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IUCrData is a peer-reviewed open-access data publication from the International Union of Crystallography (IUCr). It aims to provide short descriptions of crystallographic datasets and datasets from related scientific disciplines. The primary article category is Data Reports; these describe crystal structures of inorganic, metal-organic or organic compounds. Information on each crystal structure includes the crystallographic data (CIF and structure factors), a data validation report, figures and a text representation of the data.en-gbCopyright (c) 2024 International Union of CrystallographyInternational Union of CrystallographyInternational Union of CrystallographyOpen-access and free articles in IUCrDatahttps://journals.iucr.orgtext/htmlIUCrData is a peer-reviewed open-access data publication from the International Union of Crystallography (IUCr). It aims to provide short descriptions of crystallographic datasets and datasets from related scientific disciplines. The primary article category is Data Reports; these describe crystal structures of inorganic, metal-organic or organic compounds. Information on each crystal structure includes the crystallographic data (CIF and structure factors), a data validation report, figures and a text representation of the data.urn:issn:2414-3146text12002-01-28+00:00monthlyCopyright (c) 2024 International Union of Crystallographyurn:issn:2414-3146med@iucr.orgIUCrDataOpen-access and free articles in IUCrDatahttp://journals.iucr.org/logos/rss10x.gif
https://journals.iucr.org/x/journalhomepage.html
Still image5-Bromo-2-(phenylamino)benzoic acid
http://scripts.iucr.org/cgi-bin/paper?hb4456
The title compound, C13H10BrNO2, was obtained by the reaction of 2,5-dibromobenzoic acid and aniline. The molecule is twisted with a dihedral angle between the aromatic rings of 45.74 (11)° and an intramolecular N—H⋯O hydrogen bond is seen. In the crystal, pairwise O—H⋯O hydrogen bonds generate carboxylic acid inversion dimers.The molecules of the title compound pair up to form carboxylic acid–carboxylic acid homodimers in the crystal structure.International Union of CrystallographyenSYNTHON; HYDROGEN BOND; ACID-ACID DIMER; CRYSTAL STRUCTURE5-Bromo-2-(phenylamino)benzoic acidurn:issn:2414-3146text/htmlThe title compound, C13H10BrNO2, was obtained by the reaction of 2,5-dibromobenzoic acid and aniline. The molecule is twisted with a dihedral angle between the aromatic rings of 45.74 (11)° and an intramolecular N—H⋯O hydrogen bond is seen. In the crystal, pairwise O—H⋯O hydrogen bonds generate carboxylic acid inversion dimers.doi:10.1107/S24143146240019862024-03-06texthttps://creativecommons.org/licenses/by/4.0/Kang, L.Long, S.organic compounds2414-314632414-3146x240198March 20242024-03-06med@iucr.orghttps://creativecommons.org/licenses/by/4.0/9IUCrData4-Fluoro-2-(phenylamino)benzoic acid
http://scripts.iucr.org/cgi-bin/paper?hb4457
The title compound, C13H10FNO2, was obtained by the reaction of 2-bromo-4-fluorobenzoic acid with aniline. There are two independent molecules, A and B, in the asymmetric unit, with slight conformational differences: the dihedral angles between the aromatic rings are 55.63 (5) and 52.65 (5)°. Both molecules feature an intramolecular N—H⋯O hydrogen bond. In the crystal, the molecules are linked by pairwise O—H⋯O hydrogen bonds to form A–B acid–acid dimers and weak C—H⋯F interactions further connect the dimers.There are two crystallographically independent molecules in the asymmetric unit of the title compound, which are linked by pairwise O—H⋯O hydrogen bonds.International Union of CrystallographyenZ' = 2; TWISTED CONFORMATION; ACID-ACID DIMER; CRYSTAL STRUCTURE4-Fluoro-2-(phenylamino)benzoic acidurn:issn:2414-3146text/htmlThe title compound, C13H10FNO2, was obtained by the reaction of 2-bromo-4-fluorobenzoic acid with aniline. There are two independent molecules, A and B, in the asymmetric unit, with slight conformational differences: the dihedral angles between the aromatic rings are 55.63 (5) and 52.65 (5)°. Both molecules feature an intramolecular N—H⋯O hydrogen bond. In the crystal, the molecules are linked by pairwise O—H⋯O hydrogen bonds to form A–B acid–acid dimers and weak C—H⋯F interactions further connect the dimers.doi:10.1107/S24143146240019742024-03-06texthttps://creativecommons.org/licenses/by/4.0/Li, J.Long, S.IUCrDatamed@iucr.org2024-03-06https://creativecommons.org/licenses/by/4.0/932414-3146x240197March 2024organic compounds2414-3146cis,cis,cis-Dichloridobis(N4,N4-dimethylpyridin-4-amine-κN1)bis(dimethyl sulfoxide-κS)ruthenium(II)
http://scripts.iucr.org/cgi-bin/paper?bh4082
The structure of the title compound, [RuCl2(C7H10N2)2(C2H6OS)2], has monoclinic (P21/n) symmetry. The Ru—N distances of the coordination compound are influenced by the trans chloride or dimethylsulfoxide-κS ligands. The molecular structure exhibits disorder for two of the terminal methyl groups of a dimethyl sulfoxide ligand.In the structure of the title compound, the Ru—N distances of the DMAP ligands are influenced by the trans chloride or dimethylsulfoxide-κS ligands.International Union of CrystallographyenCRYSTAL STRUCTURE; COORDINATION COMPOUND; RUTHENIUM(II); DMAP; DMSOcis,cis,cis-Dichloridobis(N4,N4-dimethylpyridin-4-amine-κN1)bis(dimethyl sulfoxide-κS)ruthenium(II)urn:issn:2414-3146text/htmlThe structure of the title compound, [RuCl2(C7H10N2)2(C2H6OS)2], has monoclinic (P21/n) symmetry. The Ru—N distances of the coordination compound are influenced by the trans chloride or dimethylsulfoxide-κS ligands. The molecular structure exhibits disorder for two of the terminal methyl groups of a dimethyl sulfoxide ligand.doi:10.1107/S24143146240019132024-03-06texthttps://creativecommons.org/licenses/by/4.0/Park, E.H.Ortiz, S.M.Liang, T.K.Smucker, B.W.x240191March 202432414-31462414-3146metal-organic compoundsIUCrData9med@iucr.org2024-03-06https://creativecommons.org/licenses/by/4.0/Bis[S-octyl 3-(2-methylpropylidene)dithiocarbazato-κ2N3,S]nickel(II)
http://scripts.iucr.org/cgi-bin/paper?wm4208
The central NiII atom in the title complex, [Ni(C13H25N2S2)2], is located on an inversion center and adopts a roughly square-planar coordination environment defined by two chelating N,S donor sets of two symmetry-related ligands in a trans configuration. The Ni—N and Ni—S bond lenghts are 1.9193 (14) and 2.1788 (5) Å, respectively, with a chelating N—Ni—S bond angle of 86.05 (4)°. These data are compared with those measured for similar dithiocarbazato ligands that bear n-octyl or n-hexyl alkyl chains. Slight differences are observed with respect to the phenylethylidene derivative where the ligands are bound cis relative to one another.The bis-chelated mononuclear nickel(II) complex shows inversion symmetry, with the dithiocarbazato ligand in the usual trans configuration and the central metal cation in a square-planar coordination environment.International Union of CrystallographyenCRYSTAL STRUCTURE; DITHIOCARBAZATO LIGAND; NIII COMPLEX; TRANS CONFIGURATION COMPLEX; OCTYL ALKYL CHAINBis[S-octyl 3-(2-methylpropylidene)dithiocarbazato-κ2N3,S]nickel(II)urn:issn:2414-3146text/htmlThe central NiII atom in the title complex, [Ni(C13H25N2S2)2], is located on an inversion center and adopts a roughly square-planar coordination environment defined by two chelating N,S donor sets of two symmetry-related ligands in a trans configuration. The Ni—N and Ni—S bond lenghts are 1.9193 (14) and 2.1788 (5) Å, respectively, with a chelating N—Ni—S bond angle of 86.05 (4)°. These data are compared with those measured for similar dithiocarbazato ligands that bear n-octyl or n-hexyl alkyl chains. Slight differences are observed with respect to the phenylethylidene derivative where the ligands are bound cis relative to one another.doi:10.1107/S241431462400186X2024-03-06texthttps://creativecommons.org/licenses/by/4.0/Khan, S.S.Howlader, M.B.H.Sheikh, M.C.Miyatake, R.Zangrando, E.metal-organic compounds2414-314632414-3146x240186March 20242024-03-06med@iucr.orghttps://creativecommons.org/licenses/by/4.0/9IUCrDataerythro-{1-Bromo-1-[(1-phenylethyl)sulfonyl]ethyl}benzene
http://scripts.iucr.org/cgi-bin/paper?wm4209
The title compound, C16H17BrO2S, crystallizes as the erythro (RR/SS) isomer of a pair of sulfones that were diastereomeric due to chirality of the α-carbon atoms on the sulfone sulfur atom. The structural analysis was pivotal in showing that the 1,3 elimination reactions of these compounds, which lead to substituted stilbenes, occur with inversion at each asymmetric carbon atom. In the crystal, C—H⋯Br and C—H⋯O hydrogen bonds link the molecules into a tri-periodic intermolecular network.Structural analysis of the title diasteromeric sulfone determines this to be the erythro (RR/SS) isomer, and was pivotal in showing that the 1,3-elimination reactions of these compounds, which lead to substituted stilbenes, occur with inversion at each asymmetric carbon atom.International Union of CrystallographyenCRYSTAL STRUCTURE; SULFONE; DIASTEROMER; 1,3-ELIMINATION; C-H...O AND C-H...BR HYDROGEN BONDINGerythro-{1-Bromo-1-[(1-phenylethyl)sulfonyl]ethyl}benzeneurn:issn:2414-3146text/htmlThe title compound, C16H17BrO2S, crystallizes as the erythro (RR/SS) isomer of a pair of sulfones that were diastereomeric due to chirality of the α-carbon atoms on the sulfone sulfur atom. The structural analysis was pivotal in showing that the 1,3 elimination reactions of these compounds, which lead to substituted stilbenes, occur with inversion at each asymmetric carbon atom. In the crystal, C—H⋯Br and C—H⋯O hydrogen bonds link the molecules into a tri-periodic intermolecular network.doi:10.1107/S24143146240018952024-03-06texthttps://creativecommons.org/licenses/by/4.0/Corfield, P.W.R.organic compounds2414-31462414-31463March 2024x240189https://creativecommons.org/licenses/by/4.0/2024-03-06med@iucr.org9IUCrDataCrystal structure of defect scheelite-type Nd2/3[WO4]
http://scripts.iucr.org/cgi-bin/paper?wm4207
Neodymium(III) ortho-oxidotungstate(VI) was synthesized as a side-product in an unsuccessful synthesis attempt at fluoride derivatives of neodymium tungstate in fused silica ampoules, using neodymium(III) oxide, neodymium(III) fluoride and tungsten trioxide. Violet, platelet-shaped single crystals of the title compound emerged of the bulk, which crystallize in the defect scheelite type with a trigonal dodecahedral coordination of oxide anions around the Nd3+ cations and the hexavalent tungsten cations situated in the centers of oxide tetrahedra.The crystal structure of defect-scheelite type Nd2/3[WO4] consists of [WO4]2− tetrahedra and trigonal [NdO8]13– dodecahedra.International Union of CrystallographyenCRYSTAL STRUCTURE; OXIDOTUNGSTATE(VI); NEODYMIUM; SCHEELITECrystal structure of defect scheelite-type Nd2/3[WO4]urn:issn:2414-3146text/htmlNeodymium(III) ortho-oxidotungstate(VI) was synthesized as a side-product in an unsuccessful synthesis attempt at fluoride derivatives of neodymium tungstate in fused silica ampoules, using neodymium(III) oxide, neodymium(III) fluoride and tungsten trioxide. Violet, platelet-shaped single crystals of the title compound emerged of the bulk, which crystallize in the defect scheelite type with a trigonal dodecahedral coordination of oxide anions around the Nd3+ cations and the hexavalent tungsten cations situated in the centers of oxide tetrahedra.doi:10.1107/S24143146240017552024-03-06texthttps://creativecommons.org/licenses/by/4.0/Knies, B.Hartenbach, I.2414-3146inorganic compoundsMarch 2024x2401752414-314639https://creativecommons.org/licenses/by/4.0/2024-03-06med@iucr.orgIUCrDataProp-2-ynyl 3-methoxy-4-(prop-2-ynyloxy)benzoate
http://scripts.iucr.org/cgi-bin/paper?hb4463
The title compound, C14H12O4, comprises of two crystallographically independent molecules in the asymmetric unit, linked via C—H⋯O interactions to form dimeric entities. The allylic groups are twisted out of the phenyl planes with dihedral angles varying between 7.92 (13) and 25.42 (8)°. In the crystal, the packing follows a zigzag pattern along the c-axis direction. The absolute configuration of the sample could not be determined reliably.The title compound, C14H12O4, was prepared via alkylation of 4-hydroxy-3-methoxybenzoic acid with propargyl bromide in the presence of K2CO3.International Union of CrystallographyenCRYSTAL STRUCTURE; DIMER; HYDROGEN BONDINGProp-2-ynyl 3-methoxy-4-(prop-2-ynyloxy)benzoateurn:issn:2414-3146text/htmlThe title compound, C14H12O4, comprises of two crystallographically independent molecules in the asymmetric unit, linked via C—H⋯O interactions to form dimeric entities. The allylic groups are twisted out of the phenyl planes with dihedral angles varying between 7.92 (13) and 25.42 (8)°. In the crystal, the packing follows a zigzag pattern along the c-axis direction. The absolute configuration of the sample could not be determined reliably.doi:10.1107/S24143146240016392024-02-27texthttps://creativecommons.org/licenses/by/4.0/Moodley, C.Muller, A.Belay, Y.H.9https://creativecommons.org/licenses/by/4.0/2024-02-27med@iucr.orgIUCrData2414-3146organic compoundsFebruary 2024x2401632414-314621-Ethyl-3,3-dimethylspiro[indoline-2,8′-phenaleno[1,9-fg]chromene]
http://scripts.iucr.org/cgi-bin/paper?hb4461
The title pyrene-fused spiropyran derivative, C30H25NO, crystallizes with two molecules in the asymmetric unit with dihedral angles between their fused-ring sub units of 76.20 (8) and 89.38 (9)°. In the crystal, weak C—H⋯π interactions link the molecules into a three-dimensional network.Both molecules in the asymmetric unit of the title compound are twisted. In the crystal, weak C—H⋯π interactions link the molecules into a three-dimensional network.International Union of CrystallographyenCRYSTAL STRUCTURE; SPIROPYRAN; PYRENE; PACKING1-Ethyl-3,3-dimethylspiro[indoline-2,8′-phenaleno[1,9-fg]chromene]urn:issn:2414-3146text/htmlThe title pyrene-fused spiropyran derivative, C30H25NO, crystallizes with two molecules in the asymmetric unit with dihedral angles between their fused-ring sub units of 76.20 (8) and 89.38 (9)°. In the crystal, weak C—H⋯π interactions link the molecules into a three-dimensional network.doi:10.1107/S24143146240013782024-02-13texthttps://creativecommons.org/licenses/by/4.0/Zhu., X.Jiang, Z.Liu, Z.IUCrData2024-02-13med@iucr.orghttps://creativecommons.org/licenses/by/4.0/922414-3146x240137February 2024organic compounds2414-3146Bis[μ-bis(pyridin-2-yl)methanone oxime-κ3N:,N′,N′′]bis[diacetato-κ2O,O′;κO-zinc(II)]
http://scripts.iucr.org/cgi-bin/paper?zl4065
The structure of the title complex, [Zn2(C2H3O2)4(C11H9N3O)2], is triclinic containing half of the molecule in the asymmetric unit. Each zinc atom is coordinated to a pyridyl and oxime nitrogen from one di-2-pyridyl ketone oxime (dpko) ligand and a third nitrogen from the other dpko pyridyl ring. Additionally, each zinc is coordinated to two acetato anions, one of which is bidentate and the other monodentate. The uncoordinated oxygen of the monodentate acetato group is involved in a hydrogen bond with the oxime hydrogen. The packing in the crystal is assisted by weak C—H⋯O interactions between acetato groups and neighboring pyridyl rings.The structure of the title compound is triclinic containing half of the molecule in the asymmetric unit. Each zinc atom is coordinated to a pyridyl and oxime nitrogen from one ligand and a third nitrogen from the other dpko pyridyl ring and two acetato anions.International Union of CrystallographyenCRYSTAL STRUCTURE; DPKO; ZINCBis[μ-bis(pyridin-2-yl)methanone oxime-κ3N:,N′,N′′]bis[diacetato-κ2O,O′;κO-zinc(II)]urn:issn:2414-3146text/htmlThe structure of the title complex, [Zn2(C2H3O2)4(C11H9N3O)2], is triclinic containing half of the molecule in the asymmetric unit. Each zinc atom is coordinated to a pyridyl and oxime nitrogen from one di-2-pyridyl ketone oxime (dpko) ligand and a third nitrogen from the other dpko pyridyl ring. Additionally, each zinc is coordinated to two acetato anions, one of which is bidentate and the other monodentate. The uncoordinated oxygen of the monodentate acetato group is involved in a hydrogen bond with the oxime hydrogen. The packing in the crystal is assisted by weak C—H⋯O interactions between acetato groups and neighboring pyridyl rings.doi:10.1107/S24143146240012262024-02-16texthttps://creativecommons.org/licenses/by/4.0/Crundwell, G.Crundwell, N.E.Westcott, B.L.2414-3146metal-organic compoundsx240122February 202422414-314692024-02-16med@iucr.orghttps://creativecommons.org/licenses/by/4.0/IUCrDataAquabis(2,2′-bipyridine-κ2N,N′)(isonicotinamide-κN)ruthenium(II) bis(trifluoromethanesulfonate)
http://scripts.iucr.org/cgi-bin/paper?bt4147
In the title complex, [Ru(C10H8N2)2(C6H6N2O)(H2O)](CF3SO3)2, the central RuII atom is sixfold coordinated by two bidentate 2,2′-bipyridine, an isonicotinamide ligand, and a water molecule in a distorted octahedral environment with trifluoromethanesulfonate ions completing the outer coordination sphere of the complex. Hydrogen bonding involving the water molecule and weak π–π stacking interactions between the pyridyl rings in adjacent molecules contribute to the alignment of the complexes in columns parallel to the c axis.In the crystal structure of the title compound, the ruthenium(II) metal center is surrounded by two bidentate 2,2′-bipyridine, an isonicotinamide ligand, and a water in a distorted octahedral geometry. Hydrogen bonding is present between counter-ion and ligand.International Union of CrystallographyenCRYSTAL STRUCTURE; RUTHENIUM(II); OCTAHEDRAL GEOMETRY; 2,2'-BIPYRIDINE; BIDENTATE LIGAND; ISONICOTINAMIDE; HYDROGEN BONDING; [PI]-[PI] STACKINGAquabis(2,2′-bipyridine-κ2N,N′)(isonicotinamide-κN)ruthenium(II) bis(trifluoromethanesulfonate)urn:issn:2414-3146text/htmlIn the title complex, [Ru(C10H8N2)2(C6H6N2O)(H2O)](CF3SO3)2, the central RuII atom is sixfold coordinated by two bidentate 2,2′-bipyridine, an isonicotinamide ligand, and a water molecule in a distorted octahedral environment with trifluoromethanesulfonate ions completing the outer coordination sphere of the complex. Hydrogen bonding involving the water molecule and weak π–π stacking interactions between the pyridyl rings in adjacent molecules contribute to the alignment of the complexes in columns parallel to the c axis.doi:10.1107/S24143146240011472024-02-08texthttps://creativecommons.org/licenses/by/4.0/Faubert, L.Arman, H.D.Adrian, R.A.IUCrDatahttps://creativecommons.org/licenses/by/4.0/2024-02-08med@iucr.org92414-31462February 2024x240114metal-organic compounds2414-3146(2,2′-Bipyridine-κ2N,N′)(4,4′-dimethoxy-2,2′-bipyridine-κ2N,N′)palladium(II) bis(trifluoromethanesulfonate)
http://scripts.iucr.org/cgi-bin/paper?wm4206
In the title complex salt, [Pd(C10H8N2)(C12H12N2O2)](CF3SO3)2, the palladium(II) atom is fourfold coordinated by two chelating ligands, 2,2′-bipyridine and 4,4′-dimethoxy-2,2′-bipyridine, in a distorted square-planar environment. In the crystal, weak π–π stacking interactions between the 2,2′-bipyridine rings [centroid-to-centroid distances = 3.8984 (19) Å] and between the 4,4′-dimethoxy-2,2′-bipyridine rings [centroid-to-centroid distances = 3.747 (18) Å] contribute to the alignment of the complex cations in columns parallel to the b-axis direction.In the cation of the title complex, the central palladium(II) atom is surrounded by two bidentate ligands, 2,2′-bipyridine and 4,4′-dimethoxy-2,2′-bipyridine, in a distorted square-planar environment.International Union of CrystallographyenCRYSTAL STRUCTURE; PALLADIUM(II) COMPLEX; SQUARE-PLANAR COORDINATION ENVIRONMENT; 2,2'-BIPYRIDINE; 4,4'-DIMETHOXY-2,2'-BIPYRIDINE; TRIFLUOROMETHANESULFONATE SALT; [TAU]4 DESCRIPTOR(2,2′-Bipyridine-κ2N,N′)(4,4′-dimethoxy-2,2′-bipyridine-κ2N,N′)palladium(II) bis(trifluoromethanesulfonate)urn:issn:2414-3146text/htmlIn the title complex salt, [Pd(C10H8N2)(C12H12N2O2)](CF3SO3)2, the palladium(II) atom is fourfold coordinated by two chelating ligands, 2,2′-bipyridine and 4,4′-dimethoxy-2,2′-bipyridine, in a distorted square-planar environment. In the crystal, weak π–π stacking interactions between the 2,2′-bipyridine rings [centroid-to-centroid distances = 3.8984 (19) Å] and between the 4,4′-dimethoxy-2,2′-bipyridine rings [centroid-to-centroid distances = 3.747 (18) Å] contribute to the alignment of the complex cations in columns parallel to the b-axis direction.doi:10.1107/S24143146240010932024-02-08texthttps://creativecommons.org/licenses/by/4.0/Vargas, B.B.Arman, H.D.Adrian, R.A.IUCrDatahttps://creativecommons.org/licenses/by/4.0/2024-02-08med@iucr.org92414-31462February 2024x240109metal-organic compounds2414-3146Bis[2,6-bis(benzimidazol-2-yl)pyridine-κ3N,N′,N′′]nickel(II) bis(trifluoromethanesulfonate) diethyl ether monosolvate
http://scripts.iucr.org/cgi-bin/paper?vm4063
In the title complex, [Ni(C19H13N5)2](CF3SO3)2·(CH3CH2)2O, the central NiII atom is sixfold coordinated by three nitrogen atoms of each 2,6-bis(2-benzimidazolyl)pyridine ligand in a distorted octahedral geometry with two trifluoromethanesulfonate ions and a molecule of diethyl ether completing the outer coordination sphere of the complex. Hydrogen bonding contributes to the organization of the asymmetric units in columns along the a axis generating a porous supramolecular structure. The structure was refined as a two-component twin with a refined BASF value of 0.4104 (13).In the crystal structure of the title compound, the nickel(II) metal center is surrounded by two tridentate 2,6-bis(2-benzimidazolyl)pyridine ligands in a distorted octahedral geometry. Hydrogen bonding is present between counter-ion and ligand.International Union of CrystallographyenCRYSTAL STRUCTURE; NICKEL(II); TRIFLUOROMETHANESULFONATE SALT; 2,6-BIS(2-BENZIMIDAZOLYL)PYRIDINE; OCTAHEDRAL GEOMETRY; HYDROGEN BOND; DIETHYL ETHER SOLVATEBis[2,6-bis(benzimidazol-2-yl)pyridine-κ3N,N′,N′′]nickel(II) bis(trifluoromethanesulfonate) diethyl ether monosolvateurn:issn:2414-3146text/htmlIn the title complex, [Ni(C19H13N5)2](CF3SO3)2·(CH3CH2)2O, the central NiII atom is sixfold coordinated by three nitrogen atoms of each 2,6-bis(2-benzimidazolyl)pyridine ligand in a distorted octahedral geometry with two trifluoromethanesulfonate ions and a molecule of diethyl ether completing the outer coordination sphere of the complex. Hydrogen bonding contributes to the organization of the asymmetric units in columns along the a axis generating a porous supramolecular structure. The structure was refined as a two-component twin with a refined BASF value of 0.4104 (13).doi:10.1107/S24143146240008892024-01-31texthttps://creativecommons.org/licenses/by/4.0/Ruiz, S.E.Arman, H.D.Adrian, R.A.IUCrDatahttps://creativecommons.org/licenses/by/4.0/med@iucr.org2024-01-3192414-31461January 2024x240088metal-organic compounds2414-3146(4-Butyl-1-ethyl-1,2,4-triazol-5-ylidene)[(1,2,5,6-η)-cycloocta-1,5-diene](triphenylphosphane)rhodium(I) tetrafluoridoborate
http://scripts.iucr.org/cgi-bin/paper?hb4460
In the title triazole-based N-heterocyclic carbene rhodium(I) cationic complex with a tetrafluoridoborate counter-anion, [Rh(C8H12)(C8H15N3)(C18H15P)]BF4, which crystallizes with two cations and two anions in the asymmetric unit, the Rh center has a distorted square-planar coordination geometry with expected bond distances. Several nonclassical C—H⋯F hydrogen-bonding interactions help to consolidate the packing. Two of the F atoms of one of the anions are disordered over adjacent sites in a 0.814 (4):0.186 (4) ratio.In the title triazole-based N-heterocyclic carbene rhodium(I) cationic complex with a tetrafluoridoborate counter-anion, the Rh center has a distorted square-planar coordination geometry with expected bond distances.International Union of CrystallographyenCRYSTAL STRUCTURE; RHODIUM; N-HETEROCYCLIC CARBENES; CATIONIC COMPLEXES(4-Butyl-1-ethyl-1,2,4-triazol-5-ylidene)[(1,2,5,6-η)-cycloocta-1,5-diene](triphenylphosphane)rhodium(I) tetrafluoridoborateurn:issn:2414-3146text/htmlIn the title triazole-based N-heterocyclic carbene rhodium(I) cationic complex with a tetrafluoridoborate counter-anion, [Rh(C8H12)(C8H15N3)(C18H15P)]BF4, which crystallizes with two cations and two anions in the asymmetric unit, the Rh center has a distorted square-planar coordination geometry with expected bond distances. Several nonclassical C—H⋯F hydrogen-bonding interactions help to consolidate the packing. Two of the F atoms of one of the anions are disordered over adjacent sites in a 0.814 (4):0.186 (4) ratio.doi:10.1107/S24143146240006092024-01-26texthttps://creativecommons.org/licenses/by/4.0/Lerch, T.G.Gau, M.Albert, D.R.Rajaseelan, E.https://creativecommons.org/licenses/by/4.0/med@iucr.org2024-01-269IUCrDatametal-organic compounds2414-31462414-31461January 2024x240060Bis(2-hydroxy-2,3-dihydro-1H-inden-1-aminium) tetrachloridopalladate(II) hemihydrate
