(C10H8N2)(H2O)]·0.68H2O or [Cu(3-mb)2(bipy)(H2O)]·0.68H2O. The coordination environment of CuII is a distorted octahedron. The metal atom is attached to two 3-mb moieties, which bind in monodentate and bidentate fashions. One of the 3-mb units is disordered. The coordination environment is completed by one bipy ligand and a water molecule. A second water molecule is outside the coordination sphere of the CuII atom and its occupancy refined to 0.68. The structure consists of chains along the b-axis direction formed by complex units joined via hydrogen bonds between the coordinated water molecule and an O atom of a coordinated 3-mb unit. Hirshfeld surface analysis indicates that the most abundant contacts are H⋯H (56.8%), H⋯C/C⋯H (21.7%) and H⋯O/O⋯H (13.7%).urn:issn:2056-9890Qadir, A.text/htmlA new copper(II) complex with 3-methylbenzoate and 2,2′-bipyridine synthesized displays chains of hydrogen-bonded complex units along the b axis. Hirshfeld surface analysis indicates that H⋯H and H⋯C/C⋯H contacts are the most important interactions.doi:10.1107/S2056989023006904CRYSTAL STRUCTURE; COORDINATION COMPOUND; HIRSHFELD SURFACE ANALYSIS; 3-METHYLBENZOATE2023-08-15Synthesis, crystal structure and Hirshfeld surface analysis of a copper(II) complex involving 3-methylbenzoate and 2,2′-bipyridine ligands3-Methylbenzoic acid (3-mbH) and 2,2′-bipyridine (bipy) reacted with a copper(II) salt forming a new mixed ligand complex, aqua(2,2′-bipyridine-κ2N,N′)bis(3-methylbenzoato)-κ2O,O′;κO-copper(II) 0.68-hydrate, [Cu(C8H7O2)2(C10H8N2)(H2O)]·0.68H2O or [Cu(3-mb)2(bipy)(H2O)]·0.68H2O. The coordination environment of CuII is a distorted octahedron. The metal atom is attached to two 3-mb moieties, which bind in monodentate and bidentate fashions. One of the 3-mb units is disordered. The coordination environment is completed by one bipy ligand and a water molecule. A second water molecule is outside the coordination sphere of the CuII atom and its occupancy refined to 0.68. The structure consists of chains along the b-axis direction formed by complex units joined via hydrogen bonds between the coordinated water molecule and an O atom of a coordinated 3-mb unit. Hirshfeld surface analysis indicates that the most abundant contacts are H⋯H (56.8%), H⋯C/C⋯H (21.7%) and H⋯O/O⋯H (13.7%).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98909med@iucr.org79August 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/2023-08-15Synthesis, crystal structure and thermal behavior of tetrakis(3-cyanopyridine N-oxide-κO)bis(thiocyanato-κN)cobalt(II), which shows strong pseudosymmetry
http://scripts.iucr.org/cgi-bin/paper?hb8070
The title compound, [Co(SCN)2(C6H4N2O)4], was prepared by the reaction of cobalt(II)thiocyanate with 3-cyanopyridine N-oxide in ethanol. In the crystal, the cobalt(II) cations are octahedrally coordinated by two terminal N-bonded thiocyanate anions and four O-bonded 3-cyanopyridine N-oxide coligands, forming discrete complexes that are located on centers of inversion, hence forming trans-CoN2O4 octahedra. The structure refinement was performed in the monoclinic space group P21/n, for which a potential lattice translation and new symmetry elements with a fit of 100% is suggested. The structure can easily be refined in the space group I2/m, where the complexes have 2/m symmetry. However, nearly all of the reflections that violate the centering are observed with significant intensity and the refinement in P21/n leads to significantly lower R(F) values (0.027 versus 0.033). Moreover, in I2/m much larger components of the anisotropic displacement parameters are observed and therefore, the crystal structure is presented in the primitive unit cell. IR investigations confirm that the anionic ligands are only terminally bonded and that the cyano group is not involved in the metal coordination. PXRD investigations show that a pure crystalline phase has been obtained and measurements using simultaneously thermogravimetry and differential thermoanalysis reveal that the compound decomposes in an exothermic reaction upon heating, without the formation of a coligand-deficient intermediate phase.urn:issn:2056-9890Näther, C.Jess, I.text/htmlThe crystal structure of the title compound consists of discrete complexes in which the CoII cations are octahedrally coordinated and show strong pseudosymmetry.doi:10.1107/S2056989023006862SYNTHESIS; COORDINATION COMPOUND; COBALT THIOCYANATE; 3-CYANOPYRIDINE N-OXIDE; CRYSTAL STRUCTURE; PSEUDOSYMMETRY; THERMAL PROPERTIES2023-09-08Synthesis, crystal structure and thermal behavior of tetrakis(3-cyanopyridine N-oxide-κO)bis(thiocyanato-κN)cobalt(II), which shows strong pseudosymmetryThe title compound, [Co(SCN)2(C6H4N2O)4], was prepared by the reaction of cobalt(II)thiocyanate with 3-cyanopyridine N-oxide in ethanol. In the crystal, the cobalt(II) cations are octahedrally coordinated by two terminal N-bonded thiocyanate anions and four O-bonded 3-cyanopyridine N-oxide coligands, forming discrete complexes that are located on centers of inversion, hence forming trans-CoN2O4 octahedra. The structure refinement was performed in the monoclinic space group P21/n, for which a potential lattice translation and new symmetry elements with a fit of 100% is suggested. The structure can easily be refined in the space group I2/m, where the complexes have 2/m symmetry. However, nearly all of the reflections that violate the centering are observed with significant intensity and the refinement in P21/n leads to significantly lower R(F) values (0.027 versus 0.033). Moreover, in I2/m much larger components of the anisotropic displacement parameters are observed and therefore, the crystal structure is presented in the primitive unit cell. IR investigations confirm that the anionic ligands are only terminally bonded and that the cyano group is not involved in the metal coordination. PXRD investigations show that a pure crystalline phase has been obtained and measurements using simultaneously thermogravimetry and differential thermoanalysis reveal that the compound decomposes in an exothermic reaction upon heating, without the formation of a coligand-deficient intermediate phase.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext102056-98902056-9890med@iucr.org792023-09-08Acta Crystallographica Section E: Crystallographic CommunicationsOctober 2023https://creativecommons.org/licenses/by/4.0/research communicationsThe unusual (syn-/anti-)2 conformation of a dimethoxypyrimidyl-based tennimide
http://scripts.iucr.org/cgi-bin/paper?ex2073
The tennimide macrocycle, (I) (C52H40N16O16.0.167H2O), was synthesized from 2-amino-4,6-dimethoxypyrimidine and pyridine-2,6-dicarbonyl dichloride. Compound (I) represents the first tennimide incorporating pyridine rings in the macrocycle scaffold. In the macrocycle ring, the carbonyl groups at each successive dicarbonyl(pyridine) moiety adopt the (syn/anti)2 conformation. This contrasts with all previously reported tetraimide macrocycles, which exhibit the (syn)4 conformation. The effect is to close any potential cavity or niche by having two of the central pyridine C5N rings aligned close to each other [with closest pyridine Cg⋯Cg ring centroid separations of 3.5775 (19) Å; closest C⋯C = 3.467 (5) Å]. A partial occupancy water molecule (with s.o.f. = 0.167), resides with its oxygen atom on a twofold axis at hydrogen-bonding distances to the carbonyl O atom, in a molecular niche between two pyridine rings. Macrocyles of (I) have all six C=O groups and all eight methoxy O atoms present on the macrocycle surface. However, all twelve N atoms are effectively shielded on steric grounds from any potential intermolecular interactions. The remaining two C=O O atoms interact with the partial occupancy water molecule via two O—H⋯O=C hydrogen bonds. Macrocycles of (I) stack as one-dimensional chains along the b-axis direction with primary intermolecular interactions involving weak C—H⋯O=C/OCH3/H2O contacts. Chains interlock weakly via methoxy–methoxy C—H⋯O interactions into two-dimensional sheets.urn:issn:2056-9890Mocilac, P.Pohl, F.Gallagher, J.F.text/htmlThe tennimide macrocycle (I) resides on a twofold axis and adopts an alternate (syn/anti)2 conformation with no inner cavity (niche), unlike all previously reported (syn)4 tennimide conformations. A partial occupancy water molecule (with 0.167 site occupancy) at hydrogen-bonding distances to two symmetry-related carbonyl O atoms (as O—H⋯O=C) resides on the twofold axis in a molecular niche between two of the pyridine rings. Macrocycle aggregation occurs as one-dimensional chains along the (010) direction.doi:10.1107/S2056989023006837CONFORMATION; MACROCYCLE; METHOXY; PYRIDINE; PYRIMIDINE; TENNIMIDE; TETRAMER; CRYSTAL STRUCTURE2023-08-23The unusual (syn-/anti-)2 conformation of a dimethoxypyrimidyl-based tennimideThe tennimide macrocycle, (I) (C52H40N16O16.0.167H2O), was synthesized from 2-amino-4,6-dimethoxypyrimidine and pyridine-2,6-dicarbonyl dichloride. Compound (I) represents the first tennimide incorporating pyridine rings in the macrocycle scaffold. In the macrocycle ring, the carbonyl groups at each successive dicarbonyl(pyridine) moiety adopt the (syn/anti)2 conformation. This contrasts with all previously reported tetraimide macrocycles, which exhibit the (syn)4 conformation. The effect is to close any potential cavity or niche by having two of the central pyridine C5N rings aligned close to each other [with closest pyridine Cg⋯Cg ring centroid separations of 3.5775 (19) Å; closest C⋯C = 3.467 (5) Å]. A partial occupancy water molecule (with s.o.f. = 0.167), resides with its oxygen atom on a twofold axis at hydrogen-bonding distances to the carbonyl O atom, in a molecular niche between two pyridine rings. Macrocyles of (I) have all six C=O groups and all eight methoxy O atoms present on the macrocycle surface. However, all twelve N atoms are effectively shielded on steric grounds from any potential intermolecular interactions. The remaining two C=O O atoms interact with the partial occupancy water molecule via two O—H⋯O=C hydrogen bonds. Macrocycles of (I) stack as one-dimensional chains along the b-axis direction with primary intermolecular interactions involving weak C—H⋯O=C/OCH3/H2O contacts. Chains interlock weakly via methoxy–methoxy C—H⋯O interactions into two-dimensional sheets.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-98909August 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-08-2379Crystal structure of a (carboxymethyl)triethylazanium bromide–2-(triethylazaniumyl)acetate (1/1) hydrogen-bonded dimer
http://scripts.iucr.org/cgi-bin/paper?wm5689
The title compound, C8H18NO2+·Br−·C8H17NO2, crystallizes as the bromide salt of a 50:50 mixture of (triethylazaniumyl)carboxylic acid and the zwitterionic (triethylazaniumyl)carboxylate. The two organic entities are linked by a half-occupied bridging carboxylic acid hydrogen atom that is hydrogen-bonded to the carboxylate group of the second molecule. The tetralkylammonium group adopts a nearly perfect tetrahedral shape around the nitrogen atom with bond lengths that agree with known values. The carboxylic acid/carboxylate group is oriented anti to one of the ethyl groups on the ammonium group, and the carbonyl oxygen atom is engaged in intramolecular C—H⋯O hydrogen bonds.urn:issn:2056-9890Carlson, F.M.Staples, R.J.Biros, S.M.text/htmlThe crystal structure of a hydrogen-bonded dimer of (triethylazaniumyl)acetic acid and (triethylazaniumyl)acetate bromide features a carboxylic acid hydrogen atom that is engaged in an asymmetric hydrogen bond with the carboxylate oxygen. The crystal also features intramolecular C—H hydrogen bonds and a layer of bromide ions that is surrounded by alkyl groups.doi:10.1107/S2056989023006850CRYSTAL STRUCTURE; ASYMMETRIC HYDROGEN BOND; BROMIDE SALT; INTERMOLECULAR O-H...O HYDROGEN BOND; INTRAMOLECULAR C-H...O HYDROGEN BOND2023-08-10Crystal structure of a (carboxymethyl)triethylazanium bromide–2-(triethylazaniumyl)acetate (1/1) hydrogen-bonded dimerThe title compound, C8H18NO2+·Br−·C8H17NO2, crystallizes as the bromide salt of a 50:50 mixture of (triethylazaniumyl)carboxylic acid and the zwitterionic (triethylazaniumyl)carboxylate. The two organic entities are linked by a half-occupied bridging carboxylic acid hydrogen atom that is hydrogen-bonded to the carboxylate group of the second molecule. The tetralkylammonium group adopts a nearly perfect tetrahedral shape around the nitrogen atom with bond lengths that agree with known values. The carboxylic acid/carboxylate group is oriented anti to one of the ethyl groups on the ammonium group, and the carbonyl oxygen atom is engaged in intramolecular C—H⋯O hydrogen bonds.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextAugust 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-08-1079med@iucr.org2056-98902056-98909Synthesis, crystal structure and Hirshfeld surface analysis of 5-[2-(dicyanomethylidene)hydrazin-1-yl]-2,4,6-triiodoisophthalic acid ethanol monosolvate
http://scripts.iucr.org/cgi-bin/paper?tx2072
The title compound, C11H3I3N4O4·C2H6O, crystallizes in the triclinic P\overline{1} space group with one independent molecule and one ethanol solvent molecule in the asymmetric unit. The benzene ring and the methylcarbonohydrazonoyl dicyanide group of the main molecule makes a dihedral angle of 57.91 (16)°. In the crystal, O—H⋯O and N—H⋯O hydrogen bonds link pairs of molecules, forming dimers with R22(14) motifs. These dimers are connected by O—H⋯O hydrogen bonds into chains along the a-axis direction, forming R22(16) ring motifs. Further O—H⋯O interactions involving the ethanol solvent molecule connect the chains into a three-dimensional network. In addition, C—I⋯π interactions are observed. The intermolecular interactions in the crystal structure were quantified and analysed using Hirshfeld surface analysis.urn:issn:2056-9890Aliyeva, F.S.Mammadova, G.Z.Akkurt, M.Çelikesir, S.T.Bhattarai, A.text/htmlIn the crystal, pairs of molecules are linked by O—H⋯O and N—H⋯O hydrogen bonds forming dimers with R_{2}^{2}(14) motifs. These dimers are connected by O—H⋯O hydrogen bonds into chains along the a-axis direction, forming R_{2}^{2}(16) ring motifs. Further O—H⋯O interactions involving the ethanol solvent molecule connect the chains into a three-dimensional network.doi:10.1107/S205698902300676XCRYSTAL STRUCTURE; HYDROGEN BONDS; THREE DIMENSIONAL NETWORK; C-I...[PI] INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-08-04Synthesis, crystal structure and Hirshfeld surface analysis of 5-[2-(dicyanomethylidene)hydrazin-1-yl]-2,4,6-triiodoisophthalic acid ethanol monosolvateThe title compound, C11H3I3N4O4·C2H6O, crystallizes in the triclinic P\overline{1} space group with one independent molecule and one ethanol solvent molecule in the asymmetric unit. The benzene ring and the methylcarbonohydrazonoyl dicyanide group of the main molecule makes a dihedral angle of 57.91 (16)°. In the crystal, O—H⋯O and N—H⋯O hydrogen bonds link pairs of molecules, forming dimers with R22(14) motifs. These dimers are connected by O—H⋯O hydrogen bonds into chains along the a-axis direction, forming R22(16) ring motifs. Further O—H⋯O interactions involving the ethanol solvent molecule connect the chains into a three-dimensional network. In addition, C—I⋯π interactions are observed. The intermolecular interactions in the crystal structure were quantified and analysed using Hirshfeld surface analysis.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-98909research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsAugust 20232023-08-0479A nickel(II) complex with an unsymmetrical tetradentate chelating ligand derived from pyridine-2,6-dicarbaldehyde and 2-aminothiophenol
http://scripts.iucr.org/cgi-bin/paper?pk2692
[(2-{[6-(1,3-Benzothiazol-2-yl)pyridin-2-yl]carbonylazanidyl}phenyl)sulfanido]nickel(II), [Ni(C19H11N3OS2)], crystallizes in the centrosymmetric monoclinic space group P21/n with one molecule in the asymmetric unit. The expected ligand, a bis-Schiff base derived from pyridine-2,6-dicarbaldehyde and 2-aminothiophenol, had modified in situ in a both unexpected and unsymmetrical fashion. One arm had cyclized to form a benzo[d]thiazol-2-yl functionality, while the imine linkage of the second arm had oxidized to an amide group. The geometry about the central NiII atom is distorted square-planar N3S. The molecules form supramolecular face-to-face dimers via rather strong π–π stacking interactions, with these dimers then linked into chains via pairwise C—H⋯O interactions.urn:issn:2056-9890Al-Zeidaneen, F.K.Anson, C.E.Powell, A.K.text/html[(2-{[6-(1,3-Benzothiazol-2-yl)pyridin-2-yl]carbonylazanidyl}phenyl)sulfanido]nickel(II) crystallizes in the centrosymmetric monoclinic space group P21/n. Both arms of the expected bis-Schiff base ligand based on pyridine-2,6-dicarbaldehyde and 2-aminothiophenol had oxidized; one by cyclization to a benzothiazole, the other by oxidation of its imine linkage to the corresponding amide.doi:10.1107/S2056989023006692CRYSTAL STRUCTURE; NICKEL; CHELATE LIGAND; LIGAND MODIFICATION2023-08-04A nickel(II) complex with an unsymmetrical tetradentate chelating ligand derived from pyridine-2,6-dicarbaldehyde and 2-aminothiophenol[(2-{[6-(1,3-Benzothiazol-2-yl)pyridin-2-yl]carbonylazanidyl}phenyl)sulfanido]nickel(II), [Ni(C19H11N3OS2)], crystallizes in the centrosymmetric monoclinic space group P21/n with one molecule in the asymmetric unit. The expected ligand, a bis-Schiff base derived from pyridine-2,6-dicarbaldehyde and 2-aminothiophenol, had modified in situ in a both unexpected and unsymmetrical fashion. One arm had cyclized to form a benzo[d]thiazol-2-yl functionality, while the imine linkage of the second arm had oxidized to an amide group. The geometry about the central NiII atom is distorted square-planar N3S. The molecules form supramolecular face-to-face dimers via rather strong π–π stacking interactions, with these dimers then linked into chains via pairwise C—H⋯O interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2023-08-04https://creativecommons.org/licenses/by/4.0/research communicationsAugust 2023Acta Crystallographica Section E: Crystallographic Communications79med@iucr.org92056-98902056-9890Foreword to the special virtual issue on Modern approaches and tools for teaching crystallography
http://scripts.iucr.org/cgi-bin/paper?me6239
urn:issn:2056-9890Díaz de Delgado, G.Parkin, S.text/htmlA compilation of articles with a strong teaching element published since 2018 is presented alongside an overview of the articles in the special issue on this topic.doi:10.1107/S2056989023006667CRYSTALLOGRAPHIC TEACHING; SPACE-GROUP SYMMETRY; CRYSTAL GROWING; TWINNING; VALIDATION CRITERIA; DISORDER; ELECTRON DIFFRACTION2023-08-01Foreword to the special virtual issue on Modern approaches and tools for teaching crystallographyhttps://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext92056-98902056-9890med@iucr.org768792023-08-01767https://creativecommons.org/licenses/by/4.0/editorialActa Crystallographica Section E: Crystallographic CommunicationsAugust 2023Crystal structure and Hirshfeld surface analysis of 7-[(6-hydroxy-2,5,5,8a-tetramethyldecahydronaphthalen-1-yl)methoxy]-2H-chromen-2-one
http://scripts.iucr.org/cgi-bin/paper?wm5687
urn:issn:2056-9890Karimli, E.G.Khrustalev, V.N.Akkurt, M.Khalilov, A.N.Bhattarai, A.Aleskerova, A.N.Mamedov, İ.G.text/htmldoi:10.1107/S20569890230065522023-08-01Crystal structure and Hirshfeld surface analysis of 7-[(6-hydroxy-2,5,5,8a-tetramethyldecahydronaphthalen-1-yl)methoxy]-2H-chromen-2-onehttps://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext92056-98902056-9890med@iucr.org792023-08-01Acta Crystallographica Section E: Crystallographic CommunicationsAugust 2023https://creativecommons.org/licenses/by/4.0/research communicationsCrystal structure of bis(3,5-dichloro-2-hydroxybenzyl)(2-methoxyethyl)amine
http://scripts.iucr.org/cgi-bin/paper?zl5047
The title compound, systematic name 4,4′,6,6′-tetrachloro-2,2′-{[(2-methoxyethyl)azanediyl]bis(methylene)}diphenol (C17H17Cl4NO, 1), was prepared via a modified Mannich reaction between 2-methoxyethylamine, 2,4-dichlorophenol, and aqueous formaldehyde. The resulting amine bis(phenol) provides an interesting comparison to related species as a result of the electron-withdrawing substituents on the phenol rings, in combination with similar steric parameters. One of the Cl atoms was modeled as a two-component disorder with partial occupancies of 0.49 (3) and 0.51 (3), while the pendant ether group was modeled as a two-component disorder with partial occupancies of 0.867 (3) and 0.133 (3). A comparison of metrical parameters for the title compound and closely related structures provides insight into the use of these species as ligands to support transition-metal complexes for applications as homogeneous catalysts.urn:issn:2056-9890Wile, B.M.Griffith, C.L.Johnson, A.R.text/htmlThe title compound was prepared via a modified Mannich reaction between 2-methoxyethylamine, 2,4-dichlorophenol, and aqueous formaldehyde. The resulting amine bis(phenol) provides an interesting comparison to related species as a result of the electron-withdrawing substituents on the phenol rings, in combination with similar steric parameters.doi:10.1107/S2056989023006564CRYSTAL STRUCTURE; PHENOL; AMINE; ETHER; AMINEBIS(PHENOL)2023-08-04Crystal structure of bis(3,5-dichloro-2-hydroxybenzyl)(2-methoxyethyl)amineThe title compound, systematic name 4,4′,6,6′-tetrachloro-2,2′-{[(2-methoxyethyl)azanediyl]bis(methylene)}diphenol (C17H17Cl4NO, 1), was prepared via a modified Mannich reaction between 2-methoxyethylamine, 2,4-dichlorophenol, and aqueous formaldehyde. The resulting amine bis(phenol) provides an interesting comparison to related species as a result of the electron-withdrawing substituents on the phenol rings, in combination with similar steric parameters. One of the Cl atoms was modeled as a two-component disorder with partial occupancies of 0.49 (3) and 0.51 (3), while the pendant ether group was modeled as a two-component disorder with partial occupancies of 0.867 (3) and 0.133 (3). A comparison of metrical parameters for the title compound and closely related structures provides insight into the use of these species as ligands to support transition-metal complexes for applications as homogeneous catalysts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-98909August 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-08-0479Structures of rac-2,4:3,5-dimethylene xylitol derivatives
http://scripts.iucr.org/cgi-bin/paper?pk2693
The structures of three racemic (tetrahydro-[1,3]dioxino[5,4-d][1,3]dioxin-4-yl)methanol derivatives are reported, namely, 4-[(methylsulfonyloxy)methyl]-2,4,4a,6,8,8a-hexahydro-[1,3]dioxino[5,4-d][1,3]dioxine, C8H14O7S, 1, 4-[(benzyloxy)methyl]-2,4,4a,6,8,8a-hexahydro-[1,3]dioxino[5,4-d][1,3]dioxine, C14H18O5, 2, and 4-[(anilinocarbonyl)methyl]-2,4,4a,6,8,8a-hexahydro-[1,3]dioxino[5,4-d][1,3]dioxine, C14H17NO6, 3. Mesylate ester 1 at 173 K has triclinic P\overline{1} symmetry and both benzyl ether 2 at 173 K and phenyl urethane 3 have monoclinic P21/c symmetry. These structures are of interest because of the conformation of the cis-fused tetraoxadecalin ring system. This cis-bicyclo[4.4.0]decane ring system, i.e. cis-decalin, can undergo conformational equilibration. In the two most stable conformers, both six-membered rings adopt a chair conformation. However, there are significant consequences in these two stable conformers, with heteroatom substitution at the 1,3,5,7-ring positions as described. Only one conformation, denoted as `concave' or `inside', is found in these crystal structures. This is consistent with previously reported structures of the 1,1-geminal dihydroxy aldehyde and tosylate analogs.urn:issn:2056-9890Satlow, M.Williard, P.G.text/htmlThe crystal structures of three xylitol derivatives prepared directly from commercially available xylitol by treatment with formalin and acid followed by subsequent derivatization of the primary hydroxyl group of the bis-methylene ketal with mesyl chloride, benzyl bromide or phenyl isocyanate are reported.doi:10.1107/S2056989023006497XYLITOL; PENTOSE; CIS-1,3,5,7-TETRAOXADECALIN; CIS-DECALIN CONFORMATION; CRYSTAL STRUCTURE2023-08-04Structures of rac-2,4:3,5-dimethylene xylitol derivativesThe structures of three racemic (tetrahydro-[1,3]dioxino[5,4-d][1,3]dioxin-4-yl)methanol derivatives are reported, namely, 4-[(methylsulfonyloxy)methyl]-2,4,4a,6,8,8a-hexahydro-[1,3]dioxino[5,4-d][1,3]dioxine, C8H14O7S, 1, 4-[(benzyloxy)methyl]-2,4,4a,6,8,8a-hexahydro-[1,3]dioxino[5,4-d][1,3]dioxine, C14H18O5, 2, and 4-[(anilinocarbonyl)methyl]-2,4,4a,6,8,8a-hexahydro-[1,3]dioxino[5,4-d][1,3]dioxine, C14H17NO6, 3. Mesylate ester 1 at 173 K has triclinic P\overline{1} symmetry and both benzyl ether 2 at 173 K and phenyl urethane 3 have monoclinic P21/c symmetry. These structures are of interest because of the conformation of the cis-fused tetraoxadecalin ring system. This cis-bicyclo[4.4.0]decane ring system, i.e. cis-decalin, can undergo conformational equilibration. In the two most stable conformers, both six-membered rings adopt a chair conformation. However, there are significant consequences in these two stable conformers, with heteroatom substitution at the 1,3,5,7-ring positions as described. Only one conformation, denoted as `concave' or `inside', is found in these crystal structures. This is consistent with previously reported structures of the 1,1-geminal dihydroxy aldehyde and tosylate analogs.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-08-04August 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/92056-98902056-9890med@iucr.orgSynthesis and crystal structures of (E)-N′-(4-chloro-3-nitrobenzylidene)acetohydrazide and (E)-2-(4-chlorobenzylidene)-1-(quinolin-8-yl)hydrazine