http://scripts.iucr.org/cgi-bin/paper?tk4099
A new square-planar palladium complex salt hydrate, (C9H12NO)2[PdCl4]·0.5H2O, has been characterized. The asymmetric unit of the complex salt comprises two [PdCl4]2− dianions, four 2-hydroxy-2,3-dihydro-1H-inden-1-aminium cations, each derived from (1R,2S)-(+)-1-aminoindan-2-ol, and one water molecule of crystallization. In the crystal, a two-dimensional layer parallel to (001) features a number of O—H⋯O, N—H⋯O, O—H⋯Cl and N—H⋯Cl hydrogen bonds.In the title salt hydrate, (C9H12NO)2[PdCl4]·0.5H2O, the PdII atom is coordinated by four chloride anions and the charge balance is provided by two ammonium cations formed from (1R,2S)-(+)-1-aminoindan-2-ol.International Union of CrystallographyenCRYSTAL STRUCTURE; HYDROGEN BONDING; PALLADIUM TETRACHLORIDE; AMINOINDANOLBis(2-hydroxy-2,3-dihydro-1H-inden-1-aminium) tetrachloridopalladate(II) hemihydrateurn:issn:2414-3146text/htmlA new square-planar palladium complex salt hydrate, (C9H12NO)2[PdCl4]·0.5H2O, has been characterized. The asymmetric unit of the complex salt comprises two [PdCl4]2− dianions, four 2-hydroxy-2,3-dihydro-1H-inden-1-aminium cations, each derived from (1R,2S)-(+)-1-aminoindan-2-ol, and one water molecule of crystallization. In the crystal, a two-dimensional layer parallel to (001) features a number of O—H⋯O, N—H⋯O, O—H⋯Cl and N—H⋯Cl hydrogen bonds.doi:10.1107/S24143146240005922024-01-26texthttps://creativecommons.org/licenses/by/4.0/Singh, O.Mok, J.Park, H.-R.Lee, J.January 2024x2400592414-314612414-3146metal-organic compoundsIUCrData9https://creativecommons.org/licenses/by/4.0/2024-01-26med@iucr.orgCrystal structure of Ti4Ni2C
http://scripts.iucr.org/cgi-bin/paper?wm4205
Single crystals of the intermetallic phase with composition Ti4Ni2C were serendipitously obtained by high-pressure sintering of a mixture with initial chemical composition Ti2Ni. The Ti4Ni2C phase crystallizes in the Fd\overline{3}m space group and can be considered as a partially filled Ti2Ni structure with the C atom occupying an octahedral void. Ti4Ni2C is isotypic with Ti4Ni2O, Nb4Ni2C and Ta4Ni2C, all of which were studied previously by means of powder diffraction.Ti4Ni2C crystallizes isotypically with Ti4Ni2O, Nb4Ni2C and Ta4Ni2C and can be considered as a partially filled Ti2Ni structure with the C atom occupying an octahedral void.International Union of CrystallographyenCRYSTAL STRUCTURE; HIGH-PRESSURE SINTERING; INTERMETALLIC; TI4NI2C PHASECrystal structure of Ti4Ni2Curn:issn:2414-3146text/htmlSingle crystals of the intermetallic phase with composition Ti4Ni2C were serendipitously obtained by high-pressure sintering of a mixture with initial chemical composition Ti2Ni. The Ti4Ni2C phase crystallizes in the Fd\overline{3}m space group and can be considered as a partially filled Ti2Ni structure with the C atom occupying an octahedral void. Ti4Ni2C is isotypic with Ti4Ni2O, Nb4Ni2C and Ta4Ni2C, all of which were studied previously by means of powder diffraction.doi:10.1107/S24143146240004392024-01-19texthttps://creativecommons.org/licenses/by/4.0/Liu, H.Liang, X.Liu, Y.Fan, C.Wen, B.Zhang, L.2414-3146inorganic compoundsJanuary 2024x2400432414-314619https://creativecommons.org/licenses/by/4.0/med@iucr.org2024-01-19IUCrDataSynthesis and structure of trans-bis(4-amino-3-nitrobenzoato-κO)bis(4-amino-3-nitrobenzoic acid-κO)diaquamanganese(II) dihydrate
http://scripts.iucr.org/cgi-bin/paper?bv4050
The manganese title complex, [Mn(C7H5N2O4)2(C7H6N2O4)2(H2O)2]·2H2O, is one of the first 4-amino 3-nitrobenzoic acid (4 A3NBA) monoligand metal complexes to be synthesized. It crystallizes in the centrosymmetric monoclinic space group P21/n with the complex molecules located on inversion centers. Four 4 A3NBA ligand molecules are monodentately coordinated by the Mn2+ ion through the carboxylic oxygen atoms while the other two positions of the inner coordination sphere are occupied by water molecules, giving rise to a distorted octahedron, and two water molecules are in the outer coordination sphere. There are two intramolecular hydrogen bonds in the complex molecule. The first is of the common N—H⋯O=N type, while the second is a rarely occurring very strong hydrogen bond in which a common proton is shared by two uncoordinated oxygen atoms of neighboring carboxylate groups. In the crystal, an intricate system of intermolecular hydrogen bonds links the complex molecules into a three-dimensional-network.The reaction of 4-amino 3-nitrobenzoic acid and manganese dichloride tetrahydrate in an ethanol–water mixture yielded the title complex[Mn(C7H5N2O4)2(C7H6N2O4)2(H2O)2]·2H2O. In the crystal, molecules are linked by N—H⋯O, O—H⋯O and C—H⋯O hydrogen bonds.International Union of Crystallographyen4-AMINO 3-NITROBENZOIC ACID; MNII; CRYSTAL STRUCTURE; HYDROGEN BONDSynthesis and structure of trans-bis(4-amino-3-nitrobenzoato-κO)bis(4-amino-3-nitrobenzoic acid-κO)diaquamanganese(II) dihydrateurn:issn:2414-3146text/htmlThe manganese title complex, [Mn(C7H5N2O4)2(C7H6N2O4)2(H2O)2]·2H2O, is one of the first 4-amino 3-nitrobenzoic acid (4 A3NBA) monoligand metal complexes to be synthesized. It crystallizes in the centrosymmetric monoclinic space group P21/n with the complex molecules located on inversion centers. Four 4 A3NBA ligand molecules are monodentately coordinated by the Mn2+ ion through the carboxylic oxygen atoms while the other two positions of the inner coordination sphere are occupied by water molecules, giving rise to a distorted octahedron, and two water molecules are in the outer coordination sphere. There are two intramolecular hydrogen bonds in the complex molecule. The first is of the common N—H⋯O=N type, while the second is a rarely occurring very strong hydrogen bond in which a common proton is shared by two uncoordinated oxygen atoms of neighboring carboxylate groups. In the crystal, an intricate system of intermolecular hydrogen bonds links the complex molecules into a three-dimensional-network.doi:10.1107/S24143146240004032024-01-19texthttps://creativecommons.org/licenses/by/4.0/Narmanova, F.S.Turaev, K.K.Ibragimov, A.B.Ashurov, J.M.9https://creativecommons.org/licenses/by/4.0/med@iucr.org2024-01-19IUCrData2414-3146metal-organic compoundsJanuary 2024x2400402414-314612-Aminobenzoxazole–oxalic acid (2/1)
http://scripts.iucr.org/cgi-bin/paper?bv4051
In the title compound, 2C7H7N2O+·C2O42−, proton transfer from oxalic acid to the N atom of the heterocycle has occurred to form a 2:1 molecular salt. In the extended structure, N—H⋯O hydrogen bonds link the components into [100] chains, which feature R22(8) and R44(14) loops.In the title compound, proton transfer from oxalic acid to the N atom of the heterocycle has occurred to form a 2:1 molecular salt. In the extended structure, N—H⋯O hydrogen bonds link the components into [100] chains, which feature R22(8) and R44(14) loops.International Union of CrystallographyenCRYSTAL STRUCTURE; 2-AMINOBENZOXAZOLE; MOLECULAR STRUCTURE; CO-CRYSTAL; HYDROGEN BONDS2-Aminobenzoxazole–oxalic acid (2/1)urn:issn:2414-3146text/htmlIn the title compound, 2C7H7N2O+·C2O42−, proton transfer from oxalic acid to the N atom of the heterocycle has occurred to form a 2:1 molecular salt. In the extended structure, N—H⋯O hydrogen bonds link the components into [100] chains, which feature R22(8) and R44(14) loops.doi:10.1107/S24143146240003362024-01-26texthttps://creativecommons.org/licenses/by/4.0/Razzoqova, S.Torambetov, B.Todjiev, J.Kadirova, S.Ibragimov, A.Ruzmetov, A.Ashurov, J.organic compounds2414-314612414-3146x240033January 20242024-01-26med@iucr.orghttps://creativecommons.org/licenses/by/4.0/9IUCrDataDichlorido(4,7-dimethoxy-1,10-phenanthroline-κ2N,N′)zinc(II)
http://scripts.iucr.org/cgi-bin/paper?wm4203
In the title complex, [ZnCl2(C14H12N2O2)], the ZnII atom is located on a twofold rotation axis and is fourfold coordinated by two chlorido ligands and a bidentate 4,7-methoxy-1,10-phenanthroline ligand in a distorted tetrahedral environment. Weak π–π stacking interactions between adjacent 4,7-dimethoxy-1,10-phenanthroline rings [centroid-to-centroid distances = 3.5969 (11) and 3.7738 (11) Å] contribute to the alignment of the complexes in layers parallel to (\overline{2}01).In the crystal structure of the title compound, the central zinc(II) metal atom is surrounded by two N atoms of a bidentate 4,7-methoxy-1,10-phenanthroline ligand and two chlorido ligands in a distorted tetrahedral coordination environment.International Union of CrystallographyenCRYSTAL STRUCTURE; ZINC; 4,7-DIMETHOXY-1,10-PHENANTHROLINE; COORDINATING CHLORIDE IONS; DISTORTED TETRAHEDRAL COORDINATION ENVIRONMENT; METAL COMPLEX; [TAU]4 DESCRIPTORDichlorido(4,7-dimethoxy-1,10-phenanthroline-κ2N,N′)zinc(II)urn:issn:2414-3146text/htmlIn the title complex, [ZnCl2(C14H12N2O2)], the ZnII atom is located on a twofold rotation axis and is fourfold coordinated by two chlorido ligands and a bidentate 4,7-methoxy-1,10-phenanthroline ligand in a distorted tetrahedral environment. Weak π–π stacking interactions between adjacent 4,7-dimethoxy-1,10-phenanthroline rings [centroid-to-centroid distances = 3.5969 (11) and 3.7738 (11) Å] contribute to the alignment of the complexes in layers parallel to (\overline{2}01).doi:10.1107/S24143146240003732024-01-12texthttps://creativecommons.org/licenses/by/4.0/Rose, N.P.Arman, H.D.Adrian, R.A.IUCrData9med@iucr.org2024-01-12https://creativecommons.org/licenses/by/4.0/x240037January 202412414-31462414-3146metal-organic compoundstrans-Dichloridobis[(S)-(−)-1-(4-methylphenyl)ethylamine-κN]palladium(II)
http://scripts.iucr.org/cgi-bin/paper?wm4204
The title complex, [PdCl2(C9H13N)2], comprises a single molecule in the asymmetric unit. The PdII atom is tetracoordinated by two N atoms from two trans-aligned organic ligands and two Cl ligands, forming a square-planar metal coordination environment. The distances from the ortho-H atoms on the phenyl ring to the central PdII atom fall within the range 4.70–5.30 Å, precluding any significant intramolecular Pd⋯H interactions.The molecular PdII title complex exhibits a square-planar coordination about the central metal atom, provided by two trans-arranged chlorido ligands and two nitrogen atoms from the two neutral organic ligands.International Union of CrystallographyenCRYSTAL STRUCTURE; AMINE; PALLADIUM(II) COMPLEX; MONODENTATE LIGANDtrans-Dichloridobis[(S)-(−)-1-(4-methylphenyl)ethylamine-κN]palladium(II)urn:issn:2414-3146text/htmlThe title complex, [PdCl2(C9H13N)2], comprises a single molecule in the asymmetric unit. The PdII atom is tetracoordinated by two N atoms from two trans-aligned organic ligands and two Cl ligands, forming a square-planar metal coordination environment. The distances from the ortho-H atoms on the phenyl ring to the central PdII atom fall within the range 4.70–5.30 Å, precluding any significant intramolecular Pd⋯H interactions.doi:10.1107/S24143146240003612024-01-12texthttps://creativecommons.org/licenses/by/4.0/Hernández Téllez, G.Moreno Morales, G.E.Sharma, P.Gonzalez, R.Anzaldo, B.https://creativecommons.org/licenses/by/4.0/2024-01-12med@iucr.org9IUCrDatametal-organic compounds2414-31462414-31461January 2024x240036N-Methyl-2-{3-methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}hydrazinecarbothioamide
http://scripts.iucr.org/cgi-bin/paper?bt4146
The equimolar and hydrochloric acid-catalysed reaction between cis-jasmone and 4-methylthiosemicarbazide in ethanolic solution yields the title compound, C13H21N3S (common name: cis-jasmone 4-methylthiosemicarbazone). Two molecules with all atoms in general positions are present in the asymmetric unit. In one of them, the carbon chain is disordered [site occupancy ratio = 0.821 (3):0.179 (3)]. The thiosemicarbazone entities [N—N—C(=S)—N] are approximately planar, with the maximum deviation from the mean plane through the selected atoms being −0.0115 (16) Å (r.m.s.d. = 0.0078 Å) for the non-disordered molecule and 0.0052 (14) Å (r.m.s.d. = 0.0031 Å) for the disordered one. The molecules are not planar, since the jasmone groups have a chain with sp3-hybridized carbon atoms and, in addition, the thiosemicarbazone fragments are attached to the respective carbon five-membered rings and the dihedral angles between them for each molecule amount to 8.9 (1) and 6.3 (1)°. In the crystal, the molecules are connected through pairs of N—H⋯S and C—H⋯S interactions into crystallographically independent centrosymmetric dimers, in which rings of graph-set motifs R22(8) and R21(7) are observed. A Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are from H⋯H (70.6%), H⋯S/S⋯H (16.7%), H⋯C/C⋯H (7.5%) and H⋯N/N⋯H (4.9%) interactions [considering the two crystallographically independent molecules and only the disordered atoms with the highest s.o.f. for the evaluation].The synthesis, crystal structure and Hirshfeld analysis of cis-jasmone 4-methylthiosemicarbazone is reported. Two crystallographically independent molecules are observed in the asymmetric unit, one of them being disordered over the carbon chain. In the crystal, the molecules are linked by N—H⋯S and C—H⋯S interactions into independent centrosymmetric dimers.International Union of CrystallographyenTHIOSEMICARBAZONE; CIS-JASMONE; METHYLTHIOSEMICARBAZONE DERIVATIVE; CENTROSYMMETRIC DIMERS; CRYSTAL STRUCTURE; HIRSHFELD ANALYSISN-Methyl-2-{3-methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}hydrazinecarbothioamideurn:issn:2414-3146text/htmlThe equimolar and hydrochloric acid-catalysed reaction between cis-jasmone and 4-methylthiosemicarbazide in ethanolic solution yields the title compound, C13H21N3S (common name: cis-jasmone 4-methylthiosemicarbazone). Two molecules with all atoms in general positions are present in the asymmetric unit. In one of them, the carbon chain is disordered [site occupancy ratio = 0.821 (3):0.179 (3)]. The thiosemicarbazone entities [N—N—C(=S)—N] are approximately planar, with the maximum deviation from the mean plane through the selected atoms being −0.0115 (16) Å (r.m.s.d. = 0.0078 Å) for the non-disordered molecule and 0.0052 (14) Å (r.m.s.d. = 0.0031 Å) for the disordered one. The molecules are not planar, since the jasmone groups have a chain with sp3-hybridized carbon atoms and, in addition, the thiosemicarbazone fragments are attached to the respective carbon five-membered rings and the dihedral angles between them for each molecule amount to 8.9 (1) and 6.3 (1)°. In the crystal, the molecules are connected through pairs of N—H⋯S and C—H⋯S interactions into crystallographically independent centrosymmetric dimers, in which rings of graph-set motifs R22(8) and R21(7) are observed. A Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are from H⋯H (70.6%), H⋯S/S⋯H (16.7%), H⋯C/C⋯H (7.5%) and H⋯N/N⋯H (4.9%) interactions [considering the two crystallographically independent molecules and only the disordered atoms with the highest s.o.f. for the evaluation].doi:10.1107/S24143146240001302024-01-09texthttps://creativecommons.org/licenses/by/4.0/Oliveira, A.B. deBresolin, L.Beck, J.Daniels, J.2414-3146organic compoundsx240013January 202412414-31469med@iucr.org2024-01-09https://creativecommons.org/licenses/by/4.0/IUCrData2-{3-Methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}-N-phenylhydrazinecarbothioamide. Corrigendum
http://scripts.iucr.org/cgi-bin/paper?me6263
In the paper by Oliveira et al. [IUCrData (2023), 8, x230971], there was an error in the name of the first author.Corrigendum to IUCrData (2023), 8, x230971.International Union of Crystallographyen2-{3-Methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}-N-phenylhydrazinecarbothioamide. Corrigendumurn:issn:2414-3146text/htmlIn the paper by Oliveira et al. [IUCrData (2023), 8, x230971], there was an error in the name of the first author.doi:10.1107/S24143146240000992024-01-31texthttps://creativecommons.org/licenses/by/4.0/Oliveira, A.B. deBresolin, L.Beck, J.Daniels, J.2414-3146addenda and erratax240009January 202412414-314692024-01-31med@iucr.orghttps://creativecommons.org/licenses/by/4.0/IUCrDatarac-Hydroxyisovaleric acid
http://scripts.iucr.org/cgi-bin/paper?bt4145
The title compound (systematic name: rac-2-hydroxy-3-methylbutanoic acid), C5H10O3, is the constitutional isomer of α-hydroxybutanoic acid. In the crystal, hydrogen bonds involving the alcoholic hydroxyl group give rise to centrosymmetric dimers that are extended to sheets perpendicular to the crystallographic c axis.The title compound is the constitutional isomer of α-hydroxybutanoic acid. In the crystal, hydrogen bonds involving the alcoholic hydroxyl group give rise to centrosymmetric dimers that are extended to sheets perpendicular to the crystallographic c axis.International Union of CrystallographyenCRYSTAL STRUCTURE; HYDROGEN BONDING; HYDROXYCARBOXYLIC ACIDSrac-Hydroxyisovaleric acidurn:issn:2414-3146text/htmlThe title compound (systematic name: rac-2-hydroxy-3-methylbutanoic acid), C5H10O3, is the constitutional isomer of α-hydroxybutanoic acid. In the crystal, hydrogen bonds involving the alcoholic hydroxyl group give rise to centrosymmetric dimers that are extended to sheets perpendicular to the crystallographic c axis.doi:10.1107/S24143146230109332024-01-05texthttps://creativecommons.org/licenses/by/4.0/Dasi, L.Hosten, E.C.Betz, R.IUCrDatahttps://creativecommons.org/licenses/by/4.0/2024-01-05med@iucr.org92414-31461January 2024x231093organic compounds2414-3146meso-α,α-5,15-Bis(o-nicotinamidophenyl)-10,20-diphenylporphyrin n-hexane monosolvate
http://scripts.iucr.org/cgi-bin/paper?bh4080
The structure of the title solvated porphyrin, C56H38N8O2·C6H14, is reported. Two porphyrin molecules, one ordered and one disordered n-hexane solvate molecules are present in its asymmetric unit. The porphyrin macrocycle shows a characteristic saddle-shaped distortion, and the maximum deviation from the mean plane for non-hydrogen atoms is 0.48 Å. N—H⋯N, N—H⋯O, and C—H⋯O hydrogen bonds, as well as π–π interactions, are observed in the crystal structure.In the title porphyrin solvate, the macrocycle shows a characteristic saddle-shaped distortion.International Union of CrystallographyenCRYSTAL STRUCTURE; PORPHYRINS; SOLVATE; HYDROGEN BONDS; DISORDERmeso-α,α-5,15-Bis(o-nicotinamidophenyl)-10,20-diphenylporphyrin n-hexane monosolvateurn:issn:2414-3146text/htmlThe structure of the title solvated porphyrin, C56H38N8O2·C6H14, is reported. Two porphyrin molecules, one ordered and one disordered n-hexane solvate molecules are present in its asymmetric unit. The porphyrin macrocycle shows a characteristic saddle-shaped distortion, and the maximum deviation from the mean plane for non-hydrogen atoms is 0.48 Å. N—H⋯N, N—H⋯O, and C—H⋯O hydrogen bonds, as well as π–π interactions, are observed in the crystal structure.doi:10.1107/S24143146230108542023-12-22texthttps://creativecommons.org/licenses/by/4.0/Sun, X.Li, J.2414-314612December 2023x231085organic compounds2414-3146IUCrDatahttps://creativecommons.org/licenses/by/4.0/2023-12-22med@iucr.org8Bis[1,3-bis(2,4,6-trimethylphenyl)imidazolium] bis(μ-cis-1,2-diphenylethene-1,2-dithiolato-κ2S,S′:κS)bis[(cis-1,2-diphenylethene-1,2-dithiolato-κ2S,S′)iron(III)] dimethylformamide disolvate
http://scripts.iucr.org/cgi-bin/paper?im4022
The molecular structure of the solvated title salt, (C21H25N2)2[Fe2(C14H10S2)4]·2C3H7NO reveals that the anion is situated on a crystallographic inversion center in the triclinic space group P\overline{1}. The title compound crystallizes utilizing a network of weak π-stacking interactions of phenyl rings pertaining to the dithiolene unit. Moreover, the acidic imidazolium H atoms [N—C(H)—N] display non-classical hydrogen-bonding interactions of the C—H⋯O type to the oxygen atoms of the N,N-dimethyl formamide solvent, and hydrogen atoms on the backbone of imidazolium rings display weak C—H⋯S interactions with the dithiolene sulfur atoms.The solid-state structural analysis of a reduced iron bis(dithiolene) dimer reveals that the molecule crystallizes with the center of the Fe2S2 ring system on a crystallographic center of inversion. The structure shows non-classical hydrogen-bonding interactions between imidazolium H atoms and the oxygen atoms of N,N-dimethyl formamide that co-crystallized together with the title compound.International Union of CrystallographyenCRYSTAL STRUCTURE; IMIDAZOLIUM SALT; IRON BIS(DITHIOLENE) COMPLEXES; REDUCED IRON BIS(DITHIOLENE) COMPLEXESBis[1,3-bis(2,4,6-trimethylphenyl)imidazolium] bis(μ-cis-1,2-diphenylethene-1,2-dithiolato-κ2S,S′:κS)bis[(cis-1,2-diphenylethene-1,2-dithiolato-κ2S,S′)iron(III)] dimethylformamide disolvateurn:issn:2414-3146text/htmlThe molecular structure of the solvated title salt, (C21H25N2)2[Fe2(C14H10S2)4]·2C3H7NO reveals that the anion is situated on a crystallographic inversion center in the triclinic space group P\overline{1}. The title compound crystallizes utilizing a network of weak π-stacking interactions of phenyl rings pertaining to the dithiolene unit. Moreover, the acidic imidazolium H atoms [N—C(H)—N] display non-classical hydrogen-bonding interactions of the C—H⋯O type to the oxygen atoms of the N,N-dimethyl formamide solvent, and hydrogen atoms on the backbone of imidazolium rings display weak C—H⋯S interactions with the dithiolene sulfur atoms.doi:10.1107/S24143146230108302023-12-24texthttps://creativecommons.org/licenses/by/4.0/Selvakumar, J.Arumugam, K.med@iucr.org2023-12-24https://creativecommons.org/licenses/by/4.0/9IUCrDatametal-organic compounds2414-314612414-3146x231083January 20245,6-Dimethylbenzo[d][1,3]oxatellurole
http://scripts.iucr.org/cgi-bin/paper?hb4459
The structure of the title compound, C9H10OTe, at 100 K has orthorhombic (P21212) symmetry with two independent molecules in the asymmetric unit (Z′ = 2). The molecules are folded along their Te⋯O axes, with their Te–C–O planes angled at an average of 25.1° with respect to the remaining non-H atoms, which are almost coplanar (average deviation from planarity = 0.04 Å). A Hirshfeld plot shows weak intermolecular interactions between the two Te atoms located in each asymmetric molecule, with a Te⋯Te distance of 3.7191 (4) Å. The structure is strongly pseudosymmetric to the space group Pccn with Z′ = 1. The crystal chosen for data collection was found to be was an inversion twin.The title compound represents the first reported example of a [1,3]oxatellurole, prepared in three steps from 3,4-dimethylphenol. Both independent molecules are folded along their Te⋯O axes, with an average angle φ = 25.1° between the Te–C–O planes and the remaining non-hydrogen atoms. A Hirshfeld plot indicates a weak intermolecular interaction between the two tellurium atoms in the asymmetric unit.International Union of CrystallographyenTELLURIUM; HETEROCYCLIC; ORGANOTELLURIUM; OXATELLUROLE; CRYSTAL STRUCTURE5,6-Dimethylbenzo[d][1,3]oxatelluroleurn:issn:2414-3146text/htmlThe structure of the title compound, C9H10OTe, at 100 K has orthorhombic (P21212) symmetry with two independent molecules in the asymmetric unit (Z′ = 2). The molecules are folded along their Te⋯O axes, with their Te–C–O planes angled at an average of 25.1° with respect to the remaining non-H atoms, which are almost coplanar (average deviation from planarity = 0.04 Å). A Hirshfeld plot shows weak intermolecular interactions between the two Te atoms located in each asymmetric molecule, with a Te⋯Te distance of 3.7191 (4) Å. The structure is strongly pseudosymmetric to the space group Pccn with Z′ = 1. The crystal chosen for data collection was found to be was an inversion twin.doi:10.1107/S24143146230107632024-01-05texthttps://creativecommons.org/licenses/by/4.0/Ponzo, S.Turner, A.Fronczek, F.R.Junk, T.https://creativecommons.org/licenses/by/4.0/med@iucr.org2024-01-059IUCrDataorganic compounds2414-31462414-31461January 2024x231076Crystal structure of AlFe0.95
http://scripts.iucr.org/cgi-bin/paper?bh4081
Three B2-type intermetallic AlFe1 – δ phases (0.18 < δ < 0.05) in the Al–Fe binary system were synthesized by smelting and high temperature sintering methods. The exact crystal structure for δ = 0.05 was refined by single-crystal X-ray diffraction. The amount of vacancy defects at the Fe atom sites was obtained by refining the corresponding site occupancy factor, converging to the chemical formula AlFe0.95, with a structure identical to that of ideal AlFe models inferred from powder X-ray or neutron diffraction patterns.Three Fe-deficient B2-type AlFe1 – δ phases have been synthesized, and the exact crystal structure obtained from single-crystal X-ray diffraction measurements is reported for δ = 0.05.International Union of CrystallographyenCRYSTAL STRUCTURE; B2 PHASE; AL-FE SYSTEM; VACANCYCrystal structure of AlFe0.95urn:issn:2414-3146text/htmlThree B2-type intermetallic AlFe1 – δ phases (0.18 < δ < 0.05) in the Al–Fe binary system were synthesized by smelting and high temperature sintering methods. The exact crystal structure for δ = 0.05 was refined by single-crystal X-ray diffraction. The amount of vacancy defects at the Fe atom sites was obtained by refining the corresponding site occupancy factor, converging to the chemical formula AlFe0.95, with a structure identical to that of ideal AlFe models inferred from powder X-ray or neutron diffraction patterns.doi:10.1107/S24143146230106592023-12-14texthttps://creativecommons.org/licenses/by/4.0/Liu, Y.Liu, H.Fan, C.Bin, W.Zhang, L.inorganic compounds2414-3146122414-3146x231065December 20232023-12-14med@iucr.orghttps://creativecommons.org/licenses/by/4.0/8IUCrDataTetraaqua(ethane-1,2-diamine-κ2N,N′)nickel(II) naphthalene-1,5-disulfonate dihydrate
http://scripts.iucr.org/cgi-bin/paper?wm4202
The reaction of ethane-1,2-diamine (en, C2H8N2), the sodium salt of naphthalene-1,5-disulfonic acid (H2NDS, C10H8O6S2), and nickel sulfate in an aqueous solution resulted in the formation of the title salt, [Ni(C2H8N2)(H2O)4](C10H6O6S2)·2H2O or [Ni(en)(H2O)4](NDS)·2H2O. In the asymmetric unit, one half of an [Ni(en)(H2O)4]2+ cation and one half of an NDS2− anion, and one water molecule of crystallization are present. The Ni2+ cation in the complex is positioned on a twofold rotation axis and exhibits a slight tetragonal distortion of the cis-NiO4N2 octahedron, with an Ni—N bond length of 2.0782 (16) Å, and Ni—O bond lengths of 2.1170 (13) Å and 2.0648 (14) Å. The anion is completed by inversion symmetry. In the extended structure, the cations, anions, and non-coordinating water molecules are connected by intermolecular N—H⋯O and O—H⋯O hydrogen bonding, as well as C—H⋯π interactions, forming a three-dimensional network.In the title salt, [Ni(en)(H2O)4]2+·NDS2−·2H2O, the Ni2+ cation is positioned on a twofold rotation axis and exhibits a coordination number of six. The components are connected through an extensive network of O—H⋯O and N—H⋯O hydrogen bonds, and C—H⋯π interactions.International Union of CrystallographyenETHANE-1,2-DIAMINE; NAPHTHALENE-1,5-DISULFONATE; CRYSTAL STRUCTURE; HYDROGEN BONDING; C-H...[PI] INTERACTIONTetraaqua(ethane-1,2-diamine-κ2N,N′)nickel(II) naphthalene-1,5-disulfonate dihydrateurn:issn:2414-3146text/htmlThe reaction of ethane-1,2-diamine (en, C2H8N2), the sodium salt of naphthalene-1,5-disulfonic acid (H2NDS, C10H8O6S2), and nickel sulfate in an aqueous solution resulted in the formation of the title salt, [Ni(C2H8N2)(H2O)4](C10H6O6S2)·2H2O or [Ni(en)(H2O)4](NDS)·2H2O. In the asymmetric unit, one half of an [Ni(en)(H2O)4]2+ cation and one half of an NDS2− anion, and one water molecule of crystallization are present. The Ni2+ cation in the complex is positioned on a twofold rotation axis and exhibits a slight tetragonal distortion of the cis-NiO4N2 octahedron, with an Ni—N bond length of 2.0782 (16) Å, and Ni—O bond lengths of 2.1170 (13) Å and 2.0648 (14) Å. The anion is completed by inversion symmetry. In the extended structure, the cations, anions, and non-coordinating water molecules are connected by intermolecular N—H⋯O and O—H⋯O hydrogen bonding, as well as C—H⋯π interactions, forming a three-dimensional network.doi:10.1107/S24143146230103252023-12-14texthttps://creativecommons.org/licenses/by/4.0/Suyunov, J.R.Turaev, K.K.Alimnazarov, B.K.Ibragimov, A.B.Mengnorov, I.J.Rasulov, A.A.Ashurov, J.M.8https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-12-14IUCrData2414-3146metal-organic compoundsDecember 2023x2310322414-3146122-{1-[(6R,S)-3,5,5,6,8,8-Hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl]ethylidene}-N-methylhydrazinecarbothioamide
http://scripts.iucr.org/cgi-bin/paper?bt4144
The reaction between a racemic mixture of (R,S)-fixolide and 4-methylthiosemicarbazide in ethanol with a 1:1 stoichiometric ratio and catalysed with HCl, yielded the title compound, C20H31N3S [common name: (R,S)-fixolide 4-methylthiosemicarbazone]. There is one crystallographically independent molecule in the asymmetric unit, which is disordered over the aliphatic ring [site-occupancy ratio = 0.667 (13):0.333 (13)]. The disorder includes the chiral C atom, the neighbouring methylene group and the methyl H atoms of the methyl group bonded to the chiral C atom. The maximum deviations from the mean plane through the disordered aliphatic ring amount to 0.328 (6) and −0.334 (6) Å [r.m.s.d. = 0.2061 Å], and −0.3677 (12) and 0.3380 (12) Å [r.m.s.d. = 0.2198 Å] for the two different sites. Both fragments show a half-chair conformation. Additionally, the N—N—C(=S)—N entity is approximately planar, with the maximum deviation from the mean plane through the selected atoms being 0.0135 (18) Å [r.m.s.d. = 0.0100 Å]. The molecule is not planar due to the dihedral angle between the thiosemicarbazone entity and the aromatic ring, which amounts to 51.8 (1)°, and due to the sp3-hybridized carbon atoms of the fixolide fragment. In the crystal, the molecules are connected by H⋯S interactions with graph-set motif C(4), forming a mono-periodic hydrogen-bonded ribbon along [100]. The Hirshfeld surface analysis suggests that the major contributions for the crystal cohesion are [(R,S)-isomers considered separately] H⋯H (75.7%), H⋯S/S⋯H (11.6%), H⋯C/C⋯H (8.3% and H⋯N/N⋯H (4.4% for both of them).The synthesis, crystal structure and Hirshfeld analysis of (R,S)-fixolide 4-methylthiosemicarbazone is reported. The compound is disordered over the fixolide fragment and in the crystal, the molecules are linked by H⋯S interactions with graph-set motif C(4), forming mono-periodic hydrogen-bonded ribbons along [100].International Union of CrystallographyenTHIOSEMICARBAZONE; FIXOLIDE THIOSEMICARBAZONE; CHIRAL THIOSEMICARBAZONE; HYDROGEN-BONDED RIBBON; FIXOLIDE DERIVATIVE; CRYSTAL STRUCTURE2-{1-[(6R,S)-3,5,5,6,8,8-Hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl]ethylidene}-N-methylhydrazinecarbothioamideurn:issn:2414-3146text/htmlThe reaction between a racemic mixture of (R,S)-fixolide and 4-methylthiosemicarbazide in ethanol with a 1:1 stoichiometric ratio and catalysed with HCl, yielded the title compound, C20H31N3S [common name: (R,S)-fixolide 4-methylthiosemicarbazone]. There is one crystallographically independent molecule in the asymmetric unit, which is disordered over the aliphatic ring [site-occupancy ratio = 0.667 (13):0.333 (13)]. The disorder includes the chiral C atom, the neighbouring methylene group and the methyl H atoms of the methyl group bonded to the chiral C atom. The maximum deviations from the mean plane through the disordered aliphatic ring amount to 0.328 (6) and −0.334 (6) Å [r.m.s.d. = 0.2061 Å], and −0.3677 (12) and 0.3380 (12) Å [r.m.s.d. = 0.2198 Å] for the two different sites. Both fragments show a half-chair conformation. Additionally, the N—N—C(=S)—N entity is approximately planar, with the maximum deviation from the mean plane through the selected atoms being 0.0135 (18) Å [r.m.s.d. = 0.0100 Å]. The molecule is not planar due to the dihedral angle between the thiosemicarbazone entity and the aromatic ring, which amounts to 51.8 (1)°, and due to the sp3-hybridized carbon atoms of the fixolide fragment. In the crystal, the molecules are connected by H⋯S interactions with graph-set motif C(4), forming a mono-periodic hydrogen-bonded ribbon along [100]. The Hirshfeld surface analysis suggests that the major contributions for the crystal cohesion are [(R,S)-isomers considered separately] H⋯H (75.7%), H⋯S/S⋯H (11.6%), H⋯C/C⋯H (8.3% and H⋯N/N⋯H (4.4% for both of them).doi:10.1107/S24143146230102092023-11-30texthttps://creativecommons.org/licenses/by/4.0/Melo, A.P.L. deFlores, A.F.C.Bresolin, L.Tirloni, B.Oliveira, A.B. de2414-3146organic compoundsNovember 2023x2310202414-3146118https://creativecommons.org/licenses/by/4.0/2023-11-30med@iucr.orgIUCrDataA second crystalline modification of 2-{3-methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}hydrazinecarbothioamide
http://scripts.iucr.org/cgi-bin/paper?bt4143
A second crystalline modification of the title compound, C12H19N3S [common name: cis-jasmone thiosemicarbazone] was crystallized from tetrahydrofurane at room temperature. There is one crystallographic independent molecule in the asymmetric unit, showing disorder in the cis-jasmone chain [site-occupancy ratio = 0.590 (14):0.410 (14)]. The thiosemicarbazone entity is approximately planar, with the maximum deviation from the mean plane through the N/N/C/S/N atoms being 0.0463 (14) Å [r.m.s.d. = 0.0324 Å], while for the five-membered ring of the jasmone fragment, the maximum deviation from the mean plane through the carbon atoms amounts to 0.0465 (15) Å [r.m.s.d. = 0.0338 Å]. The molecule is not planar due to the dihedral angle between these two fragments, which is 8.93 (1)°, and due to the sp3-hybridized carbon atoms in the jasmone fragment chain. In the crystal, the molecules are connected by N—H⋯S and C—H⋯S interactions, with graph-set motifs R22(8) and R21(7), building mono-periodic hydrogen-bonded ribbons along [010]. A Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are H⋯H (67.8%), H⋯S/S⋯H (15.0%), H⋯C/C⋯H (8.5%) and H⋯N/N⋯H (5.6%) [only non-disordered atoms and those with the highest s.o.f. were considered]. This work reports the second crystalline modification of the cis-jasmone thiosemicarbazone structure, the first one being published recently [Orsoni et al. (2020). Int. J. Mol. Sci. 21, 8681–8697] with the crystals obtained in ethanol at 273 K.The crystal structure and Hirshfeld analysis of a second crystalline modification of the cis-jasmone thiosemicarbazone is reported. The molecular structure matches the asymmetric unit and the molecules are linked into mono-periodic hydrogen-bonded ribbons along [010].International Union of CrystallographyenJASMONE THIOSEMICARBAZONE; THIOSEMICARBAZONE; CIS-JASMONE DERIVATIVE; CRYSTALLINE MODIFICATION; CRYSTAL STRUCTURE; HIRSHFELD ANALYSISA second crystalline modification of 2-{3-methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}hydrazinecarbothioamideurn:issn:2414-3146text/htmlA second crystalline modification of the title compound, C12H19N3S [common name: cis-jasmone thiosemicarbazone] was crystallized from tetrahydrofurane at room temperature. There is one crystallographic independent molecule in the asymmetric unit, showing disorder in the cis-jasmone chain [site-occupancy ratio = 0.590 (14):0.410 (14)]. The thiosemicarbazone entity is approximately planar, with the maximum deviation from the mean plane through the N/N/C/S/N atoms being 0.0463 (14) Å [r.m.s.d. = 0.0324 Å], while for the five-membered ring of the jasmone fragment, the maximum deviation from the mean plane through the carbon atoms amounts to 0.0465 (15) Å [r.m.s.d. = 0.0338 Å]. The molecule is not planar due to the dihedral angle between these two fragments, which is 8.93 (1)°, and due to the sp3-hybridized carbon atoms in the jasmone fragment chain. In the crystal, the molecules are connected by N—H⋯S and C—H⋯S interactions, with graph-set motifs R22(8) and R21(7), building mono-periodic hydrogen-bonded ribbons along [010]. A Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are H⋯H (67.8%), H⋯S/S⋯H (15.0%), H⋯C/C⋯H (8.5%) and H⋯N/N⋯H (5.6%) [only non-disordered atoms and those with the highest s.o.f. were considered]. This work reports the second crystalline modification of the cis-jasmone thiosemicarbazone structure, the first one being published recently [Orsoni et al. (2020). Int. J. Mol. Sci. 21, 8681–8697] with the crystals obtained in ethanol at 273 K.doi:10.1107/S24143146230101802023-11-30texthttps://creativecommons.org/licenses/by/4.0/Oliveira, A.B. deBresolin, L.Gervini, V.C.Beck, J.Daniels, J.8med@iucr.org2023-11-30https://creativecommons.org/licenses/by/4.0/IUCrData2414-3146organic compoundsx231018November 2023112414-3146(E)-3-(1,3-Diphenyl-1H-pyrazol-4-yl)-1-(thiazol-2-yl)prop-2-en-1-one
http://scripts.iucr.org/cgi-bin/paper?hb4458
In the title molecule, C21H15N3OS, the C5=C6 double bond in the central enone group adopts a trans configuration. The dihedral angle between planes of the thiazole and pyrazole rings is 6.6 (2)°. In the crystal, pairs of C—H⋯O hydrogen bonds generate inversion dimers and another pair of C—H⋯N hydrogen bonds link the dimers into chains propagating along a-axis direction.The crystal structure of a heterocycles containing chalcone is reported.International Union of CrystallographyenCRYSTAL STRUCTURE; CHALCONE; HETEROCYCLES; C-H...O HYDROGEN BONDS(E)-3-(1,3-Diphenyl-1H-pyrazol-4-yl)-1-(thiazol-2-yl)prop-2-en-1-oneurn:issn:2414-3146text/htmlIn the title molecule, C21H15N3OS, the C5=C6 double bond in the central enone group adopts a trans configuration. The dihedral angle between planes of the thiazole and pyrazole rings is 6.6 (2)°. In the crystal, pairs of C—H⋯O hydrogen bonds generate inversion dimers and another pair of C—H⋯N hydrogen bonds link the dimers into chains propagating along a-axis direction.doi:10.1107/S24143146230099752023-11-21texthttps://creativecommons.org/licenses/by/4.0/Koh, D.https://creativecommons.org/licenses/by/4.0/2023-11-21med@iucr.org8IUCrDataorganic compounds2414-31462414-314611November 2023x230997Methyl 1-(4-fluorobenzyl)-1H-indazole-3-carboxylate
http://scripts.iucr.org/cgi-bin/paper?zl4059
The title compound, C16H13FN2O2, was synthesized by nucleophilic substitution of the indazole N—H hydrogen atom of methyl 1H-indazole-3-carboxylate with 1-(bromomethyl)-4-fluorobenzene. In the crystal, some hydrogen-bond-like interactions are observed.The title compound was synthesized by nucleophilic substitution of the indazole N—H hydrogen atom of methyl 1H-indazole-3-carboxylate with 1-(bromomethyl)-4-fluorobenzene. In the crystal, some hydrogen-bond-like interactions are observed.International Union of CrystallographyenCRYSTAL STRUCTURE; SYNTHETIC CANNABINOID; INTERMEDIATE COMPOUNDMethyl 1-(4-fluorobenzyl)-1H-indazole-3-carboxylateurn:issn:2414-3146text/htmlThe title compound, C16H13FN2O2, was synthesized by nucleophilic substitution of the indazole N—H hydrogen atom of methyl 1H-indazole-3-carboxylate with 1-(bromomethyl)-4-fluorobenzene. In the crystal, some hydrogen-bond-like interactions are observed.doi:10.1107/S24143146230099512023-11-23texthttps://creativecommons.org/licenses/by/4.0/Doi, T.Sakai, T.IUCrDatahttps://creativecommons.org/licenses/by/4.0/med@iucr.org2023-11-2382414-314611November 2023x230995organic compounds2414-3146trans-Bis[bis(diphenylphosphanyl)methane-κ2P,P′]dichloridoruthenium(II): a triclinic polymorph
http://scripts.iucr.org/cgi-bin/paper?wm4201
The title compound, [RuCl2(C25H22P2)2] or [RuCl2(dppm)2] (dppm = bis(diphenylphosphanyl)methane, C25H22P2) crystallizes as two half-molecules (completed by inversion symmetry) in space group P\overline{1} (Z = 2), with the RuII atoms occupying inversion centers at 0,0,0 and 1/2, 1/2, 1/2, respectively. The bidentate phosphane ligands occupy equatorial positions while the chlorido ligands complete the distorted octahedral coordination spheres at axial positions. The bite angles of the phosphane chelates are similar for the two molecules [(P—Ru—P)avg. = 71.1°], while there are significant differences in the twisting of the methylene backbone, with a distance of the methylene C atom from the RuP4 plane of 0.659 (2) and 0.299 (3) Å, respectively, and also for the phenyl substituents for both molecules due to variations in weak C—H⋯Cl interactions.The title compound crystallizes with two different inversion-symmetric molecules having a distorted octahedral {P4Cl2} coordination environment, and an average P—Ru—P bite angle of 71.1°.International Union of CrystallographyenCRYSTAL STRUCTURE; RUTHENIUM; DIMORPHISM; BIDENTATE LIGANDtrans-Bis[bis(diphenylphosphanyl)methane-κ2P,P′]dichloridoruthenium(II): a triclinic polymorphurn:issn:2414-3146text/htmlThe title compound, [RuCl2(C25H22P2)2] or [RuCl2(dppm)2] (dppm = bis(diphenylphosphanyl)methane, C25H22P2) crystallizes as two half-molecules (completed by inversion symmetry) in space group P\overline{1} (Z = 2), with the RuII atoms occupying inversion centers at 0,0,0 and 1/2, 1/2, 1/2, respectively. The bidentate phosphane ligands occupy equatorial positions while the chlorido ligands complete the distorted octahedral coordination spheres at axial positions. The bite angles of the phosphane chelates are similar for the two molecules [(P—Ru—P)avg. = 71.1°], while there are significant differences in the twisting of the methylene backbone, with a distance of the methylene C atom from the RuP4 plane of 0.659 (2) and 0.299 (3) Å, respectively, and also for the phenyl substituents for both molecules due to variations in weak C—H⋯Cl interactions.doi:10.1107/S24143146230098472023-11-14texthttps://creativecommons.org/licenses/by/4.0/Kelani, M.T.Muller, A.Lammertsma, K.IUCrData2023-11-14med@iucr.orghttps://creativecommons.org/licenses/by/4.0/8112414-3146x230984November 2023metal-organic compounds2414-3146[1,1′-Bicyclohexane]-1,1′-diol
http://scripts.iucr.org/cgi-bin/paper?bt4141
The title compound, C12H22O2, is a symmetric diol derived from the pinacol coupling of cyclohexanone. The asymmetric unit contains three complete molecules. The cyclohexane moieties adopt chair conformations. Cooperative hydrogen bonding connects the individual molecules to infinite chains propagating along the crystallographic a-axis direction.The title compound is a symmetric diol derived from the pinacol coupling of cyclohexanone. The asymmetric unit contains three complete molecules·Cooperative hydrogen bonding connects the individual molecules to infinite chains propagating along the crystallographic a-axis direction.International Union of CrystallographyenCRYSTAL STRUCTURE[1,1′-Bicyclohexane]-1,1′-diolurn:issn:2414-3146text/htmlThe title compound, C12H22O2, is a symmetric diol derived from the pinacol coupling of cyclohexanone. The asymmetric unit contains three complete molecules. The cyclohexane moieties adopt chair conformations. Cooperative hydrogen bonding connects the individual molecules to infinite chains propagating along the crystallographic a-axis direction.doi:10.1107/S24143146230096902023-11-14texthttps://creativecommons.org/licenses/by/4.0/Mtendeni, Z.Hosten, E.C.Betz, R.organic compounds2414-31462414-314611November 2023x230969https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-11-148IUCrDataN-phenyl-{3-methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}hydrazinecarbothioamide
http://scripts.iucr.org/cgi-bin/paper?bt4142
The hydrochloric acid-catalyzed equimolar reaction between cis-jasmone and 4-phenylthiosemicarbazide yielded the title compound, C18H23N3S (common name: cis-jasmone 4-phenylthiosemicarbazone). Concerning the hydrogen bonding, an N—H⋯N intramolecular interaction is observed, forming a ring with graph-set motif S(5). In the crystal, the molecules are connected into centrosymmetric dimers by pairs of N—H⋯S and C—H⋯S interactions, forming rings of graph-set motifs R22(8) and R21(7), with the sulfur atoms acting as double acceptors. The thiosemicarbazone entity is approximately planar, with the maximum deviation from the mean plane through the N/N/C/S/N atoms being 0.0376 (9) Å (the r.m.s.d. amounts to 0.0234 Å). The molecule is substantially twisted as indicated by the dihedral angle between the thiosemicarbazone fragment and the phenyl ring, which amounts to 56.1 (5)°, and because of the jasmone fragment, which bears a chain with sp3-hybridized carbon atoms in the structure. The Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are: H⋯H (65.3%), H⋯C/C⋯H (16.2%), H⋯S/S⋯H (10.9%) and H⋯N/N⋯H (5.5%).The synthesis, crystal structure and Hirshfeld analysis of the cis-jasmone 4-phenylthiosemicarbazone is reported. The molecules are linked into centrosymmetric dimers via pairs of N—H⋯S and C—H⋯S interactions, with graph-set motifs R_{2}^{2}(8) and R_{2}^{1}(7). In addition, one N—H⋯N intramolecular interaction is observed, with graph-set motif S(5). The crystal structure resembles a zigzag motif when viewed along [010].International Union of CrystallographyenCIS-JASMONE; 4-PHENYLTHIOSEMICARBAZONE; THIOSEMICARBAZONE; JASMONE; CRYSTAL STRUCTURE; HIRSHFELD ANALYSIS.N-phenyl-{3-methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}hydrazinecarbothioamideurn:issn:2414-3146text/htmlThe hydrochloric acid-catalyzed equimolar reaction between cis-jasmone and 4-phenylthiosemicarbazide yielded the title compound, C18H23N3S (common name: cis-jasmone 4-phenylthiosemicarbazone). Concerning the hydrogen bonding, an N—H⋯N intramolecular interaction is observed, forming a ring with graph-set motif S(5). In the crystal, the molecules are connected into centrosymmetric dimers by pairs of N—H⋯S and C—H⋯S interactions, forming rings of graph-set motifs R22(8) and R21(7), with the sulfur atoms acting as double acceptors. The thiosemicarbazone entity is approximately planar, with the maximum deviation from the mean plane through the N/N/C/S/N atoms being 0.0376 (9) Å (the r.m.s.d. amounts to 0.0234 Å). The molecule is substantially twisted as indicated by the dihedral angle between the thiosemicarbazone fragment and the phenyl ring, which amounts to 56.1 (5)°, and because of the jasmone fragment, which bears a chain with sp3-hybridized carbon atoms in the structure. The Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are: H⋯H (65.3%), H⋯C/C⋯H (16.2%), H⋯S/S⋯H (10.9%) and H⋯N/N⋯H (5.5%).doi:10.1107/S24143146230097192023-11-14texthttps://creativecommons.org/licenses/by/4.0/Oliveira, A.B.Bresolin, L.Beck, J.Daniels, J.https://creativecommons.org/licenses/by/4.0/2023-11-14med@iucr.org8IUCrDataorganic compounds2414-31462414-314611November 2023x2309716,7-Diphenyl-5-thia-7-azaspiro[2.6]nonan-8-one 5,5-dioxide
http://scripts.iucr.org/cgi-bin/paper?hb4455
The racemic mixture of the title compound, C19H19NO3S, crystallizes in space group P\overline{1} with two homochiral molecules in each asymmetric unit. The seven-membered ring in both molecules is in a pucker-chair conformation. The extended structure exhibits C—H⋯O hydrogen bonds, of which two connect crystallographically independent molecules to generate a chain propagating along the b-axis direction. One C—H grouping of the cyclopropyl ring is in close contact with the phenyl ring of the neighboring independent molecule in C—H⋯π type interactions with carbon atom–ring-centroid distances of 3.544 (5) and 3.596 (4) Å. Other interactions are of the parallel–reciprocal type, with the chiral carbon atom of one molecule donating a proton to an oxygen atom of the sulfone group of a symmetry-related molecule and vice-versa. Symmetry-related molecular pairs also exhibit T-type interactions between aromatic rings with interplanar angles of 74.2 (2) and 69.2 (2)° and intercentroid distances of 4.965 (4) and 5.114 (4) Å.The seven-membered 1,3-thiazepan-4-one ring system, like its six- and five-membered-ring analogues, is known to be biologically active and is of potential medicinal use. The crystal structure reported is of the sulfone of a 1,3-thiazepan-4-one in which the seven-membered ring adopts a pucker-chair conformation.International Union of CrystallographyenCRYSTAL STRUCTURE; C-H...O; C-H...[PI]; AROMATIC T-TYPE STACKING INTERACTIONS; CHAIR PUCKER6,7-Diphenyl-5-thia-7-azaspiro[2.6]nonan-8-one 5,5-dioxideurn:issn:2414-3146text/htmlThe racemic mixture of the title compound, C19H19NO3S, crystallizes in space group P\overline{1} with two homochiral molecules in each asymmetric unit. The seven-membered ring in both molecules is in a pucker-chair conformation. The extended structure exhibits C—H⋯O hydrogen bonds, of which two connect crystallographically independent molecules to generate a chain propagating along the b-axis direction. One C—H grouping of the cyclopropyl ring is in close contact with the phenyl ring of the neighboring independent molecule in C—H⋯π type interactions with carbon atom–ring-centroid distances of 3.544 (5) and 3.596 (4) Å. Other interactions are of the parallel–reciprocal type, with the chiral carbon atom of one molecule donating a proton to an oxygen atom of the sulfone group of a symmetry-related molecule and vice-versa. Symmetry-related molecular pairs also exhibit T-type interactions between aromatic rings with interplanar angles of 74.2 (2) and 69.2 (2)° and intercentroid distances of 4.965 (4) and 5.114 (4) Å.doi:10.1107/S24143146230093792023-10-31texthttps://creativecommons.org/licenses/by/4.0/Yennawar, H.P.Russell, M.W.Silverberg, L.J.2414-3146organic compoundsOctober 2023x2309372414-3146108https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-10-31IUCrDataBis(diisobutylammonium) tetrachloridobis[3-(trifluoromethyl)phenyl]stannate
http://scripts.iucr.org/cgi-bin/paper?tk4096