http://scripts.iucr.org/cgi-bin/paper?jq2029
The syntheses of two benzylidenehydrazine derivatives, namely, (E)-N′-(4-chloro-3-nitrobenzylidene)acetohydrazide, C9H8ClN3O3, and (E)-2-(4-chlorobenzylidene)-1-(quinolin-8-yl)hydrazine, C16H12ClN3, are reported. The molecules have been characterized using IR, 1H NMR, 13C NMR and mass spectroscopic and elemental analysis techniques, and their structures have been determined by single-crystal X-ray diffraction.urn:issn:2056-9890Nasr, T.Kariuki, B.M.Elansary, M.M.Elhaggar, R.Zaghary, W.text/htmlTwo benzylidenehydrazinederivatives have been synthesized and structurally characterized.doi:10.1107/S2056989023006412SYNTHESIS; CRYSTAL STRUCTURE; BENZYLIDENE; HYDRAZINE2023-07-28Synthesis and crystal structures of (E)-N′-(4-chloro-3-nitrobenzylidene)acetohydrazide and (E)-2-(4-chlorobenzylidene)-1-(quinolin-8-yl)hydrazineThe syntheses of two benzylidenehydrazine derivatives, namely, (E)-N′-(4-chloro-3-nitrobenzylidene)acetohydrazide, C9H8ClN3O3, and (E)-2-(4-chlorobenzylidene)-1-(quinolin-8-yl)hydrazine, C16H12ClN3, are reported. The molecules have been characterized using IR, 1H NMR, 13C NMR and mass spectroscopic and elemental analysis techniques, and their structures have been determined by single-crystal X-ray diffraction.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext766med@iucr.org2056-98902056-98908Acta Crystallographica Section E: Crystallographic CommunicationsJuly 2023research communicationshttps://creativecommons.org/licenses/by/4.0/2023-07-2876279Diastereotopic groups in two new single-enantiomer structures (R2)P(O)[NH-(+)CH(C2H5)(C6H5)] (R = OC6H5 and C6H5)
http://scripts.iucr.org/cgi-bin/paper?jq2028
The crystal structures of two single-enantiomer compounds, i.e. diphenyl [(R)-(+)-α-ethylbenzylamido]phosphate, C21H22NO3P or (C6H5O)2P(O)[NH-(R)-(+)CH(C2H5)(C6H5)] (I), and N-[(R)-(+)-α-ethylbenzyl]-P,P-diphenylphosphinic amide, C21H22NOP or (C6H5)2P(O)[NH-R-(+)CH(C2H5)(C6H5)] (II), were studied. The different environments at the phosphorus atoms, (O)2P(O)(N) and (C)2P(O)(N), allow the P=O/P—N bond strengths to be compared, as well as the N—H⋯O=P hydrogen-bond strengths, and P=O/N—H vibrations. The following characteristics related to diastereotopic C6H5O/C6H5 groups in I/II were considered: geometry parameters, contributions to the crystal packing, solution 13C/1H NMR chemical shifts, conformations, and NMR coupling constants. The phosphorus-carbon coupling constants nJPC (n = 2 and 3) in I and mJPC (m = 1, 2, 3 and 4) in II were evaluated. For a comparative study, chiral analogous structures were retrieved from the Cambridge Structural Database (CSD) and their geometries and conformations are discussed.urn:issn:2056-9890Eslami, F.Pourayoubi, M.Sabbaghi, F.Skořepová, E.Dušek, M.Baniyaghoob, S.text/htmlTwo new single-enantiomer phosphorus structures were studied. Their geometries, conformations and NMR features are discussed.doi:10.1107/S2056989023006278PHOSPHORAMIDE; PHOSPHINAMIDE; SINGLE-ENANTIOMER; DIASTEREOTOPIC GROUPS; X-RAY CRYSTALLOGRAPHY; CRYSTAL STRUCTURE2023-08-01Diastereotopic groups in two new single-enantiomer structures (R2)P(O)[NH-(+)CH(C2H5)(C6H5)] (R = OC6H5 and C6H5)The crystal structures of two single-enantiomer compounds, i.e. diphenyl [(R)-(+)-α-ethylbenzylamido]phosphate, C21H22NO3P or (C6H5O)2P(O)[NH-(R)-(+)CH(C2H5)(C6H5)] (I), and N-[(R)-(+)-α-ethylbenzyl]-P,P-diphenylphosphinic amide, C21H22NOP or (C6H5)2P(O)[NH-R-(+)CH(C2H5)(C6H5)] (II), were studied. The different environments at the phosphorus atoms, (O)2P(O)(N) and (C)2P(O)(N), allow the P=O/P—N bond strengths to be compared, as well as the N—H⋯O=P hydrogen-bond strengths, and P=O/N—H vibrations. The following characteristics related to diastereotopic C6H5O/C6H5 groups in I/II were considered: geometry parameters, contributions to the crystal packing, solution 13C/1H NMR chemical shifts, conformations, and NMR coupling constants. The phosphorus-carbon coupling constants nJPC (n = 2 and 3) in I and mJPC (m = 1, 2, 3 and 4) in II were evaluated. For a comparative study, chiral analogous structures were retrieved from the Cambridge Structural Database (CSD) and their geometries and conformations are discussed.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextActa Crystallographica Section E: Crystallographic CommunicationsAugust 2023research communicationshttps://creativecommons.org/licenses/by/4.0/2023-08-0179med@iucr.org2056-98902056-98909Crystal structure and Hirshfeld surface analysis of 4-cyano-N-[(4-cyanophenyl)sulfonyl]-N-[2-(5-methylfuran-2-yl)phenyl]benzenesulfonamide
http://scripts.iucr.org/cgi-bin/paper?tx2071
In the title compound, C25H17N3O5S2, intramolecular π–π interactions [centroid-to-centroid distance = 3.5640 (9) Å] are observed between the furan and benzene rings of the 4-cyanophenyl group. In the crystal, molecules are connected via C—H⋯O and C—H⋯N hydrogen bonds, forming layers parallel to the (100) plane. These layers are interconnected by C—H⋯π interactions and weak van der Waals interactions. Hirshfeld surface analysis indicates that H⋯H (30.2%), N⋯H/H⋯N (22.3%), C⋯H/H⋯C (17.9%) and O⋯H/H⋯O (15.4%) interactions make the most significant contributions to the crystal packing.urn:issn:2056-9890Mammadova, G.Z.Yakovleva, E.D.Burkin, G.M.Khrustalev, V.N.Akkurt, M.Çelikesir, S.T.Bhattarai, A.text/htmlThe crystal structure features C—H⋯O and C—H⋯N hydrogen bonds, which link the molecules into layers parallel to the (100) plane. IC—H⋯π interactions and weak van der Waals interactions occur between the layers.doi:10.1107/S2056989023006254CRYSTAL STRUCTURE; SULFONAMIDES; HYDROGEN BONDS; C-H...[PI] INTERACTIONS; [PI]-[PI] INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-07-21Crystal structure and Hirshfeld surface analysis of 4-cyano-N-[(4-cyanophenyl)sulfonyl]-N-[2-(5-methylfuran-2-yl)phenyl]benzenesulfonamideIn the title compound, C25H17N3O5S2, intramolecular π–π interactions [centroid-to-centroid distance = 3.5640 (9) Å] are observed between the furan and benzene rings of the 4-cyanophenyl group. In the crystal, molecules are connected via C—H⋯O and C—H⋯N hydrogen bonds, forming layers parallel to the (100) plane. These layers are interconnected by C—H⋯π interactions and weak van der Waals interactions. Hirshfeld surface analysis indicates that H⋯H (30.2%), N⋯H/H⋯N (22.3%), C⋯H/H⋯C (17.9%) and O⋯H/H⋯O (15.4%) interactions make the most significant contributions to the crystal packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext751med@iucr.org2056-98902056-98908research communicationshttps://creativecommons.org/licenses/by/4.0/July 2023Acta Crystallographica Section E: Crystallographic Communications2023-07-2174779N-Cyclohexyltryptamine: freebase, bromide and fumarate
http://scripts.iucr.org/cgi-bin/paper?tx2070
The solid-state structures of N-cyclohexyltryptamine (I) {systematic name: N-[2-(1H-indol-3-yl)ethyl]cyclohexanamine}, C16H22N2, and two of its salts, N-cyclohexyltryptammonium bromide (II) {systematic name: N-[2-(1H-indol-3-yl)ethyl]cyclohexanaminium bromide}, C16H23N2+·Br−, and N-cyclohexyltryptammonium fumarate (III) (systematic name: bis{N-[2-(1H-indol-3-yl)ethyl]cyclohexanaminium} (2E)-but-2-enedioate), 2C16H23N2+·C4H2O42−, were determined by single-crystal X-ray diffraction. The freebase compound forms infinite chains along [010] through N—H⋯N hydrogen bonds. The bromide salt is held together by N—H⋯Br interactions in two-dimensional sheets along (001). The fumarate salt is held together in infinite three-dimensional frameworks by N—H⋯O hydrogen bonds.urn:issn:2056-9890Naeem, M.Le, A.N.Bauer, B.E.Chadeayne, A.R.Golen, J.A.Manke, D.R.text/htmlThe crystal structure of the freebase of the monoalkyl tryptamine N-cyclohexyltryptamine is presented, along with those of its bromide and fumarate salts.doi:10.1107/S2056989023006217CRYSTAL STRUCTURE; TRYPTAMINES; INDOLES; HYDROGEN BONDS2023-07-25N-Cyclohexyltryptamine: freebase, bromide and fumarateThe solid-state structures of N-cyclohexyltryptamine (I) {systematic name: N-[2-(1H-indol-3-yl)ethyl]cyclohexanamine}, C16H22N2, and two of its salts, N-cyclohexyltryptammonium bromide (II) {systematic name: N-[2-(1H-indol-3-yl)ethyl]cyclohexanaminium bromide}, C16H23N2+·Br−, and N-cyclohexyltryptammonium fumarate (III) (systematic name: bis{N-[2-(1H-indol-3-yl)ethyl]cyclohexanaminium} (2E)-but-2-enedioate), 2C16H23N2+·C4H2O42−, were determined by single-crystal X-ray diffraction. The freebase compound forms infinite chains along [010] through N—H⋯N hydrogen bonds. The bromide salt is held together by N—H⋯Br interactions in two-dimensional sheets along (001). The fumarate salt is held together in infinite three-dimensional frameworks by N—H⋯O hydrogen bonds.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98908756med@iucr.org79https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsJuly 20232023-07-25752Synthesis, optical properties and crystal structure of (E,E)-1,3-(3,4:9,10-dibenzododeca-1,11-diene-5,7-diyne-1,12-diyl)benzene
http://scripts.iucr.org/cgi-bin/paper?pk2689
The dehydrobenzannulene (E,E)-1,3-(3,4:9,10-dibenzododeca-1,11-diene-5,7-diyne-1,12-diyl)benzene, C26H16, was successfully synthesized via photocatalyst-assisted stereoselective reductive desulfonylation of 1,3-bis{1-phenylsulfonyl-2-[2-(trimethylsilylethynyl)phenyl]ethenyl}benzene, C44H42O4S2Si2, and subsequent desilylative cyclization of the resulting (E,E)-bis-silyl-protected dienyne, C32H34Si2. The structure of the dehydrobenzannulene thus obtained was confirmed by single-crystal X-ray analysis; three benzene rings are connected to one another by a 1,3-butadiynylene and a pair of ethenylene arrays. Although the π-system expanded efficiently in the dehydrobenzannulene, it was observed that the butadiynylene and ethenylene arrays were strained, showing smaller [171.3 (2)–172.6 (2) °] and larger bond angles [122.5 (2)–131.9 (2)°] than the conventional bond angles, respectively. In CHCl3, the dehydrobenzannulene showed the longest absorption band at 377 nm. When irradiated by UV light, it emitted fluorescence at 468 nm (ΦF = 0.26) and 504 nm (ΦF = 0.24) in CHCl3 and in the powdered state, respectively.urn:issn:2056-9890Watanabe, H.Sato, T.Sumita, M.Shiroyama, M.Sugawara, D.Tokuyama, T.Okuda, Y.Wakamatsu, K.Akashi, H.Orita, A.text/htmlA dehydrobenzannulene, (E,E)-1,3-(3,4:9,10-dibenzododeca-1,11-diene-5,7-diyne-1,12-diyl)benzene, was stereoselectively synthesized, and its crystal structure and UV-Vis absorption and photoluminescence optical properties were determined.doi:10.1107/S2056989023006187CRYSTAL STRUCTURE; EXPANDED [PI]-SYSTEM; DEHYDROBENZANNULENE; REDUCTIVE DESULFONYLATION2023-07-28Synthesis, optical properties and crystal structure of (E,E)-1,3-(3,4:9,10-dibenzododeca-1,11-diene-5,7-diyne-1,12-diyl)benzeneThe dehydrobenzannulene (E,E)-1,3-(3,4:9,10-dibenzododeca-1,11-diene-5,7-diyne-1,12-diyl)benzene, C26H16, was successfully synthesized via photocatalyst-assisted stereoselective reductive desulfonylation of 1,3-bis{1-phenylsulfonyl-2-[2-(trimethylsilylethynyl)phenyl]ethenyl}benzene, C44H42O4S2Si2, and subsequent desilylative cyclization of the resulting (E,E)-bis-silyl-protected dienyne, C32H34Si2. The structure of the dehydrobenzannulene thus obtained was confirmed by single-crystal X-ray analysis; three benzene rings are connected to one another by a 1,3-butadiynylene and a pair of ethenylene arrays. Although the π-system expanded efficiently in the dehydrobenzannulene, it was observed that the butadiynylene and ethenylene arrays were strained, showing smaller [171.3 (2)–172.6 (2) °] and larger bond angles [122.5 (2)–131.9 (2)°] than the conventional bond angles, respectively. In CHCl3, the dehydrobenzannulene showed the longest absorption band at 377 nm. When irradiated by UV light, it emitted fluorescence at 468 nm (ΦF = 0.26) and 504 nm (ΦF = 0.24) in CHCl3 and in the powdered state, respectively.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext761med@iucr.org2056-98902056-98908Acta Crystallographica Section E: Crystallographic CommunicationsJuly 2023research communicationshttps://creativecommons.org/licenses/by/4.0/7572023-07-2879Crystal structure of a 1:1 co-crystal of quabodepistat (OPC-167832) with 2,5-dihydroxybenzoic acid using microcrystal electron diffraction
http://scripts.iucr.org/cgi-bin/paper?dj2052
Quabodepistat [(5-{[(3R,4R)-1-(4-chloro-2,6-difluorophenyl)-3,4-dihydroxypiperidin-4-yl]methoxy}-8-fluoro-3,4-dihydroquinolin-2(1H)-one); C21H20ClF3N2O4] and 2,5-dihydroxybenzoic acid (2,5DHBA; C7H6O4) were successfully co-crystallized. Given the small size of the crystals (1 × 0.2 × 0.2 µm) the structure was solved via microcrystal electron diffraction (MicroED). The C—O and C=O bond-length ratio of the carboxylic group in 2,5DHBA is 1.08 (1.34 Å/1.24 Å), suggesting that 2,5DHBA remains protonated. Therefore, the material is a co-crystal rather than a salt. The amide group of quabodepistat participates in a cyclic hydrogen bond with the carboxylic group of the 2,5DHBA. Additional hydrogen bonds involving the quabodepistat amide and hydroxyl groups result in a three-dimensional network.urn:issn:2056-9890Sakamoto, N.Gato, K.text/htmlA co-crystal of quabodepistat and 2,5-dihydroxybenzoic acid was obtained and the crystal structure was solved from microcrystal electron diffraction (MicroED) data.doi:10.1107/S2056989023006047CRYSTAL STRUCTURE; CO-CRYSTAL; QUABODEPISTAT; 2,5-DIHYDROXYBENZOIC ACID; MICROCRYSTAL ELECTRON DIFFRACTION2023-09-19Crystal structure of a 1:1 co-crystal of quabodepistat (OPC-167832) with 2,5-dihydroxybenzoic acid using microcrystal electron diffractionQuabodepistat [(5-{[(3R,4R)-1-(4-chloro-2,6-difluorophenyl)-3,4-dihydroxypiperidin-4-yl]methoxy}-8-fluoro-3,4-dihydroquinolin-2(1H)-one); C21H20ClF3N2O4] and 2,5-dihydroxybenzoic acid (2,5DHBA; C7H6O4) were successfully co-crystallized. Given the small size of the crystals (1 × 0.2 × 0.2 µm) the structure was solved via microcrystal electron diffraction (MicroED). The C—O and C=O bond-length ratio of the carboxylic group in 2,5DHBA is 1.08 (1.34 Å/1.24 Å), suggesting that 2,5DHBA remains protonated. Therefore, the material is a co-crystal rather than a salt. The amide group of quabodepistat participates in a cyclic hydrogen bond with the carboxylic group of the 2,5DHBA. Additional hydrogen bonds involving the quabodepistat amide and hydroxyl groups result in a three-dimensional network.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-09-19October 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/102056-98902056-9890med@iucr.orgCrystal structure and luminescence spectrum of a one-dimensional nickel(II) coordination polymer incorporating 1,4-bis[(2-methylimidazol-1-yl)methyl]benzene and adamantane-1,3-dicarboxylate co-ligands
http://scripts.iucr.org/cgi-bin/paper?hb8041
An NiII coordination polymer, namely, poly[(μ2-adamantane-1,3-dicarboxylato-κ4O1,O1′:O3,O3′)[μ2-1,4-bis(2-methyl-imidazol-1-ylmethyl)benzene-κ2N3:N3′]nickel(II)], [Ni(C12H14O4)(C16H18N4)]n or [Ni(adc)(bmib)]n, (I) [adc = adamantane-1,3-dicarboxylate, C12H14O42– and bmib = 1,4-bis(2-methyl-imidazol-1-ylmethyl)benzene, C16H18N4] was synthesized and characterized. It exhibits a one-dimensional extended structure built up from alternating [Ni2(bmib)2] 26-membered rings and [Ni2(adc)2] 16-membered rings. The nickel atom lies on a crystallographic twofold axis and both ligands are completed by mirror symmetry. The solid-state luminescence spectra of (I) and the bmib ligand show strong emissions at 442 and 410 nm, respectively.urn:issn:2056-9890Zhang, Y.Qin, H.Wu, B.text/htmlThe title one-dimensional coordination polymer features alternating 26- and 16-membered rings.doi:10.1107/S2056989023006059CRYSTAL STRUCTURE; NICKEL; COORDINATION POLYMER2023-07-14Crystal structure and luminescence spectrum of a one-dimensional nickel(II) coordination polymer incorporating 1,4-bis[(2-methylimidazol-1-yl)methyl]benzene and adamantane-1,3-dicarboxylate co-ligandsAn NiII coordination polymer, namely, poly[(μ2-adamantane-1,3-dicarboxylato-κ4O1,O1′:O3,O3′)[μ2-1,4-bis(2-methyl-imidazol-1-ylmethyl)benzene-κ2N3:N3′]nickel(II)], [Ni(C12H14O4)(C16H18N4)]n or [Ni(adc)(bmib)]n, (I) [adc = adamantane-1,3-dicarboxylate, C12H14O42– and bmib = 1,4-bis(2-methyl-imidazol-1-ylmethyl)benzene, C16H18N4] was synthesized and characterized. It exhibits a one-dimensional extended structure built up from alternating [Ni2(bmib)2] 26-membered rings and [Ni2(adc)2] 16-membered rings. The nickel atom lies on a crystallographic twofold axis and both ligands are completed by mirror symmetry. The solid-state luminescence spectra of (I) and the bmib ligand show strong emissions at 442 and 410 nm, respectively.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextresearch communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsJuly 20237222023-07-1479725med@iucr.org2056-98902056-98908Crystal structure of K6[Zn(CO3)4]
http://scripts.iucr.org/cgi-bin/paper?pk2691
The crystal structure of K6[Zn(CO3)4], hexapotassium tetracarbonatozincate(II), comprises four unique potassium cations (two located on a general position, and two on the twofold rotation axis of the space group C2/c) and a [Zn(CO3)4]6− anion. The ZnII atom of the latter is located on the twofold rotation axis and is surrounded in a slightly distorted tetrahedral manner by two pairs of monodentately binding carbonate groups, with Zn—O distances of 1.9554 (18) and 1.9839 (18) Å. Both carbonate groups exhibit a slight deviation from planarity, with the C atom being shifted by 0.008 (2) and 0.006 (3) Å, respectively, from the plane of the three O atoms. The coordination numbers of the potassium cations range from 6 to 8, using a threshold of 3.0 Å for K—O bonding interactions being significant. In the crystal structure, [KOx] polyhedra and [Zn(CO3)4]6− groups share O atoms to build up the framework structure.urn:issn:2056-9890Eder, F.Weil, M.text/htmlThe crystal structure of the title compound comprises a tetracarbonatozincate(II) anion, [Zn(CO3)4]6−, with point-group symmetry 2 where the ZnII atom is surrounded in a distorted tetrahedral manner by four monodentate carbonate groups.doi:10.1107/S2056989023006072CRYSTAL STRUCTURE; ZINC IN TETRAHEDRAL COORDINATION; CARBONATE2023-07-14Crystal structure of K6[Zn(CO3)4]The crystal structure of K6[Zn(CO3)4], hexapotassium tetracarbonatozincate(II), comprises four unique potassium cations (two located on a general position, and two on the twofold rotation axis of the space group C2/c) and a [Zn(CO3)4]6− anion. The ZnII atom of the latter is located on the twofold rotation axis and is surrounded in a slightly distorted tetrahedral manner by two pairs of monodentately binding carbonate groups, with Zn—O distances of 1.9554 (18) and 1.9839 (18) Å. Both carbonate groups exhibit a slight deviation from planarity, with the C atom being shifted by 0.008 (2) and 0.006 (3) Å, respectively, from the plane of the three O atoms. The coordination numbers of the potassium cations range from 6 to 8, using a threshold of 3.0 Å for K—O bonding interactions being significant. In the crystal structure, [KOx] polyhedra and [Zn(CO3)4]6− groups share O atoms to build up the framework structure.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext721med@iucr.org2056-98902056-98908July 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications7182023-07-1479Crystal structure and Hirshfeld surface analysis of (E)-1-(2,4-dimethylfuran-3-yl)-3-phenylprop-2-en-1-one
http://scripts.iucr.org/cgi-bin/paper?vm2287
The title compound, C15H14O2, adopts an E configuration about the C=C double bond. The furan ring is inclined to the phenyl ring by 12.03 (9)°. In the crystal, pairs of molecules are linked by C—H⋯O hydrogen bonds, forming dimers with R22(14) ring motifs. The molecules are connected via C—H⋯π interactions, forming a three dimensional network. No π–π interactions are observed.urn:issn:2056-9890Khalilov, A.N.Khrustalev, V.N.Samigullina, A.I.Akkurt, M.Rzayev, R.M.Bhattarai, A.Mamedov, İ.G.text/htmlIn the crystal, pairs of molecules are linked by C—H⋯O hydrogen bonds, forming dimers with R_{2}^{2}(14) ring motifs. Molecules are connected via C—H⋯π interactions forming a three-dimensional network.doi:10.1107/S2056989023006084CRYSTAL STRUCTURE; 2,4-DIMETHYLFURAN; CHALCONES; HYDROGEN BOND; C-H...[PI] INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-07-14Crystal structure and Hirshfeld surface analysis of (E)-1-(2,4-dimethylfuran-3-yl)-3-phenylprop-2-en-1-oneThe title compound, C15H14O2, adopts an E configuration about the C=C double bond. The furan ring is inclined to the phenyl ring by 12.03 (9)°. In the crystal, pairs of molecules are linked by C—H⋯O hydrogen bonds, forming dimers with R22(14) ring motifs. The molecules are connected via C—H⋯π interactions, forming a three dimensional network. No π–π interactions are observed.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext740med@iucr.org2056-98902056-98908https://creativecommons.org/licenses/by/4.0/research communicationsJuly 2023Acta Crystallographica Section E: Crystallographic Communications2023-07-1473679Crystal-structure determination and Hirshfeld surface analysis of two new thiophene derivatives: (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]-5-fluorophenyl}benzenesulfonamide and (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]-5-fluorophenyl}-N-(but-2-yn-1-yl)benzenesulfonamide
http://scripts.iucr.org/cgi-bin/paper?zn2029
In the title compounds, C22H16FNO2S2 (I) and C26H20FNO2S2 (II), the benzothiophene rings are essentially planar with maximum deviations of 0.009 (1) and 0.001 (1) Å for the carbon and sulfur atom in compounds I and II, respectively. In I, the thiophene ring system is almost orthogonal to the phenyl ring attached to the sulfonyl group, with a dihedral angle of 77.7 (1)°. In compound I, the molecular structure is stabilized by weak C—H⋯O intramolecular interactions formed by the sulfone oxygen atoms, which generate two S(5) ring motifs. In the crystal of I, N—H⋯O hydrogen bonds link the molecules into R22(8) rings, which are connected into a C(10) chain via C—H⋯F hydrogen bonds. Intermolecular C—H⋯π interactions are also observed. In compound II, the molecules are linked via C—H⋯O and C—H⋯F hydrogen bonding, generating infinite C(11) and C(13) chains running parallel to [010].urn:issn:2056-9890Madhan, S.NizamMohideen, M.Pavunkumar, V.MohanaKrishnan, A.K.text/htmlThe crystal structures of two benzothiophene derivatives are described and the intermolecular contacts in the crystals analysed using Hirshfeld surface analysis and two-dimensional fingerprint plots.doi:10.1107/S2056989023006096CRYSTAL STRUCTURE; THIOPHENE; BENZOTHIOPHENE; FLUROPHENYL; PHENYLSULFONAMIDE HYDROGEN BONDING; HIRSHFELD SURFACE ANALYSIS2023-07-21Crystal-structure determination and Hirshfeld surface analysis of two new thiophene derivatives: (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]-5-fluorophenyl}benzenesulfonamide and (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]-5-fluorophenyl}-N-(but-2-yn-1-yl)benzenesulfonamideIn the title compounds, C22H16FNO2S2 (I) and C26H20FNO2S2 (II), the benzothiophene rings are essentially planar with maximum deviations of 0.009 (1) and 0.001 (1) Å for the carbon and sulfur atom in compounds I and II, respectively. In I, the thiophene ring system is almost orthogonal to the phenyl ring attached to the sulfonyl group, with a dihedral angle of 77.7 (1)°. In compound I, the molecular structure is stabilized by weak C—H⋯O intramolecular interactions formed by the sulfone oxygen atoms, which generate two S(5) ring motifs. In the crystal of I, N—H⋯O hydrogen bonds link the molecules into R22(8) rings, which are connected into a C(10) chain via C—H⋯F hydrogen bonds. Intermolecular C—H⋯π interactions are also observed. In compound II, the molecules are linked via C—H⋯O and C—H⋯F hydrogen bonding, generating infinite C(11) and C(13) chains running parallel to [010].https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext82056-98902056-9890med@iucr.org746792023-07-21741Acta Crystallographica Section E: Crystallographic CommunicationsJuly 2023https://creativecommons.org/licenses/by/4.0/research communicationsCrystal structures of four organic salts of trihexyphenidyl at 90 K
http://scripts.iucr.org/cgi-bin/paper?vm2286