The asymmetric unit in the title salt, (C8H20N)2[SnCl4(C7H4Cl2F3)2], features a di-isobutylammonium cation in a general position and a diorganotin tetrachloride dianion, i.e. tetrachloridobis(3-trifuoromethylphenyl)stannate(IV), located on a centre of inversion; the SnIV atom is octahedrally coordinated. In the crystal, charge-assisted N+—H⋯Cl hydrogen bonds along with C—H⋯F contacts occur within supramolecular layers that interdigitate along the a-axis direction.The title salt comprises di-isobutylammonium cations and centrosymmetric tetrachlorobis-(3-trifuoromethylphenyl)stannate(IV) anions, which are connected in the crystal by N—H⋯Cl and C—H⋯F interactions.International Union of CrystallographyenSTANNATE; AMMONIUM CATION; CRYSTAL STRUCTURE; HYDROGEN BONDING; SALTBis(diisobutylammonium) tetrachloridobis[3-(trifluoromethyl)phenyl]stannateurn:issn:2414-3146text/htmlThe asymmetric unit in the title salt, (C8H20N)2[SnCl4(C7H4Cl2F3)2], features a di-isobutylammonium cation in a general position and a diorganotin tetrachloride dianion, i.e. tetrachloridobis(3-trifuoromethylphenyl)stannate(IV), located on a centre of inversion; the SnIV atom is octahedrally coordinated. In the crystal, charge-assisted N+—H⋯Cl hydrogen bonds along with C—H⋯F contacts occur within supramolecular layers that interdigitate along the a-axis direction.doi:10.1107/S24143146230091362023-10-24texthttps://creativecommons.org/licenses/by/4.0/Song, X.Li, W.IUCrData2023-10-24med@iucr.orghttps://creativecommons.org/licenses/by/4.0/8102414-3146x230913October 2023metal-organic compounds2414-3146[(1,2,5,6-η)-Cycloocta-1,5-diene](1-ethyl-4-isopropyl-1,2,4-triazol-5-ylidene)(triphenylphosphane)iridium(I) tetrafluoridoborate dichloromethane sesquisolvate
http://scripts.iucr.org/cgi-bin/paper?hb4453
The synthesis and crystal structure of a new triazole-based N-heterocyclic carbene iridium(I) cationic complex with a tetrafluoridoborate counter-anion and solvating dichloromethane, [Ir(C8H12)(C7H13N3)(C18H15P)]BF4·1.5CH2Cl2, is reported. The IrI center of the cationic complex has a distorted square-planar conformation, formed by a bidentate cycloocta-1,5-diene (COD) ligand, an N-heterocyclic carbene, and a triphenylphosphane ligand. There are weak hydrogen-bonding interactions between C—H groupings of the iridium complex and F atoms of the [BF4]− counter-ions. The atoms of the COD ligand are disordered over two sets of sites in a 0.65:0.35 ratio and two of the F atoms of the anion are disordered over adjacent sites in a 0.6:0.4 ratio. One of the dichloromethane solvent molecules is disordered about an inversion center with 0.5 occupancy.The synthesis and crystal structure of a new triazole-based N-heterocyclic carbene iridium(I) cationic complex with a tetrafluoridoborate counter-anion and solvating dichloromethane is reported. The IrI center of the cationic complex has a distorted square-planar conformation, formed by a bidentate cycloocta-1,5-diene (COD) ligand, an N-heterocyclic carbene, and a tripheylphosphane ligand. There are weak hydrogen-bonding interactions between C—H groupings of the iridium complex and F atoms of the [BF4]− counter-ions.International Union of CrystallographyenCRYSTAL STRUCTURE; IRIDIUM; N-HETEROCYCLIC CARBENES[(1,2,5,6-η)-Cycloocta-1,5-diene](1-ethyl-4-isopropyl-1,2,4-triazol-5-ylidene)(triphenylphosphane)iridium(I) tetrafluoridoborate dichloromethane sesquisolvateurn:issn:2414-3146text/htmlThe synthesis and crystal structure of a new triazole-based N-heterocyclic carbene iridium(I) cationic complex with a tetrafluoridoborate counter-anion and solvating dichloromethane, [Ir(C8H12)(C7H13N3)(C18H15P)]BF4·1.5CH2Cl2, is reported. The IrI center of the cationic complex has a distorted square-planar conformation, formed by a bidentate cycloocta-1,5-diene (COD) ligand, an N-heterocyclic carbene, and a triphenylphosphane ligand. There are weak hydrogen-bonding interactions between C—H groupings of the iridium complex and F atoms of the [BF4]− counter-ions. The atoms of the COD ligand are disordered over two sets of sites in a 0.65:0.35 ratio and two of the F atoms of the anion are disordered over adjacent sites in a 0.6:0.4 ratio. One of the dichloromethane solvent molecules is disordered about an inversion center with 0.5 occupancy.doi:10.1107/S24143146230090332023-10-19texthttps://creativecommons.org/licenses/by/4.0/Maynard, A.Gau, M.Albert, D.R.Rajaseelan, E.8https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-10-19IUCrData2414-3146metal-organic compoundsOctober 2023x2309032414-3146102-[4-(2-Chlorobenzyl)-3-methyl-6-oxo-1,6-dihydropyridazin-1-yl]-N-(4-fluorophenyl)acetamide
http://scripts.iucr.org/cgi-bin/paper?hb4454
The conformation of the title molecule, C20H17ClFN3O2, is partly determined by an intramolecular C—H⋯O hydrogen bond, which leads to a dihedral angle of 14.7 (4)° between the fluorobenzene ring and the acetamide group. The 2-chlorobenzyl group is rotationally disordered over two orientations in a 0.656 (2): 0.344 (2) ratio. In the crystal, a layered structure is formed by N—H⋯O, C—H⋯O and C—H⋯F hydrogen bonds plus slipped π–π stacking interactions.An intramolecular C—H⋯O hydrogen bond helps to determine the conformation of the title molecule in which the 2-chlorobenzyl group is rotationally disordered.International Union of CrystallographyenCRYSTAL STRUCTURE; PYRIDAZINE; HYDROGEN BOND; [PI]-STACKING; ARYLACETAMIDE; CRYSTAL STRUCTURE2-[4-(2-Chlorobenzyl)-3-methyl-6-oxo-1,6-dihydropyridazin-1-yl]-N-(4-fluorophenyl)acetamideurn:issn:2414-3146text/htmlThe conformation of the title molecule, C20H17ClFN3O2, is partly determined by an intramolecular C—H⋯O hydrogen bond, which leads to a dihedral angle of 14.7 (4)° between the fluorobenzene ring and the acetamide group. The 2-chlorobenzyl group is rotationally disordered over two orientations in a 0.656 (2): 0.344 (2) ratio. In the crystal, a layered structure is formed by N—H⋯O, C—H⋯O and C—H⋯F hydrogen bonds plus slipped π–π stacking interactions.doi:10.1107/S241431462300901X2023-10-19texthttps://creativecommons.org/licenses/by/4.0/Assila, H.Ameziane El Hassani, I.El Moutaouakil Ala Allah, A.Alsubari, A.Mague, J.T.Ramli, Y.Ansar, M.H.organic compounds2414-3146102414-3146x230901October 20232023-10-19med@iucr.orghttps://creativecommons.org/licenses/by/4.0/8IUCrDataPoly[bis(O-ethylhydroxylaminium) [di-μ-chlorido-dichloridocadmate(II)]]
http://scripts.iucr.org/cgi-bin/paper?wm4199
The title compound, {(CH3CH2ONH3)2[CdCl4]}n, consists of bilayers of organic CH3CH2ONH3+ cations and infinite [CdCl4]n2n− inorganic layers. It can be described as an organic–inorganic hybrid layered perovskite. In the crystal structure, the CdII cation is situated at an inversion center and is coordinated by six chloride ions, forming a slightly distorted octahedral coordination polyhedron. By corner-sharing of the [CdCl6] octahedra, infinite [CdCl4]n2n− inorganic layers are formed, extending parallel to (100). The inorganic layers alternate with bilayers of CH3CH2ONH3+ cations, whereby the connection of the cationic and anionic layers is achieved through N—H⋯Cl hydrogen bonds and Coulombic interactions.In the crystal structure of the title organic–inorganic hybrid layered perovskite, organic bilayers alternate with [CdCl4]n2n− inorganic layers along [100].International Union of CrystallographyenCRYSTAL STRUCTURE; O-ETHYLHYDROXYLAMMONIUM; ORGANIC-INORGANIC HYBRID; LAYERED PEROVSKITEPoly[bis(O-ethylhydroxylaminium) [di-μ-chlorido-dichloridocadmate(II)]]urn:issn:2414-3146text/htmlThe title compound, {(CH3CH2ONH3)2[CdCl4]}n, consists of bilayers of organic CH3CH2ONH3+ cations and infinite [CdCl4]n2n− inorganic layers. It can be described as an organic–inorganic hybrid layered perovskite. In the crystal structure, the CdII cation is situated at an inversion center and is coordinated by six chloride ions, forming a slightly distorted octahedral coordination polyhedron. By corner-sharing of the [CdCl6] octahedra, infinite [CdCl4]n2n− inorganic layers are formed, extending parallel to (100). The inorganic layers alternate with bilayers of CH3CH2ONH3+ cations, whereby the connection of the cationic and anionic layers is achieved through N—H⋯Cl hydrogen bonds and Coulombic interactions.doi:10.1107/S24143146230089822023-10-19texthttps://creativecommons.org/licenses/by/4.0/Tong, Y.-Q.Lei, Z.-Q.Huang, B.102414-3146x230898October 2023metal-organic compounds2414-3146IUCrData2023-10-19med@iucr.orghttps://creativecommons.org/licenses/by/4.0/8Rerefinement of the crystal structure of α-ThBr4
http://scripts.iucr.org/cgi-bin/paper?wm4200
Single crystals of α-ThBr4, thorium(IV) tetrabromide, were obtained as a side product from the reaction of CuBr with β-ThBr4 at 753 K. In the crystal structure, the Th atom (site symmetry \overline{4}..) is surrounded by eight Br atoms in the form of a tetragonal-disphenoidal coordination polyhedron. The connectivity of these polyhedra is 3∞[ThBr4/2Br4/2]. In comparison with the previous crystal structure refinement [Mason et al. (1974). J. Less-Common Met. 35, 331–338], the current rerefinement resulted in much higher preciscion of the lattice parameters and the atomic coordinates.The rerefinement of the crystal structure of α-ThBr4 (α-ThCl4 structure type) results in higher precision of the lattice parameters and the atomic coordinates.International Union of CrystallographyenCRYSTAL STRUCTURE; THORIUM; THORIUM BROMIDE; ACTINIDE BROMIDERerefinement of the crystal structure of α-ThBr4urn:issn:2414-3146text/htmlSingle crystals of α-ThBr4, thorium(IV) tetrabromide, were obtained as a side product from the reaction of CuBr with β-ThBr4 at 753 K. In the crystal structure, the Th atom (site symmetry \overline{4}..) is surrounded by eight Br atoms in the form of a tetragonal-disphenoidal coordination polyhedron. The connectivity of these polyhedra is 3∞[ThBr4/2Br4/2]. In comparison with the previous crystal structure refinement [Mason et al. (1974). J. Less-Common Met. 35, 331–338], the current rerefinement resulted in much higher preciscion of the lattice parameters and the atomic coordinates.doi:10.1107/S24143146230089082023-10-17texthttps://creativecommons.org/licenses/by/4.0/Graubner, T.Kraus, F.IUCrData8https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-10-17October 2023x2308902414-3146102414-3146inorganic compoundsPoly[[(μ3-adamantane-1,3-diacetato)[μ-N-(pyridin-3-yl)isonicotinamide]nickel(II)] monohydrate], a layered coordination polymer with triangular (3,6) topology
http://scripts.iucr.org/cgi-bin/paper?bh4079
The title compound, {[Ni(C14H18O4)(C11H9N3O)]·H2O}n, contains octahedrally coordinated NiII ions ligated by 1,3-adamantanediacetato (ada) ligands and N-(pyridin-3-yl)isonicotinamide (3-pina) ligands, to form coordination polymer layers with a triangular (3,6) grid topology based on [Ni2(OCO)2] dimeric units. The diperiodic layer motifs stack in an ABAB pattern mediated by C—H⋯O supramolecular interactions between ada ligands and water molecules of crystallization to form the full triperiodic crystal structure of the title compound.The title inorganic NiII polymer features layers with a triangular (3,6) grid topology, stacked in a ABAB pattern to form a triperiodic structure.International Union of CrystallographyenCRYSTAL STRUCTURE; POLYMER; TOPOLOGY; NICKEL; ISONICOTINAMIDEPoly[[(μ3-adamantane-1,3-diacetato)[μ-N-(pyridin-3-yl)isonicotinamide]nickel(II)] monohydrate], a layered coordination polymer with triangular (3,6) topologyurn:issn:2414-3146text/htmlThe title compound, {[Ni(C14H18O4)(C11H9N3O)]·H2O}n, contains octahedrally coordinated NiII ions ligated by 1,3-adamantanediacetato (ada) ligands and N-(pyridin-3-yl)isonicotinamide (3-pina) ligands, to form coordination polymer layers with a triangular (3,6) grid topology based on [Ni2(OCO)2] dimeric units. The diperiodic layer motifs stack in an ABAB pattern mediated by C—H⋯O supramolecular interactions between ada ligands and water molecules of crystallization to form the full triperiodic crystal structure of the title compound.doi:10.1107/S24143146230086962023-10-05texthttps://creativecommons.org/licenses/by/4.0/Travis, J.Z.LaDuca, R.L.IUCrDatahttps://creativecommons.org/licenses/by/4.0/med@iucr.org2023-10-0582414-314610October 2023x230869metal-organic compounds2414-3146Al0.88Cu0.94Fe0.18
http://scripts.iucr.org/cgi-bin/paper?hb4450
The intermetallic phase with composition Al0.88Cu0.94Fe0.18 was synthesized by high-temperature sintering of a mixture with initial chemical composition Al78Cu48Fe13. Al0.88Cu0.94Fe0.18 adopts the CsCl structure type in space-group Pm\overline{3}m. The structure analysis revealed that one site is co-occupied by Al and Cu with a ratio of 0.88 (5):0.12 (5) and the other is co-occupied by Fe and Cu with a ratio of 0.2 (4):0.8 (4). The Al/Cu⋯Fe/Cu separation is 2.5465 (13) Å.The intermetallic phase with composition Al0.88Cu0.94Fe0.18 was synthesized by high-temperature sintering of a mixture with initial chemical composition Al78Cu48Fe13. Al0.88Cu0.94Fe0.18 adopts the CsCl structure type in space-group Pm\overline{3}m.International Union of CrystallographyenCRYSTAL STRUCTURE; HIGH-TEMPERATURE SINTERING; [BETA] PHASE; AL-CU-FE SYSTEMAl0.88Cu0.94Fe0.18urn:issn:2414-3146text/htmlThe intermetallic phase with composition Al0.88Cu0.94Fe0.18 was synthesized by high-temperature sintering of a mixture with initial chemical composition Al78Cu48Fe13. Al0.88Cu0.94Fe0.18 adopts the CsCl structure type in space-group Pm\overline{3}m. The structure analysis revealed that one site is co-occupied by Al and Cu with a ratio of 0.88 (5):0.12 (5) and the other is co-occupied by Fe and Cu with a ratio of 0.2 (4):0.8 (4). The Al/Cu⋯Fe/Cu separation is 2.5465 (13) Å.doi:10.1107/S24143146230087022023-10-12texthttps://creativecommons.org/licenses/by/4.0/Liu, Y.Liu, H.Wen, B.Fan, C.102414-3146x230870October 2023inorganic compounds2414-3146IUCrData2023-10-12med@iucr.orghttps://creativecommons.org/licenses/by/4.0/8Poly[[[μ-1,4-bis(pyridin-4-ylmethyl)piperazine][μ-4-(2-carboxylatoethyl)benzoato]copper(II)] monohydrate], a coordination polymer with twofold interpenetrated cds topology networks
http://scripts.iucr.org/cgi-bin/paper?wm4198
The title compound, {[Cu(C10H8O4)(C16H20N4)]·H2O}n, contains square-planar coordinated CuII ions linked by 4-(carboxylatoethyl)benzoato (ceb) and 1,4-bis(pyridin-4-ylmethyl)piperazine (bpmp) ligands into a tri-periodic coordination polymer with twofold interpenetrating 658 cds topology. Positional crystallographic disorder among the copper atoms, the ethylcarboxy group of the ceb ligands, and the water molecules of crystallization exists in a refined 0.655 (6)/0.345 (6) ratio.A divalent copper tri-periodic coordination polymer with twofold interpenetrating 658 cds topology, {[Cu(ceb)(bpmp)]·H2O]n, was structurally characterized by single-crystal X-ray diffraction.International Union of CrystallographyenCRYSTAL STRUCTURE; COPPER; COORDINATION POLYMER; DISORDER; TRI-PERIODIC NETWORKPoly[[[μ-1,4-bis(pyridin-4-ylmethyl)piperazine][μ-4-(2-carboxylatoethyl)benzoato]copper(II)] monohydrate], a coordination polymer with twofold interpenetrated cds topology networksurn:issn:2414-3146text/htmlThe title compound, {[Cu(C10H8O4)(C16H20N4)]·H2O}n, contains square-planar coordinated CuII ions linked by 4-(carboxylatoethyl)benzoato (ceb) and 1,4-bis(pyridin-4-ylmethyl)piperazine (bpmp) ligands into a tri-periodic coordination polymer with twofold interpenetrating 658 cds topology. Positional crystallographic disorder among the copper atoms, the ethylcarboxy group of the ceb ligands, and the water molecules of crystallization exists in a refined 0.655 (6)/0.345 (6) ratio.doi:10.1107/S24143146230085562023-10-03texthttps://creativecommons.org/licenses/by/4.0/Gaskin, G.J.LaDuca, R.L.IUCrData2023-10-03med@iucr.orghttps://creativecommons.org/licenses/by/4.0/8102414-3146x230855October 2023metal-organic compounds2414-31461-Methyl-3-(naphthalen-2-yl)cyclopentadiene
http://scripts.iucr.org/cgi-bin/paper?zl4062
The title compound, C16H14, an asymmetric naphthyl-/methyl-substituted cyclopentadiene was synthesized and one isomer of five accessible through sigmatropic rearrangement was isolated and characterized by 1H NMR and X-ray diffraction. The crystal packing features an intermolecular C—H⋯π interaction.An asymmetric naphthyl-/methyl-substituted cyclopentadiene was synthesized and one isomer of five accessible through sigmatropic rearrangement was isolated and characterized by 1H NMR and X-ray diffraction. The title compound is envisioned as a π-bonded `antenna' ligand to enhance lanthanide ion luminescence sensitization.International Union of CrystallographyenCRYSTAL STRUCTURE; CYCLOPENTADIENE; LUMINESCENCE SENSITIZATION1-Methyl-3-(naphthalen-2-yl)cyclopentadieneurn:issn:2414-3146text/htmlThe title compound, C16H14, an asymmetric naphthyl-/methyl-substituted cyclopentadiene was synthesized and one isomer of five accessible through sigmatropic rearrangement was isolated and characterized by 1H NMR and X-ray diffraction. The crystal packing features an intermolecular C—H⋯π interaction.doi:10.1107/S24143146230085682023-10-10texthttps://creativecommons.org/licenses/by/4.0/Michailidis, M.Bonitatibus Jr, P.J.med@iucr.org2023-10-10https://creativecommons.org/licenses/by/4.0/8IUCrDataorganic compounds2414-3146102414-3146x230856October 2023Poly[[μ-1,3-bis(pyridin-3-yl)urea]bis(μ4-glutarato)dicopper(II)]
http://scripts.iucr.org/cgi-bin/paper?pk4043
The title compound, [Cu2(C5H6O4)2(C11H10N4O)]n, contains square-pyramidally coordinated CuII ions linked by anti-gauche conformation glutarate (glu) ligands into [Cu2(glu)2]n di-periodic coordination polymer layers with embedded [Cu2(OCO)4] paddlewheel clusters. In turn, the layer motifs are connected by 1,3-di(pyridin-3-yl)urea (3-dpu) linkers to form a [Cu2(glu)2(3-dpu)]n tri-periodic coordination polymer network. Treating the [Cu2(OCO)4] clusters as 6-connected nodes reveals an underlying 41263 pcu topology according to TOPOSPRO software [Blatov et al. (2014). Cryst. Growth Des. 14, 3576–3586].A divalent copper tri-periodic coordination polymer with no co-crystallized species and underlying pcu topology, {[Cu2(glu)2(3-dpu)]n, was prepared and structurally characterized by single-crystal X-ray diffraction.International Union of CrystallographyenCRYSTAL STRUCTURE; COPPER; COORDINATION POLYMER; TRI-PERIODICPoly[[μ-1,3-bis(pyridin-3-yl)urea]bis(μ4-glutarato)dicopper(II)]urn:issn:2414-3146text/htmlThe title compound, [Cu2(C5H6O4)2(C11H10N4O)]n, contains square-pyramidally coordinated CuII ions linked by anti-gauche conformation glutarate (glu) ligands into [Cu2(glu)2]n di-periodic coordination polymer layers with embedded [Cu2(OCO)4] paddlewheel clusters. In turn, the layer motifs are connected by 1,3-di(pyridin-3-yl)urea (3-dpu) linkers to form a [Cu2(glu)2(3-dpu)]n tri-periodic coordination polymer network. Treating the [Cu2(OCO)4] clusters as 6-connected nodes reveals an underlying 41263 pcu topology according to TOPOSPRO software [Blatov et al. (2014). Cryst. Growth Des. 14, 3576–3586].doi:10.1107/S24143146230083372023-09-26texthttps://creativecommons.org/licenses/by/4.0/Ezenyilimba, F.C.LaDuca, R.L.IUCrData8https://creativecommons.org/licenses/by/4.0/2023-09-26med@iucr.orgSeptember 2023x2308332414-314692414-3146metal-organic compounds4-Amino-3,5-dichloropyridinium 3-hydroxypicolinate monohydrate
http://scripts.iucr.org/cgi-bin/paper?hb4452
In the title hydrated salt, C5H5Cl2N2+·C6H4NO3−·H2O, the pyridine N atom of the cation is protonated and an intramolecular O—H⋯O hydrogen bond is observed in the anion, which generates an S(6) ring. The crystal packing features N—H⋯N, O—H⋯O, N—H⋯O, C—H⋯Cl and C—H⋯O hydrogen bonds, which generate a three-dimensional network.The title hydrated salt features a dense array of hydrogen bonds, forming a three-dimensional network.International Union of CrystallographyenCRYSTAL STRUCTURE; HYDROGEN BONDING; HYDRATED SALT4-Amino-3,5-dichloropyridinium 3-hydroxypicolinate monohydrateurn:issn:2414-3146text/htmlIn the title hydrated salt, C5H5Cl2N2+·C6H4NO3−·H2O, the pyridine N atom of the cation is protonated and an intramolecular O—H⋯O hydrogen bond is observed in the anion, which generates an S(6) ring. The crystal packing features N—H⋯N, O—H⋯O, N—H⋯O, C—H⋯Cl and C—H⋯O hydrogen bonds, which generate a three-dimensional network.doi:10.1107/S24143146230082102023-09-22texthttps://creativecommons.org/licenses/by/4.0/Ashokan, A.Nehru, J.Chakkarapani, N.Khamrang, T.Kavitha, S.J.Rajakannan, V.Hemamalini, M.organic compounds2414-314692414-3146x230821September 2023med@iucr.org2023-09-22https://creativecommons.org/licenses/by/4.0/8IUCrData3-Nitrobenzonitrile
http://scripts.iucr.org/cgi-bin/paper?hb4451
The crystal structure of 3-nitrobenzonitrile, C7H4N2O2, was elucidated by low-temperature single-crystal X-ray diffraction. The compound crystallizes in the Sohncke space group P21 and features two molecules in the unit cell. Aromatic π–π stacking leads to stacks of molecules in the [100] direction. The absolute structure was established from anomalous dispersion.3-Nitrobenzonitrile crystallizes in the Sohncke space group P21.International Union of CrystallographyenNITRO; NITRILE; BENZONITRILE; CRYSTAL STRUCTURE3-Nitrobenzonitrileurn:issn:2414-3146text/htmlThe crystal structure of 3-nitrobenzonitrile, C7H4N2O2, was elucidated by low-temperature single-crystal X-ray diffraction. The compound crystallizes in the Sohncke space group P21 and features two molecules in the unit cell. Aromatic π–π stacking leads to stacks of molecules in the [100] direction. The absolute structure was established from anomalous dispersion.doi:10.1107/S24143146230081432023-09-22texthttps://creativecommons.org/licenses/by/4.0/Virant, M.Siljanovska, A.Cerkovnik, J.Lozinšek, M.IUCrData8med@iucr.org2023-09-22https://creativecommons.org/licenses/by/4.0/x230814September 202392414-31462414-3146organic compoundsPoly[[[μ-1,4-bis(pyridin-4-ylcarbonyl)piperazine-κ2N:N′][μ-2-(2-carboxylatoeth-1-en-1-yl)benzoato-κ2O:O2]zinc(II)] 2.5 hydrate]: a tri-periodic coordination polymer with a dimer-based six-connected pcu topology
http://scripts.iucr.org/cgi-bin/paper?tk4097
The title compound, {[Zn(C10H6O4)(C16H16N4O2]·2.5H2O}n, contains five-coordinate ZnII ions intermediate between square-pyramidal and trigonal–bipyramidal coordination environments. The ZnII ions are connected by 2-carboxycinnamate (cca) ligands and N,N′-bis-(pyridine-4-carboxamido)piperazine (4-pcap) ligands to construct a non-interpenetrated, tri-periodic coordination polymer with embedded [Zn2(OCO)2] dimeric units. Treating these as six-connected nodes reveals an overall (41263) pcu topology. One of the 4-pcap piperazinyl rings is disordered equally over two sets of crystallographic positions.The title compound contains five-coordinate ZnII ions intermediate between square-pyramidal and trigonal–bipyramidal coordination geometries. The ZnII ions are connected by 2-carboxycinnamate (cca) ligands and N,N′-bis-(pyridine-4-carboxamido)piperazine (4-pcap) ligands to construct a non-interpenetrated, tri-periodic coordination polymer with embedded [Zn2(OCO)2] dimeric units. Treating these as six-connected nodes reveals an overall (41263) pcu topology.International Union of CrystallographyenCRYSTAL STRUCTURE; TRI-PERIODIC COORDINATION POLYMER; PCU TOPOLOGY; CCA; 4-PCAPPoly[[[μ-1,4-bis(pyridin-4-ylcarbonyl)piperazine-κ2N:N′][μ-2-(2-carboxylatoeth-1-en-1-yl)benzoato-κ2O:O2]zinc(II)] 2.5 hydrate]: a tri-periodic coordination polymer with a dimer-based six-connected pcu topologyurn:issn:2414-3146text/htmlThe title compound, {[Zn(C10H6O4)(C16H16N4O2]·2.5H2O}n, contains five-coordinate ZnII ions intermediate between square-pyramidal and trigonal–bipyramidal coordination environments. The ZnII ions are connected by 2-carboxycinnamate (cca) ligands and N,N′-bis-(pyridine-4-carboxamido)piperazine (4-pcap) ligands to construct a non-interpenetrated, tri-periodic coordination polymer with embedded [Zn2(OCO)2] dimeric units. Treating these as six-connected nodes reveals an overall (41263) pcu topology. One of the 4-pcap piperazinyl rings is disordered equally over two sets of crystallographic positions.doi:10.1107/S24143146230081182023-09-22texthttps://creativecommons.org/licenses/by/4.0/Glatz, E.J.LaDuca, R.L.IUCrDatahttps://creativecommons.org/licenses/by/4.0/2023-09-22med@iucr.org82414-31469September 2023x230811metal-organic compounds2414-3146Tetrakis(μ-acetato-κ2O:O′)bis[(tetrahydrofuran-κO)chromium(II)]
http://scripts.iucr.org/cgi-bin/paper?wm4196
The title compound, [Cr2(C2H3O2)4(C4H8O)2] or [Cr2(OAc)4(THF)2] (OAc is acetate, THF is tetrahydrofuran), was obtained by recrystallization of anhydrous chromium(II) acetate [Cr2(OAc)4] from hot tetrahydrofuran. The centrosymmetric complex forms monoclinic crystals, space group C2/c, and consists of two CrII atoms bridged by four acetate ligands. Additionally, each CrII atom is coordinated by a terminal THF ligand, which leads to a square-pyramidal coordination.Centrosymmetric [Cr2(OAc)4(THF)2] consists of two CrII atoms that are bridged by four acetate ions to yield a typical paddle-wheel structure. Furthermore, each chromium atom bears an axially bound THF ligand to give a square-pyramidal coordination.International Union of CrystallographyenCRYSTAL STRUCTURE; CHROMIUM; ACETATE; TETRAHYDROFURANE; PADDLE WHEELTetrakis(μ-acetato-κ2O:O′)bis[(tetrahydrofuran-κO)chromium(II)]urn:issn:2414-3146text/htmlThe title compound, [Cr2(C2H3O2)4(C4H8O)2] or [Cr2(OAc)4(THF)2] (OAc is acetate, THF is tetrahydrofuran), was obtained by recrystallization of anhydrous chromium(II) acetate [Cr2(OAc)4] from hot tetrahydrofuran. The centrosymmetric complex forms monoclinic crystals, space group C2/c, and consists of two CrII atoms bridged by four acetate ligands. Additionally, each CrII atom is coordinated by a terminal THF ligand, which leads to a square-pyramidal coordination.doi:10.1107/S24143146230080152023-09-22texthttps://creativecommons.org/licenses/by/4.0/Heiser, C.Merzweiler, K.IUCrData2023-09-22med@iucr.orghttps://creativecommons.org/licenses/by/4.0/892414-3146x230801September 2023metal-organic compounds2414-31461-(Pyrrolidin-1-yl)ethan-1-iminium chloride
http://scripts.iucr.org/cgi-bin/paper?hb4444
The title compound, C6H13N2+·Cl−, is as an amidinium salt that was isolated as unexpected product from the reaction between acetonitrile, chloroform and pyrrolidine under refluxing conditions. The packing features two N—H⋯Cl hydrogen bonds to generate centrosymmetric tetramers (two cations and two anions) and van der Waals interactions.The title salt was serendipitously obtained while using a mixed solvent system during an SN2 reaction between an alkyl halide and pyrrolidine.International Union of CrystallographyenACETONITRILE; AMIDINIUM SALT; CHLOROFORM; CRYSTAL STRUCTURE; PINNER REACTION; PYRROLIDINE1-(Pyrrolidin-1-yl)ethan-1-iminium chlorideurn:issn:2414-3146text/htmlThe title compound, C6H13N2+·Cl−, is as an amidinium salt that was isolated as unexpected product from the reaction between acetonitrile, chloroform and pyrrolidine under refluxing conditions. The packing features two N—H⋯Cl hydrogen bonds to generate centrosymmetric tetramers (two cations and two anions) and van der Waals interactions.doi:10.1107/S24143146230079032023-09-12texthttps://creativecommons.org/licenses/by/4.0/Artis, R.Padgett, C.W.Quillian, B.2414-31469September 2023x230790organic compounds2414-3146IUCrDatahttps://creativecommons.org/licenses/by/4.0/med@iucr.org2023-09-128Poly[diaqua[μ-1,4-bis(pyridin-4-ylmethyl)piperazine][μ-4-(carboxylatoethyl)benzoato]nickel(II)]
http://scripts.iucr.org/cgi-bin/paper?wm4194
The title compound, [Ni(C10H8O4)(C16H20N4)(H2O)2]n, contains NiII cations octahedrally surrounded within an [O4N2] coordination set. The cations are linked by 4-(carboxyethyl)benzoate (ceb) and 1,4-bis(pyridin-4-ylmethyl)piperazine (bpmp) ligands into tri-periodic diamondoid (dia) networks. The fivefold interpenetrated dia networks are held into the crystal structure by means of O—H⋯O hydrogen bonding between bound water molecules and unligated carboxylate O atoms of the ceb ligands.The divalent nickel compound {[Ni(ceb)(bpmp)(H2O)2]n, (ceb is (4-(carboxyethyl)benzoate; bpmp is 1,4-bis(pyridin-4-ylmethyl)piperazine) crystallizes as a fivefold interpenetrated tri-periodic coordination polymer without co-crystallized species.International Union of CrystallographyenCRYSTAL STRUCTURE; NICKEL; COORDINATION POLYMER; DIAMONDOID NETWORK.Poly[diaqua[μ-1,4-bis(pyridin-4-ylmethyl)piperazine][μ-4-(carboxylatoethyl)benzoato]nickel(II)]urn:issn:2414-3146text/htmlThe title compound, [Ni(C10H8O4)(C16H20N4)(H2O)2]n, contains NiII cations octahedrally surrounded within an [O4N2] coordination set. The cations are linked by 4-(carboxyethyl)benzoate (ceb) and 1,4-bis(pyridin-4-ylmethyl)piperazine (bpmp) ligands into tri-periodic diamondoid (dia) networks. The fivefold interpenetrated dia networks are held into the crystal structure by means of O—H⋯O hydrogen bonding between bound water molecules and unligated carboxylate O atoms of the ceb ligands.doi:10.1107/S24143146230078852023-09-22texthttps://creativecommons.org/licenses/by/4.0/Gaskin, G.J.LaDuca, R.L.https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-09-228IUCrDatametal-organic compounds2414-31462414-31469September 2023x2307881-Ethyl-4-isopropyl-1,2,4-triazolium bromide
http://scripts.iucr.org/cgi-bin/paper?hb4448
An ionic compound consisting of a triazolium cation and bromide anion, C7H14N3+·Br−, has been synthesized and structurally characterized using single-crystal X-ray diffraction and NMR. The compound crystallizes in the monoclinic space group P21/m with the non-hydrogen atoms of one cation lying on general positions and the others lying on a mirror plane. One bromide ion also lies on the mirror. The extended structure exhibits only weak intermolecular interactions between heterocyclic C—H groups and Br− ions.The title compound crystallizes with Z = 6 in space group P21/m.International Union of CrystallographyenCRYSTAL STRUCTURE; TRIAZOLIUM SALT; HETEROCYCLIC IONIC COMPOUND1-Ethyl-4-isopropyl-1,2,4-triazolium bromideurn:issn:2414-3146text/htmlAn ionic compound consisting of a triazolium cation and bromide anion, C7H14N3+·Br−, has been synthesized and structurally characterized using single-crystal X-ray diffraction and NMR. The compound crystallizes in the monoclinic space group P21/m with the non-hydrogen atoms of one cation lying on general positions and the others lying on a mirror plane. One bromide ion also lies on the mirror. The extended structure exhibits only weak intermolecular interactions between heterocyclic C—H groups and Br− ions.doi:10.1107/S24143146230078482023-09-14texthttps://creativecommons.org/licenses/by/4.0/Maynard, A.Keller, T.M.Gau, M.Albert, D.R.Rajaseelan, E.September 2023x2307842414-314692414-3146organic compoundsIUCrData8https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-09-14(Z)-Benzyl 2-(5-methyl-2-oxoindolin-3-ylidene)hydrazinecarbodithioate
http://scripts.iucr.org/cgi-bin/paper?hb4449
The title compound, C17H15N3OS2 was obtained from the condensation reaction of S-benzyldithiocarbazate and 5-methylisatin. In the solid-state, the molecule adopts a Z configuration with the 5-methylisatin and dithiocarbazate groups located on the same side of the C=N bond, involving an intramolecular N—H⋯O hydrogen bond.The crystal structure of a new dithiocarbazate imine, obtained from the condensation reaction of S-benzyldithiocarbazate and 5-methylisatin, is described.International Union of CrystallographyenCRYSTAL STRUCTURE; DITHIOCARBAZATE; 5-METHYLISATIN; Z CONFIGURATION; HYDROGEN BONDING(Z)-Benzyl 2-(5-methyl-2-oxoindolin-3-ylidene)hydrazinecarbodithioateurn:issn:2414-3146text/htmlThe title compound, C17H15N3OS2 was obtained from the condensation reaction of S-benzyldithiocarbazate and 5-methylisatin. In the solid-state, the molecule adopts a Z configuration with the 5-methylisatin and dithiocarbazate groups located on the same side of the C=N bond, involving an intramolecular N—H⋯O hydrogen bond.doi:10.1107/S24143146230078242023-09-12texthttps://creativecommons.org/licenses/by/4.0/Abdul Manan, M.A.F.Cordes, D.B.McKay, A.P.Mohammat, M.F.Mohd Aluwi, M.F.F.Jumali, N.S.IUCrDatamed@iucr.org2023-09-12https://creativecommons.org/licenses/by/4.0/892414-3146x230782September 2023organic compounds2414-3146(2,4-Dichlorobenzylidene)[2-(1H-indol-3-yl)ethyl]amine
http://scripts.iucr.org/cgi-bin/paper?hb4446
In the title compound, C17H14Cl2N2, the molecule exists in an E configuration with respect to the C=N bond of the Schiff base fragment. The dihedral angle between the indole ring system and the benzene ring is 80.86 (12)°. In the crystal, molecules are connected by N—H⋯N hydrogen bonds, generating a C(7) chain extending along the a-axis direction. No aromatic π–π stacking occurs but weak C—H⋯π interactions are observed.The molecules of the title compound are linked by N—H⋯N hydrogen bonds, generating a C(7) chain extending along the a-axis direction.International Union of CrystallographyenCRYSTAL STRUCTURE; HYDROGEN BONDING; C-H...[PI] INTERACTIONS(2,4-Dichlorobenzylidene)[2-(1H-indol-3-yl)ethyl]amineurn:issn:2414-3146text/htmlIn the title compound, C17H14Cl2N2, the molecule exists in an E configuration with respect to the C=N bond of the Schiff base fragment. The dihedral angle between the indole ring system and the benzene ring is 80.86 (12)°. In the crystal, molecules are connected by N—H⋯N hydrogen bonds, generating a C(7) chain extending along the a-axis direction. No aromatic π–π stacking occurs but weak C—H⋯π interactions are observed.doi:10.1107/S24143146230078002023-09-12texthttps://creativecommons.org/licenses/by/4.0/Murugan, S.Paul, A.C.Khamrang, T.Kavitha, S.J.Rajakannan, V.Hemamalini, M.IUCrData8https://creativecommons.org/licenses/by/4.0/2023-09-12med@iucr.orgSeptember 2023x2307802414-314692414-3146organic compoundsBis(4-acetoxy-N-ethyl-N-n-propyltryptammonium) fumarate–fumaric acid (1/1)
http://scripts.iucr.org/cgi-bin/paper?hb4447
The solid-state structure of the title salt/adduct (systemic name: bis{[2-(4-acetyloxy-1H-indol-3-yl)ethyl](ethyl)propylazanium} but-2-enedioate–(E)-butenedioic acid (1/1)), 2C17H25N2O2+·C4H2O42−·C4H4O4, was determined by single-crystal X-ray diffraction. The asymmetric unit consists of a singly protonated tryptammonium cation, one half of a fumarate dianion and one half of a fumaric acid molecule. In the crystal, the ions and molecules are linked together in infinite chains propagating along [001] through a series of N—H⋯O and O—H⋯O hydrogen bonds.The structure of the synthetic psychedelic prodrug 4-hydroxy-N-ethyl-N-n-propyltryptamine is reported as its salt with a fumarate dianion and a fumaric acid adduct.International Union of CrystallographyenCRYSTAL STRUCTURE; TRYPTAMINES; INDOLES; FUMARATES; HYDROGEN BONDSBis(4-acetoxy-N-ethyl-N-n-propyltryptammonium) fumarate–fumaric acid (1/1)urn:issn:2414-3146text/htmlThe solid-state structure of the title salt/adduct (systemic name: bis{[2-(4-acetyloxy-1H-indol-3-yl)ethyl](ethyl)propylazanium} but-2-enedioate–(E)-butenedioic acid (1/1)), 2C17H25N2O2+·C4H2O42−·C4H4O4, was determined by single-crystal X-ray diffraction. The asymmetric unit consists of a singly protonated tryptammonium cation, one half of a fumarate dianion and one half of a fumaric acid molecule. In the crystal, the ions and molecules are linked together in infinite chains propagating along [001] through a series of N—H⋯O and O—H⋯O hydrogen bonds.doi:10.1107/S24143146230077942023-09-08texthttps://creativecommons.org/licenses/by/4.0/Pham, D.N.K.Sackett, N.B.Chadeayne, A.R.Golen, J.A.Manke, D.R.x230779September 202392414-31462414-3146organic compoundsIUCrData82023-09-08med@iucr.orghttps://creativecommons.org/licenses/by/4.0/(31E,32Z,71E,72Z)-4,8-Bis(3,5-dichlorophenyl)-14,33,53,73-tetrapropyl-11H,32H,51H,72H-1,5(2,5),3,7(5,2)-tetrapyrrola-2,6(2,5)-dithiophenacyclooctaphane
http://scripts.iucr.org/cgi-bin/paper?xu4052
Purple crystals of the title compound, C50H44Cl4N4S2 were obtained from the reaction of 2,5-bis(4-propyl-1H-pyrrol-2-yl)thiophene and 3,5-dichlorobenzaldehyde in the presence of trifluoroacetic acid for 3 h and subsequent addition of p-chloranil. The macrocycle in the title compound can be described as a highly planar structure wthe the average deviation of the 32 macrocyclic atoms from the least-squares plane being 0.0416 Å. Its molecular conformation is stabilized by two intramolecular N—H⋯N bonds and a three-dimensional network is formed by C—H⋯π interactions.In the title compound, [24]dithiaamethyrin(1.0.0.1.0.0); C50H44Cl4N4S2, the macrocycle can be described as a highly planar structure with a mean-plane deviation (MPD) value of 0.0416 Å. The molecular conformation is stabilized by two intramolecular N—H⋯N interactions. In the crystal, molecules are also linked via C—H⋯π interactions forming a three-dimensional network.International Union of CrystallographyenCRYSTAL STRUCTURE; ANTIAROMATIC; HETEROATOM; MACROCYCLIC COMPOUND(31E,32Z,71E,72Z)-4,8-Bis(3,5-dichlorophenyl)-14,33,53,73-tetrapropyl-11H,32H,51H,72H-1,5(2,5),3,7(5,2)-tetrapyrrola-2,6(2,5)-dithiophenacyclooctaphaneurn:issn:2414-3146text/htmlPurple crystals of the title compound, C50H44Cl4N4S2 were obtained from the reaction of 2,5-bis(4-propyl-1H-pyrrol-2-yl)thiophene and 3,5-dichlorobenzaldehyde in the presence of trifluoroacetic acid for 3 h and subsequent addition of p-chloranil. The macrocycle in the title compound can be described as a highly planar structure wthe the average deviation of the 32 macrocyclic atoms from the least-squares plane being 0.0416 Å. Its molecular conformation is stabilized by two intramolecular N—H⋯N bonds and a three-dimensional network is formed by C—H⋯π interactions.doi:10.1107/S24143146230076662023-09-08texthttps://creativecommons.org/licenses/by/4.0/Ishimaru, Y.Ikeda, R.Fujihara, T.2414-3146organic compoundsx230766September 202392414-31468med@iucr.org2023-09-08https://creativecommons.org/licenses/by/4.0/IUCrDatacatena-Poly[[diaquabis(1,3-dihydro-3-oxoisobenzofuran-1-acetato)copper(II)]-μ-N,N′-(ethane-1,2-diyl)dinicotinamide]
http://scripts.iucr.org/cgi-bin/paper?zl4058
The title compound, {[Cu(C10H7O4)2(C14H14N4O2)(H2O)2]n, contains octahedrally coordinated CuII ions ligated by two bis(1,3-dihydro-3-oxo-1-isobenzofuranacetate (dibf) ligands and two trans water molecules, linked by N,N′-(ethane-1,2-diyl)dinicotinamide (edn) ligands into mono-periodic coordination polymer chains. The dibf ligands exhibit a pseudo-mirror positional disorder over two positions in a 89.2 (3)/10.8 (3) ratio; the central amide groups of the edn ligands are disordered pseudo-rotationally in the same ratio. These mono-periodic chain motifs are held into supramolecular di-periodic supramolecular layers by means of N—H⋯O hydrogen bonding between edn amide groups and unligated dibf carboxylate O atoms. In turn, the supramolecular layers are held by crystal packing forces into the full crystal structure of the title compound.In situ lactonization of 2-carboxycinnamic acid to form bis(1,3-dihydro-3-oxo-1-isobenzofuranacetate (dibf) resulted in the the crystallization of [Cu(dibf)(edn)(H2O)2]n coordination polymer chains [edn = N,N′-(ethane-1,2-diyl)dinicotinamide].International Union of CrystallographyenCRYSTAL STRUCTURE; COORDINATION POLYMER; IN SITU LACTONIZATION; DIBF; EDNcatena-Poly[[diaquabis(1,3-dihydro-3-oxoisobenzofuran-1-acetato)copper(II)]-μ-N,N′-(ethane-1,2-diyl)dinicotinamide]urn:issn:2414-3146text/htmlThe title compound, {[Cu(C10H7O4)2(C14H14N4O2)(H2O)2]n, contains octahedrally coordinated CuII ions ligated by two bis(1,3-dihydro-3-oxo-1-isobenzofuranacetate (dibf) ligands and two trans water molecules, linked by N,N′-(ethane-1,2-diyl)dinicotinamide (edn) ligands into mono-periodic coordination polymer chains. The dibf ligands exhibit a pseudo-mirror positional disorder over two positions in a 89.2 (3)/10.8 (3) ratio; the central amide groups of the edn ligands are disordered pseudo-rotationally in the same ratio. These mono-periodic chain motifs are held into supramolecular di-periodic supramolecular layers by means of N—H⋯O hydrogen bonding between edn amide groups and unligated dibf carboxylate O atoms. In turn, the supramolecular layers are held by crystal packing forces into the full crystal structure of the title compound.doi:10.1107/S24143146230076422023-09-08texthttps://creativecommons.org/licenses/by/4.0/Pumford, S.R.LaDuca, R.L.IUCrData8med@iucr.org2023-09-08https://creativecommons.org/licenses/by/4.0/x230764September 202392414-31462414-3146metal-organic compoundsPoly[[(μ3-adamantane-1,3-dicarboxylato)aqua[μ-N-(pyridin-3-yl)isonicotinamide]nickel(II)] monohydrate], a layered coordination polymer with (4,4) topology
http://scripts.iucr.org/cgi-bin/paper?vm4062
The title compound, {[Ni(C12H14O4)(C11H9N3O)(H2O)]·H2O}n, contains octahedrally coordinated NiII ions ligated by adamantane-1,3-dicarboxylate (adc) and N-(pyridin-3-yl)isonicotinamide (3-pina) ligands forming coordination polymer layers with a (4,4) grid topology. These diperiodic layer motifs aggregate in an AAA pattern mediated by supramolecular C—H⋯O interactions to form the full triperiodic crystal structure of the title compound.The title compound contains octahedrally coordinated NiII ions ligated by adamantane-1,3-dicarboxylate and N-(pyridin-3-yl)isonicotinamide ligands forming coordination polymer layers with a (4,4) grid topology.International Union of CrystallographyenCRYSTAL STRUCTURE; COORDINATION POLYMER; ADAMANTANE-1,3-DICARBOXYLATE; N-(PYRIDIN-3-YL)ISONICOTINAMIDE; NICKEL(II)Poly[[(μ3-adamantane-1,3-dicarboxylato)aqua[μ-N-(pyridin-3-yl)isonicotinamide]nickel(II)] monohydrate], a layered coordination polymer with (4,4) topologyurn:issn:2414-3146text/htmlThe title compound, {[Ni(C12H14O4)(C11H9N3O)(H2O)]·H2O}n, contains octahedrally coordinated NiII ions ligated by adamantane-1,3-dicarboxylate (adc) and N-(pyridin-3-yl)isonicotinamide (3-pina) ligands forming coordination polymer layers with a (4,4) grid topology. These diperiodic layer motifs aggregate in an AAA pattern mediated by supramolecular C—H⋯O interactions to form the full triperiodic crystal structure of the title compound.doi:10.1107/S24143146230075872023-09-08texthttps://creativecommons.org/licenses/by/4.0/Travis, J.Z.LaDuca, R.L.IUCrData2023-09-08med@iucr.orghttps://creativecommons.org/licenses/by/4.0/892414-3146x230758September 2023metal-organic compounds2414-3146Poly[[μ-1,3-bis(pyridin-3-yl)urea]bis(μ4-succinato)dicopper(II)], a ribbon-like coordination polymer
http://scripts.iucr.org/cgi-bin/paper?bh4078
In the title compound, [Cu2(C4H4O4)2(C11H10N4O)]n, mono-periodic coordination polymer ribbons are held into the crystal structure by means of N—H⋯O hydrogen bonding and crystal packing forces.A divalent copper one-dimensional ribbon copper(II) coordination polymer, with 1,3-bis(pyridin-3-yl)urea and succinate ligands, was structurally characterized by single-crystal X-ray diffraction.International Union of CrystallographyenCRYSTAL STRUCTURE; COORDINATION POLYMER; RIBBON TOPOLOGY; COPPER; SUCCINATEPoly[[μ-1,3-bis(pyridin-3-yl)urea]bis(μ4-succinato)dicopper(II)], a ribbon-like coordination polymerurn:issn:2414-3146text/htmlIn the title compound, [Cu2(C4H4O4)2(C11H10N4O)]n, mono-periodic coordination polymer ribbons are held into the crystal structure by means of N—H⋯O hydrogen bonding and crystal packing forces.doi:10.1107/S24143146230074722023-09-08texthttps://creativecommons.org/licenses/by/4.0/Ezenyilimba, F.LaDuca, R.L.2414-3146metal-organic compoundsSeptember 2023x2307472414-314698https://creativecommons.org/licenses/by/4.0/2023-09-08med@iucr.orgIUCrDataPoly[[μ-1,4-bis(pyridin-4-ylmethyl)piperazine]bis[μ3-4-(2-carboxylatoethyl)benzoato]dicopper(II)]
http://scripts.iucr.org/cgi-bin/paper?wm4195
In the title coordination polymer, [Cu2(C9H6O4)2(C16H20N4)]n, the CuII atoms in {NO4} square-pyramidal coordination environments are conjoined into diperiodic coordination polymer slabs by the full span of the bridging 1,4-bis(pyridin-4-ylmethyl)piperazine (bpmp) and 4-(carboxylethyl)benzoate (ceb) ligands. The slab motifs are expanded into the full crystal structure by means of longer-range C—H⋯O attractive interactions.The title compound is a diperiodic slab copper(II) coordination polymer held together via longer-range C—H⋯O attractive interactions.International Union of CrystallographyenCRYSTAL STRUCTURE; COPPER(II); JAHN-TELLER DISTORTION; COORDINATION POLYMERPoly[[μ-1,4-bis(pyridin-4-ylmethyl)piperazine]bis[μ3-4-(2-carboxylatoethyl)benzoato]dicopper(II)]urn:issn:2414-3146text/htmlIn the title coordination polymer, [Cu2(C9H6O4)2(C16H20N4)]n, the CuII atoms in {NO4} square-pyramidal coordination environments are conjoined into diperiodic coordination polymer slabs by the full span of the bridging 1,4-bis(pyridin-4-ylmethyl)piperazine (bpmp) and 4-(carboxylethyl)benzoate (ceb) ligands. The slab motifs are expanded into the full crystal structure by means of longer-range C—H⋯O attractive interactions.doi:10.1107/S24143146230074592023-08-30texthttps://creativecommons.org/licenses/by/4.0/Jia, J.LaDuca, R.L.x230745August 202382414-31462414-3146metal-organic compoundsIUCrData82023-08-30med@iucr.orghttps://creativecommons.org/licenses/by/4.0/N,N′-[1,4-Phenylenebis(iminocarbonyl)]bis(l-phenylalanine) tetrahydrofuran disolvate
http://scripts.iucr.org/cgi-bin/paper?bh4077
The title compound, C26H26N4O6·2C4H8O, representing a bis-urea with terminal phenylalanine units, crystallized with two tetrahydrofuran (THF) molecules. The main molecule is located on a crystallographic twofold axis, while the solvent molecule is disordered over two positions, with occupancies of 0.571 (15) and 0.429 (15). The host molecules are linked by N—H⋯O=C hydrogen bonds and C—H⋯O contacts with R21(6) and R21(7) ring motifs. The THF molecules enclosed in the crystal are connected to the bis-urea compound via O—H⋯O and C—H⋯O interactions.In the crystal structure of the title bis-urea derivative, the host molecules are linked by N—H⋯O=C hydrogen bonds and C—H⋯O contacts with R_{2}^{1}(6) and R_{2}^{1}(7) ring motifs.International Union of CrystallographyenCRYSTAL STRUCTURE; UREA; AMINO ACID; HYDROGEN BONDING; TETRAHYDROFURAN SOLVATEN,N′-[1,4-Phenylenebis(iminocarbonyl)]bis(l-phenylalanine) tetrahydrofuran disolvateurn:issn:2414-3146text/htmlThe title compound, C26H26N4O6·2C4H8O, representing a bis-urea with terminal phenylalanine units, crystallized with two tetrahydrofuran (THF) molecules. The main molecule is located on a crystallographic twofold axis, while the solvent molecule is disordered over two positions, with occupancies of 0.571 (15) and 0.429 (15). The host molecules are linked by N—H⋯O=C hydrogen bonds and C—H⋯O contacts with R21(6) and R21(7) ring motifs. The THF molecules enclosed in the crystal are connected to the bis-urea compound via O—H⋯O and C—H⋯O interactions.doi:10.1107/S24143146230074352023-09-08texthttps://creativecommons.org/licenses/by/4.0/Stapf, M.Schwarzer, A.x230743September 202392414-31462414-3146organic compoundsIUCrData82023-09-08med@iucr.orghttps://creativecommons.org/licenses/by/4.0/Bis(dimethoxyethane-1κ2O,O′)pentakis(1,1,1,3,3,3-hexafluoropropan-2-olato)-2κ3O,3κ2O-μ-hydroxido-1:3κ2O-μ3-oxido-1:2:3κ3O-magnesiumdialuminium
http://scripts.iucr.org/cgi-bin/paper?hb4443
Partial hydrolysis of a sample of [Mg(dme)3][Al(hfip)4]2 crystals led to the formation of the title complex, [Mg(dme)2{HOAl(hfip)2OAl(hfip)3}] (dme = dimethoxyethane and hfipH = hexafluoroisopropanol) or [Mg(C4H10O2)2O(OH)Al2(C3HF6O)5]. The magnesium cation exhibits a distorted octahedral coordination with two bidentate dimethoxyethane molecules and a dinuclear aluminate anion, coordinated to Mg2+ via oxido and hydroxido units. The anion is an oxido-bridged species, [HOAl(hfip)2(μ-O)Al(hfip)3]2–, with one Al3+ cation tetrahedrally coordinated by an oxido (O2–) anion, a hydroxido anion, and two hfip groups, whereas the second Al3+ cation is coordinated by the oxido anion and three hfip groups.The title complex was formed as a partial hydrolysis product of [Mg(dme)3][Al(hfip)4]2 (dme = dimethoxyethane and hfipH = hexafluoroisopropanol), a promising electrolyte salt for magnesium batteries.International Union of CrystallographyenFLUORINATED ALKOXYALUMINATE; HFIP; MAGNESIUM BATTERY ELECTROLYTE; CRYSTAL STRUCTUREBis(dimethoxyethane-1κ2O,O′)pentakis(1,1,1,3,3,3-hexafluoropropan-2-olato)-2κ3O,3κ2O-μ-hydroxido-1:3κ2O-μ3-oxido-1:2:3κ3O-magnesiumdialuminiumurn:issn:2414-3146text/htmlPartial hydrolysis of a sample of [Mg(dme)3][Al(hfip)4]2 crystals led to the formation of the title complex, [Mg(dme)2{HOAl(hfip)2OAl(hfip)3}] (dme = dimethoxyethane and hfipH = hexafluoroisopropanol) or [Mg(C4H10O2)2O(OH)Al2(C3HF6O)5]. The magnesium cation exhibits a distorted octahedral coordination with two bidentate dimethoxyethane molecules and a dinuclear aluminate anion, coordinated to Mg2+ via oxido and hydroxido units. The anion is an oxido-bridged species, [HOAl(hfip)2(μ-O)Al(hfip)3]2–, with one Al3+ cation tetrahedrally coordinated by an oxido (O2–) anion, a hydroxido anion, and two hfip groups, whereas the second Al3+ cation is coordinated by the oxido anion and three hfip groups.doi:10.1107/S24143146230071622023-09-08texthttps://creativecommons.org/licenses/by/4.0/Lozinšek, M.Pavčnik, T.Bitenc, J.IUCrData8https://creativecommons.org/licenses/by/4.0/2023-09-08med@iucr.orgSeptember 2023x2307162414-314692414-3146metal-organic compoundsμ-1,6-Dioxo-1,6-diphenylhexane-3,4-diolato-bis[(2,2′-bipyridine)chloridocopper(II)] dihydrate
http://scripts.iucr.org/cgi-bin/paper?tk4095