The syntheses and crystal structure studies of four organic salts of trihexyphenidyl, viz., trihexyphenidylium [1-(3-cyclohexyl-3-hydroxy-3-phenylpropyl)piperidin-1-ium] 4-nitrobenzoate, C20H32NO+·C7H4NO4− (I), trihexyphenidylium 4-hydroxybenzoate, C20H32NO+·C7H5O− (II), trihexyphenidylium 4-bromobenzoate, C20H32NO+·C7H4BrO2− (III), and trihexyphenidylium thiophene-2-carboxylate hemihydrate, 2C20H32NO+·2C5H3O2S−·H2O (IV), conducted at 90 K are described. Structures I, II, and III are solvent free with one cation–anion pair per asymmetric unit, while IV crystallizes as a hemihydrate, having two cation–anion pairs and one water of crystallization in its asymmetric unit. Structures I and III exhibit configurational disorder of the cation. Structure IV also exhibits disorder, but only of the thiophene-2-carboxylate anions. Structure II is a non-merohedric twin by a twofold rotation about [403]. The main supramolecular motifs in I, II, and III are similar R22(10) rings between cation–anion pairs, although their packing within the crystals is distinct. As a consequence of having two cation–anion pairs and a water molecule in its asymmetric unit, the packing in IV is by far the most complex of the four structures, its hydrogen-bonding patterns being quite different from I, II, or III. In all the crystals studied, N—H⋯O, O—H⋯O, and C—H⋯O interactions are observed, plus C—H⋯Br close contacts for III.urn:issn:2056-9890VinayaBasavaraju, Y.B.Yathirajan, H.S.Parkin, S.text/htmlThe low-temperature crystal structures of four organic salts of the anti-spasmodic drug trihexyphenidyl are presented.doi:10.1107/S2056989023005960TRIHEXYPHENIDYL; TRIHEXYPHENIDYLIUM CATION; CRYSTAL STRUCTURE; DISORDER; TWINNING; NON-MEROHEDRY; HYDROGEN BONDING2023-07-14Crystal structures of four organic salts of trihexyphenidyl at 90 KThe syntheses and crystal structure studies of four organic salts of trihexyphenidyl, viz., trihexyphenidylium [1-(3-cyclohexyl-3-hydroxy-3-phenylpropyl)piperidin-1-ium] 4-nitrobenzoate, C20H32NO+·C7H4NO4− (I), trihexyphenidylium 4-hydroxybenzoate, C20H32NO+·C7H5O− (II), trihexyphenidylium 4-bromobenzoate, C20H32NO+·C7H4BrO2− (III), and trihexyphenidylium thiophene-2-carboxylate hemihydrate, 2C20H32NO+·2C5H3O2S−·H2O (IV), conducted at 90 K are described. Structures I, II, and III are solvent free with one cation–anion pair per asymmetric unit, while IV crystallizes as a hemihydrate, having two cation–anion pairs and one water of crystallization in its asymmetric unit. Structures I and III exhibit configurational disorder of the cation. Structure IV also exhibits disorder, but only of the thiophene-2-carboxylate anions. Structure II is a non-merohedric twin by a twofold rotation about [403]. The main supramolecular motifs in I, II, and III are similar R22(10) rings between cation–anion pairs, although their packing within the crystals is distinct. As a consequence of having two cation–anion pairs and a water molecule in its asymmetric unit, the packing in IV is by far the most complex of the four structures, its hydrogen-bonding patterns being quite different from I, II, or III. In all the crystals studied, N—H⋯O, O—H⋯O, and C—H⋯O interactions are observed, plus C—H⋯Br close contacts for III.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext735med@iucr.org2056-98902056-98908research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsJuly 20237302023-07-1479Crystal structure of poly[(acetonitrile-κN)(μ3-7-{[bis(pyridin-2-ylmethyl)amino]methyl}-8-hydroxyquinoline-5-sulfonato-κ4N,O:O′:O′′)sodium]
http://scripts.iucr.org/cgi-bin/paper?yz2037
In the title compound, [Na(C22H19N4O4S)(CH3CN)]n, the NaI atom adopts a distorted square-pyramidal coordination geometry, formed by one N and one O atom of the qunolinol moiety in the ligand, two O atoms of sulfonate moieties of two adjacent ligands and the N atom of the coordinated acetonitrile solvent. The NaI atom is located well above the mean basal plane of the square-based pyramid. The apical position is occupied by a sulfonate O atom of a neighboring ligand. Three N atoms of the bis(pyridin-2-ylmethyl)amine moiety in the ligand are not coordinated by the sodium atom. The molecule forms an intramolecular bifurcated O—H⋯[N(tertiary amine),N(pyridine)] hydrogen bond, generating S(6) and S(5) rings. In the crystal, four molecules are linked by four Na—O(sulfonato) bridged coordination bonds, forming a supramolecular centrosymmetric tetramer unit comprising an eight-membered ring, and generating a two-dimensional network sheet. The molecules of different sheets form intermolecular C—H⋯O hydrogen bonds, and thereby a three-dimensional network structure.urn:issn:2056-9890Kubono, K.Tanaka, R.Kashiwagi, Y.Tani, K.Yokoi, K.text/htmlIn the title compound, the NaI atom has a distorted square-pyramidal coordination environment. The molecular structure exhibits an intramolecular bifurcated O—H⋯[N(tertiary amine), N(pyridyl)] hydrogen bond. In the crystal, the molecules are linked by the bridging Na—O(sulfonato) coordination bonds and the intermolecular C—H⋯O hydrogen bonds, forming a three-dimensional network structure.doi:10.1107/S2056989023005959CRYSTAL STRUCTURE; COORDINATION POLYMER; SODIUM COMPLEX; 8-HYDROXYQUINOLINE SULFONATO; C-H...O INTERACTIONS2023-07-14Crystal structure of poly[(acetonitrile-κN)(μ3-7-{[bis(pyridin-2-ylmethyl)amino]methyl}-8-hydroxyquinoline-5-sulfonato-κ4N,O:O′:O′′)sodium]In the title compound, [Na(C22H19N4O4S)(CH3CN)]n, the NaI atom adopts a distorted square-pyramidal coordination geometry, formed by one N and one O atom of the qunolinol moiety in the ligand, two O atoms of sulfonate moieties of two adjacent ligands and the N atom of the coordinated acetonitrile solvent. The NaI atom is located well above the mean basal plane of the square-based pyramid. The apical position is occupied by a sulfonate O atom of a neighboring ligand. Three N atoms of the bis(pyridin-2-ylmethyl)amine moiety in the ligand are not coordinated by the sodium atom. The molecule forms an intramolecular bifurcated O—H⋯[N(tertiary amine),N(pyridine)] hydrogen bond, generating S(6) and S(5) rings. In the crystal, four molecules are linked by four Na—O(sulfonato) bridged coordination bonds, forming a supramolecular centrosymmetric tetramer unit comprising an eight-membered ring, and generating a two-dimensional network sheet. The molecules of different sheets form intermolecular C—H⋯O hydrogen bonds, and thereby a three-dimensional network structure.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext729med@iucr.org2056-98902056-98908Acta Crystallographica Section E: Crystallographic CommunicationsJuly 2023research communicationshttps://creativecommons.org/licenses/by/4.0/2023-07-1472679Crystal structure of bis{S-octyl-3-[(thiophen-2-yl)methylidene]dithiocarbazato-κ2N3,S}nickel(II)
http://scripts.iucr.org/cgi-bin/paper?pk2690
In the title complex, [Ni(C14H21N2S3)2], the nickel(II) atom is located on a crystallographic inversion center and exhibits a square-planar coordination environment, being coordinated by two negatively charged N,S-chelating ligands in a trans configuration. In the crystal, the non-H atoms of the complex are practically coplanar (r.m.s. deviation of fitted atoms = 0.135 Å), and the angle between the thienyl and the chelating rings is 6.7 (1)°. The molecules stack at a distance of 3.623 (2) Å along the b-axis direction.urn:issn:2056-9890Khan, S.S.Howlader, M.B.H.Sheikh, M.C.Miyatake, R.Zangrando, E.text/htmlThe mononuclear nickel(II) complex is bis-chelated by dithiocarbazato ligands bearing a thienyl ring and an n-octyl alkyl chain.doi:10.1107/S2056989023005935CRYSTAL STRUCTURE; NICKEL(II) COMPLEX; DITHIOCARBAZATO LIGAND2023-07-11Crystal structure of bis{S-octyl-3-[(thiophen-2-yl)methylidene]dithiocarbazato-κ2N3,S}nickel(II)In the title complex, [Ni(C14H21N2S3)2], the nickel(II) atom is located on a crystallographic inversion center and exhibits a square-planar coordination environment, being coordinated by two negatively charged N,S-chelating ligands in a trans configuration. In the crystal, the non-H atoms of the complex are practically coplanar (r.m.s. deviation of fitted atoms = 0.135 Å), and the angle between the thienyl and the chelating rings is 6.7 (1)°. The molecules stack at a distance of 3.623 (2) Å along the b-axis direction.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext82056-98902056-9890med@iucr.org717792023-07-11714https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsJuly 2023Synthesis and crystal structures of three Schiff bases derived from 3-formylacetylacetone and benzyl-, tert-butyl- and (S)-methylbenzylamine
http://scripts.iucr.org/cgi-bin/paper?wm5685
Treatment of 3-formylacetylacetone with the amines benzylamine, tert-butylamine and (S)-methylbenzylamine led to the formation of the corresponding Schiff bases 3-[(benzylamino)methylidene]pentane-2,4-dione, C13H15NO2 (1), 3-[(tert-butylamino)methylidene]pentan-2,4-dione, C10H17NO2 (2) and 3-{[(S)-benzyl(methyl)amino]methylidene}pentane-2,4-dione, C14H17NO2 (3). The molecules of all three compounds exist as enamine tautomers that contain a nearly planar amino-methylene-pentane-2,4-dione core with a strong intramolecular N—H⋯O hydrogen bridge. The R group attached to the enamine N atom has no significant influence on the bond lengths and angles of the amino-methylene-pentane-2,4-dione core. The supramolecular structures in 1–3 are mainly based on weak C—H⋯O hydrogen bonds.urn:issn:2056-9890Halz, J.H.Hentsch, A.Wagner, C.Merzweiler, K.text/htmlThe crystal structures of three Schiff bases synthesized from 3-formylaceylacetone and different primary amines were determined and compared with simulated gas phase structures based on DFT calculations.doi:10.1107/S205698902300587XCRYSTAL STRUCTURE; ENAMINE; 3-FORMYLACETYLACETONE; SCHIFF BASE2023-07-11Synthesis and crystal structures of three Schiff bases derived from 3-formylacetylacetone and benzyl-, tert-butyl- and (S)-methylbenzylamineTreatment of 3-formylacetylacetone with the amines benzylamine, tert-butylamine and (S)-methylbenzylamine led to the formation of the corresponding Schiff bases 3-[(benzylamino)methylidene]pentane-2,4-dione, C13H15NO2 (1), 3-[(tert-butylamino)methylidene]pentan-2,4-dione, C10H17NO2 (2) and 3-{[(S)-benzyl(methyl)amino]methylidene}pentane-2,4-dione, C14H17NO2 (3). The molecules of all three compounds exist as enamine tautomers that contain a nearly planar amino-methylene-pentane-2,4-dione core with a strong intramolecular N—H⋯O hydrogen bridge. The R group attached to the enamine N atom has no significant influence on the bond lengths and angles of the amino-methylene-pentane-2,4-dione core. The supramolecular structures in 1–3 are mainly based on weak C—H⋯O hydrogen bonds.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext7072023-07-11research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsJuly 202379med@iucr.org71382056-98902056-9890(NH4)2[UO2Cl4]·2H2O, a new uranyl tetrachloride with ammonium charge-balancing cations
http://scripts.iucr.org/cgi-bin/paper?pk2687
A new uranyl tetrachloride salt with chemical formula, (NH4)2[UO2Cl4]·2H2O, namely, diammonium uranyl tetrachloride dihydrate, 1, was prepared and crystallized via slow evaporation from a solution of 2 M hydrochloric acid. As confirmed by powder X-ray diffraction, the title compound crystallizes with an ammonium chloride impurity that formed as a result of the breakdown of a triazine precursor. The (UO2Cl4)2− dianion is charge balanced by ammonium cations, while an extensive hydrogen-bond network donated from structural water molecules stabilize the overall assembly. Compound 1 adds to the extensive collection of actinyl tetrachloride salts, but it represents the first without an alkali cation for purely inorganic compounds. Diffuse reflectance and luminescence spectra show typical absorption and emission behavior, respectively, of uranyl materials.urn:issn:2056-9890Kohlgruber, T.A.Surbella III, R.G.text/htmlWhile several actinyl tetrahalides have been synthesized and their structures reported, (NH4)2(UO2Cl4)·2H2O represents a new uranyl tetrachloride salt synthesized in a slow evaporation from a 2 M hydrochloric acid solution. Its optical properties were measured by diffuse reflectance and luminescence spectroscopies, while powder X-ray diffraction confirmed an ammonium chloride impurity phase.doi:10.1107/S2056989023005753AMMONIUM; OPTICAL PROPERTIES; URANYL TETRACHLORIDE; X-RAY DIFFRACTION; CRYSTAL STRUCTURE2023-07-07(NH4)2[UO2Cl4]·2H2O, a new uranyl tetrachloride with ammonium charge-balancing cationsA new uranyl tetrachloride salt with chemical formula, (NH4)2[UO2Cl4]·2H2O, namely, diammonium uranyl tetrachloride dihydrate, 1, was prepared and crystallized via slow evaporation from a solution of 2 M hydrochloric acid. As confirmed by powder X-ray diffraction, the title compound crystallizes with an ammonium chloride impurity that formed as a result of the breakdown of a triazine precursor. The (UO2Cl4)2− dianion is charge balanced by ammonium cations, while an extensive hydrogen-bond network donated from structural water molecules stabilize the overall assembly. Compound 1 adds to the extensive collection of actinyl tetrachloride salts, but it represents the first without an alkali cation for purely inorganic compounds. Diffuse reflectance and luminescence spectra show typical absorption and emission behavior, respectively, of uranyl materials.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext706med@iucr.org2056-98902056-98908Acta Crystallographica Section E: Crystallographic CommunicationsJuly 2023https://creativecommons.org/licenses/by/4.0/research communications7022023-07-0779Synthesis and crystal structure of a bench-stable pyridinium ketene hemiaminal: 1-(1-ethoxyethenyl)-2-[methyl(phenyl)amino]pyridin-1-ium trifluoromethanesulfonate
http://scripts.iucr.org/cgi-bin/paper?zl5048
The novel bench-stable N-quaternized ketene N,O-acetal, C16H19N2O+·CF3O3S−, was synthesized and its structure determined. The title compound is a rare example of a pyridinium ketene hemiaminal for which a crystal structure has been determined, joining the 2-chloro-1-(1-ethyoxyethenyl)pyridin-1-ium trifluoromethanesulfonate salt from which it was synthesized. The cationic species of the title compound can be defined by three individually planar fragments assembling into a non-coplanar cation. The phenyl substituent extending from the amino nitrogen atom and the ethyoxyvinyl substituent extending from the pyridine N atom are oriented on the same side of the molecule and maintain the closest coplanar relationship of the three fragments. Supramolecular interactions are dominated by C—H⋯O interactions from the cation to the SO3 side of the trifluoromethanesulfonate anion, forming a two-dimensional substructure.urn:issn:2056-9890Krevlin, Z.A.Bote, I.C.Crespo, M.C.F.Lam, C.C.McMillen, C.D.Majireck, M.M.text/htmlThe N-quaternized ketene N,O-acetal, 1-(1-ethoxyvinyl)-2-(methyl(phenyl)amino)pyridin-1-ium trifluoromethanesulfonate was synthesized and its structure determined, making it a rare example of this class of compounds to be structurally characterized.doi:10.1107/S2056989023005741CRYSTAL STRUCTURE; KETENE HEMIAMINAL; N-QUATERNIZED KETENE N,O-ACETAL2023-07-07Synthesis and crystal structure of a bench-stable pyridinium ketene hemiaminal: 1-(1-ethoxyethenyl)-2-[methyl(phenyl)amino]pyridin-1-ium trifluoromethanesulfonateThe novel bench-stable N-quaternized ketene N,O-acetal, C16H19N2O+·CF3O3S−, was synthesized and its structure determined. The title compound is a rare example of a pyridinium ketene hemiaminal for which a crystal structure has been determined, joining the 2-chloro-1-(1-ethyoxyethenyl)pyridin-1-ium trifluoromethanesulfonate salt from which it was synthesized. The cationic species of the title compound can be defined by three individually planar fragments assembling into a non-coplanar cation. The phenyl substituent extending from the amino nitrogen atom and the ethyoxyvinyl substituent extending from the pyridine N atom are oriented on the same side of the molecule and maintain the closest coplanar relationship of the three fragments. Supramolecular interactions are dominated by C—H⋯O interactions from the cation to the SO3 side of the trifluoromethanesulfonate anion, forming a two-dimensional substructure.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79Acta Crystallographica Section E: Crystallographic CommunicationsJuly 2023research communicationshttps://creativecommons.org/licenses/by/4.0/2023-07-076982056-98902056-98908701med@iucr.orgCo-crystallization of N′-benzylidenepyridine-4-carbohydrazide and benzoic acid via autoxidation of benzaldehyde
http://scripts.iucr.org/cgi-bin/paper?ex2072
The 1:1 co-crystal N′-[(2-methylphenyl)methylidene]pyridine-4-carbohydrazide–benzoic acid (1/1), C13H11N3O·C7H6O2, formed unexpectedly after autoxidation of benzaldehyde during the slow evaporation process of a solution of isoniazid in benzaldehyde. The original intent of the synthesis was to modify isoniazid with benzaldehyde and crystallize the product in order to improve efficacy against Mycobacteria species, but benzoic acid formed spontaneously and co-crystallized with the intended product, N′-benzylidenepyridine-4-carbohydrazide.urn:issn:2056-9890Setshedi, I.B.Lemmerer, A.Smith, M.G.text/htmlThe 1:1 co-crystal N′-[(2-methylphenyl)methylidene]pyridine-4-carbohydrazide–benzoic acid (1/1) formed unexpectedly after autoxidation of benzaldehyde during the slow evaporation process of a solution of isoniazid in benzaldehyde. The original intent of the synthesis was to modify isoniazid with benzaldehyde and crystallize the product in order to improve efficacy against Mycobacteria species, but benzoic acid formed spontaneously and co-crystallized with the intended product, N′-benzylidenepyridine-4-carbohydrazide.doi:10.1107/S2056989023005698CRYSTAL STRUCTURE; AUTOXIDATION; BENZOIC ACID; ISONIAZID2023-07-04Co-crystallization of N′-benzylidenepyridine-4-carbohydrazide and benzoic acid via autoxidation of benzaldehydeThe 1:1 co-crystal N′-[(2-methylphenyl)methylidene]pyridine-4-carbohydrazide–benzoic acid (1/1), C13H11N3O·C7H6O2, formed unexpectedly after autoxidation of benzaldehyde during the slow evaporation process of a solution of isoniazid in benzaldehyde. The original intent of the synthesis was to modify isoniazid with benzaldehyde and crystallize the product in order to improve efficacy against Mycobacteria species, but benzoic acid formed spontaneously and co-crystallized with the intended product, N′-benzylidenepyridine-4-carbohydrazide.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext82056-98902056-9890med@iucr.org792023-07-04Acta Crystallographica Section E: Crystallographic CommunicationsJuly 2023https://creativecommons.org/licenses/by/4.0/research communicationsThe synthesis, crystal structure and spectroscopic analysis of (E)-3-(4-chlorophenyl)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)prop-2-en-1-one
http://scripts.iucr.org/cgi-bin/paper?vm2285
The synthesis, crystal structure and spectroscopic analysis of (E)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-3-(4-chlorophenyl)prop-2-en-1-one (C17H13ClO3), a substituted chalcone, are described. The overall geometry of the molecule is largely planar (r.m.s. deviation = 0.1742 Å), but slightly kinked, leading to a dihedral angle between the planes of the benzene rings at either side of the molecule of 8.31 (9)°. In the crystal, only weak interactions determine the packing motifs. These include C—H⋯O and C—H⋯Cl hydrogen bonds and π–π overlap of aromatic rings.urn:issn:2056-9890VinayaRichard, A.S.Murthy, S.M.Basavaraju, Y.B.Yathirajan, H.S.Parkin, S.text/htmlThe synthesis, crystal structure and some spectroscopic details for (E)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-3-(4-chlorophenyl)prop-2-en-1-one are presented.doi:10.1107/S2056989023005613CRYSTAL STRUCTURE; CHALCONE; [PI]-[PI] INTERACTION2023-06-30The synthesis, crystal structure and spectroscopic analysis of (E)-3-(4-chlorophenyl)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)prop-2-en-1-oneThe synthesis, crystal structure and spectroscopic analysis of (E)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-3-(4-chlorophenyl)prop-2-en-1-one (C17H13ClO3), a substituted chalcone, are described. The overall geometry of the molecule is largely planar (r.m.s. deviation = 0.1742 Å), but slightly kinked, leading to a dihedral angle between the planes of the benzene rings at either side of the molecule of 8.31 (9)°. In the crystal, only weak interactions determine the packing motifs. These include C—H⋯O and C—H⋯Cl hydrogen bonds and π–π overlap of aromatic rings.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org67772056-98902056-98906742023-06-30https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsJune 202379Synthesis, crystal structure and Hirshfeld surface analysis of naphthalene-2,3-diyl bis(3-benzyloxy)benzoate
http://scripts.iucr.org/cgi-bin/paper?hb8069
In the title compound, C38H28O6, the dihedral angles between the naphthalene ring system and its pendant benzyloxy rings A and B are 88.05 (7) and 80.84 (7)°, respectively. The dihedral angles between the A and B rings and their attached phenyl rings are 49.15 (8) and 80.78 (8)°, respectively. In the extended structure, the molecules are linked by weak C—H⋯O and C—H⋯π hydrogen bonds, and π–π stacking interactions, which variously generate C(11) chains and R22(12) loops as part of a three-dimensional network. The Hirshfeld surface [fingerprint contributions = H⋯H (42.3%), C⋯H/H⋯C (40.3%) and O⋯H/H⋯O (15.7%)] and intermolecular interaction energies are reported, with dispersion (Edis = −428.6 kJ mol−1) being the major contributor.urn:issn:2056-9890Anil Kumar, H.Selvanandan, S.Srinivasa, H.T.Venkateshappa, G.Palakshamurthy, B.S.text/htmlIn the title compound, C38H28O6, the dihedral angles between the naphthalene ring system and its pendant benzyloxy rings A and B are 88.05 (7) and 80.84 (7)°, respectively. The dihedral angles between the A and B rings and their attached phenyl rings are 49.15 (8) and 80.78 (8)°, respectively. In the extended structure, the molecules are linked by weak C—H⋯O and C—H⋯π bonds and π–π stacking interactions, which variously generate C(11) chains and R_{2}^{2}(12) loops as part of a three-dimensional network. The Hirshfeld surface [fingerprint contributions = H⋯H (42.3%), C⋯H/H⋯C (40.3%) and O⋯H/H⋯O (15.7%)] and intermolecular interaction energies are reported, with dispersion, Edis at −428.6 kJ mol−1 being the major contributor.doi:10.1107/S2056989023005571CRYSTAL STRUCTURE; NAPHTHALENE; HIRSHFELD SURFACE; BENZOATE2023-07-04Synthesis, crystal structure and Hirshfeld surface analysis of naphthalene-2,3-diyl bis(3-benzyloxy)benzoateIn the title compound, C38H28O6, the dihedral angles between the naphthalene ring system and its pendant benzyloxy rings A and B are 88.05 (7) and 80.84 (7)°, respectively. The dihedral angles between the A and B rings and their attached phenyl rings are 49.15 (8) and 80.78 (8)°, respectively. In the extended structure, the molecules are linked by weak C—H⋯O and C—H⋯π hydrogen bonds, and π–π stacking interactions, which variously generate C(11) chains and R22(12) loops as part of a three-dimensional network. The Hirshfeld surface [fingerprint contributions = H⋯H (42.3%), C⋯H/H⋯C (40.3%) and O⋯H/H⋯O (15.7%)] and intermolecular interaction energies are reported, with dispersion (Edis = −428.6 kJ mol−1) being the major contributor.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext82056-98902056-9890med@iucr.org792023-07-04Acta Crystallographica Section E: Crystallographic CommunicationsJuly 2023https://creativecommons.org/licenses/by/4.0/research communicationsCrystal structures and Hirshfeld surface analyses of N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol tribromide (1/1), N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol dibromidoiodate (1/1) and N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol dichloridoiodate (1/1)
http://scripts.iucr.org/cgi-bin/paper?yz2034
In the title compounds, N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol tribromide (1/1), C4H9NO·C4H10NO+·Br3− or [(C4H9NO)·(C4H10NO)](Br3), (I), N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol dibromidoiodate (1/1), C4H9NO·C4H10NO+·Br2I− or [(C4H9NO)·(C4H10NO)](Br2I), (II), and N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol dichloridoiodate (1/1), C4H9NO·C4H10NO+·Cl2I− or [(C4H9NO)·(C4H10NO)]·(Cl2I), (III), all the anions are almost linear in geometry and all the cations, except for the methyl H atoms, are essentially planar. In the crystal structure of (I), the cations are linked by pairs of C—H⋯O hydrogen bonds, forming inversion dimers with an R22(8) ring motif. These dimers also exhibit O—H⋯O hydrogen bonding. Dimerized cation pairs and anions are arranged in columns along the a axis. In the crystal of (II), the cations are linked by pairs of O—H⋯O and C—H⋯O hydrogen bonds, forming an R44(14) ring motif. These groups of cations and the anions form individual columns along the a axis and jointly reside in planes roughly parallel to (011). In the crystal of (III), cations and anions also form columns parallel to the a axis, resulting in layers parallel to the (020) plane. Furthermore, the crystal structures of (I), (II) and (III) are consolidated by strong halogen (Br and/or I and/or Cl)⋯H and weak van der Waals interactions. In addition to the structural evaluation, a Hirshfeld surface analysis was carried out.urn:issn:2056-9890Mammadova, G.Z.Mertsalov, D.F.Shchevnikov, D.M.Grigoriev, M.S.Akkurt, M.Yıldırım, S. Ö.Bhattarai, A.text/htmlIn all three title crystals, the cations are linked by O—H⋯O and/or C—H⋯O hydrogen bonds. The three-dimensional packing is further consolidated by strong halogen–hydrogen and weak van der Waals interactions.doi:10.1107/S2056989023005509CRYSTAL STRUCTURE; DIMETHYLACETAMIDE; TRIHALIDE; HYDROGEN BOND; HIRSHFELD SURFACE ANALYSIS2023-07-04Crystal structures and Hirshfeld surface analyses of N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol tribromide (1/1), N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol dibromidoiodate (1/1) and N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol dichloridoiodate (1/1)In the title compounds, N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol tribromide (1/1), C4H9NO·C4H10NO+·Br3− or [(C4H9NO)·(C4H10NO)](Br3), (I), N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol dibromidoiodate (1/1), C4H9NO·C4H10NO+·Br2I− or [(C4H9NO)·(C4H10NO)](Br2I), (II), and N,N-dimethylacetamide–1-(dimethyl-λ4-azanylidene)ethan-1-ol dichloridoiodate (1/1), C4H9NO·C4H10NO+·Cl2I− or [(C4H9NO)·(C4H10NO)]·(Cl2I), (III), all the anions are almost linear in geometry and all the cations, except for the methyl H atoms, are essentially planar. In the crystal structure of (I), the cations are linked by pairs of C—H⋯O hydrogen bonds, forming inversion dimers with an R22(8) ring motif. These dimers also exhibit O—H⋯O hydrogen bonding. Dimerized cation pairs and anions are arranged in columns along the a axis. In the crystal of (II), the cations are linked by pairs of O—H⋯O and C—H⋯O hydrogen bonds, forming an R44(14) ring motif. These groups of cations and the anions form individual columns along the a axis and jointly reside in planes roughly parallel to (011). In the crystal of (III), cations and anions also form columns parallel to the a axis, resulting in layers parallel to the (020) plane. Furthermore, the crystal structures of (I), (II) and (III) are consolidated by strong halogen (Br and/or I and/or Cl)⋯H and weak van der Waals interactions. In addition to the structural evaluation, a Hirshfeld surface analysis was carried out.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytexthttps://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsJuly 20232023-07-0479med@iucr.org2056-98902056-98908Crystallographic and spectroscopic characterization of two 1-phenyl-1H-imidazoles: 4-(1H-imidazol-1-yl)benzaldehyde and 1-(4-methoxyphenyl)-1H-imidazole
http://scripts.iucr.org/cgi-bin/paper?jy2032
The title compounds, C10H8N2O, (I), and C10H10N2O, (II), are two 1-phenyl-1H-imidazole derivatives, which differ in the substituent para to the imidazole group on the arene ring, i.e. a benzaldehyde, (I), and an anisole, (II). Both molecules pack with different motifs via similar weak C—H⋯N/O interactions and differ with respect to the angles between the mean planes of the imidazole and arene rings [24.58 (7)° in (I) and 43.67 (4)° in (II)].urn:issn:2056-9890McClements, I.F.Wiesler, C.R.Tanski, J.M.text/htmlTwo 1-phenyl-1H-imidazoles, 4-(1H-imidazol-1-yl)benzaldehyde and 1-(4-methoxyphenyl)-1H-imidazole, differ in the substituent para to the imidazole group on the arene ring. Both molecules pack with different motifs via similar weak C—H⋯N/O interactions and differ with respect to the angles between the mean planes of the imidazole and arene rings.doi:10.1107/S2056989023005480CRYSTAL STRUCTURE; 1-PHENYL-1H-IMIDAZOLE DERIVATIVES; WEAK INTERMOLECULAR INTERACTIONS; NON-CENTROSYMMETRIC SPACE GROUP2023-06-30Crystallographic and spectroscopic characterization of two 1-phenyl-1H-imidazoles: 4-(1H-imidazol-1-yl)benzaldehyde and 1-(4-methoxyphenyl)-1H-imidazoleThe title compounds, C10H8N2O, (I), and C10H10N2O, (II), are two 1-phenyl-1H-imidazole derivatives, which differ in the substituent para to the imidazole group on the arene ring, i.e. a benzaldehyde, (I), and an anisole, (II). Both molecules pack with different motifs via similar weak C—H⋯N/O interactions and differ with respect to the angles between the mean planes of the imidazole and arene rings [24.58 (7)° in (I) and 43.67 (4)° in (II)].https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98907681med@iucr.org79June 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-06-30678Synthesis, crystal structure and Hirshfeld surface analysis of tert-butyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate
http://scripts.iucr.org/cgi-bin/paper?zn2030
The 1,4-dihydropyridine ring of the title compound, C24H29F2NO4, adopts a distorted boat conformation, while the cyclohexene ring is in an almost twist-boat conformation. In the crystal, N—H⋯O and C—H⋯O hydrogen bonds as well as C—H⋯π interactions connect molecules, forming layers parallel to the (100) plane. These layers are linked by van der Waals forces and C—H⋯F interactions, which consolidate the crystal structure. Hirshfeld surface analysis shows the major contributions to the crystal packing are from H⋯H (54.1%), F⋯H/H⋯F (16.9%), O⋯H/H⋯O (15.4%) and C⋯H/H⋯C (12.6%) contacts.urn:issn:2056-9890Pehlivanlar, E.Yıldırım, S. Ö.Şimşek, R.Akkurt, M.Butcher, R.J.Bhattarai, A.text/htmlIn the crystal, molecules are connected via N—H⋯O and C—H⋯O hydrogen bonds and C—H⋯π interactions, forming layers parallel to the (100) plane. van der Waals forces and C—H⋯F interactions connect these layers, consolidating the crystal structure.doi:10.1107/S2056989023005455CRYSTAL STRUCTURE; HYDROGEN BONDS; VAN DER WAALS FORCES; C-H...F INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-06-30Synthesis, crystal structure and Hirshfeld surface analysis of tert-butyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylateThe 1,4-dihydropyridine ring of the title compound, C24H29F2NO4, adopts a distorted boat conformation, while the cyclohexene ring is in an almost twist-boat conformation. In the crystal, N—H⋯O and C—H⋯O hydrogen bonds as well as C—H⋯π interactions connect molecules, forming layers parallel to the (100) plane. These layers are linked by van der Waals forces and C—H⋯F interactions, which consolidate the crystal structure. Hirshfeld surface analysis shows the major contributions to the crystal packing are from H⋯H (54.1%), F⋯H/H⋯F (16.9%), O⋯H/H⋯O (15.4%) and C⋯H/H⋯C (12.6%) contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79June 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/6642023-06-302056-98902056-98907668med@iucr.orgcatena-Poly[[bis(diaqualithium)]-μ4-3,3′,5,5′-tetranitro-4,4′-bipyrazole-1,1′-diido]: a new moisture-insensitive alkali-metal energetic salt with a well-defined network structure
http://scripts.iucr.org/cgi-bin/paper?pk2688
In the structure of the title salt, [Li2(C6N8O8)(H2O)4]n, the 3,3′,5,5′-tetranitro-4,4′-bipyrazole-1,1′-diide dianion [{TNBPz}2−] is situated across the twofold axis. The distorted coordination octahedra around Li+ involve four short bonds with two pyrazolate N atoms and two aqua ligands [Li—N(O) = 1.999 (3)–2.090 (2) Å] and two longer contacts with nitro-O atoms [2.550 (2), 2.636 (2) Å]. When combined with μ4-{TNBPz}2−, this generates a mono-periodic polymeric structure incorporating discrete centrosymmeric [(H2O)2Li–(dinitropyrazolato)2–Li(H2O)2] units. The three-dimensional stack of mutually orthogonal coordination chains is reminiscent of a Lincoln log pattern. It is influenced by conventional hydrogen bonding [O⋯O = 2.8555 (17)–3.0010 (15) Å] and multiple lone pair–π hole interactions of the nitro groups [N⋯O = 3.0349 (15) and 3.0887 (15) Å]. The Hirshfeld surface and two-dimensional fingerprint plots also support the significance of non-covalent bonding. Coordinative saturation and a favorable geometry at the Li+ ions, dense packing of the polymeric subconnectivities and particularly extensive interanion interactions may be involved in the stabilization of the structure. The title salt is a rare example of an energetic Li nitroazolate, which nicely crystallizes from aqueous solution and is neither hygroscopic nor efflorescent. The TG/DTA data reveal total dehydration in the range of 330–430 K and stability of the anhydrous material up to 633–653 K.urn:issn:2056-9890Domasevitch, K.V.Senchyk, G.A.Krautscheid, H.text/htmlIn the title salt, the 3,3′,5,5′-tetranitro-4,4′-bipyrazole-1,1′-diide dianion [{TNBPz}2−] is situated across the twofold axis. The distorted coordination octahedra around Li+ involve four short bonds with two pyrazolate N atoms and two aqua ligands and two longer contacts with nitro-O atoms. When combined with μ4-{TNBPz}2−, this generates a mono-periodic polymeric structure incorporating discrete centrosymmeric [(H2O)2Li–(dinitropyrazolato)2–Li(H2O)2] units. The three-dimensional stack of mutually orthogonal coordination chains is reminiscent of a Lincoln log pattern.doi:10.1107/S2056989023005339CRYSTAL STRUCTURE; LITHIUM; NITROPYRAZOLES; ENERGETIC MATERIALS; HYDROGEN BONDING2023-06-20catena-Poly[[bis(diaqualithium)]-μ4-3,3′,5,5′-tetranitro-4,4′-bipyrazole-1,1′-diido]: a new moisture-insensitive alkali-metal energetic salt with a well-defined network structureIn the structure of the title salt, [Li2(C6N8O8)(H2O)4]n, the 3,3′,5,5′-tetranitro-4,4′-bipyrazole-1,1′-diide dianion [{TNBPz}2−] is situated across the twofold axis. The distorted coordination octahedra around Li+ involve four short bonds with two pyrazolate N atoms and two aqua ligands [Li—N(O) = 1.999 (3)–2.090 (2) Å] and two longer contacts with nitro-O atoms [2.550 (2), 2.636 (2) Å]. When combined with μ4-{TNBPz}2−, this generates a mono-periodic polymeric structure incorporating discrete centrosymmeric [(H2O)2Li–(dinitropyrazolato)2–Li(H2O)2] units. The three-dimensional stack of mutually orthogonal coordination chains is reminiscent of a Lincoln log pattern. It is influenced by conventional hydrogen bonding [O⋯O = 2.8555 (17)–3.0010 (15) Å] and multiple lone pair–π hole interactions of the nitro groups [N⋯O = 3.0349 (15) and 3.0887 (15) Å]. The Hirshfeld surface and two-dimensional fingerprint plots also support the significance of non-covalent bonding. Coordinative saturation and a favorable geometry at the Li+ ions, dense packing of the polymeric subconnectivities and particularly extensive interanion interactions may be involved in the stabilization of the structure. The title salt is a rare example of an energetic Li nitroazolate, which nicely crystallizes from aqueous solution and is neither hygroscopic nor efflorescent. The TG/DTA data reveal total dehydration in the range of 330–430 K and stability of the anhydrous material up to 633–653 K.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org66372056-98902056-98906572023-06-20June 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications79Crystal structure of 5-(β-d-glucopyranosylthio)-N-(4-methylphenyl)-1,3,4-thiadiazol-2-amine
http://scripts.iucr.org/cgi-bin/paper?yz2035
In the structure of the title compound, C15H19N3O5S2, the bond lengths at the linking sulfur atom are significantly different [1.7473 (17) and 1.811 (2) Å], and the angle at the exocyclic nitrogen atom is wide at 128.45 (18)°. The interplanar angle between the tolyl and thiadiazole rings is 9.2 (1)°. The complex hydrogen-bonding pattern, involving five donors and five acceptors, can be broken down into a one-dimensional ribbon parallel to the b axis, involving hydrogen bonds of the sugar residues only, and a two-dimensional layer structure parallel to the ab plane, based on the N—H⋯O and O—H⋯N hydrogen bonds.urn:issn:2056-9890Abu-Zaied, M.A.Hebishy, A.M.S.Elgemeie, G.H.Salama, H.T.Jones, P.G.text/htmlIn the title compound, the angle between the tolyl and thiadiazole rings is 9.2 (1)°. The hydrogen bonding is a combination of a ribbon involving hydrogen bonds of the sugar residues, and a layer based on N—H⋯O and O—H⋯N hydrogen bonds.doi:10.1107/S2056989023005248GLUCOSE; THIADIAZOLE; CRYSTAL STRUCTURE; HYDROGEN BONDS2023-06-20Crystal structure of 5-(β-d-glucopyranosylthio)-N-(4-methylphenyl)-1,3,4-thiadiazol-2-amineIn the structure of the title compound, C15H19N3O5S2, the bond lengths at the linking sulfur atom are significantly different [1.7473 (17) and 1.811 (2) Å], and the angle at the exocyclic nitrogen atom is wide at 128.45 (18)°. The interplanar angle between the tolyl and thiadiazole rings is 9.2 (1)°. The complex hydrogen-bonding pattern, involving five donors and five acceptors, can be broken down into a one-dimensional ribbon parallel to the b axis, involving hydrogen bonds of the sugar residues only, and a two-dimensional layer structure parallel to the ab plane, based on the N—H⋯O and O—H⋯N hydrogen bonds.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98907656med@iucr.org79research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsJune 20232023-06-206523,5-Lutidine pentaaqua sulfate complexes of first-row transition metals: [M(3,5-lutidine)(H2O)5]SO4, with M = Mn, Co, Ni, and Zn
http://scripts.iucr.org/cgi-bin/paper?zv2026
The reactions of MnSO4·H2O, CoSO4·7H2O, NiSO4·6H2O and ZnSO4·7H2O with 3,5-lutidine (3,5-dimethylpyridine) yield crystals of pentaaqua(3,5-dimethylpyridine-κN)manganese(II) sulfate, [Mn(C7H9N)(H2O)5]SO4, (1), pentaaqua(3,5-dimethylpyridine-κN)cobalt(II) sulfate, [Co(C7H9N)(H2O)5]SO4, (2), pentaaqua(3,5-dimethylpyridine-κN)nickel(II) sulfate, [Ni(C7H9N)(H2O)5]SO4, (3), and pentaaqua(3,5-dimethylpyridine-κN)zinc(II) sulfate, [Zn(C7H9N)(H2O)5]SO4, (4), which were characterized by single-crystal X-ray diffraction. The four crystals are isostructural, demonstrating near identical unit-cell parameters and atomic positions. The metal atoms are all octahedrally coordinated, with one lutidine ligand and five water ligands. The sulfate dianion hydrogen bonds with the coordinated water molecules of the dicationic metal complex salts, generating infinite three-dimensional networks.urn:issn:2056-9890Golen, J.A.Manke, D.R.text/htmlThe structures of four metal 3,5-lutidine pentaaqua sulfates (Mn, Co, Ni, Zn) are presented and are shown to be isostructural.doi:10.1107/S2056989023005261CRYSTAL STRUCTURE; LUTIDINE; SULFATE; TRANSITION METAL; COORDINATION CHEMISTRY2023-06-163,5-Lutidine pentaaqua sulfate complexes of first-row transition metals: [M(3,5-lutidine)(H2O)5]SO4, with M = Mn, Co, Ni, and ZnThe reactions of MnSO4·H2O, CoSO4·7H2O, NiSO4·6H2O and ZnSO4·7H2O with 3,5-lutidine (3,5-dimethylpyridine) yield crystals of pentaaqua(3,5-dimethylpyridine-κN)manganese(II) sulfate, [Mn(C7H9N)(H2O)5]SO4, (1), pentaaqua(3,5-dimethylpyridine-κN)cobalt(II) sulfate, [Co(C7H9N)(H2O)5]SO4, (2), pentaaqua(3,5-dimethylpyridine-κN)nickel(II) sulfate, [Ni(C7H9N)(H2O)5]SO4, (3), and pentaaqua(3,5-dimethylpyridine-κN)zinc(II) sulfate, [Zn(C7H9N)(H2O)5]SO4, (4), which were characterized by single-crystal X-ray diffraction. The four crystals are isostructural, demonstrating near identical unit-cell parameters and atomic positions. The metal atoms are all octahedrally coordinated, with one lutidine ligand and five water ligands. The sulfate dianion hydrogen bonds with the coordinated water molecules of the dicationic metal complex salts, generating infinite three-dimensional networks.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79Acta Crystallographica Section E: Crystallographic CommunicationsJune 2023https://creativecommons.org/licenses/by/4.0/research communications6482023-06-162056-98902056-98907651med@iucr.orgCrystal structure and Hirshfeld surface analysis of bis{(Z)-N′-[(E)-(furan-2-yl)methylidene]carbamohydrazonothioato}nickel(II) methanol disolvate
http://scripts.iucr.org/cgi-bin/paper?jy2031
In the title complex, [Ni(C6H6N3OS)2]·2CH3OH, the NiII atom is coordinated by the S and N atoms of two N′-[(Z)-(furan-2-yl)methylidene]carbamohydrazonothioic acid ligands in a distorted square-planar geometry. The two mutual ligands bound to NiII are also connected by C—H⋯S interactions, while the H atoms of the NH2 group of the ligands form R44(8) motifs with the O atoms of the solvent ethyl alcohol molecules. At the same time, the OH groups of the solvent ethyl alcohol molecules form parallel layers to the (011) plane by the O—H⋯N interactions with the ligand N atom that is not bonded to the NiII atom.. The layers are connected by van der Waals interactions. A Hirshfeld surface analysis indicates that the most important contacts are H⋯H (37.7%), C⋯H/H⋯C (14.6%), O⋯H/H⋯O (11.5%) and S⋯H/H⋯S (10.6%).urn:issn:2056-9890Azizova, A.N.Mammadova, G.Z.Çelikesir, S.T.Akkurt, M.Bhattarai, A.text/htmlIn the title complex, the NiII atom is coordinated by the S and N atoms of two N′-[(Z)-(furan-2-yl)methylidene]carbamohydrazonothioic acid ligands in a distorted square-planar geometry.doi:10.1107/S2056989023005182CRYSTAL STRUCTURE; LIGANDS; DISTORTED SQUARE-PLANAR GEOMETRY; HYDROGEN BONDS; HIRSHFELD SURFACE ANALYSIS2023-06-30Crystal structure and Hirshfeld surface analysis of bis{(Z)-N′-[(E)-(furan-2-yl)methylidene]carbamohydrazonothioato}nickel(II) methanol disolvateIn the title complex, [Ni(C6H6N3OS)2]·2CH3OH, the NiII atom is coordinated by the S and N atoms of two N′-[(Z)-(furan-2-yl)methylidene]carbamohydrazonothioic acid ligands in a distorted square-planar geometry. The two mutual ligands bound to NiII are also connected by C—H⋯S interactions, while the H atoms of the NH2 group of the ligands form R44(8) motifs with the O atoms of the solvent ethyl alcohol molecules. At the same time, the OH groups of the solvent ethyl alcohol molecules form parallel layers to the (011) plane by the O—H⋯N interactions with the ligand N atom that is not bonded to the NiII atom.. The layers are connected by van der Waals interactions. A Hirshfeld surface analysis indicates that the most important contacts are H⋯H (37.7%), C⋯H/H⋯C (14.6%), O⋯H/H⋯O (11.5%) and S⋯H/H⋯S (10.6%).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsJune 20232023-06-306692056-98902056-98907673med@iucr.orgCrystal structures and Hirshfeld surface analyses of (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-phenyldiazene, (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(4-methylphenyl)diazene, (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(4-methoxyphenyl)diazene and (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(3-methylphenyl)diazene
http://scripts.iucr.org/cgi-bin/paper?wm5684
The crystal structures and Hirshfeld surface analyses of four similar azo compounds are reported. (E)-1-[1-(4-tert-Butylphenyl)-2,2-dichloroethenyl]-2-phenyldiazene, C18H18Cl2N2, (I), and (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(4-methylphenyl)diazene, C19H20Cl2N2, (II), crystallize in the monoclinic space group C2/c with Z = 8, and (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(4-methoxyphenyl)diazene, C19H20Cl2N2O, (III), in the monoclinic space group P21/c with Z = 4. (E)-1-[1-(4-tert-Butylphenyl)-2,2-dichloroethenyl]-2-(3-methylphenyl)diazene, C19H20Cl2N2, (IV), crystallizes in the triclinic space group P\overline{1} with Z = 4 and comprises two molecules (A and B) in the asymmetric unit. In the crystal structures of (I) and (II), molecules are linked by C—H⋯π and C—Cl⋯π interactions, forming layers parallel to (\overline{2}02), while molecules of (III) are linked by C—H⋯O contacts, C—H⋯π and C—Cl⋯π interactions forming layers parallel to (\overline{3}02). The stability of the molecular packing is ensured by van der Waals forces between these layers. In the crystal structure of (IV), molecules are linked by C—H⋯π and C—Cl⋯π interactions, forming a tri-periodic network.urn:issn:2056-9890Maharramov, A.Shikhaliyev, N.Q.Qajar, A.Atakishiyeva, G.T.Niyazova, A.Khrustalev, V.N.Akkurt, M.Yıldırım, S. Ö.Bhattarai, A.text/htmlC—H⋯π and C—Cl⋯π interactions are the most important intermolecular interactions in the crystal structures of the title compounds.doi:10.1107/S205698902300511XCRYSTAL STRUCTURE; AZO COMPOUNDS; C-H...[PI] AND C-CL...[PI] INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-06-13Crystal structures and Hirshfeld surface analyses of (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-phenyldiazene, (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(4-methylphenyl)diazene, (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(4-methoxyphenyl)diazene and (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(3-methylphenyl)diazeneThe crystal structures and Hirshfeld surface analyses of four similar azo compounds are reported. (E)-1-[1-(4-tert-Butylphenyl)-2,2-dichloroethenyl]-2-phenyldiazene, C18H18Cl2N2, (I), and (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(4-methylphenyl)diazene, C19H20Cl2N2, (II), crystallize in the monoclinic space group C2/c with Z = 8, and (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(4-methoxyphenyl)diazene, C19H20Cl2N2O, (III), in the monoclinic space group P21/c with Z = 4. (E)-1-[1-(4-tert-Butylphenyl)-2,2-dichloroethenyl]-2-(3-methylphenyl)diazene, C19H20Cl2N2, (IV), crystallizes in the triclinic space group P\overline{1} with Z = 4 and comprises two molecules (A and B) in the asymmetric unit. In the crystal structures of (I) and (II), molecules are linked by C—H⋯π and C—Cl⋯π interactions, forming layers parallel to (\overline{2}02), while molecules of (III) are linked by C—H⋯O contacts, C—H⋯π and C—Cl⋯π interactions forming layers parallel to (\overline{3}02). The stability of the molecular packing is ensured by van der Waals forces between these layers. In the crystal structure of (IV), molecules are linked by C—H⋯π and C—Cl⋯π interactions, forming a tri-periodic network.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext796372023-06-13Acta Crystallographica Section E: Crystallographic CommunicationsJune 2023https://creativecommons.org/licenses/by/4.0/research communications72056-98902056-9890med@iucr.org643Synthesis, crystal structure and Hirshfeld surface analysis of bis(caffeinium) hexachloridoplatinum(IV) in comparison with some related compounds
http://scripts.iucr.org/cgi-bin/paper?zv2027
The molecular and crystal structure of the title compound, (C8H11N4O2)2[PtCl6], synthesized from hexachloroplatinic acid and caffeine in methanol, was studied by single-crystal X-ray diffraction. The caffeinium cations form a double layer via hydrogen bonds and π-stacking interactions. The Hirshfeld surface analysis showed that the largest contribution to the crystal packing is made by H⋯H (31.2%), H⋯Cl/Cl⋯H (22.6%), O⋯H/H⋯O (21.9%) contacts for the cation and H⋯Cl/Cl⋯H (79.3%) contacts for the anion.urn:issn:2056-9890Zagidullin, K.A.Novikov, A.P.Zelenina, D.A.Grigoriev, M.S.German, K.E.text/htmlIn the crystal, the cations and anions form a layered structure via strong N—H⋯Cl, weak C—H⋯Cl and C—H⋯O hydrogen bonds and π-stacking interactions.doi:10.1107/S2056989023005157CRYSTAL STRUCTURE; PLATINUM; PT; CAFFEINE; HIRSHFELD SURFACE ANALYSIS; HEXAHALIDE; [PI]-STACKING2023-06-16Synthesis, crystal structure and Hirshfeld surface analysis of bis(caffeinium) hexachloridoplatinum(IV) in comparison with some related compoundsThe molecular and crystal structure of the title compound, (C8H11N4O2)2[PtCl6], synthesized from hexachloroplatinic acid and caffeine in methanol, was studied by single-crystal X-ray diffraction. The caffeinium cations form a double layer via hydrogen bonds and π-stacking interactions. The Hirshfeld surface analysis showed that the largest contribution to the crystal packing is made by H⋯H (31.2%), H⋯Cl/Cl⋯H (22.6%), O⋯H/H⋯O (21.9%) contacts for the cation and H⋯Cl/Cl⋯H (79.3%) contacts for the anion.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext647med@iucr.org2056-98902056-98907https://creativecommons.org/licenses/by/4.0/research communicationsJune 2023Acta Crystallographica Section E: Crystallographic Communications2023-06-1664479Crystal structure of 1-(4-bromophenyl)but-3-yn-1-one
http://scripts.iucr.org/cgi-bin/paper?dx2053
The title compound, 1-(4-bromophenyl)but-3-yn-1-one, C10H7BrO, crystallizes in the monoclinic space group P21/n with one molecule in the asymmetric unit. The structure displays a planar geometry. The crystal structure is consolidated by C—H⋯O hydrogen bonding and a short C=O⋯C≡C (acetylene) contacts. Hirshfeld surface analysis indicates that H⋯H, C⋯H/H⋯C and H⋯Br/Br⋯H interactions play a more important role in consolidating the crystal structure compared to H⋯O/O⋯H and C⋯C contacts.urn:issn:2056-9890Siddiqui, S.K.Ramana, C.V.Gonnade, R.G.text/htmlThe title compound crystallizes in the monoclinic crystal system in the centrosymmetric space group P21/n. The crystal structure features C—H⋯O hydrogen bonding and a short C=O⋯C≡C (acetylene) contacts.doi:10.1107/S205698902300508XCRYSTAL STRUCTURE; INTERMOLECULAR INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-06-13Crystal structure of 1-(4-bromophenyl)but-3-yn-1-oneThe title compound, 1-(4-bromophenyl)but-3-yn-1-one, C10H7BrO, crystallizes in the monoclinic space group P21/n with one molecule in the asymmetric unit. The structure displays a planar geometry. The crystal structure is consolidated by C—H⋯O hydrogen bonding and a short C=O⋯C≡C (acetylene) contacts. Hirshfeld surface analysis indicates that H⋯H, C⋯H/H⋯C and H⋯Br/Br⋯H interactions play a more important role in consolidating the crystal structure compared to H⋯O/O⋯H and C⋯C contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsJune 20232023-06-136332056-98902056-98907636med@iucr.orgCyclopentadienone triisocyanide iron complexes: general synthesis and crystal structures of tris(2,6-dimethylphenyl isocyanide)(η4-tetraphenylcyclopentadienone)iron and tris(naphthalen-2-yl isocyanide)(η4-tetraphenylcyclopentadienone)iron acetone hemisolvate
http://scripts.iucr.org/cgi-bin/paper?mw2197
Irradiation of a toluene solution containing cyclopentadienone tricarbonyl iron complexes and isocyanides with blue LEDs afforded the formation and isolation of 12 triisocyanide complexes, two of which, namely tris(2,6-dimethylphenyl isocyanide)(η4-tetraphenylcyclopenatedienone)iron, [Fe(C9H9N)3(C29H20O)], and tris(naphthalen-2-yl isocyanide)(η4-tetraphenylcyclopenatedienone)iron acetone hemisolvate, [Fe(C11H7N)3(C29H20O)]2·C3H6O, could be characterized crystallographically. The air-stable compounds were purified by column chromatography and were characterized by 1H NMR, 13C NMR, elemental analysis and HRMS. NMR and XRD data indicate generally more electron-rich Fe0 centers compared to the corresponding tricarbonyl compounds.urn:issn:2056-9890Bütikofer, A.Chen, P.text/htmlCyclopentadienone triisocyanide iron complexes were isolated and fully characterized for the first time. Two of the twelve isolated complexes could be crystallographically characterized.doi:10.1107/S205698902300498XCRYSTAL STRUCTURE; ISOCYANIDE; CYCLOPENTADIENONE IRON COMPLEX; LEDS2023-06-13Cyclopentadienone triisocyanide iron complexes: general synthesis and crystal structures of tris(2,6-dimethylphenyl isocyanide)(η4-tetraphenylcyclopentadienone)iron and tris(naphthalen-2-yl isocyanide)(η4-tetraphenylcyclopentadienone)iron acetone hemisolvateIrradiation of a toluene solution containing cyclopentadienone tricarbonyl iron complexes and isocyanides with blue LEDs afforded the formation and isolation of 12 triisocyanide complexes, two of which, namely tris(2,6-dimethylphenyl isocyanide)(η4-tetraphenylcyclopenatedienone)iron, [Fe(C9H9N)3(C29H20O)], and tris(naphthalen-2-yl isocyanide)(η4-tetraphenylcyclopenatedienone)iron acetone hemisolvate, [Fe(C11H7N)3(C29H20O)]2·C3H6O, could be characterized crystallographically. The air-stable compounds were purified by column chromatography and were characterized by 1H NMR, 13C NMR, elemental analysis and HRMS. NMR and XRD data indicate generally more electron-rich Fe0 centers compared to the corresponding tricarbonyl compounds.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2023-06-13626Acta Crystallographica Section E: Crystallographic CommunicationsJune 2023research communicationshttps://creativecommons.org/licenses/by/4.0/79med@iucr.org63272056-98902056-9890Crystal structures of two SmIII complexes with dipicolinate [DPA]2− ligands: comparison of luminescent properties of products obtained at different pH values