The reaction of CuCl2 with 1,6-diphenyl-1,3,5,6-hexanetetrone and 2,2′-bipyridine (bipy) in ethanol gave crystals of the corresponding bimetallic complex, [Cu2(C18H12O4)Cl2(C10H8N2)2]·2H2O. The molecule is centrosymmetric with each CuII ion coordinated to two oxygen atoms from the tetronediate, two nitrogen atoms from a bipy ligand and one coordinated chloride ion. A water molecule of crystallization forms hydrogen bonds to the chloride ions, linking the molecules into a chain parallel to the bc-face diagonal.The title complex sits astride an inversion center with each CuII atom having an N2O2Cl coordination sphere. Charge balance is achieved via the tetronediate and one coordinated chloride ion per CuII. Hydrogen bonding to a solvent water molecule links the molecules into a chain parallel to the bc-face diagonal.International Union of CrystallographyenCUII; HYDRATE; HYDROGEN-BONDING; TETRONEDIOATE; CRYSTAL STRUCTUREμ-1,6-Dioxo-1,6-diphenylhexane-3,4-diolato-bis[(2,2′-bipyridine)chloridocopper(II)] dihydrateurn:issn:2414-3146text/htmlThe reaction of CuCl2 with 1,6-diphenyl-1,3,5,6-hexanetetrone and 2,2′-bipyridine (bipy) in ethanol gave crystals of the corresponding bimetallic complex, [Cu2(C18H12O4)Cl2(C10H8N2)2]·2H2O. The molecule is centrosymmetric with each CuII ion coordinated to two oxygen atoms from the tetronediate, two nitrogen atoms from a bipy ligand and one coordinated chloride ion. A water molecule of crystallization forms hydrogen bonds to the chloride ions, linking the molecules into a chain parallel to the bc-face diagonal.doi:10.1107/S24143146230071372023-08-30texthttps://creativecommons.org/licenses/by/4.0/Nye, L.Telfer, S.G.Turnbull, M.M.IUCrData82023-08-30med@iucr.orghttps://creativecommons.org/licenses/by/4.0/x230713August 202382414-31462414-3146metal-organic compoundsDiethyl 2,2′-[({2-chloro-5-[(2-ethoxy-2-oxoethyl)(2-methylindolin-1-yl)carbamoyl]phenyl}sulfonyl)azanediyl]diacetate
http://scripts.iucr.org/cgi-bin/paper?tk4094
The majority of the title molecule, C28H34ClN3O9S, is disordered over two closely spaced sets of sites; the site occupancy of the major component = 0.542 (3). The conformation of each component is approximately U-shaped with the chlorobenzene ring forming the base and the indolinyl and sulfamoyl groups the sides; an intramolecular C—H⋯Cl hydrogen bond possibly contributes to the stabilization of the conformation. In the crystal, a corrugated layer structure parallel to the ab plane is formed by C—H⋯O and C—H⋯Cl hydrogen bonds together with C—H⋯π(ring) interactions.The majority of the title molecule is disordered over two closely spaced locations; the conformation is approximately U-shaped. In the crystal, chains of molecules extending along the a-axis direction are formed by C—H⋯O and C—H⋯Cl hydrogen bonds and are connected into a corrugated layer structure parallel to the ab plane by C—H⋯O hydrogen bonds and C—H⋯π(ring) interactions.International Union of CrystallographyenCRYSTAL STRUCTURE; HYDROGEN BOND; C-H...[PI](RING) INTERACTION; INDAPAMIDE; INDOLE; SULFAMATE ESTERDiethyl 2,2′-[({2-chloro-5-[(2-ethoxy-2-oxoethyl)(2-methylindolin-1-yl)carbamoyl]phenyl}sulfonyl)azanediyl]diacetateurn:issn:2414-3146text/htmlThe majority of the title molecule, C28H34ClN3O9S, is disordered over two closely spaced sets of sites; the site occupancy of the major component = 0.542 (3). The conformation of each component is approximately U-shaped with the chlorobenzene ring forming the base and the indolinyl and sulfamoyl groups the sides; an intramolecular C—H⋯Cl hydrogen bond possibly contributes to the stabilization of the conformation. In the crystal, a corrugated layer structure parallel to the ab plane is formed by C—H⋯O and C—H⋯Cl hydrogen bonds together with C—H⋯π(ring) interactions.doi:10.1107/S24143146230069952023-08-24texthttps://creativecommons.org/licenses/by/4.0/Ramli, Y.Al Garadi, W.El Hafi, M.Lhoussaine, E.Essassi, E.M.Alsubari, A.Mague, J.T.8med@iucr.org2023-08-24https://creativecommons.org/licenses/by/4.0/IUCrData2414-3146organic compoundsx230699August 202382414-3146Poly[[[μ3-3-(2-carboxylatophenyl)propionato][μ2-N,N′-(ethane-1,2-diyl)bis(pyridine-4-carboxamide)]copper(II)] monohydrate], a layered coordination polymer with (4,4) topology
http://scripts.iucr.org/cgi-bin/paper?bh4076
In the title compound, {[Cu(C10H8O4)(C14H14N4O2)]·H2O}n, the CuII cations are coordinated in a square-pyramidal fashion, with trans pyridyl-N donor atoms from two N-(2-(pyridin-3-ylamino)ethyl)isonicotinamide (pein) ligands in the basal plane. The other three coordination sites are taken up by carboxylate O-atom donors from three different 3-(2-carboxyphenyl)propionate (cpp) ligands. The central ethylenediamine segments of the pein ligands are disordered equally over two sets of positions. {Cu2O2} rhomboid clusters are connected into [Cu(cpp)(pein)]n (4,4) coordination polymer grids by the full span of the cpp and pein ligands. Individual layer motifs stack in an AAA pattern along the a axis by means of interlayer hydrogen-bonding interactions.A layered CuII coordination polymer with (4,4) topology was prepared by hydrothermal methods and structurally characterized by single-crystal X-ray diffraction.International Union of CrystallographyenCRYSTAL STRUCTURE; COORDINATION POLYMER; LAYER; COPPERPoly[[[μ3-3-(2-carboxylatophenyl)propionato][μ2-N,N′-(ethane-1,2-diyl)bis(pyridine-4-carboxamide)]copper(II)] monohydrate], a layered coordination polymer with (4,4) topologyurn:issn:2414-3146text/htmlIn the title compound, {[Cu(C10H8O4)(C14H14N4O2)]·H2O}n, the CuII cations are coordinated in a square-pyramidal fashion, with trans pyridyl-N donor atoms from two N-(2-(pyridin-3-ylamino)ethyl)isonicotinamide (pein) ligands in the basal plane. The other three coordination sites are taken up by carboxylate O-atom donors from three different 3-(2-carboxyphenyl)propionate (cpp) ligands. The central ethylenediamine segments of the pein ligands are disordered equally over two sets of positions. {Cu2O2} rhomboid clusters are connected into [Cu(cpp)(pein)]n (4,4) coordination polymer grids by the full span of the cpp and pein ligands. Individual layer motifs stack in an AAA pattern along the a axis by means of interlayer hydrogen-bonding interactions.doi:10.1107/S241431462300679X2023-08-10texthttps://creativecommons.org/licenses/by/4.0/Gaskin, G.J.LaDuca, R.L.IUCrDatahttps://creativecommons.org/licenses/by/4.0/2023-08-10med@iucr.org82414-31468August 2023x230679metal-organic compounds2414-31469-(4-Methoxyphenyl)-9H-carbazole
http://scripts.iucr.org/cgi-bin/paper?hb4441
In the title compound, C19H15NO, the dihedral angle between the benzene rings of the carbazole moiety is 1.73 (12)° and the methoxy-substituted phenyl ring deviates from the mean plane of the carbazole grouping (r.m.s. deviation = 0.020 Å) by 56.78 (8)°. In the crystal, weak C—H⋯π interactions link the molecules. The two-dimensional fingerprint plots derived from the Hirshfeld surface indicate that H⋯H (51.2%) and C⋯H/H⋯C (39.9%) contacts dominate the packing.In the title carbazole derivative, the dihedral angle between the carbazole ring system and the pendant phenyl ring is 56.78 (8)°.International Union of CrystallographyenCARBAZOLE; DIHEDRAL ANGLE; TORSION ANGLE; HIRSHFELD SURFACE ANALYSIS; CRYSTAL STRUCTURE9-(4-Methoxyphenyl)-9H-carbazoleurn:issn:2414-3146text/htmlIn the title compound, C19H15NO, the dihedral angle between the benzene rings of the carbazole moiety is 1.73 (12)° and the methoxy-substituted phenyl ring deviates from the mean plane of the carbazole grouping (r.m.s. deviation = 0.020 Å) by 56.78 (8)°. In the crystal, weak C—H⋯π interactions link the molecules. The two-dimensional fingerprint plots derived from the Hirshfeld surface indicate that H⋯H (51.2%) and C⋯H/H⋯C (39.9%) contacts dominate the packing.doi:10.1107/S24143146230067402023-08-10texthttps://creativecommons.org/licenses/by/4.0/Ganesan, P.Jasmine, N.J.Darious, R.S.Soundararajan, K.Rajalingam, R.IUCrDatahttps://creativecommons.org/licenses/by/4.0/2023-08-10med@iucr.org82414-31468August 2023x230674organic compounds2414-31462-[5-(2,3-Dimethoxynaphthalen-1-yl)-4,5-dihydro-1H-pyrazol-3-yl]-3-methoxyphenol
http://scripts.iucr.org/cgi-bin/paper?hb4442
In the title compound, C22H22N2O4, the central pyrazoline ring exhibits a nearly planar structure (r.m.s. deviation = 0.025 Å) despite having two sp3 carbon atoms. The pyrazoline ring subtends dihedral angles of 4.61 (1) and 87.31 (1)° with the pendant benzene ring and naphthalene ring system, respectively. The dihedral angle between the planes of the benzene ring and the naphthalene ring system is 89.76 (2)°. An intramolecular O—H⋯N hydrogen bond forms an S(6) ring motif. In the crystal, inversion dimers formed by pairwise weak N—H⋯N hydrogen bonds generate R22(4) loops and the dimers are linked by pairwise C—H⋯O hydrogen bonds [which generate R22(8) loops] into [100] chains.In the title compound, the central pyrazoline ring subtends dihedral angles of 4.61 (1) and 87.31 (1)° with the pendant benzene ring and naphthalene ring system, respectively. In the crystal, inversion dimers formed by pairwise weak N—H⋯N hydrogen bonds are linked by pairwise C—H⋯O hydrogen bonds into [100] chains.International Union of CrystallographyenCRYSTAL STRUCTURE; PYRAZOLINE; N-H...N HYDROGEN BONDS; INVERSION DIMERS2-[5-(2,3-Dimethoxynaphthalen-1-yl)-4,5-dihydro-1H-pyrazol-3-yl]-3-methoxyphenolurn:issn:2414-3146text/htmlIn the title compound, C22H22N2O4, the central pyrazoline ring exhibits a nearly planar structure (r.m.s. deviation = 0.025 Å) despite having two sp3 carbon atoms. The pyrazoline ring subtends dihedral angles of 4.61 (1) and 87.31 (1)° with the pendant benzene ring and naphthalene ring system, respectively. The dihedral angle between the planes of the benzene ring and the naphthalene ring system is 89.76 (2)°. An intramolecular O—H⋯N hydrogen bond forms an S(6) ring motif. In the crystal, inversion dimers formed by pairwise weak N—H⋯N hydrogen bonds generate R22(4) loops and the dimers are linked by pairwise C—H⋯O hydrogen bonds [which generate R22(8) loops] into [100] chains.doi:10.1107/S24143146230066852023-08-10texthttps://creativecommons.org/licenses/by/4.0/Sung, J.August 2023x2306682414-314682414-3146organic compoundsIUCrData8https://creativecommons.org/licenses/by/4.0/2023-08-10med@iucr.org6,8-Dichloro-3-(pyridin-2-yl)-2-[1-(pyridin-2-yl)ethyl]-1,2-dihydroquinoxaline
http://scripts.iucr.org/cgi-bin/paper?hb4436
The crystal structure of the racemic title compound, C20H16Cl2N4 is described, where the formation of a di-substituted 6,8-dichloro quinoxaline, containing two stereogenic centres, is confirmed.The synthesis and single-crystal X-ray structure of a substituted quinoxaline compound is described.International Union of CrystallographyenCRYSTAL STRUCTURE; QUINOXALINE DERIVATIVE; CHIRAL COMPOUND6,8-Dichloro-3-(pyridin-2-yl)-2-[1-(pyridin-2-yl)ethyl]-1,2-dihydroquinoxalineurn:issn:2414-3146text/htmlThe crystal structure of the racemic title compound, C20H16Cl2N4 is described, where the formation of a di-substituted 6,8-dichloro quinoxaline, containing two stereogenic centres, is confirmed.doi:10.1107/S241431462300665X2023-08-04texthttps://creativecommons.org/licenses/by/4.0/Malan, F.P.Mansour, A.M.Manicum, A.-L.E.https://creativecommons.org/licenses/by/4.0/2023-08-04med@iucr.org8IUCrDataorganic compounds2414-31462414-31468August 2023x230665Tetra-μ3-selenido-1:2:3κ3Se;1:2:4κ3Se;1:3:4κ3Se;2:3:4κ3Se-tetrakis[(η5-methylcyclopentadienyl)molybdenum(III)](6 Mo—Mo)
http://scripts.iucr.org/cgi-bin/paper?hb4439
The title cluster compound, [Mo4(η5-C5H4Me)4(μ3-Se)4], was synthesized from the reaction of [Mo(η5-C5H4Me)(CO)3]2 with grey selenium in refluxing xylene solution under a nitrogen atmosphere. The complete cluster is generated by a crystallographic twofold axis and contains an Mo4Se4 cubane-like core surrounded by four η5-methylcyclopentadienyl ligands. In the core, the four molybdenum atoms are connected to each other to form a tetrahedron, with a selenium atom capping each face. The Mo—Mo bond lengths vary from 2.9857 (5) to 3.0083 (3) Å and the Mo—Se separations range from 2.4633 (4) to 2.4693 (5) Å.The title cluster contains an Mo tetrahedron capped on each face with a μ3-selenide ligand.International Union of CrystallographyenCRYSTAL STRUCTURE; MOLYBDENUM CLUSTER; SELENIDE LIGANDTetra-μ3-selenido-1:2:3κ3Se;1:2:4κ3Se;1:3:4κ3Se;2:3:4κ3Se-tetrakis[(η5-methylcyclopentadienyl)molybdenum(III)](6 Mo—Mo)urn:issn:2414-3146text/htmlThe title cluster compound, [Mo4(η5-C5H4Me)4(μ3-Se)4], was synthesized from the reaction of [Mo(η5-C5H4Me)(CO)3]2 with grey selenium in refluxing xylene solution under a nitrogen atmosphere. The complete cluster is generated by a crystallographic twofold axis and contains an Mo4Se4 cubane-like core surrounded by four η5-methylcyclopentadienyl ligands. In the core, the four molybdenum atoms are connected to each other to form a tetrahedron, with a selenium atom capping each face. The Mo—Mo bond lengths vary from 2.9857 (5) to 3.0083 (3) Å and the Mo—Se separations range from 2.4633 (4) to 2.4693 (5) Å.doi:10.1107/S24143146230065702023-08-01texthttps://creativecommons.org/licenses/by/4.0/Ouchi, A.Takase, T.Inomata, S.IUCrDatamed@iucr.org2023-08-01https://creativecommons.org/licenses/by/4.0/882414-3146x230657August 2023metal-organic compounds2414-3146Poly[[aqua[μ2-1,3-bis(pyridin-4-yl)urea-κ2N4:N4′]bis(μ3-5-tert-butylisophthalato-κ3O1:O1′:O3)dizinc(II)] trihydrate], a double-strand coordination polymer
http://scripts.iucr.org/cgi-bin/paper?im4021
In the title compound, {[Zn2(C12H12O4)2(C11H10N4O)(H2O)]·3H2O}n, monoperiodic coordination polymer double strands are held into the triperiodic crystal structure by means of N—H⋯O hydrogen-bonding patterns between the amide groups of the 1,3-di(pyridin-4-yl)urea ligands and unligated O atoms belonging to 5-tert-butylisophthalate ligands. One of the Zn atoms displays a tetrahedral coordination environment, while the other Zn atom adopts a five-coordinate geometry intermediate between square pyramidal and trigonal bipyramidal. Additionally, O—H⋯O hydrogen-bonding patterns involving the water molecules of crystallization serve as a structure-stabilizing element by aggregating the double-strand motifs.A divalent zinc one-dimensional double-strand coordination polymer, [Zn2(tbuip)2(dpu)]n, was structurally characterized by single-crystal X-ray diffraction.International Union of CrystallographyenCRYSTAL STRUCTURE; DOUBLE-STRAND COORDINATION POLYMER; 1,3-DI(PYRIDIN-4-YL)UREA; 5-TERT-BUTYLISOPHTHALATE; ZINCPoly[[aqua[μ2-1,3-bis(pyridin-4-yl)urea-κ2N4:N4′]bis(μ3-5-tert-butylisophthalato-κ3O1:O1′:O3)dizinc(II)] trihydrate], a double-strand coordination polymerurn:issn:2414-3146text/htmlIn the title compound, {[Zn2(C12H12O4)2(C11H10N4O)(H2O)]·3H2O}n, monoperiodic coordination polymer double strands are held into the triperiodic crystal structure by means of N—H⋯O hydrogen-bonding patterns between the amide groups of the 1,3-di(pyridin-4-yl)urea ligands and unligated O atoms belonging to 5-tert-butylisophthalate ligands. One of the Zn atoms displays a tetrahedral coordination environment, while the other Zn atom adopts a five-coordinate geometry intermediate between square pyramidal and trigonal bipyramidal. Additionally, O—H⋯O hydrogen-bonding patterns involving the water molecules of crystallization serve as a structure-stabilizing element by aggregating the double-strand motifs.doi:10.1107/S24143146230065942023-08-04texthttps://creativecommons.org/licenses/by/4.0/Jia, J.LaDuca, R.L.8med@iucr.org2023-08-04https://creativecommons.org/licenses/by/4.0/IUCrData2414-3146metal-organic compoundsx230659August 202382414-3146Poly[bis[μ2-1,3-bis(pyridin-4-yl)urea-κ2N4:N4′]bis(μ2-5-methylisophthalato-κ2O1:O3)dizinc(II)], a parallel interpenetrated slab-like coordination polymer with {3.648}{326.728} 4,4-connected binodal topology
http://scripts.iucr.org/cgi-bin/paper?pk4042
In the title compound, [Zn2(C9H6O4)2(C11H10N4O)2]n, diperiodic coordination polymer slabs with {3.648}{326.728} 4,4-connected binodal topology are held into a parallel interpenetrated triperiodic crystal structure by means of N—H⋯O hydrogen-bonding patterns.A divalent zinc one-dimensional ribbon coordination polymer, [Zn2(tbuip)2(bpu)]n, was structurally characterized by single-crystal X-ray diffraction.International Union of CrystallographyenCRYSTAL STRUCTURE; COORDINATION POLYMER; {3.648}{326.728} 4,4-CONNECTED BINODAL TOPOLOGYPoly[bis[μ2-1,3-bis(pyridin-4-yl)urea-κ2N4:N4′]bis(μ2-5-methylisophthalato-κ2O1:O3)dizinc(II)], a parallel interpenetrated slab-like coordination polymer with {3.648}{326.728} 4,4-connected binodal topologyurn:issn:2414-3146text/htmlIn the title compound, [Zn2(C9H6O4)2(C11H10N4O)2]n, diperiodic coordination polymer slabs with {3.648}{326.728} 4,4-connected binodal topology are held into a parallel interpenetrated triperiodic crystal structure by means of N—H⋯O hydrogen-bonding patterns.doi:10.1107/S24143146230066002023-08-04texthttps://creativecommons.org/licenses/by/4.0/Jia, J.LaDuca, R.L.x230660August 202382414-31462414-3146metal-organic compoundsIUCrData82023-08-04med@iucr.orghttps://creativecommons.org/licenses/by/4.0/M-type Gd2[Si2O7]
http://scripts.iucr.org/cgi-bin/paper?wm4193
The title compound, digadolinium(III) oxidodisilicate, Gd2[Si2O7], was obtained in its M-type crystal structure after attempts to synthesize Gd5Br3[AsO3]4 as a by-product from fused silica ampoules. It crystallizes isotypically with M-type Eu2[Si2O7]. This structure consists of layers of ecliptically arranged oxidodisilicate [Si2O7]6− units separated from each other by bilayers consisting of GdIII cations.M-type Gd2[Si2O7] crystallizes isotypically with Eu2[Si2O7].International Union of CrystallographyenCRYSTAL STRUCTURE; OXIDODISILICATE; RARE-EARTH METAL; GADOLINIUM; ISOTYPISMM-type Gd2[Si2O7]urn:issn:2414-3146text/htmlThe title compound, digadolinium(III) oxidodisilicate, Gd2[Si2O7], was obtained in its M-type crystal structure after attempts to synthesize Gd5Br3[AsO3]4 as a by-product from fused silica ampoules. It crystallizes isotypically with M-type Eu2[Si2O7]. This structure consists of layers of ecliptically arranged oxidodisilicate [Si2O7]6− units separated from each other by bilayers consisting of GdIII cations.doi:10.1107/S24143146230065452023-08-01texthttps://creativecommons.org/licenses/by/4.0/Locke, R.J.C.Schleid, T.IUCrData8https://creativecommons.org/licenses/by/4.0/2023-08-01med@iucr.orgAugust 2023x2306542414-314682414-3146inorganic compoundsPoly[[(μ-aqua)[μ4-4-(carboxylatomethyl)benzoato]cobalt(II)] hemi[1,4-bis(pyridin-4-ylmethyl)piperazine] hemihydrate]
http://scripts.iucr.org/cgi-bin/paper?bt4140
In the title compound, {[Co(C9H6O4)(H2O)]·0.5C16H20N4·0.5H2O}n, two-dimensional coordination polymer slabs are held together in the three-dimensional crystal structure by means of O—H⋯N hydrogen bonding between bound water molecules and pyridyl N atoms of cocrystallized 1,4-bis(pyridin-4-ylmethyl)piperazine molecules.A divalent cobalt two-dimensional slab coordination polymer with cocrystallized species, {[Co(cmb)(H2O)].0.5(bpmp)·0.5H2O}n (where cmb is 4-(carboxylatomethyl)benzoate and bpmp is 1,4-bis(pyridin-4-ylmethyl)piperazine, was structurally characterized by single-crystal X-ray diffraction.International Union of CrystallographyenCRYSTAL STRUCTURE; COORDINATION POLYMER; PIPERAZINE; COBALTPoly[[(μ-aqua)[μ4-4-(carboxylatomethyl)benzoato]cobalt(II)] hemi[1,4-bis(pyridin-4-ylmethyl)piperazine] hemihydrate]urn:issn:2414-3146text/htmlIn the title compound, {[Co(C9H6O4)(H2O)]·0.5C16H20N4·0.5H2O}n, two-dimensional coordination polymer slabs are held together in the three-dimensional crystal structure by means of O—H⋯N hydrogen bonding between bound water molecules and pyridyl N atoms of cocrystallized 1,4-bis(pyridin-4-ylmethyl)piperazine molecules.doi:10.1107/S241431462300648X2023-07-28texthttps://creativecommons.org/licenses/by/4.0/Gaskin, G.J.LaDuca, R.L.x230648July 202372414-31462414-3146metal-organic compoundsIUCrData82023-07-28med@iucr.orghttps://creativecommons.org/licenses/by/4.0/5,6-Dihydro-1,4-dithiine-2,3-dicarboxylic anhydride
http://scripts.iucr.org/cgi-bin/paper?hb4438
In the title compound (systematic name: 2,3-dihydro-1,4-dithiino[2,3-c]furan-5,7-dione), C6H4O3S2, the observed geometry agrees well with those of its phthalamide, thieno and hydroxy analogs, and with a calculated geometry obtained by density functional theory (DFT) calculations. Specific structural features are an S—C—C—S torsion angle of −70.39 (17)° and S—C bonds to sp2-hybridized C atoms approximately 0.1 Å shorter than those to sp3-hybridized C atoms. Unlike the extended structures of the analogs, there are no directed intermolecular interactions and the head-to-tail rows of molecules that are a prominent structural motif of the packing can be rationalized in terms of optimized dipole–dipole interactions.The heterocyclic fused ring geometry of the title compound coincides with the geometries of related molecules but without directed intermolecular contacts determining the crystal packing.International Union of CrystallographyenCRYSTAL STRUCTURE; FUSED RING; HETEROCYCLE; DITHIINE; ANHYDRIDE5,6-Dihydro-1,4-dithiine-2,3-dicarboxylic anhydrideurn:issn:2414-3146text/htmlIn the title compound (systematic name: 2,3-dihydro-1,4-dithiino[2,3-c]furan-5,7-dione), C6H4O3S2, the observed geometry agrees well with those of its phthalamide, thieno and hydroxy analogs, and with a calculated geometry obtained by density functional theory (DFT) calculations. Specific structural features are an S—C—C—S torsion angle of −70.39 (17)° and S—C bonds to sp2-hybridized C atoms approximately 0.1 Å shorter than those to sp3-hybridized C atoms. Unlike the extended structures of the analogs, there are no directed intermolecular interactions and the head-to-tail rows of molecules that are a prominent structural motif of the packing can be rationalized in terms of optimized dipole–dipole interactions.doi:10.1107/S24143146230064782023-08-04texthttps://creativecommons.org/licenses/by/4.0/Bullock, O.Rice, S.Bond, M.R.August 2023x2306472414-314682414-3146organic compoundsIUCrData8https://creativecommons.org/licenses/by/4.0/2023-08-04med@iucr.orgN-(5-Cyanononan-5-yl)benzamide
http://scripts.iucr.org/cgi-bin/paper?bv4049
N-(5-Cyanononan-5-yl)benzamide, C17H24N2O, synthesized from the reaction between benzoyl chloride and 2-amino-2-butylhexanenitrile, is an important intermediate in amino acid synthesis. Intermolecular N—H⋯O and C—H⋯O hydrogen bonds with N⋯O and C⋯O distances of 3.083 (2) and 3.304 (2) Å, respectively, link adjacent molecules into chains along the a axis. The dihedral angle between the mean plane of the phenyl group and the plane of the amide group is 19.504 (4)°.The title compound crystallizes in the orthorhombic space group Pbca with eight formula units per unit cell. The N—H group forms an intermolecular N—H⋯O hydrogen bond to the amide carbonyl O atom, generating chains.International Union of CrystallographyenCRYSTAL STRUCTURE; HYDROGEN BONDING; STRECKER REACTION; AMINO ACID SYNTHESISN-(5-Cyanononan-5-yl)benzamideurn:issn:2414-3146text/htmlN-(5-Cyanononan-5-yl)benzamide, C17H24N2O, synthesized from the reaction between benzoyl chloride and 2-amino-2-butylhexanenitrile, is an important intermediate in amino acid synthesis. Intermolecular N—H⋯O and C—H⋯O hydrogen bonds with N⋯O and C⋯O distances of 3.083 (2) and 3.304 (2) Å, respectively, link adjacent molecules into chains along the a axis. The dihedral angle between the mean plane of the phenyl group and the plane of the amide group is 19.504 (4)°.doi:10.1107/S24143146230063992023-07-28texthttps://creativecommons.org/licenses/by/4.0/Song, X.Li, W.x230639July 202372414-31462414-3146organic compoundsIUCrData8med@iucr.org2023-07-28https://creativecommons.org/licenses/by/4.0/Tetrel bond in the triphenyltin(IV) chloride–cyclohexyldiphenylphosphane oxide (1/1) cocrystal
http://scripts.iucr.org/cgi-bin/paper?bv4048
The single-crystal X-ray diffraction structure of the title compound, [SnCl(C6H5)3]·C18H21OP, is reported. The 1:1 cocrystal features a short and directional tetrel bond between tin and oxygen. The tin–oxygen distance is 2.346 (4) Å, representing 62% of the sum of the van der Waals radii of Sn and O. The Cl—Sn⋯O angle is 174.0 (1)° and this nearly linear arrangement is consistent with a tetrel bond formed via a σ-hole opposite the tin–chlorine covalent bond. Some weak C—H⋯Cl interactions are noted between adjacent molecules.A short and directional tetrel bond between tin and oxygen is identified in the title compound.International Union of CrystallographyenCRYSTAL STRUCTURE; TETREL BOND; NONCOVALENT INTERACTION; COCRYSTALTetrel bond in the triphenyltin(IV) chloride–cyclohexyldiphenylphosphane oxide (1/1) cocrystalurn:issn:2414-3146text/htmlThe single-crystal X-ray diffraction structure of the title compound, [SnCl(C6H5)3]·C18H21OP, is reported. The 1:1 cocrystal features a short and directional tetrel bond between tin and oxygen. The tin–oxygen distance is 2.346 (4) Å, representing 62% of the sum of the van der Waals radii of Sn and O. The Cl—Sn⋯O angle is 174.0 (1)° and this nearly linear arrangement is consistent with a tetrel bond formed via a σ-hole opposite the tin–chlorine covalent bond. Some weak C—H⋯Cl interactions are noted between adjacent molecules.doi:10.1107/S24143146230063752023-08-01texthttps://creativecommons.org/licenses/by/4.0/Liyanage, S.Ovens, J.S.Bryce, D.L.x230637August 202382414-31462414-3146metal-organic compoundsIUCrData8med@iucr.org2023-08-01https://creativecommons.org/licenses/by/4.0/Methyl 4-amino-3-methoxyisoxazole-5-carboxylate