http://scripts.iucr.org/cgi-bin/paper?wm5678
The formation of the two title compounds, Na3[Sm(DPA)3]·14H2O trisodium tris(pyridine-2,6-dicarboxylato-κ3O2,N,O6)samarate(III) tetradecahydrate, Na3[Sm(C7H3NO4)3]·14H2O, and catena-poly[[[diaqua(6-carboxypyridine-2-carboxylato-κ3O2,N,O6)samarium(III)]-μ-pyridine-2,6-dicarboxylato-κ4O2,N,O6:O2] tetrahydrate], {[Sm(C7H3NO4)(C7H4NO4)(H2O)2]·4H2O}n, depends on the pH value adjusted with NaOH solution. In both crystal structures, the coordination spheres of the SmIII cations were found to be best described by a tricapped trigonal prism (TTP), with a more regular O6N3 donor set for Na3[Sm(DPA)3]·14H2O than that of O7N2 for [Sm(DPA)(HDPA)(H2O)2]·4H2O. The supramolecular features of both crystal structures are dominated by O—H⋯O hydrogen bonds between water molecules and the O atoms of the dipicolinato ligands. Samples were made from solutions at pH = 2, pH = 5, pH = 7, and pH = 10, and the crystals present in each sample were ground to a powder. The powder samples were analyzed with powder X-ray diffraction and luminescence spectroscopy. The splitting of the bands in the luminescence spectra recorded on powders at 77 K was observed to vary with the pH.urn:issn:2056-9890Mortensen, S.S.Sørensen, T.J.text/htmlCrystallization of the title compounds, synthesized from Sm(CF3SO3)3 and dipicolinic acid solution, was found to change as a function of pH.doi:10.1107/S2056989023004814CRYSTAL STRUCTURE; LUMINESCENCE; SAMARIUM(III); PXRD; HYDROGEN BONDING2023-06-09Crystal structures of two SmIII complexes with dipicolinate [DPA]2− ligands: comparison of luminescent properties of products obtained at different pH valuesThe formation of the two title compounds, Na3[Sm(DPA)3]·14H2O trisodium tris(pyridine-2,6-dicarboxylato-κ3O2,N,O6)samarate(III) tetradecahydrate, Na3[Sm(C7H3NO4)3]·14H2O, and catena-poly[[[diaqua(6-carboxypyridine-2-carboxylato-κ3O2,N,O6)samarium(III)]-μ-pyridine-2,6-dicarboxylato-κ4O2,N,O6:O2] tetrahydrate], {[Sm(C7H3NO4)(C7H4NO4)(H2O)2]·4H2O}n, depends on the pH value adjusted with NaOH solution. In both crystal structures, the coordination spheres of the SmIII cations were found to be best described by a tricapped trigonal prism (TTP), with a more regular O6N3 donor set for Na3[Sm(DPA)3]·14H2O than that of O7N2 for [Sm(DPA)(HDPA)(H2O)2]·4H2O. The supramolecular features of both crystal structures are dominated by O—H⋯O hydrogen bonds between water molecules and the O atoms of the dipicolinato ligands. Samples were made from solutions at pH = 2, pH = 5, pH = 7, and pH = 10, and the crystals present in each sample were ground to a powder. The powder samples were analyzed with powder X-ray diffraction and luminescence spectroscopy. The splitting of the bands in the luminescence spectra recorded on powders at 77 K was observed to vary with the pH.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytexthttps://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsJune 20236192023-06-0979625med@iucr.org2056-98902056-98907Metal halide coordination compounds with quinazolin-4(3H)-one
http://scripts.iucr.org/cgi-bin/paper?wm5681
Three coordination compounds of quinazolin-4(3H)-one (quinoz; C8H6N2O) with divalent group 12 halides are reported. In all complexes, coordination occurs via the nitrogen atom ortho to the quinazolinone carbonyl group. In the two chain polymers with composition [MX2(quinoz)], viz. (M = Cd, X = Br), catena-poly[[[quinazolin-4(3H)-one-κN3]cadmium(II)]-di-μ-bromido], [CdBr2(C8H6N2O)]n (I), and M = Hg, X = Cl, catena-poly[[[quinazolin-4(3H)-one-κN3]mercury(II)]-di-μ-chlorido], [HgCl2(C8H6N2O)]n (II), the divalent cations are five-coordinate, with four bridging halide and one terminal quinoz ligand. The CdII atom in (I) has an almost trigonal–bipyramidal coordination environment, whereas the HgII atom in (II) has a more distorted coordination environment. Likewise, the halide bridges in (II) are significantly more asymmetric than in (I). In both (I) and (II), quinoz ligands at adjacent cations along each strand are oriented in opposite directions, and the organic ligands of neighboring strands interdigitate with resulting π–π interactions. In contrast to the halide-bridged chain polymers (I) and (II), the adduct of quinoz with CdI2 is the tetrahedral complex [CdI2(quinoz)2], diiodidobis[quinazolin-4(3H)-one-κN3]cadmium(II), [CdI2(C16H12N4O2)], (III). The CdII atom in this discrete complex is located on a twofold rotation axis. Disorder in (III) is reflected in an alternative minority orientation of the molecules for which the iodine sites closely match the position of the majority orientation. In view of the low site occupancy of only 0.0318 (8) Å, only the CdII position for this alternative orientation was taken into account during refinement. In all three compounds, classical N—H⋯O hydrogen bonds with donor–acceptor distances of ca 2.9 Å occur; they link the polymer chains in (I) and (II) into di-periodic networks and connect adjacent discrete complexes in (III) to mono-periodic strands.urn:issn:2056-9890Turgunov, K.K.Englert, U.text/htmlThe cadmium(II) and mercury (II) coordination compounds with composition [CdBr2(quinoz)] and [HgCl2(quinoz)], respectively, where quinoz = quinazolin-4(3H)-one, are chain polymers with bridging halogen atoms. The structure of [CdI2(quinoz)2] was re-determined at 100 K, modeling minor disorder.doi:10.1107/S2056989023004802CRYSTAL STRUCTURE; CADMIUM(II) COORDINATION POLYMER; HALIDE-BRIDGED COORDINATION POLYMERS; MERCURY(II) COORDINATION POLYMER; QUINAZOLINONE COORDINATION; TETRAHEDRAL CADMIUM(II) COMPLEX.2023-06-06Metal halide coordination compounds with quinazolin-4(3H)-oneThree coordination compounds of quinazolin-4(3H)-one (quinoz; C8H6N2O) with divalent group 12 halides are reported. In all complexes, coordination occurs via the nitrogen atom ortho to the quinazolinone carbonyl group. In the two chain polymers with composition [MX2(quinoz)], viz. (M = Cd, X = Br), catena-poly[[[quinazolin-4(3H)-one-κN3]cadmium(II)]-di-μ-bromido], [CdBr2(C8H6N2O)]n (I), and M = Hg, X = Cl, catena-poly[[[quinazolin-4(3H)-one-κN3]mercury(II)]-di-μ-chlorido], [HgCl2(C8H6N2O)]n (II), the divalent cations are five-coordinate, with four bridging halide and one terminal quinoz ligand. The CdII atom in (I) has an almost trigonal–bipyramidal coordination environment, whereas the HgII atom in (II) has a more distorted coordination environment. Likewise, the halide bridges in (II) are significantly more asymmetric than in (I). In both (I) and (II), quinoz ligands at adjacent cations along each strand are oriented in opposite directions, and the organic ligands of neighboring strands interdigitate with resulting π–π interactions. In contrast to the halide-bridged chain polymers (I) and (II), the adduct of quinoz with CdI2 is the tetrahedral complex [CdI2(quinoz)2], diiodidobis[quinazolin-4(3H)-one-κN3]cadmium(II), [CdI2(C16H12N4O2)], (III). The CdII atom in this discrete complex is located on a twofold rotation axis. Disorder in (III) is reflected in an alternative minority orientation of the molecules for which the iodine sites closely match the position of the majority orientation. In view of the low site occupancy of only 0.0318 (8) Å, only the CdII position for this alternative orientation was taken into account during refinement. In all three compounds, classical N—H⋯O hydrogen bonds with donor–acceptor distances of ca 2.9 Å occur; they link the polymer chains in (I) and (II) into di-periodic networks and connect adjacent discrete complexes in (III) to mono-periodic strands.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext618med@iucr.org2056-98902056-98907research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsJune 20236142023-06-0679Synthesis, crystal structure, Hirshfeld surface analysis and DFT study of the 1,1′-(buta-1,3-diyne-1,4-diyl)bis(cyclohexan-1-ol)
http://scripts.iucr.org/cgi-bin/paper?zv2024
The title compound, C16H22O2, was synthesized in order to obtain its guest-free form because `wheel-and-axle'-shaped molecules tend to crystallize from solutions as solvates or host–guest molecules. It crystallizes in the monoclinic space group P2/c with two crystallographically non-equivalent molecules, one situated on an inversion center and the other on a twofold axis. The rod-like 1,3-diyne fragments have the usual linear geometry. In the crystal, O—H ⋯ O bonds form eight-membered rings of the R44(8) type, linking molecules into layers. The Hirshfeld surface analysis indicates that the largest contributions are from intermolecular H⋯H (ca 71%) and H⋯C/C⋯H (ca 19%) contacts. The energies of the frontier molecular orbitals were determined by DFT calculations at the B3LYP/def2-TZVP level of theory.urn:issn:2056-9890Tirkasheva, S.I.Ziyadullaev, O.E.Eshimbetov, A.G.Ibragimov, B.T.Ashurov, J.M.text/htmlThe two crystallographically non-equivalent molecules in the title compound have C2 and Ci symmetries. The crystal structure features strong intermolecular O—H⋯O hydrogen bonds, which form eight-membered rings with R_{4}^{4}(8) graph-set motifs, linking the molecules into layers.doi:10.1107/S2056989023004772SYNTHESIS; 1,1'-(BUTA-1,3-DIYNE-1,4-DIYL)BIS(CYCLOHEXAN-1-OL); CRYSTAL STRUCTURE; HYDROGEN BOND; HIRSHFELD SURFACE ANALYSIS; DFT STUDY.2023-06-02Synthesis, crystal structure, Hirshfeld surface analysis and DFT study of the 1,1′-(buta-1,3-diyne-1,4-diyl)bis(cyclohexan-1-ol)The title compound, C16H22O2, was synthesized in order to obtain its guest-free form because `wheel-and-axle'-shaped molecules tend to crystallize from solutions as solvates or host–guest molecules. It crystallizes in the monoclinic space group P2/c with two crystallographically non-equivalent molecules, one situated on an inversion center and the other on a twofold axis. The rod-like 1,3-diyne fragments have the usual linear geometry. In the crystal, O—H ⋯ O bonds form eight-membered rings of the R44(8) type, linking molecules into layers. The Hirshfeld surface analysis indicates that the largest contributions are from intermolecular H⋯H (ca 71%) and H⋯C/C⋯H (ca 19%) contacts. The energies of the frontier molecular orbitals were determined by DFT calculations at the B3LYP/def2-TZVP level of theory.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-98907June 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/2023-06-0279Crystal structure and Hirshfeld surface analysis of (1H-imidazole-κN3)[N-(2-oxidobenzylidene)tyrosinato-κ3O,N,O′]copper(II)
http://scripts.iucr.org/cgi-bin/paper?ex2071
The title copper(II) complex, [Cu(C16H13NO4)(C3H4N2)], consists of a tridentate ligand synthesized from l-tyrosine and salicylaldehyde. One imidazole molecule is additionally coordinating to the copper(II) ion. The crystal structure features N—H⋯O, O—H⋯O and C—H⋯O hydrogen bonds. The Hirshfeld surface analysis indicates that the most important contributions to the packing are from H⋯H (37.9%), C⋯H (28.2%) and O⋯H/H⋯O (21.2%) contacts.urn:issn:2056-9890Suzuki, S.Akiyama, Y.Nakane, D.Akitsu, T.text/htmlThe amino acid Schiff base copper(II) title complex consists of a tridentate ligand synthesized from l-tyrosine and salicylaldehyde. One imidazole molecule is additionally coordinating to the copper(II) ion. The crystal structure features N—H⋯O, O—H⋯O and C—H⋯O hydrogen bonds.doi:10.1107/S2056989023004735SCHIFF BASE COMPLEX; COPPER; AMINO ACID; HIRSHFELD ANALYSIS; CRYSTAL STRUCTURE2023-06-02Crystal structure and Hirshfeld surface analysis of (1H-imidazole-κN3)[N-(2-oxidobenzylidene)tyrosinato-κ3O,N,O′]copper(II)The title copper(II) complex, [Cu(C16H13NO4)(C3H4N2)], consists of a tridentate ligand synthesized from l-tyrosine and salicylaldehyde. One imidazole molecule is additionally coordinating to the copper(II) ion. The crystal structure features N—H⋯O, O—H⋯O and C—H⋯O hydrogen bonds. The Hirshfeld surface analysis indicates that the most important contributions to the packing are from H⋯H (37.9%), C⋯H (28.2%) and O⋯H/H⋯O (21.2%) contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79June 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-06-022056-98902056-98907med@iucr.orgCrystal structure of Ag3Dy2(NO3)9 and quantitative comparison to isotypic compounds
http://scripts.iucr.org/cgi-bin/paper?pk2686
Single crystals of Ag3Dy2(NO3)9 (trisilver didysprosium nonanitrate) were obtained from a mixture of AgNO3 and Dy(NO3)3·5 H2O. The new compound crystallizes in space group P4132 (No. 213) with a = 13.2004 (4) Å, V = 2300.2 (2) Å3, Z = 4. The Ag and Dy cations are coordinated by five and six bidentate nitrate anions, respectively. Ag3Dy2(NO3)9 is isostructural to several compounds that include alkali metals or ammonium and lanthanide cations, but silver and dysprosium are included for the first time and feature the smallest ion radii observed for this structure type to date. Crystal structures of isotypic compounds are compared.urn:issn:2056-9890Klein, W.text/htmlThe crystal structure of the title compound and its particular relation to isotypic compounds is considered.doi:10.1107/S2056989023004747CRYSTAL STRUCTURE; DYSPROSIUM; SILVER; NITRATE2023-06-02Crystal structure of Ag3Dy2(NO3)9 and quantitative comparison to isotypic compoundsSingle crystals of Ag3Dy2(NO3)9 (trisilver didysprosium nonanitrate) were obtained from a mixture of AgNO3 and Dy(NO3)3·5 H2O. The new compound crystallizes in space group P4132 (No. 213) with a = 13.2004 (4) Å, V = 2300.2 (2) Å3, Z = 4. The Ag and Dy cations are coordinated by five and six bidentate nitrate anions, respectively. Ag3Dy2(NO3)9 is isostructural to several compounds that include alkali metals or ammonium and lanthanide cations, but silver and dysprosium are included for the first time and feature the smallest ion radii observed for this structure type to date. Crystal structures of isotypic compounds are compared.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org2056-98902056-98907Acta Crystallographica Section E: Crystallographic CommunicationsJune 2023research communicationshttps://creativecommons.org/licenses/by/4.0/2023-06-0279Crystal structure and Hirshfeld-surface analysis of a monoclinic polymorph of 2-amino-5-chlorobenzophenone oxime at 90 K
http://scripts.iucr.org/cgi-bin/paper?tx2069
The synthesis and crystal structure of a monoclinic polymorph of 2-amino-5-chlorobenzophenone oxime, C13H11ClN2O, are presented. The molecular conformation results from twisting of the phenyl and 2-amino-5-chloro benzene rings attached to the oxime group, which subtend a dihedral angle of 80.53 (4)°. In the crystal, centrosymmetric dimers are formed as a result of pairs of strong O—H⋯N hydrogen bonds. A comparison is made to a previously known triclinic polymorph, including differences in atom–atom contacts obtained via a Hirshfeld-surface analysis.urn:issn:2056-9890Geetha, D.Kavitha, C.N.Divakara, T.R.Basavaraju, Y.B.Yathirajan, H.S.Parkin, S.text/htmlThe synthesis and crystal structure of a monoclinic polymorph of 2-amino-5-chlorobenzophenone oxime, C13H11ClN2O, are presented along with a comparison to a previously determined triclinic form.doi:10.1107/S2056989023004668CRYSTAL STRUCTURE; BENZOPHENONE OXIME; POLYMORPH; HIRSHFELD SURFACE2023-06-06Crystal structure and Hirshfeld-surface analysis of a monoclinic polymorph of 2-amino-5-chlorobenzophenone oxime at 90 KThe synthesis and crystal structure of a monoclinic polymorph of 2-amino-5-chlorobenzophenone oxime, C13H11ClN2O, are presented. The molecular conformation results from twisting of the phenyl and 2-amino-5-chloro benzene rings attached to the oxime group, which subtend a dihedral angle of 80.53 (4)°. In the crystal, centrosymmetric dimers are formed as a result of pairs of strong O—H⋯N hydrogen bonds. A comparison is made to a previously known triclinic polymorph, including differences in atom–atom contacts obtained via a Hirshfeld-surface analysis.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-06-06610June 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/72056-98902056-9890med@iucr.org613Structure of (R,R)-4-bromo-2-{4-[4-bromo-1-(4-toluenesulfonyl)-1H-pyrrol-2-yl]-1,3-dinitrobutan-2-yl}-1-(4-toluenesulfonyl)-1H-pyrrole, another ostensible by-product in the synthesis of geminal-dimethyl hydrodipyrrins
http://scripts.iucr.org/cgi-bin/paper?vm2284
The crystal structure of (R,R)-4-bromo-2-{4-[4-bromo-1-(4-toluenesulfonyl)-1H-pyrrol-2-yl]-1,3-dinitrobutan-2-yl}-1-(4-toluenesulfonyl)-1H-pyrrole (1, C26H24Br2N4O8S2) is presented. The title compound was isolated in suitable yield as a by-product in our synthesis of geminal-dimethyl hydrodipyrrins. We observe an unforeseen enantiomeric resolution both in the bulk sample and the crystal of 1, with distinct C—H⋯O (Cmethyl—H⋯Onitro, Csp3—H⋯Osulfonyl) interactions observed in the enantiomers present, along with other interactions, namely C5-pyrrolyl—H⋯Osulfonyl, forming a polymer along the crystallographic c-axis direction. Whilst pyrrolic fragments are well documented in the literature, little data is found surrounding the 1,3-dinitrobutane scaffold.urn:issn:2056-9890Sample, H.C.Twamley, B.Senge, M.O.text/htmlThe crystal structure of a by-product in the synthesis of geminal-dimethyl hydrodipyrrins is reported; (R,R)-4-bromo-2-{4-[4-bromo-1-(4-toluenesulfonyl)-1H-pyrrol-2-yl]-1,3-dinitrobutan-2-yl}-1-(4-toluenesulfonyl)-1H-pyrrole (1, C26H24N4O8S2Br2). Generated through a nitronate-mediated dimerization, this compound presents unforeseen enantiomeric resolution, something previously not noted in its singular prior report. This crystal adds to the ever-growing library of by-products arising from these syntheses.doi:10.1107/S2056989023004644CRYSTAL STRUCTURE; ENANTIOMER; RESOLUTION; PYRROLE; BY-PRODUCT2023-06-02Structure of (R,R)-4-bromo-2-{4-[4-bromo-1-(4-toluenesulfonyl)-1H-pyrrol-2-yl]-1,3-dinitrobutan-2-yl}-1-(4-toluenesulfonyl)-1H-pyrrole, another ostensible by-product in the synthesis of geminal-dimethyl hydrodipyrrinsThe crystal structure of (R,R)-4-bromo-2-{4-[4-bromo-1-(4-toluenesulfonyl)-1H-pyrrol-2-yl]-1,3-dinitrobutan-2-yl}-1-(4-toluenesulfonyl)-1H-pyrrole (1, C26H24Br2N4O8S2) is presented. The title compound was isolated in suitable yield as a by-product in our synthesis of geminal-dimethyl hydrodipyrrins. We observe an unforeseen enantiomeric resolution both in the bulk sample and the crystal of 1, with distinct C—H⋯O (Cmethyl—H⋯Onitro, Csp3—H⋯Osulfonyl) interactions observed in the enantiomers present, along with other interactions, namely C5-pyrrolyl—H⋯Osulfonyl, forming a polymer along the crystallographic c-axis direction. Whilst pyrrolic fragments are well documented in the literature, little data is found surrounding the 1,3-dinitrobutane scaffold.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79June 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-06-022056-98902056-98907med@iucr.orgGolden oldies: ten crystallography articles that we think must be read
http://scripts.iucr.org/cgi-bin/paper?dj2066
We have selected a set of ten `golden oldies', diverse crystallography articles to illustrate important moments in the development of our field of science and which form landmark papers in crystallography. They are a mixture of `science pull and technology push'. For each of our choices, we firstly created a new title that emphasizes how the paper's importance worked out from today's perspective. Then we describe the core details and impacts of each paper, with some quotations and a selected figure or two. Ten is an arbitrary number of highlights and our choice is personal.urn:issn:2056-9890Massera, C.Helliwell, J.R.text/htmlWe have selected a set of ten diverse crystallography articles to illustrate important moments in the development of our field of science. They are a mixture of `science pull and technology push'. Ten is an arbitrary number and our choice is personal, so many others might have been chosen.doi:10.1107/S2056989023004619LANDMARK PAPERS IN CRYSTALLOGRAPHY; SCIENCE PULL; TECHNOLOGY PUSH2023-06-06Golden oldies: ten crystallography articles that we think must be readWe have selected a set of ten `golden oldies', diverse crystallography articles to illustrate important moments in the development of our field of science and which form landmark papers in crystallography. They are a mixture of `science pull and technology push'. For each of our choices, we firstly created a new title that emphasizes how the paper's importance worked out from today's perspective. Then we describe the core details and impacts of each paper, with some quotations and a selected figure or two. Ten is an arbitrary number of highlights and our choice is personal.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79June 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications5802023-06-062056-98902056-98907591med@iucr.orgSynthesis and crystal structure of bis(2-phthalimidoethyl)ammonium chloride dihydrate
http://scripts.iucr.org/cgi-bin/paper?ex2070
The title compound {systematic name: bis[2-(1,3-dioxoisoindol-2-yl)ethyl]azanium chloride dihydrate}, C20H18N3O4+·Cl−·2H2O, is a phthalimide-protected polyamine that was synthesized by a previous method. It was characterized by ESI–MS, 1H NMR, and FT–IR. Crystals were grown from a solution of H2O and 0.1 M HCl. The central nitrogen atom is protonated and forms hydrogen bonds with the chloride ion and a water molecule. The two phthalimide units make a dihedral angle of 22.07 (3)°. The crystal packing features a hydrogen-bond network, two-coordinated chloride, and off-set π–π stacking.urn:issn:2056-9890Young, B.S.Lee, J.L.Gembicky, M.Bailey, J.Smith, G.L.N.text/htmlThe title compound is a phthalimide-protected polyamine with a protonated central nitrogen atom. The crystal packing features a hydrogen-bond network, a two-coordinated chloride ion, and off-set π–π stacking.doi:10.1107/S2056989023004565CRYSTAL STRUCTURE; PHTHALIMIDES; [PI]-[PI] INTERACTIONS; TRIPODAL LIGAND2023-05-26Synthesis and crystal structure of bis(2-phthalimidoethyl)ammonium chloride dihydrateThe title compound {systematic name: bis[2-(1,3-dioxoisoindol-2-yl)ethyl]azanium chloride dihydrate}, C20H18N3O4+·Cl−·2H2O, is a phthalimide-protected polyamine that was synthesized by a previous method. It was characterized by ESI–MS, 1H NMR, and FT–IR. Crystals were grown from a solution of H2O and 0.1 M HCl. The central nitrogen atom is protonated and forms hydrogen bonds with the chloride ion and a water molecule. The two phthalimide units make a dihedral angle of 22.07 (3)°. The crystal packing features a hydrogen-bond network, two-coordinated chloride, and off-set π–π stacking.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79Acta Crystallographica Section E: Crystallographic CommunicationsMay 2023https://creativecommons.org/licenses/by/4.0/research communications2023-05-265752056-98902056-98906577med@iucr.orgCrystal structure and Hirshfeld surface analysis of 5-oxo-7-phenyl-2-(phenylamino)-1H-[1,2,4]triazolo[1,5-a]pyridine-6,8-dicarbonitrile dimethyl sulfoxide monosolvate
http://scripts.iucr.org/cgi-bin/paper?tx2068
In the title compound, C20H12N6O·C2H6OS, the [1,2,4]triazolo[1,5-a]pyridine ring system is almost planar and makes dihedral angles of 16.33 (7) and 46.80 (7)°, respectively, with the phenylamino and phenyl rings. In the crystal, molecules are linked by intermolecular N—H⋯O and C—H⋯O hydrogen bonds into chains along the b-axis direction through the dimethyl sulfoxide solvent molecule, forming C(10)R21(6) motifs. These chains are connected via S—O⋯π interactions, π–π stacking interactions between the pyridine rings [centroid-to-centroid distance = 3.6662 (9) Å] and van der Waals interactions. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions to the crystal packing are from H⋯H (28.1%), C⋯H/H⋯C (27.2%), N⋯H/H⋯N (19.4%) and O⋯H/H⋯O (9.8%) interactions.urn:issn:2056-9890Naghiyev, F.N.Khrustalev, V.N.Mamedov, H.M.Akkurt, M.Khalilov, A.N.Bhattarai, A.Mamedov, İ.G.text/htmlIn the crystal, intermolecular N—H⋯O and C—H⋯O hydrogen bonds connect molecules into chains along the b-axis direction through the dimethyl sulfoxide solvent molecule, forming C(10)R_{1}^{2}(6) motifs. These chains are connected via S—O⋯π interactions, π–π stacking interactions and van der Waals interactions.doi:10.1107/S2056989023004383CRYSTAL STRUCTURE; [1,2,4]TRIAZOLO[1,5-A]PYRIDINE; HYDROGEN BOND; HIRSHFELD SURFACE ANALYSIS2023-05-26Crystal structure and Hirshfeld surface analysis of 5-oxo-7-phenyl-2-(phenylamino)-1H-[1,2,4]triazolo[1,5-a]pyridine-6,8-dicarbonitrile dimethyl sulfoxide monosolvateIn the title compound, C20H12N6O·C2H6OS, the [1,2,4]triazolo[1,5-a]pyridine ring system is almost planar and makes dihedral angles of 16.33 (7) and 46.80 (7)°, respectively, with the phenylamino and phenyl rings. In the crystal, molecules are linked by intermolecular N—H⋯O and C—H⋯O hydrogen bonds into chains along the b-axis direction through the dimethyl sulfoxide solvent molecule, forming C(10)R21(6) motifs. These chains are connected via S—O⋯π interactions, π–π stacking interactions between the pyridine rings [centroid-to-centroid distance = 3.6662 (9) Å] and van der Waals interactions. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions to the crystal packing are from H⋯H (28.1%), C⋯H/H⋯C (27.2%), N⋯H/H⋯N (19.4%) and O⋯H/H⋯O (9.8%) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79May 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/2023-05-265672056-98902056-98906570med@iucr.orgSynthesis and crystal structure of 2-[(2,3,5,6-tetrafluoropyridin-4-yl)amino]ethyl methacrylate