http://scripts.iucr.org/cgi-bin/paper?hb4437
The title compound, C6H8N2O4, a new derivative of isoxazole, has been synthesized and structurally characterized. The crystal structure shows the molecule to be almost planar (r.m.s. deviation for the non-hydrogen atoms = 0.029 Å), this conformation being supported by an intramolecular N—H⋯O hydrogen bond. In the extended structure, the molecules are linked by N—H⋯O hydrogen bonds into chains propagating along [010].The crystal structure of the title compound obtained from the reduction of its nitro precursor, methyl 3-methoxy-4-nitroisoxazole-5-carboxylate, is described.International Union of CrystallographyenCRYSTAL STRUCTURE; ISOXAZOLE; HYDROGEN-BONDED CHAINMethyl 4-amino-3-methoxyisoxazole-5-carboxylateurn:issn:2414-3146text/htmlThe title compound, C6H8N2O4, a new derivative of isoxazole, has been synthesized and structurally characterized. The crystal structure shows the molecule to be almost planar (r.m.s. deviation for the non-hydrogen atoms = 0.029 Å), this conformation being supported by an intramolecular N—H⋯O hydrogen bond. In the extended structure, the molecules are linked by N—H⋯O hydrogen bonds into chains propagating along [010].doi:10.1107/S24143146230062352023-08-01texthttps://creativecommons.org/licenses/by/4.0/Abdul Manan, M.A.F.Cordes, D.B.Slawin, A.M.Z.med@iucr.org2023-08-01https://creativecommons.org/licenses/by/4.0/8IUCrDataorganic compounds2414-314682414-3146x230623August 2023Poly[[bis[μ4-3-(2-carboxylatophenyl)propionato]{N-[2-(pyridine-3-amido)ethyl]nicotinamide}dicopper(II)] pentahydrate]
http://scripts.iucr.org/cgi-bin/paper?zl4055
In the title compound, {[Cu2(C10H8O4)2(C14H14N4O2)]·5H2O}n, the CuII cations are coordinated in a square-pyramidal fashion, with four 3-(2-carboxyphenyl)propionate (cpp) carboxylate O-atom donors in the basal plane, along with an N-atom donor from a N-[2-(pyridin-3-ylamino)ethyl]nicotinamide (pen) ligand in the apical position. [Cu2(cpp)2]n coordination polymer layer motifs with embedded {Cu2(OCO)4} paddlewheel clusters are thereby constructed. These layer motifs are connected into a three-dimensional [Cu2(cpp)2(pen)]n coordination polymer network by tethering pen ligands. Treating the {Cu2(OCO)4 paddelwheel clusters as 6-connected nodes reveals an underlying cross-pillared self-penetrated rob network with 48668 topology. The water molecules of crystallization are held to the coordination polymer network by N—H⋯O and O—H⋯O hydrogen-bonding patterns.A divalent copper three-dimensional self-penetrated coordination polymer with rob topology, {[Cu2(3-(2-carboxyphenyl)propionate)2(ethylenediamine(bis(nicotinamide)] .5H2O}n, was structurally characterized by single-crystal X-ray diffraction.International Union of CrystallographyenCRYSTAL STRUCTURE; COPPER(II); SELF-PENETRATION; COORDINATION POLYMERPoly[[bis[μ4-3-(2-carboxylatophenyl)propionato]{N-[2-(pyridine-3-amido)ethyl]nicotinamide}dicopper(II)] pentahydrate]urn:issn:2414-3146text/htmlIn the title compound, {[Cu2(C10H8O4)2(C14H14N4O2)]·5H2O}n, the CuII cations are coordinated in a square-pyramidal fashion, with four 3-(2-carboxyphenyl)propionate (cpp) carboxylate O-atom donors in the basal plane, along with an N-atom donor from a N-[2-(pyridin-3-ylamino)ethyl]nicotinamide (pen) ligand in the apical position. [Cu2(cpp)2]n coordination polymer layer motifs with embedded {Cu2(OCO)4} paddlewheel clusters are thereby constructed. These layer motifs are connected into a three-dimensional [Cu2(cpp)2(pen)]n coordination polymer network by tethering pen ligands. Treating the {Cu2(OCO)4 paddelwheel clusters as 6-connected nodes reveals an underlying cross-pillared self-penetrated rob network with 48668 topology. The water molecules of crystallization are held to the coordination polymer network by N—H⋯O and O—H⋯O hydrogen-bonding patterns.doi:10.1107/S24143146230062232023-07-22texthttps://creativecommons.org/licenses/by/4.0/Gaskin, G.J.LaDuca, R.L.IUCrDatahttps://creativecommons.org/licenses/by/4.0/2023-07-22med@iucr.org82414-31467July 2023x230622metal-organic compounds2414-31464,6-Diferrocenyl-5-(morpholin-4-yl)-1,2,3-triazine
http://scripts.iucr.org/cgi-bin/paper?bh4075
The structure of the title Fe complex, [Fe(C5H5)2(C17H16N4O)], was determined at 130 K, and has orthorhombic (Pna21) symmetry. It is of interest with respect to the class of triazine heterocyclic compounds: the triazine ring is substituted by two ferrocenyl and one morpholine groups. The crystal structure features C—H⋯O and C—H⋯N non-classical hydrogen bonds.The title complex crystallizes with two independent molecules in the asymmetric unit of the orthorhombic unit cell. The crystal structure features C—H⋯O and C—H⋯N non-classical hydrogen bonds.International Union of CrystallographyenCRYSTAL STRUCTURE; MORPHOLINE; FERROCENYL; TRIAZINE4,6-Diferrocenyl-5-(morpholin-4-yl)-1,2,3-triazineurn:issn:2414-3146text/htmlThe structure of the title Fe complex, [Fe(C5H5)2(C17H16N4O)], was determined at 130 K, and has orthorhombic (Pna21) symmetry. It is of interest with respect to the class of triazine heterocyclic compounds: the triazine ring is substituted by two ferrocenyl and one morpholine groups. The crystal structure features C—H⋯O and C—H⋯N non-classical hydrogen bonds.doi:10.1107/S24143146230061682023-08-01texthttps://creativecommons.org/licenses/by/4.0/Aguilar-Lugo, C.Flores-Alamo, M.Sánchez García, J.J.Klimova, E.I.IUCrDatahttps://creativecommons.org/licenses/by/4.0/2023-08-01med@iucr.org82414-31468August 2023x230616metal-organic compounds2414-3146Bis(tetrabutylammonium) tetrachloridomanganate(II) dichloromethane disolvate
http://scripts.iucr.org/cgi-bin/paper?wm4191
The title compound, (C16H36N)2[MnCl4]·2CH2Cl2, is an ionic organic–inorganic hybride compound consisting of a tetrabutylammonium cation and a tetrachloridomanganate(II) anion in a 2:1 stoichiometric ratio. The cation contains a central nitrogen atom bonded to four n-butyl groups in a tetrahedral arrangement, while the anion contains a central MnII atom tetrahedrally coordinated by four chlorido ligands. It co-crystallized with two equivalents of dichloromethane solvent, CH2Cl2, to give the following empirical formula: [(C4H9)4N]2[MnCl4]·(CH2Cl2)2. The crystal structure is mainly stabilized by Coulombic interactions.The ionic title compound consists of a 2:1 ratio of the tetrabutylammonium cation (1+) and the tetrachloridomanganate(II) anion (2–). The structure reported contains two dichloromethane solvent molecules co-crystallized per anion.International Union of CrystallographyenCRYSTAL STRUCTURE; ORGANIC-INORGANIC SALT; MANGANESE(II) COMPLEX; TETRABUTYLAMMONIUM SALT; SOLVATEBis(tetrabutylammonium) tetrachloridomanganate(II) dichloromethane disolvateurn:issn:2414-3146text/htmlThe title compound, (C16H36N)2[MnCl4]·2CH2Cl2, is an ionic organic–inorganic hybride compound consisting of a tetrabutylammonium cation and a tetrachloridomanganate(II) anion in a 2:1 stoichiometric ratio. The cation contains a central nitrogen atom bonded to four n-butyl groups in a tetrahedral arrangement, while the anion contains a central MnII atom tetrahedrally coordinated by four chlorido ligands. It co-crystallized with two equivalents of dichloromethane solvent, CH2Cl2, to give the following empirical formula: [(C4H9)4N]2[MnCl4]·(CH2Cl2)2. The crystal structure is mainly stabilized by Coulombic interactions.doi:10.1107/S24143146230061072023-07-14texthttps://creativecommons.org/licenses/by/4.0/Hay, M.T.Yennawar, H.P.72414-3146x230610July 2023metal-organic compounds2414-3146IUCrDatamed@iucr.org2023-07-14https://creativecommons.org/licenses/by/4.0/84-(3-Chloroanilino)benzoic acid
http://scripts.iucr.org/cgi-bin/paper?bt4139
The title compound, C13H10ClNO2, was synthesized by a Buchwald–Hartwig reaction and its crystal structure was investigated for the first time. Crystallization in a variety of solvents led to the discovery of one crystal form. High-quality single crystals were obtained by slow evaporation and the crystal structure was determined by single-crystal X-ray diffraction. The molecules in the crystal structures are highly twisted [the dihedral angle between the aromatic rings is 34.66 (6)°] and pair up to form acid–acid dimers.High quality crystals of 4-(3-chloroanilino)benzoic acid were grown in acetonitrile and its crystal structure was determined by single-crystal X-ray diffraction.International Union of CrystallographyenCRYSTAL STRUCTURE; 4-(3-CHLOROANILINO)BENZOIC ACID; ACID-ACID DIMERS4-(3-Chloroanilino)benzoic acidurn:issn:2414-3146text/htmlThe title compound, C13H10ClNO2, was synthesized by a Buchwald–Hartwig reaction and its crystal structure was investigated for the first time. Crystallization in a variety of solvents led to the discovery of one crystal form. High-quality single crystals were obtained by slow evaporation and the crystal structure was determined by single-crystal X-ray diffraction. The molecules in the crystal structures are highly twisted [the dihedral angle between the aromatic rings is 34.66 (6)°] and pair up to form acid–acid dimers.doi:10.1107/S24143146230059892023-07-14texthttps://creativecommons.org/licenses/by/4.0/Liu, X.Long, S.organic compounds2414-314672414-3146x230598July 2023med@iucr.org2023-07-14https://creativecommons.org/licenses/by/4.0/8IUCrData4-Methyl-2-(2-methylanilino)benzoic acid
http://scripts.iucr.org/cgi-bin/paper?bv4047
The title compound, C15H15NO2, was obtained by the reaction of 2-chloro-4-methyl-benzoic acid and o-toluidine using 2-ethoxyethanol as solvent. Crystals of the title compounds were obtained from crystallization in acetone. The molecule in the crystal is twisted with a dihedral angle between the aromatic rings of 50.86 (5)°. In the crystal structure, the molecules associate to form acid–acid hydrogen-bonded dimers linked by pairwise O—H⋯O hydrogen bonds.Single crystals of 4-methyl-2-(o-tolylamino)benzoic acid were obtained from slow evaporation of an acetone solution. The molecule is highly twisted with a dihedral angle between the aromatic rings of 50.86 (5)°. In the crystal structure, the molecules associate to form acid–acid dimers.International Union of CrystallographyenCRYSTAL STRUCTURE; TWISTED CONFORMATION; ACID-ACID DIMER4-Methyl-2-(2-methylanilino)benzoic acidurn:issn:2414-3146text/htmlThe title compound, C15H15NO2, was obtained by the reaction of 2-chloro-4-methyl-benzoic acid and o-toluidine using 2-ethoxyethanol as solvent. Crystals of the title compounds were obtained from crystallization in acetone. The molecule in the crystal is twisted with a dihedral angle between the aromatic rings of 50.86 (5)°. In the crystal structure, the molecules associate to form acid–acid hydrogen-bonded dimers linked by pairwise O—H⋯O hydrogen bonds.doi:10.1107/S24143146230059902023-07-14texthttps://creativecommons.org/licenses/by/4.0/Liu, C.Long, S.82023-07-14med@iucr.orghttps://creativecommons.org/licenses/by/4.0/IUCrData2414-3146organic compoundsx230599July 202372414-31463-Methyl-2-(4-methylphenoxy)benzoic acid
http://scripts.iucr.org/cgi-bin/paper?hb4431
In the title compound, C15H14O3, the dihedral angle between the aromatic rings is 86.7 (9)°. In the crystal, carboxylic acid inversion dimers linked by pairwise O—H⋯O hydrogen bonds are formed.The title compound features carboxylic acid inversion dimers in its extended structure.International Union of CrystallographyenCRYSTAL STRUCTURE; CARBOXYLIC ACID INVERSION DIMER3-Methyl-2-(4-methylphenoxy)benzoic acidurn:issn:2414-3146text/htmlIn the title compound, C15H14O3, the dihedral angle between the aromatic rings is 86.7 (9)°. In the crystal, carboxylic acid inversion dimers linked by pairwise O—H⋯O hydrogen bonds are formed.doi:10.1107/S24143146230060042023-07-14texthttps://creativecommons.org/licenses/by/4.0/Lu, K.Long, S.72414-3146x230600July 2023organic compounds2414-3146IUCrData2023-07-14med@iucr.orghttps://creativecommons.org/licenses/by/4.0/84-Oxo-N-phenyl-1,4-dihydropyridine-3-carboxamide
http://scripts.iucr.org/cgi-bin/paper?im4020
The title compound, C12H10N2O2, shows a nearly planar conformation. The crystal structure is sustained by hydrogen bonds between the NH and the carbonyl O function of the 4-oxo-1,4-dihydropyridine ring of the molecules, forming infinite chains along the b-axis direction.Single crystals of 4-oxo-N-phenyl-1,4-dihydropyridine-3-carboxamide were obtained by slow evaporation of a solution of the title compound in acetone. The crystal structure is sustained by hydrogen bonds between the NH and the carbonyl O function of the 4-oxo-1,4-dihydropyridine ring of the molecules, forming infinite chains along the b-axis direction.International Union of CrystallographyenCRYSTAL STRUCTURE; HYDROGEN BONDING4-Oxo-N-phenyl-1,4-dihydropyridine-3-carboxamideurn:issn:2414-3146text/htmlThe title compound, C12H10N2O2, shows a nearly planar conformation. The crystal structure is sustained by hydrogen bonds between the NH and the carbonyl O function of the 4-oxo-1,4-dihydropyridine ring of the molecules, forming infinite chains along the b-axis direction.doi:10.1107/S24143146230060162023-07-14texthttps://creativecommons.org/licenses/by/4.0/Shu, X.Long, S.IUCrData8med@iucr.org2023-07-14https://creativecommons.org/licenses/by/4.0/x230601July 202372414-31462414-3146organic compoundsN-(3-Chloro-2-methylphenyl)-6-oxo-1,6-dihydropyridine-3-carboxamide
http://scripts.iucr.org/cgi-bin/paper?vm4061
In the crystal structure of the title compound, C13H11ClN2O2, the molecules form a three-dimensional network based on two types of hydrogen bonds between NH groups and the carbonyl oxygen atoms and amides. The molecule is highly twisted, as evidenced by the dihedral angle between the 6-oxo-1,6-dihydropyridine and benzene rings [88.1 (2)°].The title compound was synthesized with 6-oxo-1,6-dihydropyridine-3-carboxylic acid and 3-chloro-2-methylaniline as starting materials. The crystal packing is characterized by two types of N—H⋯O hydrogen bonds.International Union of CrystallographyenCRYSTAL STRUCTURE; 6-OXO-1,6-DIHYDROPYRIDINE; N-H...O HYDROGEN BONDSN-(3-Chloro-2-methylphenyl)-6-oxo-1,6-dihydropyridine-3-carboxamideurn:issn:2414-3146text/htmlIn the crystal structure of the title compound, C13H11ClN2O2, the molecules form a three-dimensional network based on two types of hydrogen bonds between NH groups and the carbonyl oxygen atoms and amides. The molecule is highly twisted, as evidenced by the dihedral angle between the 6-oxo-1,6-dihydropyridine and benzene rings [88.1 (2)°].doi:10.1107/S24143146230060282023-07-14texthttps://creativecommons.org/licenses/by/4.0/Tian, G.Long, S.https://creativecommons.org/licenses/by/4.0/2023-07-14med@iucr.org8IUCrDataorganic compounds2414-31462414-31467July 2023x230602N-(2,6-Dichlorophenyl)-2-oxo-1,2-dihydropyridine-3-carboxamide
http://scripts.iucr.org/cgi-bin/paper?wm4188
Crystals of the title compound, C12H8Cl2N2O2, were obtained by slow evaporation of an ethanolic solution. An intramolecular amideN—H⋯O=Clactam hydrogen bond is observed. In the crystal, two molecules pair up to form a centrosymmetric lactam–lactam dimers (LLD) by N—H⋯O=C hydrogen bonds, whereas the O=Camide group of the molecule does not participate in hydrogen bonding.The title molecule has a highly twisted conformation with the two aromatic rings being almost perpendicular to each other. Through mutual N—H⋯O hydrogen bonds, the molecules form centrosymmetric lactam–lactam dimers in the crystal.International Union of CrystallographyenCRYSTAL STRUCTURE; HIGHLY TWISTED CONFORMATION; LACTAM-LACTAM DIMER; N-H...O HYDROGEN BONDSN-(2,6-Dichlorophenyl)-2-oxo-1,2-dihydropyridine-3-carboxamideurn:issn:2414-3146text/htmlCrystals of the title compound, C12H8Cl2N2O2, were obtained by slow evaporation of an ethanolic solution. An intramolecular amideN—H⋯O=Clactam hydrogen bond is observed. In the crystal, two molecules pair up to form a centrosymmetric lactam–lactam dimers (LLD) by N—H⋯O=C hydrogen bonds, whereas the O=Camide group of the molecule does not participate in hydrogen bonding.doi:10.1107/S241431462300603X2023-07-14texthttps://creativecommons.org/licenses/by/4.0/Tu, N.Long, S.IUCrData8https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-07-14July 2023x2306032414-314672414-3146organic compoundsH-type Ce2[Si2O7]
http://scripts.iucr.org/cgi-bin/paper?wm4192
The title compound, dicerium(III) oxidodisilicate, Ce2[Si2O7], was obtained as a by-product in its H-type structure after attempts to synthesize CeSb2O4Cl from fused silica ampoules. It crystallizes isotypically with H-La2[Si2O7]. The four crystallographically distinct CeIII cations form distorted square antiprisms, capped square antiprisms, and bicapped square antiprisms as coordination polyhedra consisting of oxygen atoms. Four crystallographically different silicon atoms recruit the centers of two different isolated [Si2O7]6– units.Ce2[Si2O7] was obtained in its H-type structure and crystallizes isotypically with H-La2[Si2O7].International Union of CrystallographyenCRYSTAL STRUCTURE; OXIDODISILICATE; RARE-EARTH METAL; CERIUM; ISOTYPISMH-type Ce2[Si2O7]urn:issn:2414-3146text/htmlThe title compound, dicerium(III) oxidodisilicate, Ce2[Si2O7], was obtained as a by-product in its H-type structure after attempts to synthesize CeSb2O4Cl from fused silica ampoules. It crystallizes isotypically with H-La2[Si2O7]. The four crystallographically distinct CeIII cations form distorted square antiprisms, capped square antiprisms, and bicapped square antiprisms as coordination polyhedra consisting of oxygen atoms. Four crystallographically different silicon atoms recruit the centers of two different isolated [Si2O7]6– units.doi:10.1107/S24143146230059162023-07-07texthttps://creativecommons.org/licenses/by/4.0/Locke, R.J.C.Weis, M.Schleid, T.inorganic compounds2414-314672414-3146x230591July 2023med@iucr.org2023-07-07https://creativecommons.org/licenses/by/4.0/8IUCrData5-Fluoro-3-(1H-indol-3-ylmethyl)-1H-indole
http://scripts.iucr.org/cgi-bin/paper?xu4049
The title compound, C17H13FN2, was synthesized as a potential ligand for the construction of metal–organic frameworks. The two indole motifs present two potential coordination modes. It crystallizes in the orthorhombic system with space group P212121. The dihedral angle between the fused ring systems is 68.77 (10)°. Weak F⋯H interactions are observed in the crystal.The title compound was synthesized as a potential ligand for the construction of metal–organic frameworks. The two indole motifs present two potential coordination modes. Weak F⋯H interactions are observed in the crystal.International Union of CrystallographyenCRYSTAL STRUCTURE5-Fluoro-3-(1H-indol-3-ylmethyl)-1H-indoleurn:issn:2414-3146text/htmlThe title compound, C17H13FN2, was synthesized as a potential ligand for the construction of metal–organic frameworks. The two indole motifs present two potential coordination modes. It crystallizes in the orthorhombic system with space group P212121. The dihedral angle between the fused ring systems is 68.77 (10)°. Weak F⋯H interactions are observed in the crystal.doi:10.1107/S24143146230059042023-08-04texthttps://creativecommons.org/licenses/by/4.0/Guo, G.IUCrDatahttps://creativecommons.org/licenses/by/4.0/med@iucr.org2023-08-0482414-31468August 2023x230590organic compounds2414-31461-[1,4-Bis(but-3-en-1-yloxy)]-2,3,4,5-(1,4-dimethoxy)pillar[5]arene–1,4-dibromobutane 1:1 inclusion complex
http://scripts.iucr.org/cgi-bin/paper?xu4051
In the title compound, C51H58O10·C4H8Br2, both the host and guest are completed by crystallographic twofold symmetry (one carbon atom of the host lies on the rotation axis). The pentagonal-shaped macrocycle has a pair of buteneoxy substituents on one of its faces and one molecule of 1,4-dibromobutane is encapsulated within the cavity of the pillararene, forming a 1:1 inclusion complex. The terminal alkene parts, which project outwards from the pillararene ring, exhibit positional disorder over two sets of sites in a 0.52 (2): 0.48 (2) ratio. The host and guest interact via C—H⋯O, C—H⋯Br and C—H⋯π interactions and adjacent host molecules interact via C—H⋯O and C—H⋯π bonds.In the title compound, both the host and guest are completed by crystallographic twofold symmetry (one carbon atom of the host lies on the rotation axis). The pentagonal-shaped macrocycle has a pair of buteneoxy substituents on one of its faces and one molecule of 1,4-dibromobutane is encapsulated within the cavity of the pillararene, forming a 1:1 inclusion complex.International Union of CrystallographyenCRYSTAL STRUCTURE; A1/A2-DIBUTENOXY PILLAR[5]ARENE; DIBROMOBUTANE; HOST-GUEST SYSTEM1-[1,4-Bis(but-3-en-1-yloxy)]-2,3,4,5-(1,4-dimethoxy)pillar[5]arene–1,4-dibromobutane 1:1 inclusion complexurn:issn:2414-3146text/htmlIn the title compound, C51H58O10·C4H8Br2, both the host and guest are completed by crystallographic twofold symmetry (one carbon atom of the host lies on the rotation axis). The pentagonal-shaped macrocycle has a pair of buteneoxy substituents on one of its faces and one molecule of 1,4-dibromobutane is encapsulated within the cavity of the pillararene, forming a 1:1 inclusion complex. The terminal alkene parts, which project outwards from the pillararene ring, exhibit positional disorder over two sets of sites in a 0.52 (2): 0.48 (2) ratio. The host and guest interact via C—H⋯O, C—H⋯Br and C—H⋯π interactions and adjacent host molecules interact via C—H⋯O and C—H⋯π bonds.doi:10.1107/S24143146230058862023-07-14texthttps://creativecommons.org/licenses/by/4.0/Vinodh, M.Al-Azemi, T.F.2414-3146organic compoundsJuly 2023x2305882414-314678https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-07-14IUCrDataN-(4-Ethoxyphenyl)-3-oxobutanamide
http://scripts.iucr.org/cgi-bin/paper?hb4435
The title compound, C12H15NO3, crystallizes with Z′ = 2 in space group Pca21 with the two independent molecules having almost the same conformation, differing mostly at the end of the butanamide chain. A local inversion center near 1/8, 3/4, z relates the two molecules, as is common for structures in this space group with Z′ = 2. The molecule crystallizes as the keto tautomer, and the β-diketone moieties are twisted out of planarity, with O—C⋯C—O pseudo torsion angles of −74.4 (5) and −83.9 (5)°. The N—H group of each independent molecule donates an intermolecular hydrogen bond to an amide carbonyl oxygen atom by positive or negative translations along the b axis, thus forming antiparallel chains propagating in the [010] direction.The title compound, C12H15NO3, crystallizes with Z′ = 2 in space group Pca21 with the two independent molecules having almost the same conformation, differing mostly at the end of the butanamide chain. A local inversion center near 1/8, 3/4, z relates the two molecules, as is common for structures in this space group with Z′ = 2. The molecule crystallizes as the keto tautomer, and the β-diketone moieties are twisted out of planarity, with O—C⋯C—O pseudo torsion angles of −74.4 (5) and −83.9 (5)°.International Union of CrystallographyenCRYSTAL STRUCTURE; METABOLIC INTERMEDIATES; NONOPIOD ANALGESICS; PHENACETIN CONGENERSN-(4-Ethoxyphenyl)-3-oxobutanamideurn:issn:2414-3146text/htmlThe title compound, C12H15NO3, crystallizes with Z′ = 2 in space group Pca21 with the two independent molecules having almost the same conformation, differing mostly at the end of the butanamide chain. A local inversion center near 1/8, 3/4, z relates the two molecules, as is common for structures in this space group with Z′ = 2. The molecule crystallizes as the keto tautomer, and the β-diketone moieties are twisted out of planarity, with O—C⋯C—O pseudo torsion angles of −74.4 (5) and −83.9 (5)°. The N—H group of each independent molecule donates an intermolecular hydrogen bond to an amide carbonyl oxygen atom by positive or negative translations along the b axis, thus forming antiparallel chains propagating in the [010] direction.doi:10.1107/S24143146230056552023-07-04texthttps://creativecommons.org/licenses/by/4.0/Yerramsetty, S.Fronczek, F.R.Uppu, R.M.2414-31467July 2023x230565organic compounds2414-3146IUCrDatahttps://creativecommons.org/licenses/by/4.0/2023-07-04med@iucr.org82-Amino-4-(4-methoxyphenyl)-5-oxo-4H,5H-pyrano[3,2-c]chromene-3-carbonitrile acetic acid monosolvate