http://scripts.iucr.org/cgi-bin/paper?hb8066
In the title compound, C11H10F4N2O2, the conformation about the N—C—C—O bond is gauche [torsion angle = 61.84 (13)°]. In the crystal, N—H⋯O hydrogen bonds link the molecules into [010] chains, which are cross-linked by C—H⋯F and C—H⋯π contacts. Hirshfeld surface analysis was conducted to aid in the visualization of these various influences on the packing. This analysis showed that the largest contribution to the surface contacts arises from F⋯H/H⋯F interactions (35.6%), followed by O⋯H/H⋯O (17.8%) and H⋯H (12.7%).urn:issn:2056-9890Overstreet, S.M.J.Genzia, I.M.Nguyen, A.Auleciems, Z.J.Jennings, A.R.Peloquin, A.J.text/htmlIn the crystal structure of the title compound, the packing is driven by C—H⋯F, N—H⋯O and C—H⋯π contacts. Hirshfeld surface analysis showed that the largest contribution to the surface contacts arise from F⋯H/H⋯F interactions.doi:10.1107/S2056989023004334CRYSTAL STRUCTURE; PERFLUOROPYRIDINE; C-H...F INTERACTION2023-05-26Synthesis and crystal structure of 2-[(2,3,5,6-tetrafluoropyridin-4-yl)amino]ethyl methacrylateIn the title compound, C11H10F4N2O2, the conformation about the N—C—C—O bond is gauche [torsion angle = 61.84 (13)°]. In the crystal, N—H⋯O hydrogen bonds link the molecules into [010] chains, which are cross-linked by C—H⋯F and C—H⋯π contacts. Hirshfeld surface analysis was conducted to aid in the visualization of these various influences on the packing. This analysis showed that the largest contribution to the surface contacts arises from F⋯H/H⋯F interactions (35.6%), followed by O⋯H/H⋯O (17.8%) and H⋯H (12.7%).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org57462056-98902056-98902023-05-26571https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsMay 202379Synthesis and crystal structure studies of 5-(trifluoromethyl)-1,3,4-thiadiazol-2(3H)-one at 180 K
http://scripts.iucr.org/cgi-bin/paper?vm2283
The synthesis and crystal structure of C3HF3N2OS, systematic name 5-(trifluoromethyl)-1,3,4-thiadiazol-2(3H)-one (5-TMD-2-one), a compound containing the pharmacologically important heterocycle 1,3,4-thiadiazole, is presented. The asymmetric unit comprises six independent molecules (Z′ = 6), all of which are planar. The r.m.s. deviations from each mean plane range from 0.0063 to 0.0381 Å, not including the CF3 fluorine atoms. Within the crystal, two of the molecules form hydrogen-bonded dimers that in turn combine with inversion-related copies to form tetrameric constructs. Similar tetramers, but lacking inversion symmetry, are formed by the remaining four molecules. The tetramers are linked into tape-like motifs by S⋯O and O⋯O close contacts. The environments of each symmetry-independent molecule were compared via a Hirshfeld surface analysis. The most abundant atom–atom contacts are between fluorine atoms, while the strongest result from N—H⋯O hydrogen bonds.urn:issn:2056-9890Geetha, D.Mohan Kumar, T.M.Anil Kumar, H.G.Shreenivas, M.T.Basavaraju, Y.B.Yathirajan, H.S.Parkin, S.text/htmlThe synthesis and crystal structure of 5-(trifluoromethyl)-1,3,4-thiadiazol-2(3H)-one, a heterocycle of importance as a pharmaceutical building block, are presented.doi:10.1107/S20569890230042671,3,4-THIADIAZOLE; HETEROCYCLE; HIGH Z'; Z' = 6; HYDROGEN BONDING; DISORDER; CRYSTAL STRUCTURE2023-05-19Synthesis and crystal structure studies of 5-(trifluoromethyl)-1,3,4-thiadiazol-2(3H)-one at 180 KThe synthesis and crystal structure of C3HF3N2OS, systematic name 5-(trifluoromethyl)-1,3,4-thiadiazol-2(3H)-one (5-TMD-2-one), a compound containing the pharmacologically important heterocycle 1,3,4-thiadiazole, is presented. The asymmetric unit comprises six independent molecules (Z′ = 6), all of which are planar. The r.m.s. deviations from each mean plane range from 0.0063 to 0.0381 Å, not including the CF3 fluorine atoms. Within the crystal, two of the molecules form hydrogen-bonded dimers that in turn combine with inversion-related copies to form tetrameric constructs. Similar tetramers, but lacking inversion symmetry, are formed by the remaining four molecules. The tetramers are linked into tape-like motifs by S⋯O and O⋯O close contacts. The environments of each symmetry-independent molecule were compared via a Hirshfeld surface analysis. The most abundant atom–atom contacts are between fluorine atoms, while the strongest result from N—H⋯O hydrogen bonds.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext62056-98902056-9890med@iucr.org561792023-05-19557research communicationshttps://creativecommons.org/licenses/by/4.0/May 2023Acta Crystallographica Section E: Crystallographic Communications2-[3-(1H-Benzimidazol-2-yl)propyl]-1H-benzimidazol-3-ium 3,4,5-trihydroxybenzoate–1,3-bis(1H-benzimidazol-2-yl)propane–ethyl acetate (2/1/2.94): co-crystallization between a salt, a neutral molecule and a solvent
http://scripts.iucr.org/cgi-bin/paper?wm5683
The chemical formula of the title compound, 2C17H17N4+·2C7H5O5−·C17H16N4·2.94C4H8O2, was established by X-ray diffraction of a single-crystal obtained by reacting 1,3-bis(benzimidazol-2-yl)propane (L) and gallic acid (HGal) in ethyl acetate. The molecular structure can be described as a salt (HL)+(Gal)− co-crystallized with a molecule L, with a stoichiometric relation of 2:1. Moreover, large voids in the crystal are filled with ethyl acetate, the amount of which was estimated by using a solvent mask during structure refinement, affording the chemical formula (HL+·Gal−)2·L·(C4H8O2)2.94. The arrangement of components in the crystal is driven by O—H⋯O, N—H⋯O and O—H⋯N hydrogen bonds rather than by π–π or C—H⋯π interactions. In the crystal, molecules and ions shape the boundary of cylindrical tunnels parallel to [100] via R (rings) and D (discrete) supramolecular motifs. These voids, which account for about 28% of the unit-cell volume, contain disordered solvent molecules.urn:issn:2056-9890Palacios Rodríguez, J.C.Mendoza, A.Sosa Rivadeneyra, M.Bernès, S.text/htmlThe title compound can be described as a salt (HL)+(Gal)− (L = 1,3-bis(benzimidazol-2-yl)propane (L); HGal = gallic acid) co-crystallized with a neutral molecule L. The crystal also comprises disordered solvent ethyl acetate molecules.doi:10.1107/S2056989023004279CRYSTAL STRUCTURE; CO-CRYSTAL; HYDROGEN BONDS; SUPRAMOLECULAR STRUCTURE; SOLVENT MASK2023-05-232-[3-(1H-Benzimidazol-2-yl)propyl]-1H-benzimidazol-3-ium 3,4,5-trihydroxybenzoate–1,3-bis(1H-benzimidazol-2-yl)propane–ethyl acetate (2/1/2.94): co-crystallization between a salt, a neutral molecule and a solventThe chemical formula of the title compound, 2C17H17N4+·2C7H5O5−·C17H16N4·2.94C4H8O2, was established by X-ray diffraction of a single-crystal obtained by reacting 1,3-bis(benzimidazol-2-yl)propane (L) and gallic acid (HGal) in ethyl acetate. The molecular structure can be described as a salt (HL)+(Gal)− co-crystallized with a molecule L, with a stoichiometric relation of 2:1. Moreover, large voids in the crystal are filled with ethyl acetate, the amount of which was estimated by using a solvent mask during structure refinement, affording the chemical formula (HL+·Gal−)2·L·(C4H8O2)2.94. The arrangement of components in the crystal is driven by O—H⋯O, N—H⋯O and O—H⋯N hydrogen bonds rather than by π–π or C—H⋯π interactions. In the crystal, molecules and ions shape the boundary of cylindrical tunnels parallel to [100] via R (rings) and D (discrete) supramolecular motifs. These voids, which account for about 28% of the unit-cell volume, contain disordered solvent molecules.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98906566med@iucr.org79May 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-05-23562Syntheses, crystal structures and Hirshfeld surface analysis of 2-(benzylsulfanyl)-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazole and 2-[(2-chloro-6-fluorobenzyl)sulfanyl]-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazole
http://scripts.iucr.org/cgi-bin/paper?dx2051
The title compounds were synthesized by alkylation of 5-[(4-dimethylamino)phenyl]-1,3,4-oxadiazole-2-thiol with benzyl chloride or 2-chloro-6-fluorobenzyl chloride in the presence of potassium carbonate. The yields of 2-(benzylsulfanyl)-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazole, C17H17N3OS (I), and 2-[(2-chloro-6-fluorobenzyl)sulfanyl]-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazole, C17H15ClFN3OS (II), were 96 and 92%, respectively. In the crystal structures of (I) and (II), C–H⋯π interactions are observed between neighboring molecules. Hirshfeld surface analysis indicates that H⋯H and H⋯C/C⋯H interactions make the most important contributions to the crystal packing.urn:issn:2056-9890Okmanov, R.Y.Ziyaev, A.A.Abdukarimov, A.S.Toshmurodov, T.T.Kholikov, T.S.text/htmlThe title molecules were synthesized by alkylation of 5-[(4-dimethylamino)phenyl]-1,3,4-oxadiazole-2-thiol. In the crystals, C–H⋯π interactions are observed between neighboring molecules. Hirshfeld surface analysis indicates that H⋯H and H⋯C/C⋯H interactions make the most important contributions to the crystal packing.doi:10.1107/S2056989023004164SYNTHESIS; 1,3,4-OXADIAZOLE; CRYSTAL STRUCTURE; HIRSHFELD SURFACE ANALYSIS2023-05-19Syntheses, crystal structures and Hirshfeld surface analysis of 2-(benzylsulfanyl)-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazole and 2-[(2-chloro-6-fluorobenzyl)sulfanyl]-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazoleThe title compounds were synthesized by alkylation of 5-[(4-dimethylamino)phenyl]-1,3,4-oxadiazole-2-thiol with benzyl chloride or 2-chloro-6-fluorobenzyl chloride in the presence of potassium carbonate. The yields of 2-(benzylsulfanyl)-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazole, C17H17N3OS (I), and 2-[(2-chloro-6-fluorobenzyl)sulfanyl]-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazole, C17H15ClFN3OS (II), were 96 and 92%, respectively. In the crystal structures of (I) and (II), C–H⋯π interactions are observed between neighboring molecules. Hirshfeld surface analysis indicates that H⋯H and H⋯C/C⋯H interactions make the most important contributions to the crystal packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org55662056-98902056-98902023-05-19552https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsMay 202379Synthesis, crystal structure and Hirshfeld surface analysis of (E)-benzo[d][1,3]dioxole-5-carbaldehyde oxime
http://scripts.iucr.org/cgi-bin/paper?hb8064
The asymmetric unit of the title molecule, C8H7NO3, consists of two molecules differing slightly in conformation and in their intermolecular interactions in the solid. The dihedral angle between the benzene and dioxolane rings is 0.20 (7)° in one molecule and 0.31 (7)° in the other. In the crystal, the two molecules are linked into dimers through pairwise O—H⋯N hydrogen bonds, with these units being formed into stacks by two different sets of aromatic π-stacking interactions. The stacks are connected by C—H⋯O hydrogen bonds. A Hirshfeld surface analysis indicates that the most significant contacts in the crystal packing are H⋯O/O⋯H (36.7%), H⋯H (32.2%) and C⋯H/H⋯C (12.7%).urn:issn:2056-9890Radhakrishnan, R.Mustaphi, N.E.H.Sebbar, N.K.Mague, J.T.Thiruvalluvar, A.A.text/htmlThe asymmetric unit of the title compound consists of two independent molecules differing slightly in conformation and in their intermolecular interactions in the solid.doi:10.1107/S2056989023004139SYNTHESIS; CRYSTAL STRUCTURE; BENZODIOXOLANE; OXIME; O-H...N; C-H...O; HYDROGEN BONDS; [PI]-STACKING; HIRSHFELD SURFACE ANALYSIS.2023-05-16Synthesis, crystal structure and Hirshfeld surface analysis of (E)-benzo[d][1,3]dioxole-5-carbaldehyde oximeThe asymmetric unit of the title molecule, C8H7NO3, consists of two molecules differing slightly in conformation and in their intermolecular interactions in the solid. The dihedral angle between the benzene and dioxolane rings is 0.20 (7)° in one molecule and 0.31 (7)° in the other. In the crystal, the two molecules are linked into dimers through pairwise O—H⋯N hydrogen bonds, with these units being formed into stacks by two different sets of aromatic π-stacking interactions. The stacks are connected by C—H⋯O hydrogen bonds. A Hirshfeld surface analysis indicates that the most significant contacts in the crystal packing are H⋯O/O⋯H (36.7%), H⋯H (32.2%) and C⋯H/H⋯C (12.7%).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext62056-98902056-9890med@iucr.org548792023-05-16545https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsMay 2023Synthesis and structure of photodegradable 1-(4,5-dimethoxy-2,3-dinitrophenyl)-2-methylpropyl N-butylcarbamate
http://scripts.iucr.org/cgi-bin/paper?ex2069
The reaction of 1-(4,5-dimethoxy-2,3-dinitrophenyl)-2-methylpropan-1-ol and butylisocyanate using dibutyltin dilaurate as a catalyst afforded 1-(4,5-dimethoxy-2,3-dinitrophenyl)-2-methylpropyl N-butylcarbamate, C17H25N3O8, which released butylamine upon photoirradiation. Single crystals of the title compound were grown in a 1:1 mixed solution of hexane and ethyl acetate. Two nitro groups and one methoxy group are twisted out of the plane of the aromatic ring in the novel photo-protecting group. Intermolecular hydrogen bonds are observed between N-butylcarbamate moieties parallel to the a axis.urn:issn:2056-9890Honda, T.Ito, M.Yamaguchi, K.Kasuga, N.C.Sato, H.text/html1-(4,5-Dimethoxy-2,3-dinitrophenyl)-2-methylpropyl butylcarbamate, which affords butylamine on photoirradiation, was prepared by the reaction of 1-(4,5-dimethoxy-2,3-dinitrophenyl)-2-methylpropan-1-ol and butylisocyanate using dibutyltin dilaurate as a catalyst. Single crystals of the carbamate were grown in a 1:1 mixed solution of hexane and ethyl acetate. Two nitro groups and one methoxy group of the novel photo-protecting group were twisted out of the plane of the aromatic ring and intermolecular hydrogen bonds are observed between carbamate moieties.doi:10.1107/S2056989023004103PHOTOLABILE CARBAMATE; 2,3-DINITROBENZYL GROUP; INTERMOLECULAR HYDROGEN BONDING; CRYSTAL STRUCTURE2023-05-16Synthesis and structure of photodegradable 1-(4,5-dimethoxy-2,3-dinitrophenyl)-2-methylpropyl N-butylcarbamateThe reaction of 1-(4,5-dimethoxy-2,3-dinitrophenyl)-2-methylpropan-1-ol and butylisocyanate using dibutyltin dilaurate as a catalyst afforded 1-(4,5-dimethoxy-2,3-dinitrophenyl)-2-methylpropyl N-butylcarbamate, C17H25N3O8, which released butylamine upon photoirradiation. Single crystals of the title compound were grown in a 1:1 mixed solution of hexane and ethyl acetate. Two nitro groups and one methoxy group are twisted out of the plane of the aromatic ring in the novel photo-protecting group. Intermolecular hydrogen bonds are observed between N-butylcarbamate moieties parallel to the a axis.https://creativecommons.org/licenses/by/4.0/enInternational Union of CrystallographytextActa Crystallographica Section E: Crystallographic CommunicationsMay 2023https://creativecommons.org/licenses/by/4.0/research communications5492023-05-1679551med@iucr.org2056-98902056-98906Syntheses, crystal structures, Hirshfeld surface analyses and energy frameworks of two 4-aminoantipyrine Schiff base compounds: (E)-4-{[4-(diethylamino)benzylidene]amino}-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-one and (E)-4-[(4-fluorobenzylidene)amino]-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-one
http://scripts.iucr.org/cgi-bin/paper?hb8065
The title Schiff base compounds, C22H26N4O (I) and C18H16FN3O (II), were each synthesized by a single-step condensation reaction. The substituted benzylidene ring is inclined to the pyrazole ring mean planes by 22.92 (7)° in I and 12.70 (9)° in II. The phenyl ring of the 4-aminoantipyrine unit is inclined to the pyrazole ring mean plane by 54.87 (7)° in I and by 60.44 (8)° in II. In the crystal of I, the molecules are linked by C—H⋯O hydrogen bonds and C—H⋯π interactions to form layers lying parallel to (001). In the crystal of II, the molecules are linked by C—H⋯O and C—H⋯F hydrogen bonds and C—H⋯π interactions, thereby forming layers lying parallel to (010). Hirshfeld surface analysis was employed to further quantify the interatomic interactions in the crystals of both compounds.urn:issn:2056-9890Shankar, M.G.Kumaravel, R.Subashini, A.Ramamurthi, K.Kučeráková, M.Dušek, M.Stoeckli-Evans, H.text/htmlThe title 4-aminoantipyrine Schiff base compounds both deviate from planarity with the phenyl ring and the substituted benzylidene ring being inclined to the pyrazole ring mean plane by 54.87 (7) and 22.92 (7)°, respectively, in the first compound and by 60.44 (8) and 12.70 (9)° in the second.doi:10.1107/S2056989023004085CRYSTAL STRUCTURE; 4-AMINOANTIPYRINE; HIRSHFELD SURFACE ANALYSIS; ENERGY FRAMEWORKS2023-05-12Syntheses, crystal structures, Hirshfeld surface analyses and energy frameworks of two 4-aminoantipyrine Schiff base compounds: (E)-4-{[4-(diethylamino)benzylidene]amino}-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-one and (E)-4-[(4-fluorobenzylidene)amino]-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-oneThe title Schiff base compounds, C22H26N4O (I) and C18H16FN3O (II), were each synthesized by a single-step condensation reaction. The substituted benzylidene ring is inclined to the pyrazole ring mean planes by 22.92 (7)° in I and 12.70 (9)° in II. The phenyl ring of the 4-aminoantipyrine unit is inclined to the pyrazole ring mean plane by 54.87 (7)° in I and by 60.44 (8)° in II. In the crystal of I, the molecules are linked by C—H⋯O hydrogen bonds and C—H⋯π interactions to form layers lying parallel to (001). In the crystal of II, the molecules are linked by C—H⋯O and C—H⋯F hydrogen bonds and C—H⋯π interactions, thereby forming layers lying parallel to (010). Hirshfeld surface analysis was employed to further quantify the interatomic interactions in the crystals of both compounds.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext62056-98902056-9890med@iucr.org544795382023-05-12Acta Crystallographica Section E: Crystallographic CommunicationsMay 2023https://creativecommons.org/licenses/by/4.0/research communicationsPolymorphic structures of 3-phenyl-1H-1,3-benzodiazol-2(3H)-one
http://scripts.iucr.org/cgi-bin/paper?vm2281
The polymorphic structures (I and II) of 3-phenyl-1H-1,3-benzodiazol-2(3H)-one, C13H10N2O, acquired from pentane diffusion into the solution in THF, are reported. The structures show negligible differences in bond distances and angles, but the C—N—C—C torsion angles between the backbone and the phenyl substituent, 123.02 (15)° for I and 137.18 (11)° for II, are different. Compound I features a stronger C=O⋯H—N hydrogen bond than that in II, while the structure of II exhibits a stronger π–π interaction than in I, as confirmed by the shorter intercentroid distance [3.3257 (8) Å in II in comparison to 3.6862 (7) Å in I]. Overall, the supramolecular interactions of I and II are distinct, presumably originating from the variation in the dihedral angle.urn:issn:2056-9890Hong, D.Lee, K.text/htmlThe two polymorphic structures of 3-phenyl-1H-1,3-benzodiazol-2(3H)-one (I and II) exhibit identical bond distances and angles except for the C—N—C—C torsion angle between the benzimidazolone backbone and the phenyl substituent, which has an effect on the crystal packing and supramolecular features. The structure of I contains a stronger C=O⋯H—N hydrogen-bonding interaction and a weaker π–π interaction between adjacent bezimidazolone moieties in comparison to II.doi:10.1107/S2056989023003961CRYSTAL STRUCTURE; BENZIMIDAZOLONE; HYDROGEN BOND2023-05-12Polymorphic structures of 3-phenyl-1H-1,3-benzodiazol-2(3H)-oneThe polymorphic structures (I and II) of 3-phenyl-1H-1,3-benzodiazol-2(3H)-one, C13H10N2O, acquired from pentane diffusion into the solution in THF, are reported. The structures show negligible differences in bond distances and angles, but the C—N—C—C torsion angles between the backbone and the phenyl substituent, 123.02 (15)° for I and 137.18 (11)° for II, are different. Compound I features a stronger C=O⋯H—N hydrogen bond than that in II, while the structure of II exhibits a stronger π–π interaction than in I, as confirmed by the shorter intercentroid distance [3.3257 (8) Å in II in comparison to 3.6862 (7) Å in I]. Overall, the supramolecular interactions of I and II are distinct, presumably originating from the variation in the dihedral angle.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsMay 20235342023-05-122056-98902056-98906537med@iucr.orgCrystal structure of 4-[(4-methylbenzyl)oxy]-N′-(4-nitrobenzylidene)benzohydrazide: a new hydrazone derivative
http://scripts.iucr.org/cgi-bin/paper?wm5682
The molecular structure of the title compound, C22H19N3O4, shows a non-coplanar conformation, with dihedral angles between the phenyl rings of 73.3 (1) and 80.9 (1)°. These deformations are induced by the crystal packing that is mainly governed by N—H⋯O and C—H⋯O hydrogen bonds, forming a mono-periodic arrangement parallel to the b axis.urn:issn:2056-9890Banna, M.H.A.Sheikh, M.C.Miyatake, R.Howlader, M.B.H.Zangrando, E.text/htmlThe title aroylhydrazone ether exists in an E-configuration with respect to the double bond of the hydrazone bridge and with an acyl–hydrazone (—CH=N—NH—CO—) torsion angle of 166.0 (3)°. The molecule exhibits a non-planar conformation, likely induced by packing requirements.doi:10.1107/S2056989023003948CRYSTAL STRUCTURE; HYDRAZINE; HYDRAZONE2023-05-05Crystal structure of 4-[(4-methylbenzyl)oxy]-N′-(4-nitrobenzylidene)benzohydrazide: a new hydrazone derivativeThe molecular structure of the title compound, C22H19N3O4, shows a non-coplanar conformation, with dihedral angles between the phenyl rings of 73.3 (1) and 80.9 (1)°. These deformations are induced by the crystal packing that is mainly governed by N—H⋯O and C—H⋯O hydrogen bonds, forming a mono-periodic arrangement parallel to the b axis.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79May 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/2023-05-052056-98902056-98906med@iucr.orgCrystal structure and Hirshfeld surface analysis of 2-amino-6-[(1-phenylethyl)amino]-4-(thiophen-2-yl)pyridine-3,5-dicarbonitrile
http://scripts.iucr.org/cgi-bin/paper?vm2282
In the title compound, C19H15N5S, the thiophene ring is disordered in a 0.6:0.4 ratio by an approximate 180° rotation of the ring around the C—C bond linking it to the pyridine ring. In the crystal, the molecules are linked by N—H⋯N hydrogen bonds into dimers with an R22(12) motif, forming chains along the b-axis direction. These chains are connected to each other by further N—H⋯N hydrogen bonds, forming a three-dimensional network. Furthermore, N—H⋯π and π–π [centroid–centroid separations = 3.899 (8) and 3.7938 (12) Å] interactions also contribute to the crystal cohesion. A Hirshfeld surface analysis indicated that the most important contributions to the surface contacts are from H⋯H (46.1%), N⋯H/H⋯N (20.4%) and C⋯H/H⋯C (17.4%) interactions.urn:issn:2056-9890Naghiyev, F.N.Khrustalev, V.N.Asadov, K.A.Akkurt, M.Khalilov, A.N.Bhattarai, A.Mamedov, İ.G.text/htmlIn the crystal, the molecules are connected by N—H⋯N hydrogen bonds into dimers with an R_{2}^{2}(12) motif, forming chains along the b-axis direction. These chains are linked to each other by N—H⋯N hydrogen bonds, N–H⋯π and π–π interactions, forming a three-dimensional network.doi:10.1107/S2056989023003845CRYSTAL STRUCTURE; PYRIDINE RING; THIOPHENE RING; DISORDER; HIRSHFELD SURFACE ANALYSIS2023-05-05Crystal structure and Hirshfeld surface analysis of 2-amino-6-[(1-phenylethyl)amino]-4-(thiophen-2-yl)pyridine-3,5-dicarbonitrileIn the title compound, C19H15N5S, the thiophene ring is disordered in a 0.6:0.4 ratio by an approximate 180° rotation of the ring around the C—C bond linking it to the pyridine ring. In the crystal, the molecules are linked by N—H⋯N hydrogen bonds into dimers with an R22(12) motif, forming chains along the b-axis direction. These chains are connected to each other by further N—H⋯N hydrogen bonds, forming a three-dimensional network. Furthermore, N—H⋯π and π–π [centroid–centroid separations = 3.899 (8) and 3.7938 (12) Å] interactions also contribute to the crystal cohesion. A Hirshfeld surface analysis indicated that the most important contributions to the surface contacts are from H⋯H (46.1%), N⋯H/H⋯N (20.4%) and C⋯H/H⋯C (17.4%) interactions.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-05-05research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsMay 202362056-98902056-9890med@iucr.orgThe synthesis, crystal structure and Hirshfeld surface analysis of the thiophene derivatives 5-(phenylsulfonyl)-5,6-dihydrobenzo[4,5]thieno[3,2-j]phenanthridine and (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]phenyl}-N-(prop-2-yn-1-yl)benzenesulfonamide
http://scripts.iucr.org/cgi-bin/paper?zn2028
In both of the title compounds, C26H19NO2S2, (I), and C25H19NO2S2, (II), the benzothiophene rings are essentially planar with maximum deviations of 0.026 (1) and −0.016 (1) Å for the carbon and sulfur atoms in compounds (I) and (II), respectively. In (I), the thiophene ring system is almost orthogonal to the phenyl ring attached to the sulfonyl group, subtending a dihedral angle of 88.1 (1)°, and the dihydropyridine ring adopts a screw–boat conformation. In both compounds, the molecular structure is consolidated by weak C—H⋯O intramolecular interactions formed by the sulfone oxygen atoms, which generate S(5) ring motifs. In the crystal of II, molecules are linked via C—H⋯O hydrogen bonds, generating C(7) chains running along the [100] direction. No significant intermolecular interactions are observed in I.urn:issn:2056-9890Madhan, S.NizamMohideen, M.Pavunkumar, V.MohanaKrishnan, A.K.text/htmlThe crystal structures of two benzothiophene derivatives are described along with an analysis of the intermolecular contacts in the crystals performed using Hirshfeld surface analysis and two-dimensional fingerprint plots.doi:10.1107/S2056989023003821CRYSTAL STRUCTURE; THIOPHENE; BENZOTHIOPHENE; DIHYDROBENZENE; DIHYDROPYRIDINE 5-(PHENYLSULFONYL); 12-(PHENYLSULFONYL); PHENANTHRIDINE HYDROGEN BONDING; HIRSHFELD SURFACE ANALYSIS.2023-05-05The synthesis, crystal structure and Hirshfeld surface analysis of the thiophene derivatives 5-(phenylsulfonyl)-5,6-dihydrobenzo[4,5]thieno[3,2-j]phenanthridine and (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]phenyl}-N-(prop-2-yn-1-yl)benzenesulfonamideIn both of the title compounds, C26H19NO2S2, (I), and C25H19NO2S2, (II), the benzothiophene rings are essentially planar with maximum deviations of 0.026 (1) and −0.016 (1) Å for the carbon and sulfur atoms in compounds (I) and (II), respectively. In (I), the thiophene ring system is almost orthogonal to the phenyl ring attached to the sulfonyl group, subtending a dihedral angle of 88.1 (1)°, and the dihydropyridine ring adopts a screw–boat conformation. In both compounds, the molecular structure is consolidated by weak C—H⋯O intramolecular interactions formed by the sulfone oxygen atoms, which generate S(5) ring motifs. In the crystal of II, molecules are linked via C—H⋯O hydrogen bonds, generating C(7) chains running along the [100] direction. No significant intermolecular interactions are observed in I.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org62056-98902056-98902023-05-05https://creativecommons.org/licenses/by/4.0/research communicationsMay 2023Acta Crystallographica Section E: Crystallographic Communications79Crystal structure and Hirshfeld analysis of trans-diiodidobis[(methylsulfanyl)benzene-κS]platinum(II)
http://scripts.iucr.org/cgi-bin/paper?jy2030
The title complex, [PtI2(C7H8I2)2], represents a further example of a square-planar PtII–dithioether complex. It crystallizes in the monoclinic space group P21/c. Additional Hirshfeld analyses indicate a C—H⋯π interaction along the [010] axis to be the most important packing factor.urn:issn:2056-9890Schmidt, A.Jourdain, I.Knorr, M.Strohmann, C.text/htmlThe title complex represents a further example of a square-planar PtII–dithioether complex. It crystallizes in the monoclinic space group P21/c. Additional Hirshfeld analyses indicate a C—H⋯π interaction along the [010] axis to be the most important packing factor.doi:10.1107/S2056989023003717CRYSTAL STRUCTURE; HIRSHFELD SURFACE ANALYSIS; DITHIOETHER2023-04-28Crystal structure and Hirshfeld analysis of trans-diiodidobis[(methylsulfanyl)benzene-κS]platinum(II)The title complex, [PtI2(C7H8I2)2], represents a further example of a square-planar PtII–dithioether complex. It crystallizes in the monoclinic space group P21/c. Additional Hirshfeld analyses indicate a C—H⋯π interaction along the [010] axis to be the most important packing factor.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-04-28516April 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/52056-98902056-9890med@iucr.org520Synthesis, crystal structure and Hirshfeld surface analysis of N-(4-fluorophenyl)-N-isopropyl-2-(methylsulfonyl)acetamide
http://scripts.iucr.org/cgi-bin/paper?hb8062
The synthesis and crystal structure of the title compound, C12H16FNO3S, which is related to the herbicide flufenacet, are presented. The dihedral angle between the amide group and the fluorinated benzene ring is 87.30 (5)° and the N—C—C—S torsion angle defining the orientation of the methylsulfonyl substituent relative to the amide group is 106.91 (11)°. In the crystal, inversion-related molecules form dimers as a result of pairwise C—H⋯O hydrogen bonds, which appear to be reinforced by short O⋯π contacts [O⋯Cg = 3.0643 (11) Å]. A Hirshfeld surface analysis was used to quantify the various types of intermolecular contacts, which are dominated by H atoms.urn:issn:2056-9890Geetha, D.Anil Kumar, H.G.Mohan Kumar, T.M.Srinivasa, G.R.Basavaraju, Y.B.Yathirajan, H.S.Parkin, S.text/htmlIn the title compound, which is related to the herbicide flufenacet, the amide group and fluorobenzene ring are almost perpendicular. A short O⋯π contact is observed in the crystal.doi:10.1107/S2056989023003675N-(SUBSTITUTED PHENYL)ACETAMIDE; FLUFENACET METABOLITE; CRYSTAL STRUCTURE; HIRSHFELD SURFACE ANALYSIS2023-04-28Synthesis, crystal structure and Hirshfeld surface analysis of N-(4-fluorophenyl)-N-isopropyl-2-(methylsulfonyl)acetamideThe synthesis and crystal structure of the title compound, C12H16FNO3S, which is related to the herbicide flufenacet, are presented. The dihedral angle between the amide group and the fluorinated benzene ring is 87.30 (5)° and the N—C—C—S torsion angle defining the orientation of the methylsulfonyl substituent relative to the amide group is 106.91 (11)°. In the crystal, inversion-related molecules form dimers as a result of pairwise C—H⋯O hydrogen bonds, which appear to be reinforced by short O⋯π contacts [O⋯Cg = 3.0643 (11) Å]. A Hirshfeld surface analysis was used to quantify the various types of intermolecular contacts, which are dominated by H atoms.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org51552056-98902056-98902023-04-28512https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsApril 202379Synthesis and crystal structure of catena-poly[[[aqua{2-[(E)-(1-cyano-2-imino-2-methoxyethylidene)hydrazinyl]benzenesulfonato}sodium]-di-μ-aqua] dihydrate]
http://scripts.iucr.org/cgi-bin/paper?wm5680
In the polymeric title compound, {[Na(C10H9N4O4S)(H2O)3]·2H2O}n, sixfold coordinated Na+ cations are linked into a chain parallel to [010] by sharing common water molecules. Next to the four bridging water molecules, each Na+ cation of the chain is bonded to the O atom of a terminal water molecule and an O atom of the SO3− group of the sulfonate anion. Classical O—H⋯O, O—H⋯N and N—H⋯O hydrogen bonds and additional π–π interactions connect these chains into a three-dimensional network.urn:issn:2056-9890Aliyeva, V.A.Aliyeva, F.S.Akkurt, M.Yıldırım, S. Ö.Bhattarai, A.text/htmlIn the crystal struture of the title compound, Na+ cations form a chain parallel to [010] through bonding to common water molecules.doi:10.1107/S2056989023003602CRYSTAL STRUCTURE; HYDROGEN BONDS; [PI]-[PI] STACKING INTERACTION; CHAIN STRUCTURE; HYDRAZONE2023-04-28Synthesis and crystal structure of catena-poly[[[aqua{2-[(E)-(1-cyano-2-imino-2-methoxyethylidene)hydrazinyl]benzenesulfonato}sodium]-di-μ-aqua] dihydrate]In the polymeric title compound, {[Na(C10H9N4O4S)(H2O)3]·2H2O}n, sixfold coordinated Na+ cations are linked into a chain parallel to [010] by sharing common water molecules. Next to the four bridging water molecules, each Na+ cation of the chain is bonded to the O atom of a terminal water molecule and an O atom of the SO3− group of the sulfonate anion. Classical O—H⋯O, O—H⋯N and N—H⋯O hydrogen bonds and additional π–π interactions connect these chains into a three-dimensional network.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext511med@iucr.org2056-98902056-98905Acta Crystallographica Section E: Crystallographic CommunicationsApril 2023https://creativecommons.org/licenses/by/4.0/research communications2023-04-2850879Synthesis, crystal structure and thermal decomposition pathway of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)manganese(II)
http://scripts.iucr.org/cgi-bin/paper?hb8063
The reaction of MnCl2·2H2O with KSeCN and pyridine in water leads to the formation of the title complex, [Mn(NCSe)2(C5H5N)4], which is isotypic to its Fe, Co, Ni, Zn and Cd analogues. In its crystal structure, discrete complexes are observed that are located on centres of inversion. The Mn cations are octahedrally coordinated by four pyridine coligands and two selenocyanate anions that coordinate via the N atom to the metal centres to generate trans-MnN(s)2N(p)4 octahedra (s = selenocyanate and p = pyridine). In the extended structure, weak C—H⋯Se contacts are observed. Powder X-ray diffraction (PXRD) investigations prove that a pure sample was obtained and in the IR and Raman spectra, the C—N stretching vibrations are observed at 2058 and 2060 cm−1, respectively, in agreement with the terminal coordination of the selenocyanate anions. Thermogravimetric investigations reveal that the pyridine coligands are removed in two separate steps. In the first mass loss, a compound with the composition Mn(NCSe)2(C5H5N)2 is formed, whereas in the second mass loss, the remaining pyridine ligands are removed, which is superimposed with the decomposition of Mn(NCSe)2 formed after ligand removal. In the intermediate compound Mn(NCSe)2(C5H5N)2, the CN stretching vibration is observed at 2090 cm−1 in the Raman and at 2099 cm−1 in the IR spectra, indicating that the Mn cations are linked by μ-1,3-bridging anionic ligands. PXRD measurements show that a compound has formed that is of poor crystallinity. A comparison of the powder pattern with that calculated for the previously reported Cd(NCSe)2(C5H5N)2 indicates that these compounds are isotypic, which was proven by a Pawley fit.urn:issn:2056-9890Näther, C.Mangelsen, S.Boeckmann, J.text/htmlIn the crystal structure of the title compound, discrete complexes are observed, in which the Ni cations are octahedrally coordinated by two terminal N-bonded selenocyanate anions and four pyridine coligands. Weak C—H⋯Se interactions occur in the extended structure.doi:10.1107/S2056989023003535CRYSTAL STRUCTURE; NICKEL SELENOCYANATE; DISCRETE COMPLEX; THERMAL PROPERTIES2023-04-21Synthesis, crystal structure and thermal decomposition pathway of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)manganese(II)The reaction of MnCl2·2H2O with KSeCN and pyridine in water leads to the formation of the title complex, [Mn(NCSe)2(C5H5N)4], which is isotypic to its Fe, Co, Ni, Zn and Cd analogues. In its crystal structure, discrete complexes are observed that are located on centres of inversion. The Mn cations are octahedrally coordinated by four pyridine coligands and two selenocyanate anions that coordinate via the N atom to the metal centres to generate trans-MnN(s)2N(p)4 octahedra (s = selenocyanate and p = pyridine). In the extended structure, weak C—H⋯Se contacts are observed. Powder X-ray diffraction (PXRD) investigations prove that a pure sample was obtained and in the IR and Raman spectra, the C—N stretching vibrations are observed at 2058 and 2060 cm−1, respectively, in agreement with the terminal coordination of the selenocyanate anions. Thermogravimetric investigations reveal that the pyridine coligands are removed in two separate steps. In the first mass loss, a compound with the composition Mn(NCSe)2(C5H5N)2 is formed, whereas in the second mass loss, the remaining pyridine ligands are removed, which is superimposed with the decomposition of Mn(NCSe)2 formed after ligand removal. In the intermediate compound Mn(NCSe)2(C5H5N)2, the CN stretching vibration is observed at 2090 cm−1 in the Raman and at 2099 cm−1 in the IR spectra, indicating that the Mn cations are linked by μ-1,3-bridging anionic ligands. PXRD measurements show that a compound has formed that is of poor crystallinity. A comparison of the powder pattern with that calculated for the previously reported Cd(NCSe)2(C5H5N)2 indicates that these compounds are isotypic, which was proven by a Pawley fit.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org52056-98902056-98902023-04-21Acta Crystallographica Section E: Crystallographic CommunicationsApril 2023https://creativecommons.org/licenses/by/4.0/research communications79Crystal structure and Hirshfeld surface analysis of N-[2-(5-methylfuran-2-yl)phenyl]-3-nitro-N-[(3-nitrophenyl)sulfonyl]benzenesulfonamide
http://scripts.iucr.org/cgi-bin/paper?tx2067
In the title compound, C23H17N3O9S2, C—H⋯O hydrogen bonds link adjacent molecules in a three-dimensional network, while π–π stacking interactions, with centroid–centroid distances of 3.8745 (9) Å, between the furan and an arene ring of one of the two (3-nitrophenyl)sulfonyl groups, result in chains parallel to the a axis. The Hirshfeld surface analysis indicates that O⋯H/H⋯O (40.1%), H⋯H (27.5%) and C⋯H/H⋯C (12.4%) interactions are the most significant contributors to the crystal packing.urn:issn:2056-9890Mammadova, G.Z.Annadurdyyeva, S.Burkin, G.M.Khrustalev, V.N.Akkurt, M.Yıldırım, S. Ö.Bhattarai, A.text/htmlIn the crystal, C—H⋯O hydrogen bonds link adjacent molecules in the three-dimensional network, while π–π stacking interactions, with centroid–centroid distances of 3.8745 (9) Å, propagate into chains parallel to the a axis.doi:10.1107/S2056989023003523CRYSTAL STRUCTURE; SULFONAMIDES; HYDROGEN BONDS; [PI]-[PI] STACKING INTERACTIONS; HIRSHFELD SURFACE ANALYSIS2023-04-25Crystal structure and Hirshfeld surface analysis of N-[2-(5-methylfuran-2-yl)phenyl]-3-nitro-N-[(3-nitrophenyl)sulfonyl]benzenesulfonamideIn the title compound, C23H17N3O9S2, C—H⋯O hydrogen bonds link adjacent molecules in a three-dimensional network, while π–π stacking interactions, with centroid–centroid distances of 3.8745 (9) Å, between the furan and an arene ring of one of the two (3-nitrophenyl)sulfonyl groups, result in chains parallel to the a axis. The Hirshfeld surface analysis indicates that O⋯H/H⋯O (40.1%), H⋯H (27.5%) and C⋯H/H⋯C (12.4%) interactions are the most significant contributors to the crystal packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-04-25499research communicationshttps://creativecommons.org/licenses/by/4.0/April 2023Acta Crystallographica Section E: Crystallographic Communications52056-98902056-9890med@iucr.org503Crystal structure of 3-(benzo[d]thiazol-2-yl)-6-methyl-2H-chromen-2-one
http://scripts.iucr.org/cgi-bin/paper?yz2033
The molecule of the title compound, C17H11NO2S, is almost planar, with an interplanar angle of 3.01 (3)° between the benzothiazole and chromene ring systems. A short intramolecular S⋯O=C contact of 2.727 (2) Å is observed. The crystal packing involves a layer structure parallel to (211), containing dimeric inversion-symmetric units connected by a `weak' C—H⋯O=C hydrogen bond.urn:issn:2056-9890Abdallah, A.E.M.Elgemeie, G.H.Jones, P.G.text/htmlThe title molecule is almost planar, with an intramolecular S⋯O=C contact. The packing is a layer structure with dimeric units connected by a C—H⋯O=C hydrogen bond.doi:10.1107/S205698902300347XBENZOTHIAZOLE; COUMARIN; CRYSTAL STRUCTURE2023-04-25Crystal structure of 3-(benzo[d]thiazol-2-yl)-6-methyl-2H-chromen-2-oneThe molecule of the title compound, C17H11NO2S, is almost planar, with an interplanar angle of 3.01 (3)° between the benzothiazole and chromene ring systems. A short intramolecular S⋯O=C contact of 2.727 (2) Å is observed. The crystal packing involves a layer structure parallel to (211), containing dimeric inversion-symmetric units connected by a `weak' C—H⋯O=C hydrogen bond.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytexthttps://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsApril 20235042023-04-2579507med@iucr.org2056-98902056-98905Crystal structure and Hirshfeld surface analysis of bis(μ-4-tert-butoxy-4-oxobut-2-en-2-olato)bis[(4-tert-butoxy-4-oxobut-2-en-2-olato)ethanolzinc(II)]
http://scripts.iucr.org/cgi-bin/paper?yz2031
The molecular and crystal structure of the title binuclear Zn2+ complex, [Zn2(C8H13O3)4(C2H5OH)2], with enolated anionic tert-butylacetoacetate and ethanol was analysed. The coordination polyhedra of the Zn atoms are distorted octahedra formed by six oxygen atoms that belong to three ligand molecules and a coordinated ethanol molecule. In the crystal phase, alternating layers can be distinguished parallel to the ac plane. A Hirshfeld surface analysis showed that there are no strong intermolecular interactions in the structure. The most significant contributions to the overall crystal packing are from H⋯H intermolecular contacts.urn:issn:2056-9890Shtokvysh, O.O.Dyakonenko, V.V.Koval, L.I.Pekhnyo, V.I.text/htmlThe crystal structure of bis(μ-4-tert-butoxy-4-oxobut-2-en-2-olato)bis[(4-tert-butoxy-4-oxobut-2-en-2-olato)ethanolzinc(II)] is reported and discussed.doi:10.1107/S2056989023003377CRYSTAL STRUCTURE; COMPLEX; ZINC; TERT-BUTYL ACETOACETATE; KETO ESTER; ETHANOL; BINUCLEAR STRUCTURE2023-04-21Crystal structure and Hirshfeld surface analysis of bis(μ-4-tert-butoxy-4-oxobut-2-en-2-olato)bis[(4-tert-butoxy-4-oxobut-2-en-2-olato)ethanolzinc(II)]The molecular and crystal structure of the title binuclear Zn2+ complex, [Zn2(C8H13O3)4(C2H5OH)2], with enolated anionic tert-butylacetoacetate and ethanol was analysed. The coordination polyhedra of the Zn atoms are distorted octahedra formed by six oxygen atoms that belong to three ligand molecules and a coordinated ethanol molecule. In the crystal phase, alternating layers can be distinguished parallel to the ac plane. A Hirshfeld surface analysis showed that there are no strong intermolecular interactions in the structure. The most significant contributions to the overall crystal packing are from H⋯H intermolecular contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98905med@iucr.org79research communicationshttps://creativecommons.org/licenses/by/4.0/Acta Crystallographica Section E: Crystallographic CommunicationsApril 20232023-04-21Structure of racemic duloxetine hydrochloride
http://scripts.iucr.org/cgi-bin/paper?hb8060
Duloxetine hydrochloride (trade name Cymbalta) is marketed as a single enantiomer (S)-N-methyl-3-(naphthalen-1-yloxy)-3-(thiophen-2-yl)propylaminium chloride, C18H20NOS+·Cl−, which is twice as effective as the (R)-enantiomer in serotonin uptake. Here, we report the crystal structure of duloxetine hydrochloride in its racemic form (space group Pna21), where it shows significant differences in the molecular conformation and packing in its extended structure compared to the previously reported (S)-enantiomer crystal structure. Molecules of this type, comprising aromatic groups with a single side chain terminated in a protonated secondary amine, are commonly found in active antidepressants. A Cambridge Structural Database survey of molecules with these features reveals a strong correlation between side-chain conformation and the crystal packing: an extended side chain leads to molecules packed into separated layers of hydrophobic and ionic hydrophilic phases. By comparison, molecules with bent side chains, such as racemic duloxetine hydrochloride, lead to crystal-packing motifs where an ionic hydrophilic phase is encapsulated within a hydrophobic shell.urn:issn:2056-9890Bhadbhade, M.M.Gao, J.Rich, A.M.Marjo, C.E.text/htmlThe structure of the hydrochloride salt of the anti-depressant drug duloxetine in its racemic form shows differences in the side chain conformation and molecular packing compared to its chirally pure crystal form. A Cambridge Database search of anti-depressant structures shows a high correlation between the side-chain conformation and the packing of molecules, a feature of interest from a crystal engineering perspective.doi:10.1107/S2056989023003353ANTI-DEPRESSANT DRUG; DULOXETINE; RACEMATE; CRYSTAL STRUCTURE; SIDE CHAIN CONFORMATION; MOLECULAR PACKING2023-04-21Structure of racemic duloxetine hydrochlorideDuloxetine hydrochloride (trade name Cymbalta) is marketed as a single enantiomer (S)-N-methyl-3-(naphthalen-1-yloxy)-3-(thiophen-2-yl)propylaminium chloride, C18H20NOS+·Cl−, which is twice as effective as the (R)-enantiomer in serotonin uptake. Here, we report the crystal structure of duloxetine hydrochloride in its racemic form (space group Pna21), where it shows significant differences in the molecular conformation and packing in its extended structure compared to the previously reported (S)-enantiomer crystal structure. Molecules of this type, comprising aromatic groups with a single side chain terminated in a protonated secondary amine, are commonly found in active antidepressants. A Cambridge Structural Database survey of molecules with these features reveals a strong correlation between side-chain conformation and the crystal packing: an extended side chain leads to molecules packed into separated layers of hydrophobic and ionic hydrophilic phases. By comparison, molecules with bent side chains, such as racemic duloxetine hydrochloride, lead to crystal-packing motifs where an ionic hydrophilic phase is encapsulated within a hydrophobic shell.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext52056-98902056-9890med@iucr.org792023-04-21Acta Crystallographica Section E: Crystallographic CommunicationsApril 2023https://creativecommons.org/licenses/by/4.0/research communicationsCrystal structure and Hirshfeld surface analysis of (5aS,8aR)-3,5a-dimethyl-8-methylidene-2-oxododecahydrooxireno[2′,3′:6,7]naphtho[1,2-b]furan-6-yl (Z)-2-methylbut-2-enoate extracted from Ferula persica
http://scripts.iucr.org/cgi-bin/paper?wm5679
In the title compound, C20H26O5, the two cyclohexane rings adopt boat and half-chair conformations. In the crystal, adjacent molecules are connected by intermolecular C—H⋯O hydrogen bonds, forming a three-dimensional network. According to a Hirshfeld surface study, H⋯H interactions are the most significant contributors to the crystal packing (63.0%).urn:issn:2056-9890Karimli, E.G.Khrustalev, V.N.Kurasova, M.N.Akkurt, M.Khalilov, A.N.Bhattarai, A.Mamedov, İ.G.text/htmlIn the crystal of the title compound, adjacent molecules are connected by intermolecular C—H⋯O hydrogen bonds, forming a three-dimensional network.doi:10.1107/S205698902300333XCRYSTAL STRUCTURE; HYDROGEN BONDS; SESQUITERPENE LACTONES; FERULA PERSICA; HIRSHFELD SURFACE ANALYSIS2023-04-21Crystal structure and Hirshfeld surface analysis of (5aS,8aR)-3,5a-dimethyl-8-methylidene-2-oxododecahydrooxireno[2′,3′:6,7]naphtho[1,2-b]furan-6-yl (Z)-2-methylbut-2-enoate extracted from Ferula persicaIn the title compound, C20H26O5, the two cyclohexane rings adopt boat and half-chair conformations. In the crystal, adjacent molecules are connected by intermolecular C—H⋯O hydrogen bonds, forming a three-dimensional network. According to a Hirshfeld surface study, H⋯H interactions are the most significant contributors to the crystal packing (63.0%).https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext52056-98902056-9890med@iucr.org792023-04-21https://creativecommons.org/licenses/by/4.0/research communicationsApril 2023Acta Crystallographica Section E: Crystallographic CommunicationsSyntheses, crystal structures and Hirshfeld surface analyses of four molecular salts of amitriptynol
http://scripts.iucr.org/cgi-bin/paper?hb8061
The syntheses and crystal structures of four salts of amitriptynol (C20H25NO) with different carboxylic acids are described. The salts formed directly from solutions of amitriptyline (which first hydrolysed to amitriptynol) and the corresponding acid in acetonitrile to form amitriptynolium [systematic name: (3-{2-hydroxytricyclo[9.4.0.03,8]pentadeca-1(11),3,5,7,12,14-hexaen-2-yl}propyl)dimethylazanium] 4-methoxybenzoate monohydrate, C20H26NO+·C8H7O3−·H2O, (I), amitriptynolium 3,4-dimethoxybenzoate trihydrate, C20H26NO+·C9H9O4−·3H2O, (II), amitriptynolium 2-chlorobenzoate, C20H26NO+·C7H4ClO2−, (III), and amitriptynolium thiophene-2-carboxylate monohydrate, C20H26NO+·C5H3O2S−·H2O, (IV). Compound (III) crystallizes with two cations, two anions and six water molecules in the asymmetric unit. The different conformations of the amitriptynolium cations are determined by the torsion angles in the dimethylamino-propyl chains and the –CH2–CH2- bridge between the benzene rings in the tricyclic ring system, and are complicated by disorder of the bridging unit in II and III. The packing in all four salts is dominated by N—H⋯O and O—H⋯O hydrogen bonds. Hirshfeld surface analyses show that the amitriptynolium cations make similar inter-species contacts, despite the distinctly different packing in each salt.urn:issn:2056-9890VinayaAnil Kumar, H.G.Mohan Kumar, T.M.Lakshmana, B.Basavaraju, Y.B.Yathirajan, H.S.Parkin, S.text/htmlThe syntheses and low-temperature crystal structures of four organic salts of amitriptynol, a common impurity in the anti-depressant drug amitriptyline, are described.doi:10.1107/S2056989023003225AMITRIPTYNOL; AMITRIPTYLINE; HYDROGEN BONDING; HIRSHFELD-SURFACE ANALYSIS; CRYSTAL STRUCTURE2023-04-14Syntheses, crystal structures and Hirshfeld surface analyses of four molecular salts of amitriptynolThe syntheses and crystal structures of four salts of amitriptynol (C20H25NO) with different carboxylic acids are described. The salts formed directly from solutions of amitriptyline (which first hydrolysed to amitriptynol) and the corresponding acid in acetonitrile to form amitriptynolium [systematic name: (3-{2-hydroxytricyclo[9.4.0.03,8]pentadeca-1(11),3,5,7,12,14-hexaen-2-yl}propyl)dimethylazanium] 4-methoxybenzoate monohydrate, C20H26NO+·C8H7O3−·H2O, (I), amitriptynolium 3,4-dimethoxybenzoate trihydrate, C20H26NO+·C9H9O4−·3H2O, (II), amitriptynolium 2-chlorobenzoate, C20H26NO+·C7H4ClO2−, (III), and amitriptynolium thiophene-2-carboxylate monohydrate, C20H26NO+·C5H3O2S−·H2O, (IV). Compound (III) crystallizes with two cations, two anions and six water molecules in the asymmetric unit. The different conformations of the amitriptynolium cations are determined by the torsion angles in the dimethylamino-propyl chains and the –CH2–CH2- bridge between the benzene rings in the tricyclic ring system, and are complicated by disorder of the bridging unit in II and III. The packing in all four salts is dominated by N—H⋯O and O—H⋯O hydrogen bonds. Hirshfeld surface analyses show that the amitriptynolium cations make similar inter-species contacts, despite the distinctly different packing in each salt.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org52056-98902056-98902023-04-14April 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications79Crystal structure and Hirshfeld surface analysis of 1,6-diamino-2-oxo-4-(thiophen-2-yl)-1,2-dihydropyridine-3,5-dicarbonitrile
http://scripts.iucr.org/cgi-bin/paper?tx2066
The asymmetric unit of the title compound, C11H7N5OS, contains two independent molecules (1 and 2). The thiophene ring in molecule 2 is rotationally disordered (flip disorder) by ca 180° (around the single C—C bond, to which it is attached) over two sites with the site-occupation factors of 0.9 and 0.1. These two orientations of the thiophene ring in molecule 2 are not equivalent. In the crystal, molecules are linked by intermolecular N—H⋯O and N—H⋯N hydrogen bonds into ribbons parallel to (022) along the a axis. Within the (022) planes, these ribbons are connected by van der Waals interactions and between the (022) planes by N—H⋯O hydrogen bonds. In molecule 1, Hirshfeld surface analysis showed that the most important contributions to the crystal packing are from N⋯H/H⋯N (27.1%), H⋯H (17.6%), C⋯H/H⋯C (13.6%) and O⋯H/H⋯O (9.3%) interactions, while in molecule 2, H⋯H (25.4%) interactions are the most significant contributors to the crystal packing.urn:issn:2056-9890Naghiyev, F.N.Khrustalev, V.N.Akkurt, M.Khalilov, A.N.Bhattarai, A.Kerimli, F.S.Mamedov, İ.G.text/htmlIn the crystal, molecules are linked by intermolecular N—H⋯O and N—H⋯N hydrogen bonds into ribbons parallel to (022) along the a axis. These ribbons are connected by N—H⋯O, N—H⋯N hydrogen bonds and van der Waals interactions.doi:10.1107/S2056989023003237CRYSTAL STRUCTURE; 1,2-DIHYDROPYRIDINE; HYDROGEN BOND; DISORDER; HIRSHFELD SURFACE ANALYSIS2023-04-21Crystal structure and Hirshfeld surface analysis of 1,6-diamino-2-oxo-4-(thiophen-2-yl)-1,2-dihydropyridine-3,5-dicarbonitrileThe asymmetric unit of the title compound, C11H7N5OS, contains two independent molecules (1 and 2). The thiophene ring in molecule 2 is rotationally disordered (flip disorder) by ca 180° (around the single C—C bond, to which it is attached) over two sites with the site-occupation factors of 0.9 and 0.1. These two orientations of the thiophene ring in molecule 2 are not equivalent. In the crystal, molecules are linked by intermolecular N—H⋯O and N—H⋯N hydrogen bonds into ribbons parallel to (022) along the a axis. Within the (022) planes, these ribbons are connected by van der Waals interactions and between the (022) planes by N—H⋯O hydrogen bonds. In molecule 1, Hirshfeld surface analysis showed that the most important contributions to the crystal packing are from N⋯H/H⋯N (27.1%), H⋯H (17.6%), C⋯H/H⋯C (13.6%) and O⋯H/H⋯O (9.3%) interactions, while in molecule 2, H⋯H (25.4%) interactions are the most significant contributors to the crystal packing.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79April 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications2023-04-212056-98902056-98905med@iucr.orgFormation of Ba3Nb0.75Mn2.25O9-6H during thermochemical reduction of Ba4NbMn3O12-12R
http://scripts.iucr.org/cgi-bin/paper?wm5677
The resurgence of interest in hydrogen-related technologies has stimulated new studies aimed at advancing lesser-developed water-splitting processes, such as solar thermochemical hydrogen production (STCH). Progress in STCH has been largely hindered by a lack of new materials able to efficiently split water at a rate comparable to ceria under identical experimental conditions. BaCe0.25Mn0.75O3 (BCM) recently demonstrated enhanced hydrogen production over ceria and has the potential to further our understanding of two-step thermochemical cycles. A significant feature of the 12R hexagonal perovskite structure of BCM is the tendency to, in part, form a 6H polytype at high temperatures and reducing environments (i.e., during the first step of the thermochemical cycle), which may serve to mitigate degradation of the complex oxide. An analogous compound, namely BaNb0.25Mn0.75O3 (BNM) with a 12R structure was synthesized and displays nearly complete conversion to the 6H structure under identical reaction conditions as BCM. The structure of the BNM-6H polytype was determined from Rietveld refinement of synchrotron powder X-ray diffraction data and is presented within the context of the previously established BCM-6H structure.urn:issn:2056-9890Strange, N.A.Bell, R.T.Park, J.E.Stone, K.H.Coker, E.N.Ginley, D.S.text/htmlNearly complete conversion to a Ba3Nb0.75Mn2.25O9-6H structure was observed following thermochemical reduction of the parent Ba4NbMn3O12-12R material. The Ba3Nb0.75Mn2.25O9-6H structure represents a hexagonal perovskite that displays substitution of Mn onto Nb sites in order to satisfy the 3:1 Mn:Nb ratio within the 6H structural motif.doi:10.1107/S2056989023003213CRYSTAL STRUCTURE; POWDER SYNCHROTRON DIFFRACTION; COMPLEX OXIDES; HEXAGONAL PEROVSKITES; SOLAR THERMOCHEMICAL HYDROGEN PRODUCTION2023-04-14Formation of Ba3Nb0.75Mn2.25O9-6H during thermochemical reduction of Ba4NbMn3O12-12RThe resurgence of interest in hydrogen-related technologies has stimulated new studies aimed at advancing lesser-developed water-splitting processes, such as solar thermochemical hydrogen production (STCH). Progress in STCH has been largely hindered by a lack of new materials able to efficiently split water at a rate comparable to ceria under identical experimental conditions. BaCe0.25Mn0.75O3 (BCM) recently demonstrated enhanced hydrogen production over ceria and has the potential to further our understanding of two-step thermochemical cycles. A significant feature of the 12R hexagonal perovskite structure of BCM is the tendency to, in part, form a 6H polytype at high temperatures and reducing environments (i.e., during the first step of the thermochemical cycle), which may serve to mitigate degradation of the complex oxide. An analogous compound, namely BaNb0.25Mn0.75O3 (BNM) with a 12R structure was synthesized and displays nearly complete conversion to the 6H structure under identical reaction conditions as BCM. The structure of the BNM-6H polytype was determined from Rietveld refinement of synchrotron powder X-ray diffraction data and is presented within the context of the previously established BCM-6H structure.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext79Acta Crystallographica Section E: Crystallographic CommunicationsApril 2023research communicationshttps://creativecommons.org/licenses/by/4.0/2023-04-142056-98902056-98905med@iucr.orgCrystal structure and Hirshfeld surface analysis of 2,2′-[(3,5-di-tert-butyl-4-hydroxyphenyl)methanediyl]bis(3-hydroxy-5,5-dimethylcyclohex-2-en-1-one)
http://scripts.iucr.org/cgi-bin/paper?zn2027
In the title compound, C31H44O5, molecules are connected by O—H⋯O and C—H⋯O hydrogen bonds, forming hydrogen-bonded zigzag chains running along the b axis and parallel to the (001) plane. The molecular packing is stabilized by van der Waals interactions between these chains along the a and c axes. The intermolecular interactions in the crystal structure were quantified and analysed using Hirshfeld surface analysis.urn:issn:2056-9890Khalilov, A.N.Khrustalev, V.N.Aleksandrova, L.V.Akkurt, M.Rzayev, R.M.Bhattarai, A.Mamedov, İ.G.text/htmlIn the title compound, molecules are linked together by O—H⋯O and C—H⋯O hydrogen bonds, forming zigzag chains that are parallel to the (001) plane and run along the b-axis direction. van der Waals interactions between these chains along the a and c axes maintain the molecular packing.doi:10.1107/S2056989023003171CRYSTAL STRUCTURE; HYDROGEN BONDS; HYDROGEN-BONDED ZIGZAG CHAINS; VAN DER WAALS INTERACTIONS; 1,8-DIOXO-OCTAHYDROXANTHENE; HIRSHFELD SURFACE ANALYSIS2023-04-14Crystal structure and Hirshfeld surface analysis of 2,2′-[(3,5-di-tert-butyl-4-hydroxyphenyl)methanediyl]bis(3-hydroxy-5,5-dimethylcyclohex-2-en-1-one)In the title compound, C31H44O5, molecules are connected by O—H⋯O and C—H⋯O hydrogen bonds, forming hydrogen-bonded zigzag chains running along the b axis and parallel to the (001) plane. The molecular packing is stabilized by van der Waals interactions between these chains along the a and c axes. The intermolecular interactions in the crystal structure were quantified and analysed using Hirshfeld surface analysis.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext52056-98902056-9890med@iucr.org792023-04-14Acta Crystallographica Section E: Crystallographic CommunicationsApril 2023research communicationshttps://creativecommons.org/licenses/by/4.0/Structural, Hirshfeld surface and three-dimensional interaction-energy studies of 1,3,5-triethyl 2-amino-3,5-dicyano-4,6-bis(4-fluorophenyl)cyclohex-1-ene-1,3,5-tricarboxylate
http://scripts.iucr.org/cgi-bin/paper?ex2065
In the title compound, C29H27F2N3O6, which crystallizes in the monoclinic space group P21/c, the cyclohexenone ring is puckered and adopts an envelope conformation. The crystal structure features various intermolecular interactions, such as N—H⋯O, C—H⋯N and C—H⋯O. These interactions were investigated using Hirshfeld surface analysis and the three-dimensional interaction energies were calculated using the B3LYP/6–31 G(d,p) energy density model.urn:issn:2056-9890Chandana, S.N.Ganesha, D.P.Sreenatha, N.R.Harisha, A.S.Lakshminarayana, B.N.text/htmlThe various intermolecular interactions, such as N—H⋯O, C—H⋯N and C—H⋯O, were investigated using Hirshfeld surface analysis and the three-dimensional interaction energies were calculated.doi:10.1107/S2056989023003134SINGLE-CRYSTAL XRD; ENVELOPE CONFORMATION; HIRSHFELD SURFACES; THREE-DIMENSIONAL INTERACTION ENERGIES2023-04-14Structural, Hirshfeld surface and three-dimensional interaction-energy studies of 1,3,5-triethyl 2-amino-3,5-dicyano-4,6-bis(4-fluorophenyl)cyclohex-1-ene-1,3,5-tricarboxylateIn the title compound, C29H27F2N3O6, which crystallizes in the monoclinic space group P21/c, the cyclohexenone ring is puckered and adopts an envelope conformation. The crystal structure features various intermolecular interactions, such as N—H⋯O, C—H⋯N and C—H⋯O. These interactions were investigated using Hirshfeld surface analysis and the three-dimensional interaction energies were calculated using the B3LYP/6–31 G(d,p) energy density model.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext52056-98902056-9890med@iucr.org792023-04-14https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsApril 2023Crystal structures and Hirshfeld surface analyses of tetrakis(4,5-dihydrofuran-2-yl)silane and tetrakis(4,5-dihydrofuran-2-yl)germane
http://scripts.iucr.org/cgi-bin/paper?hb8058
The title compounds Si(C4H5O)4 (1) and Ge(C4H5O)4 (2) are dihydrofuryl compounds of silicon and germanium and are useful building blocks for the functionalization of these elements. Both structures crystallize in space group P21/n in the monoclinic crystal system with two molecules in the asymmetric unit: the Si and Ge atoms adopt slightly distorted tetrahedral geometries, while the C4H5O moieties exhibit shallow envelope conformations. Through a Hirshfeld surface analysis of the structures, interactions within the crystal packing could be elucidated: compound 1 features a polymeric chain in the (101) plane via C—H⋯O hydrogen bonds whereas in 2 C—H⋯O hydrogen bonds create a polymeric chain in the (010) plane.urn:issn:2056-9890Ressel, A.Krupp, A.Strohmann, C.text/htmlThe crystal structures of a dihydrofurylsilane and a dihydrofurylgermane are reported. Hirshfeld surface analyses were performed to investigate the intermolecular interactions.doi:10.1107/S2056989023003158CRYSTAL STRUCTURE; DIHYDROFURANYL GROUPS (DHF); HIRSHFELD SURFACE ANALYSIS; DIHYDROFURYLSILAN; DIHYDROFURYLGERMANE2023-04-14Crystal structures and Hirshfeld surface analyses of tetrakis(4,5-dihydrofuran-2-yl)silane and tetrakis(4,5-dihydrofuran-2-yl)germaneThe title compounds Si(C4H5O)4 (1) and Ge(C4H5O)4 (2) are dihydrofuryl compounds of silicon and germanium and are useful building blocks for the functionalization of these elements. Both structures crystallize in space group P21/n in the monoclinic crystal system with two molecules in the asymmetric unit: the Si and Ge atoms adopt slightly distorted tetrahedral geometries, while the C4H5O moieties exhibit shallow envelope conformations. Through a Hirshfeld surface analysis of the structures, interactions within the crystal packing could be elucidated: compound 1 features a polymeric chain in the (101) plane via C—H⋯O hydrogen bonds whereas in 2 C—H⋯O hydrogen bonds create a polymeric chain in the (010) plane.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-04-14https://creativecommons.org/licenses/by/4.0/research communicationsApril 2023Acta Crystallographica Section E: Crystallographic Communications52056-98902056-9890med@iucr.orgElectron crystallography and dedicated electron-diffraction instrumentation
http://scripts.iucr.org/cgi-bin/paper?pk2676
Electron diffraction (known also as ED, 3D ED or microED) is gaining momentum in science and industry. The application of electron diffraction in performing nano-crystallography on crystals smaller than 1 µm is a disruptive technology that is opening up fascinating new perspectives for a wide variety of compounds required in the fields of chemical, pharmaceutical and advanced materials research. Electron diffraction enables the characterization of solid compounds complementary to neutron, powder X-ray and single-crystal X-ray diffraction, as it has the unique capability to measure nanometre-sized crystals. The recent introduction of dedicated instrumentation to perform ED experiments is a key aspect of the continued growth and success of this technology. In addition to the ultra-high-speed hybrid-pixel detectors enabling ED data collection in continuous rotation mode, a high-precision goniometer and horizontal layout have been determined as essential features of an electron diffractometer, both of which are embodied in the Eldico ED-1. Four examples of data collected on an Eldico ED-1 are showcased to demonstrate the potential and advantages of a dedicated electron diffractometer, covering selected applications and challenges of electron diffraction: (i) multiple reciprocal lattices, (ii) absolute structure of a chiral compound, and (iii) R-values achieved by kinematic refinement comparable to X-ray data.urn:issn:2056-9890Simoncic, P.Romeijn, E.Hovestreydt, E.Steinfeld, G.Santiso-Quiñones, G.Merkelbach, J.text/htmlRecent years have seen a flurry of research activity in the field of electron diffraction. The introduction of the electron diffractometer, designed to be fully dedicated to its task of providing the best data from electron-diffraction experiments, will be a crucial factor for the continued growth and success of this technology.doi:10.1107/S20569890230031093D ELECTRON DIFFRACTION; NANO CRYSTALLOGRAPHY; INSTRUMENTATION; ELECTRON DIFFRACTOMETER; 3D ELECTRON DIFFRACTION, NANO CRYSTALLOGRAPHY, INSTRUMENTATION, ELECTRON DIFFRACTOMETER2023-04-14Electron crystallography and dedicated electron-diffraction instrumentationElectron diffraction (known also as ED, 3D ED or microED) is gaining momentum in science and industry. The application of electron diffraction in performing nano-crystallography on crystals smaller than 1 µm is a disruptive technology that is opening up fascinating new perspectives for a wide variety of compounds required in the fields of chemical, pharmaceutical and advanced materials research. Electron diffraction enables the characterization of solid compounds complementary to neutron, powder X-ray and single-crystal X-ray diffraction, as it has the unique capability to measure nanometre-sized crystals. The recent introduction of dedicated instrumentation to perform ED experiments is a key aspect of the continued growth and success of this technology. In addition to the ultra-high-speed hybrid-pixel detectors enabling ED data collection in continuous rotation mode, a high-precision goniometer and horizontal layout have been determined as essential features of an electron diffractometer, both of which are embodied in the Eldico ED-1. Four examples of data collected on an Eldico ED-1 are showcased to demonstrate the potential and advantages of a dedicated electron diffractometer, covering selected applications and challenges of electron diffraction: (i) multiple reciprocal lattices, (ii) absolute structure of a chiral compound, and (iii) R-values achieved by kinematic refinement comparable to X-ray data.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-04-14April 2023Acta Crystallographica Section E: Crystallographic Communicationsresearch communicationshttps://creativecommons.org/licenses/by/4.0/52056-98902056-9890med@iucr.orgSynthesis and crystal structure of a new copper(II) complex based on 5-ethyl-3-(pyridin-2-yl)-1,2,4-triazole
http://scripts.iucr.org/cgi-bin/paper?jy2029
The title compound, bis[μ-3-ethyl-5-(pyridin-2-yl)-1H-1,2,4-triazol-1-ido]bis[acetato(dimethylformamide)copper(II)], [Cu2(C9H9N4)2(C2H3O2)2(C3H7NO)2] or [Cu2(LEt)2(OAc)2(dmf)2], is a triazolate complex, which contains two 3-(2-pyridyl)-5-ethyl-triazolates (LEt)− in bidentate-bridged coordination modes. Both copper atoms are involved in the formation of a planar six-membered metallocycle Cu–[N—N]2–Cu. The inversion center of the complex is located at the mid-point of the Cu⋯Cu vector. Each CuII atom has a distorted trigonal–bipyramidal environment formed by the three nitrogen atoms of the deprotonated bridging 3-(2-pyridyl)-5-ethyl-triazolate unit, oxygen atoms of the OAc− group and dmf molecule. In the crystal, C—H⋯O hydrogen bonds link the molecules into chains running along the c-axis direction.urn:issn:2056-9890Petrenko, Y.P.Khomenko, D.M.Doroshchuk, R.O.Raspertova, I.V.Shova, S.Lampeka, R.D.text/htmlA new copper(II) coordination compound [Cu2(LEt)2(OAc)2(dmf)2], where HLEt = 3-(2-pyridyl)-5-ethyl-1,2,4-triazole, was synthesized and structurally characterized by single-crystal X-ray diffraction.doi:10.1107/S2056989023003079COPPER(II) COMPLEX; X-RAY CRYSTALLOGRAPHY; ACETATE ANION; 3-(2-PYRIDYL)-1,2,4-TRIAZOLE; CRYSTAL PACKING2023-04-14Synthesis and crystal structure of a new copper(II) complex based on 5-ethyl-3-(pyridin-2-yl)-1,2,4-triazoleThe title compound, bis[μ-3-ethyl-5-(pyridin-2-yl)-1H-1,2,4-triazol-1-ido]bis[acetato(dimethylformamide)copper(II)], [Cu2(C9H9N4)2(C2H3O2)2(C3H7NO)2] or [Cu2(LEt)2(OAc)2(dmf)2], is a triazolate complex, which contains two 3-(2-pyridyl)-5-ethyl-triazolates (LEt)− in bidentate-bridged coordination modes. Both copper atoms are involved in the formation of a planar six-membered metallocycle Cu–[N—N]2–Cu. The inversion center of the complex is located at the mid-point of the Cu⋯Cu vector. Each CuII atom has a distorted trigonal–bipyramidal environment formed by the three nitrogen atoms of the deprotonated bridging 3-(2-pyridyl)-5-ethyl-triazolate unit, oxygen atoms of the OAc− group and dmf molecule. In the crystal, C—H⋯O hydrogen bonds link the molecules into chains running along the c-axis direction.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytextmed@iucr.org52056-98902056-98902023-04-14research communicationshttps://creativecommons.org/licenses/by/4.0/April 2023Acta Crystallographica Section E: Crystallographic Communications79Crystal and molecular structure of 4-fluoro-1H-pyrazole at 150 K
http://scripts.iucr.org/cgi-bin/paper?vm2280
Only two 4-halo-1H-pyrazole crystal structures are known to date (chloro and bromo, the structure of 4-iodo-1H-pyrazole has not been reported yet). The triclinic structure of 4-fluoro-1H-pyrazole, C3H3FN2 (P\overline{1}), reported here is not isomorphous with those of the chloro and bromo analogues (which are isomorphous, orthorhombic Pnma). To avoid sublimation during the measurement, diffraction data were collected at 150 K. Two crystallographically unique 4-fluoro-1H-pyrazole moieties linked by an N—H⋯N hydrogen bond are found in the asymmetric unit. Unlike the trimeric supramolecular motifs found in the structures of the chloro and bromo analogues, 4-fluoro-1H-pyrazole forms one-dimensional chains by intermolecular hydrogen bonding in the crystal.urn:issn:2056-9890Ahmed, B.M.Zeller, M.Mezei, G.text/htmlTwo crystallographically unique 4-fluoro-1H-pyrazole moieties linked by an N—H⋯N hydrogen bond are found in the asymmetric unit. Unlike the trimeric supramolecular motifs found in the structures of the chloro and bromo analogues, 4-fluoro-1H-pyrazole forms one-dimensional chains by intermolecular hydrogen bonding in the crystal.doi:10.1107/S2056989023003055PYRAZOLE; CRYSTAL STRUCTURE; LOW TEMPERATURE; HYDROGEN-BONDING MOTIFS2023-04-06Crystal and molecular structure of 4-fluoro-1H-pyrazole at 150 KOnly two 4-halo-1H-pyrazole crystal structures are known to date (chloro and bromo, the structure of 4-iodo-1H-pyrazole has not been reported yet). The triclinic structure of 4-fluoro-1H-pyrazole, C3H3FN2 (P\overline{1}), reported here is not isomorphous with those of the chloro and bromo analogues (which are isomorphous, orthorhombic Pnma). To avoid sublimation during the measurement, diffraction data were collected at 150 K. Two crystallographically unique 4-fluoro-1H-pyrazole moieties linked by an N—H⋯N hydrogen bond are found in the asymmetric unit. Unlike the trimeric supramolecular motifs found in the structures of the chloro and bromo analogues, 4-fluoro-1H-pyrazole forms one-dimensional chains by intermolecular hydrogen bonding in the crystal.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2023-04-06April 2023Acta Crystallographica Section E: Crystallographic Communicationshttps://creativecommons.org/licenses/by/4.0/research communications79med@iucr.org52056-98902056-9890Syntheses and crystal structures of three salts of 1-(4-nitrophenyl)piperazine
http://scripts.iucr.org/cgi-bin/paper?hb8051
The crystal structures and Hirshfeld surface analyses of three salts of 1-(4-nitrophenyl)piperazine with 2-chlorobenzoic acid, 2-bromobenzoic acid and 2-iodobenzoic acid are reported. The chlorobenzoate salt, C10H14N3O2+·C7H4ClO2−, contains whole-ion-disordered cations and anions, which were modeled with two equivalent conformations with occupancies of 0.745 (10)/0.255 (10) and 0.563 (13)/0.437 (13), respectively. The bromobenzoate and iodobenzoate derivatives are isomorphous and crystallize as hemihydrates, viz. C10H14N3O2+·C7H4BrO2−·0.5H2O and C10H14N3O2+·C7H4IO2−·0.5H2O, respectively [the water molecule is disordered over two locations with occupancies of 0.276 (3)/0.223 (3) for the iodobenzoate derivative]. In the extended structures, all three salts feature an R44(12) loop of two anions and two cations linked by N—H⋯O hydrogen bonds.urn:issn:2056-9890Prasad, H.J.S.DevarajuYathirajan, H.S.Akkurt, M.Foro, S.Balerao, R.Butcher, R.J.text/htmlThe crystal structures and Hirshfeld surface analyses of three salts of 1-(4-nitrophenyl)piperazine with 2-chlorobenzoic acid, 2-bromobenzoic acid and 2-iodobenzoic acid are reported.doi:10.1107/S205698902300302XCRYSTAL STRUCTURE; PIPERAZINIUM CATION; CARBOXYLATE ANION; SUPRAMOLECULAR FEATURES; HIRSHFELD ANALYSIS2023-04-06Syntheses and crystal structures of three salts of 1-(4-nitrophenyl)piperazineThe crystal structures and Hirshfeld surface analyses of three salts of 1-(4-nitrophenyl)piperazine with 2-chlorobenzoic acid, 2-bromobenzoic acid and 2-iodobenzoic acid are reported. The chlorobenzoate salt, C10H14N3O2+·C7H4ClO2−, contains whole-ion-disordered cations and anions, which were modeled with two equivalent conformations with occupancies of 0.745 (10)/0.255 (10) and 0.563 (13)/0.437 (13), respectively. The bromobenzoate and iodobenzoate derivatives are isomorphous and crystallize as hemihydrates, viz. C10H14N3O2+·C7H4BrO2−·0.5H2O and C10H14N3O2+·C7H4IO2−·0.5H2O, respectively [the water molecule is disordered over two locations with occupancies of 0.276 (3)/0.223 (3) for the iodobenzoate derivative]. In the extended structures, all three salts feature an R44(12) loop of two anions and two cations linked by N—H⋯O hydrogen bonds.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext792023-04-06https://creativecommons.org/licenses/by/4.0/research communicationsApril 2023Acta Crystallographica Section E: Crystallographic Communications52056-98902056-9890med@iucr.orgCrystal structure of N-[3-(benzo[d]thiazol-2-yl)-6-bromo-2H-chromen-2-ylidene]-4-methylbenzenamine
http://scripts.iucr.org/cgi-bin/paper?yz2032
The title compound, C23H15BrN2OS, was the unexpected product in an attempted synthesis of the isomeric 3-(benzo[d]thiazol-2-yl)-6-bromo-1-p-tolylquinolin-2(1H)-one. The Cchromene=N—C angle is wide [125.28 (8)°]. The benzothiazole and chromene ring systems are almost coplanar, with their planes parallel to (1\overline{1}0); the toluene ring system is rotated by ca 40° out of the chromene plane. The molecular packing involves layers with π-stacking, borderline `weak' hydrogen bonds and possible C—H⋯π contacts.urn:issn:2056-9890Abdallah, A.E.M.Elgemeie, G.H.Jones, P.G.text/htmlIn the crystal structure of the title compound, the C=N—C angle is wide [125.28 (8)°]. The benzothiazole and chromene ring systems are almost coplanar and lie parallel to (1\overline{1}0); the toluene ring system is rotated by ca 40° out of the chromene plane.doi:10.1107/S2056989023002979CRYSTAL STRUCTURE; BENZO[D]THIAZOLE; CHROMENE; IMINE; [PI]-[PI]-STACKING2023-04-14Crystal structure of N-[3-(benzo[d]thiazol-2-yl)-6-bromo-2H-chromen-2-ylidene]-4-methylbenzenamineThe title compound, C23H15BrN2OS, was the unexpected product in an attempted synthesis of the isomeric 3-(benzo[d]thiazol-2-yl)-6-bromo-1-p-tolylquinolin-2(1H)-one. The Cchromene=N—C angle is wide [125.28 (8)°]. The benzothiazole and chromene ring systems are almost coplanar, with their planes parallel to (1\overline{1}0); the toluene ring system is rotated by ca 40° out of the chromene plane. The molecular packing involves layers with π-stacking, borderline `weak' hydrogen bonds and possible C—H⋯π contacts.https://creativecommons.org/licenses/by/4.0/enInternational Union of Crystallographytext2056-98902056-98905med@iucr.org79https://creativecommons.org/licenses/by/4.0/research communicationsActa Crystallographica Section E: Crystallographic CommunicationsApril 20232023-04-14