http://scripts.iucr.org/cgi-bin/paper?hb4427
In the title co-crystal, C20H14N2O4·C2H4O2, the expected proton transfer from acetic acid to amine has not occurred. In the crystal, the chromene molecules are linked by N—H⋯O and N—H⋯N hydrogen bonds to generate [100] columns. The acetic acid molecules form inversion dimers linked by pairwise O—H⋯O hydrogen bonds and occupy voids between the columns.The crystal structure of the title compound contains the host molecule and acetic acid in 1:1 ratio without undergoing salt formation.International Union of CrystallographyenCRYSTAL STRUCTURE; CO-CRYSTAL; ACETIC ACID DIMER; CHROMENE; CARBONITRILE2-Amino-4-(4-methoxyphenyl)-5-oxo-4H,5H-pyrano[3,2-c]chromene-3-carbonitrile acetic acid monosolvateurn:issn:2414-3146text/htmlIn the title co-crystal, C20H14N2O4·C2H4O2, the expected proton transfer from acetic acid to amine has not occurred. In the crystal, the chromene molecules are linked by N—H⋯O and N—H⋯N hydrogen bonds to generate [100] columns. The acetic acid molecules form inversion dimers linked by pairwise O—H⋯O hydrogen bonds and occupy voids between the columns.doi:10.1107/S24143146230055882023-06-30texthttps://creativecommons.org/licenses/by/4.0/Chakraborty, B.B.Paul, S.Anwar, S.Choudhury, S.2023-06-30med@iucr.orghttps://creativecommons.org/licenses/by/4.0/8IUCrDataorganic compounds2414-314662414-3146x230558June 2023l-Methionyl-l-tyrosine monohydrate
http://scripts.iucr.org/cgi-bin/paper?hb4434
The study of the oxidation of various proteins necessitates scrutiny of the amino acid sequence. Since methionine (Met) and tyrosine (Tyr) are easily oxidized, peptides that contain these amino acids are frequently studied using a variety of oxidation methods, including, but not limited to, pulse radiolysis, electrochemical oxidation, and laser flash photolysis. To date, the oxidation of the Met–Tyr dipeptide is not fully understood. Several investigators have proposed a mechanism of intramolecular electron transfer between the sulfide radical of Met and the Tyr residue. Our elucidation of the structure and absolute configuration of l-Met–l-Tyr monohydrate, C14H20N2O4S·H2O (systematic name: (2S)-2-{[(2S)-2-amino-4-methylsulfanylbutanoyl]amino}-3-(4-hydroxyphenyl)propanoic acid monohydrate) is presented herein and provides information about the zwitterionic nature of the dipeptide. We suspect that the zwitterionic state of the dipeptide and its interaction within the solvent medium may play a major role in the oxidation of the dipeptide. In the crystal, all the potential donor atoms interact via strong N—H⋯O, C—H⋯O, O—H⋯S, and O—H⋯O hydrogen bonds.The hydrated title compound is zwitterionic with the amine group of the methionyl moiety protonated and the carboxyl group of tyrosine deprotonated.International Union of CrystallographyenCRYSTAL STRUCTURE; ZWITTERION; OXIDATION; NITRATIONl-Methionyl-l-tyrosine monohydrateurn:issn:2414-3146text/htmlThe study of the oxidation of various proteins necessitates scrutiny of the amino acid sequence. Since methionine (Met) and tyrosine (Tyr) are easily oxidized, peptides that contain these amino acids are frequently studied using a variety of oxidation methods, including, but not limited to, pulse radiolysis, electrochemical oxidation, and laser flash photolysis. To date, the oxidation of the Met–Tyr dipeptide is not fully understood. Several investigators have proposed a mechanism of intramolecular electron transfer between the sulfide radical of Met and the Tyr residue. Our elucidation of the structure and absolute configuration of l-Met–l-Tyr monohydrate, C14H20N2O4S·H2O (systematic name: (2S)-2-{[(2S)-2-amino-4-methylsulfanylbutanoyl]amino}-3-(4-hydroxyphenyl)propanoic acid monohydrate) is presented herein and provides information about the zwitterionic nature of the dipeptide. We suspect that the zwitterionic state of the dipeptide and its interaction within the solvent medium may play a major role in the oxidation of the dipeptide. In the crystal, all the potential donor atoms interact via strong N—H⋯O, C—H⋯O, O—H⋯S, and O—H⋯O hydrogen bonds.doi:10.1107/S24143146230055152023-06-30texthttps://creativecommons.org/licenses/by/4.0/Babu, S.Claville, M.O.Fronczek, F.R.Uppu, R.M.organic compounds2414-314662414-3146x230551June 2023med@iucr.org2023-06-30https://creativecommons.org/licenses/by/4.0/8IUCrData9,10-Bis(iodoethynyl)anthracene
http://scripts.iucr.org/cgi-bin/paper?hb4433
The title compound, C18H8I2, is an ethynyl-substituted anthracene. The C—C—I bond angles deviate from 180°, being affected by intermolecular I⋯π interactions. These interactions form a two-dimensional supramolecular structure further supported by offset π–π stacking of neighboring anthracene moieties.The title compound exhibits I⋯π halogen bonding and π-stacking in its extended structure.International Union of CrystallographyenCRYSTAL STRUCTURE; 9,10-BIS(IODOETHYNYL); ANTHRACENE; HALOGEN BONDING; [PI]-STACKING9,10-Bis(iodoethynyl)anthraceneurn:issn:2414-3146text/htmlThe title compound, C18H8I2, is an ethynyl-substituted anthracene. The C—C—I bond angles deviate from 180°, being affected by intermolecular I⋯π interactions. These interactions form a two-dimensional supramolecular structure further supported by offset π–π stacking of neighboring anthracene moieties.doi:10.1107/S24143146230055392023-07-04texthttps://creativecommons.org/licenses/by/4.0/Antoine, N.James, M.Dungey, K.McMillen, C.Pienkos, J.8https://creativecommons.org/licenses/by/4.0/2023-07-04med@iucr.orgIUCrData2414-3146organic compoundsJuly 2023x2305532414-314676,6′-Diheptyl-3,3′-bis[(pyridin-3-yl)ethynyl]-5H,5′H-dipyrrolo[1,2-b:1′,2′-g][2,6]naphthyridine-5,5′-dione
http://scripts.iucr.org/cgi-bin/paper?hb4432
The complete molecule of the title compound, C42H42N4O2, is generated by a crystallographic centre of symmetry. The pendant heptyl chains adopt extended conformations and the dihedral angle between the pyrrole and pyridine rings is 8.18 (15)°. In the crystal, the molecules are arranged in columnar stacks propagating in the [010] direction via slipped aromatic π–π stacking interactions.The complete molecule of the title compound is generated by a crystallographic centre of symmetry. The pendant heptyl chains adopt extended conformations and the dihedral angle between the pyrrole and pyridine rings is 8.18 (15)°·In the crystal, the molecules are arranged in columnar stacks propagating in the [010] direction via slipped aromatic π–π stacking interactions.International Union of CrystallographyenCRYSTAL STRUCTURE; CROSS-CONJUGATED DYE; DIPYRROLO; PHOTOLUMINESCENCE SPECTROSCOPY6,6′-Diheptyl-3,3′-bis[(pyridin-3-yl)ethynyl]-5H,5′H-dipyrrolo[1,2-b:1′,2′-g][2,6]naphthyridine-5,5′-dioneurn:issn:2414-3146text/htmlThe complete molecule of the title compound, C42H42N4O2, is generated by a crystallographic centre of symmetry. The pendant heptyl chains adopt extended conformations and the dihedral angle between the pyrrole and pyridine rings is 8.18 (15)°. In the crystal, the molecules are arranged in columnar stacks propagating in the [010] direction via slipped aromatic π–π stacking interactions.doi:10.1107/S24143146230051382023-06-09texthttps://creativecommons.org/licenses/by/4.0/Xiang, J.Gao, H.Ma, Z.Cai, X.Zhang, Y.-P.8https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-06-09IUCrData2414-3146organic compoundsJune 2023x2305132414-31466Low-temperature modification of Ba(BF4)2(H2O)3
http://scripts.iucr.org/cgi-bin/paper?wm4190
The crystal structure of the low-temperature modification of Ba(BF4)2(H2O)3, barium bis(tetrafluoridoborate) trihydrate, was determined at 150 K. In contrast to the room-temperature modification, which crystallizes in the space group C2221 [a = 7.1763 (6), b = 18.052 (2), c = 7.1631 (6) Å, V = 927.93 (15) Å3 at 300 K, Z = 4; Charkin et al. (2023). J. Struct. Chem. 64, 253–261], the low-temperature phase is monoclinic, space group P21 [a = 7.0550 (4), b = 7.1706 (3), c = 9.4182 (6) Å, β = 109.295 (7)o, V = 449.68 (5) Å3, Z = 2]. The structure of the low-temperature modification of Ba(BF4)2(H2O)3 features O—H⋯F and O—H⋯O hydrogen bonding between water molecules and BF4− anions. One of the coordinating water molecules in the low-temperature modification is disordered over two sets of sites.Ba(BF4)2(H2O)3, orthorhombic, space group C2221 at 300 K, becomes monoclinic at 280 K, space group P21. The spread of Ba—F distances is significantly larger in the LT modification, and one of the water molecules in the LT form exhibits positional disorder.International Union of CrystallographyenLOW-TEMPERATURE MODIFICATION; PHASE TRANSITION; BARIUM TETRAFLUORIDOBORATE; CRYSTAL STRUCTURELow-temperature modification of Ba(BF4)2(H2O)3urn:issn:2414-3146text/htmlThe crystal structure of the low-temperature modification of Ba(BF4)2(H2O)3, barium bis(tetrafluoridoborate) trihydrate, was determined at 150 K. In contrast to the room-temperature modification, which crystallizes in the space group C2221 [a = 7.1763 (6), b = 18.052 (2), c = 7.1631 (6) Å, V = 927.93 (15) Å3 at 300 K, Z = 4; Charkin et al. (2023). J. Struct. Chem. 64, 253–261], the low-temperature phase is monoclinic, space group P21 [a = 7.0550 (4), b = 7.1706 (3), c = 9.4182 (6) Å, β = 109.295 (7)o, V = 449.68 (5) Å3, Z = 2]. The structure of the low-temperature modification of Ba(BF4)2(H2O)3 features O—H⋯F and O—H⋯O hydrogen bonding between water molecules and BF4− anions. One of the coordinating water molecules in the low-temperature modification is disordered over two sets of sites.doi:10.1107/S24143146230048812023-06-09texthttps://creativecommons.org/licenses/by/4.0/Goreshnik, E.Vakulka, A.Tavčar, G.https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-06-098IUCrDatainorganic compounds2414-31462414-31466June 2023x230488Aqua{μ-1,4-bis[(1,4,7,10-tetraazacyclododecan-1-yl)methyl]benzene}(nitrato-κO)dicopper(II) tris(nitrate) trihydrate
http://scripts.iucr.org/cgi-bin/paper?zl4054
In the title dinuclear CuII complex, [Cu2(NO3)(C24H46N8)(H2O)](NO3)3·3H2O, the two CuII molecules both have a square-pyramidal geometry, but the ligands in the axial positions are different: a water molecule and a nitrate ion. All nitrate ions, water molecules, and N—H groups are involved in an intermolecular hydrogen-bond network.The title dinuclear CuII complex, the two CuII molecules both have a five-coordinate square-pyramidal geometry, but the molecules in the axial positions are different: a water molecule and a nitrate ion. All nitrate ions, water molecules, and N—H groups are involved in an intermolecular hydrogen-bond network.International Union of CrystallographyenCRYSTAL STRUCTURE; COPPER(II) COMPLEX; CYCLEN; P-XYLENE; DINUCLEAR COMPLEXAqua{μ-1,4-bis[(1,4,7,10-tetraazacyclododecan-1-yl)methyl]benzene}(nitrato-κO)dicopper(II) tris(nitrate) trihydrateurn:issn:2414-3146text/htmlIn the title dinuclear CuII complex, [Cu2(NO3)(C24H46N8)(H2O)](NO3)3·3H2O, the two CuII molecules both have a square-pyramidal geometry, but the ligands in the axial positions are different: a water molecule and a nitrate ion. All nitrate ions, water molecules, and N—H groups are involved in an intermolecular hydrogen-bond network.doi:10.1107/S24143146230046252023-06-02texthttps://creativecommons.org/licenses/by/4.0/Ichimaru, Y.Kato, K.Sugiura, K.Ogawa, S.Jin, W.Kurihara, M.Yamaguchi, Y.Imai, M.Kurosaki, H.metal-organic compounds2414-31462414-31466June 2023x230462https://creativecommons.org/licenses/by/4.0/2023-06-02med@iucr.org8IUCrDataPyridin-4-ylmethanaminium perchlorate monohydrate
http://scripts.iucr.org/cgi-bin/paper?wm4189
Pyridin-4-ylmethanaminium perchlorate monohydrate (synonym: 4-picolylammonium perchlorate monohydrate), C6H9N2+·ClO4−·H2O, crystallizes in the monoclinic system (space group P21/n) with the asymmetric unit comprising two formula units (Z′ = 2). All molecular entities are located on general positions. The two crystallographically distinct 4-picolylammonium cations exhibit different conformations. The two unique perchlorate anions are non-disordered, showing an r.m.s. deviation of 0.011 Å from molecular Td symmetry. The supramolecular structure in the solid state features an intricate tri-periodic network of N—H⋯O, O—H⋯N and O—H⋯O hydrogen bonds.The title compound crystallizes in the monoclinic space group P21/n with two formula units per asymmetric unit (Z′ = 2) and features an intricate tri-periodic hydrogen-bonding network.International Union of CrystallographyenCRYSTAL STRUCTURE; 4-PICOLYLAMINE; PERCHLORATE; CONFORMATION; HETEROCYCLE; HYDROGEN BONDINGPyridin-4-ylmethanaminium perchlorate monohydrateurn:issn:2414-3146text/htmlPyridin-4-ylmethanaminium perchlorate monohydrate (synonym: 4-picolylammonium perchlorate monohydrate), C6H9N2+·ClO4−·H2O, crystallizes in the monoclinic system (space group P21/n) with the asymmetric unit comprising two formula units (Z′ = 2). All molecular entities are located on general positions. The two crystallographically distinct 4-picolylammonium cations exhibit different conformations. The two unique perchlorate anions are non-disordered, showing an r.m.s. deviation of 0.011 Å from molecular Td symmetry. The supramolecular structure in the solid state features an intricate tri-periodic network of N—H⋯O, O—H⋯N and O—H⋯O hydrogen bonds.doi:10.1107/S24143146230045952023-05-26texthttps://creativecommons.org/licenses/by/4.0/Seidel, R.W.Kolev, T.M.IUCrData8https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-05-26May 2023x2304592414-314652414-3146organic compounds(E)-5-(4-Methoxyphenyl)-N′-(2-oxoindolin-3-ylidene)-1-phenyl-1H-pyrazole-3-carbohydrazide
http://scripts.iucr.org/cgi-bin/paper?hb4430
The asymmetric unit of the title compound, C25H19N5O3, is composed of two independent molecules with slightly different conformations. The extended structure features N—H⋯O hydrogen bonds as well as π–π interactions.The asymmetric unit of the title compound consists of two molecules with slightly different conformations.International Union of CrystallographyenCRYSTAL STRUCTURE; PYRAZOLES; CARBOHYDRAZIDES; ISATIN; HETEROCYCLES; SYNTHESIS(E)-5-(4-Methoxyphenyl)-N′-(2-oxoindolin-3-ylidene)-1-phenyl-1H-pyrazole-3-carbohydrazideurn:issn:2414-3146text/htmlThe asymmetric unit of the title compound, C25H19N5O3, is composed of two independent molecules with slightly different conformations. The extended structure features N—H⋯O hydrogen bonds as well as π–π interactions.doi:10.1107/S24143146230045582023-05-26texthttps://creativecommons.org/licenses/by/4.0/Abdel-Wahab, B.F.Farahat, A.A.Bekheit, M.S.Yousif, E.Kariuki, B.M.El-Hiti, G.A.2414-3146organic compoundsx230455May 202352414-314682023-05-26med@iucr.orghttps://creativecommons.org/licenses/by/4.0/IUCrData1-Benzyl-3-[(4-methoxyphenyl)imino]indolin-2-one
http://scripts.iucr.org/cgi-bin/paper?bh4074
The title compound, C22H18N2O2, is a Schiff base obtained by condensing p-arnisidine (4-methoxyaniline) with N-benzylisatin (1-benzyl-1H-indole-2,3-dione), which crystallizes in the triclinic P\overline{1} space group. The benzyl and phenyl rings subtend dihedral angles of 76.08 (7) and 60.70 (6)°, respectively, with the isatin group. The imino C=N double bond exists in an E conformation.The title Schiff base was obtained from the reaction of N-benzylisatin with p-arnisidine. The imino C=N double bond, exists in an E conformation.International Union of CrystallographyenCRYSTAL STRUCTURE; N-BENZYLISATIN; P-ARNISIDINE; SCHIFF BASE1-Benzyl-3-[(4-methoxyphenyl)imino]indolin-2-oneurn:issn:2414-3146text/htmlThe title compound, C22H18N2O2, is a Schiff base obtained by condensing p-arnisidine (4-methoxyaniline) with N-benzylisatin (1-benzyl-1H-indole-2,3-dione), which crystallizes in the triclinic P\overline{1} space group. The benzyl and phenyl rings subtend dihedral angles of 76.08 (7) and 60.70 (6)°, respectively, with the isatin group. The imino C=N double bond exists in an E conformation.doi:10.1107/S24143146230041822023-05-19texthttps://creativecommons.org/licenses/by/4.0/Odedokun, O.A.Ikotun, A.A.Ajaelu, C.J.Bhuvanesh, N.organic compounds2414-314652414-3146x230418May 2023med@iucr.org2023-05-19https://creativecommons.org/licenses/by/4.0/8IUCrData5,6,7,8-Tetrahydro-[1,2,4]triazolo[5,1-b]quinazolin-9(4H)-one
http://scripts.iucr.org/cgi-bin/paper?tk4091
The triazole ring in the title molecule, C9H10N4O, is not quite coplanar with the six-membered ring to which it is fused, the dihedral angle between the two least-squares planes being 2.52 (6)°. In the crystal, a layered structure is formed by N—H⋯N and C—H⋯O hydrogen bonds plus slipped π-stacking interactions, with the fused cyclohexene rings projecting to either side.The triazole ring in the title molecule is not quite coplanar with the six-membered ring to which it is fused, the dihedral angle between the two least-squares planes being 2.52 (6)°. In the crystal, a layer structure is formed by N—H⋯N and C—H⋯O hydrogen bonds plus slipped π-stacking interactions, with the fused cyclohexene rings projecting to either side.International Union of CrystallographyenCRYSTAL STRUCTURE; [PI]-STACKING; HYDROGEN BONDING; TRIAZOLE; TETRAHYDROQUINAZOLINE5,6,7,8-Tetrahydro-[1,2,4]triazolo[5,1-b]quinazolin-9(4H)-oneurn:issn:2414-3146text/htmlThe triazole ring in the title molecule, C9H10N4O, is not quite coplanar with the six-membered ring to which it is fused, the dihedral angle between the two least-squares planes being 2.52 (6)°. In the crystal, a layered structure is formed by N—H⋯N and C—H⋯O hydrogen bonds plus slipped π-stacking interactions, with the fused cyclohexene rings projecting to either side.doi:10.1107/S24143146230040912023-05-12texthttps://creativecommons.org/licenses/by/4.0/Ettahiri, W.Dalbouha, A.Baouid, A.Alsubari, A.Mague, J.T.Taleb, M.Ramli, Y.https://creativecommons.org/licenses/by/4.0/2023-05-12med@iucr.org8IUCrDataorganic compounds2414-31462414-31465May 2023x230409Tetrakis(triethylenediamin-1-ium) dodeca-μ2-chlorido-hexakis(thiocyanato-κN)hexa-octahedro-niobate
http://scripts.iucr.org/cgi-bin/paper?wm4186
The crystal structure of the cluster complex salt, (C6H13N2)4[Nb6(NCS)6Cl12] or (H-DABCO)4[Nb6Cl12(NCS)6] (DABCO = triethylenediamine or 1,4-diazabicyclo[2.2.2]octane), comprises octahedral Nb6 cluster cores, which are μ2-coordinated by 12 chloride ligands (bridging the octahedral edges, inner ligand sphere). Furthermore, each Nb atom is N-bonded to a terminal thiocyanate ligand (outer ligand sphere). The discrete clusters carry a charge of −4, which is compensated by four monoprotonated DABCO molecules. These are arranged in rows, which are N—H⋯Cl and N—H⋯N hydrogen bonded to the anions and among each other.The anion of the cluster complex salt, (H-DABCO)4[Nb6Cl12(NCS)6], comprises octahedral Nb6 cluster units, which are coordinated by twelve μ2-bridging chlorido ligands and six terminal N-bound thiocyanato ligands.International Union of CrystallographyenCRYSTAL STRUCTURE; NIOBIUM; CLUSTER; CHLORIDE; DABCOTetrakis(triethylenediamin-1-ium) dodeca-μ2-chlorido-hexakis(thiocyanato-κN)hexa-octahedro-niobateurn:issn:2414-3146text/htmlThe crystal structure of the cluster complex salt, (C6H13N2)4[Nb6(NCS)6Cl12] or (H-DABCO)4[Nb6Cl12(NCS)6] (DABCO = triethylenediamine or 1,4-diazabicyclo[2.2.2]octane), comprises octahedral Nb6 cluster cores, which are μ2-coordinated by 12 chloride ligands (bridging the octahedral edges, inner ligand sphere). Furthermore, each Nb atom is N-bonded to a terminal thiocyanate ligand (outer ligand sphere). The discrete clusters carry a charge of −4, which is compensated by four monoprotonated DABCO molecules. These are arranged in rows, which are N—H⋯Cl and N—H⋯N hydrogen bonded to the anions and among each other.doi:10.1107/S241431462300398X2023-05-12texthttps://creativecommons.org/licenses/by/4.0/Sperlich, E.Köckerling, M.med@iucr.org2023-05-12https://creativecommons.org/licenses/by/4.0/8IUCrDatametal-organic compounds2414-314652414-3146x230398May 2023(2,2′-Bipyridyl)(η6-p-cymene)iodidoruthenium(II) hexafluoridophosphate
http://scripts.iucr.org/cgi-bin/paper?zl4053
The title compound, having the molecular formula [RuI(η6-C10H14)(C10H8N2)]PF6, crystallizes in the triclinic P\overline{1} (Z = 2) space group as a half-sandwich complex resembling a three-legged piano stool. Important geometrical parameters include Ru—cymene centroid = 1.6902 (17) Å, Ru—I = 2.6958 (5) Å, [Ru—N]avg = 2.072 (3) Å, N1—Ru—N2 = 76.86 (12)° and a dihedral angle between the planes of the two rings of the bipyridyl system of 5.9 (2)°. The PF6− ion was treated with a twofold disorder model, refining to a 65.0 (8):35.0 (8) occupancy ratio. The crystal packing features C—H⋯F/I interactions.The title compound crystallizes in the triclinic P\overline{1} (Z = 2) space group as a half-sandwich complex resembling a three-legged piano stool. The crystal packing features C—H⋯F/I interactions.International Union of CrystallographyenRUTHENIUM; P-CYMENE; 2,2'-BIPYRIDYL; CRYSTAL STRUCTURE(2,2′-Bipyridyl)(η6-p-cymene)iodidoruthenium(II) hexafluoridophosphateurn:issn:2414-3146text/htmlThe title compound, having the molecular formula [RuI(η6-C10H14)(C10H8N2)]PF6, crystallizes in the triclinic P\overline{1} (Z = 2) space group as a half-sandwich complex resembling a three-legged piano stool. Important geometrical parameters include Ru—cymene centroid = 1.6902 (17) Å, Ru—I = 2.6958 (5) Å, [Ru—N]avg = 2.072 (3) Å, N1—Ru—N2 = 76.86 (12)° and a dihedral angle between the planes of the two rings of the bipyridyl system of 5.9 (2)°. The PF6− ion was treated with a twofold disorder model, refining to a 65.0 (8):35.0 (8) occupancy ratio. The crystal packing features C—H⋯F/I interactions.doi:10.1107/S24143146230039292023-05-12texthttps://creativecommons.org/licenses/by/4.0/Kelani, M.T.Muller, A.Lammertsma, K.IUCrData8med@iucr.org2023-05-12https://creativecommons.org/licenses/by/4.0/x230392May 202352414-31462414-3146metal-organic compoundsN-Methylserotonin hydrogen oxalate
http://scripts.iucr.org/cgi-bin/paper?bx4024
The solid-state structure of N-methylserotonin {systematic name: [2-(5-hydroxy-1H-indol-3-yl)ethyl](methyl)azanium hydrogen oxalate}, C11H15N2O+·C2HO4−, is reported. The structure possesses a singly protonated N-methylserotonin cation and one hydrogen oxalate anion in the asymmetric unit. In the crystal, the molecules are linked by N—H⋯O and O—H⋯O hydrogen bonds into a three-dimensional network.The structure of the natural product N-methylserotonin is reported as its hydrogen oxalate salt.International Union of CrystallographyenCRYSTAL STRUCTURE; TRYPTAMINES; INDOLES; HYDROGEN BONDINGN-Methylserotonin hydrogen oxalateurn:issn:2414-3146text/htmlThe solid-state structure of N-methylserotonin {systematic name: [2-(5-hydroxy-1H-indol-3-yl)ethyl](methyl)azanium hydrogen oxalate}, C11H15N2O+·C2HO4−, is reported. The structure possesses a singly protonated N-methylserotonin cation and one hydrogen oxalate anion in the asymmetric unit. In the crystal, the molecules are linked by N—H⋯O and O—H⋯O hydrogen bonds into a three-dimensional network.doi:10.1107/S24143146230037842023-05-05texthttps://creativecommons.org/licenses/by/4.0/Naeem, M.Anas, N.A.Chadeayne, A.R.Golen, J.A.Manke, D.R.IUCrData8https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-05-05May 2023x2303782414-314652414-3146organic compoundsSynthesis and crystal structure of a PdII complex of ortho-xylylenebis(pyridyltriazole)
http://scripts.iucr.org/cgi-bin/paper?xu4050
A tetradentate ligand, namely, ortho-xylylenebis(pyridyltriazole), o-xpt, was synthesized using the `click' method and complexed with Pd(BF4)2. In the title complex, bis{μ-1,1′-(o-xylylene)bis[4-(pyridin-2-yl)triazole]-κN3:N3′}dipalladium(II) tetrakis(tetrafluoridoborate)–dimethylformamide–diethyl ether (1/2/1), as the BF4 salt, and including dimethylformamide and diethyl ether solvent molecules, with stoichiometry [Pd2(C22H18N8)2](BF4)4·2C3H7NO·C4H10O, the Pd complex and the disordered diethyl ether molecule lie on inversion centers. The ligand coordinates to the PdII centers with square-planar geometry, forming a dimeric macrocycle. The Pd⋯Pd separation in the complex [Pd2(o-xpt)2]4+ cation is 3.6184 (4) Å. In the crystal, the complex molecules are stacked along the b axis, with π–π interactions between the pyridyltriazole ligands of two molecules.The ortho-xylylenebis(pyridyltriazole) ligand coordinate with PdII giving dimeric square-planar complexes on which the Pd⋯Pd separation is 3.6184 (4) Å.International Union of CrystallographyenO-XYLYLENEBISPYRIDYLTRIAZOLE; PDII COMPLEX; X-RAY CRYSTALLOGRAPHY; METAL-ORGANIC SUPRAMOLECULES; SQUARE-PLANAR GEOMETRYSynthesis and crystal structure of a PdII complex of ortho-xylylenebis(pyridyltriazole)urn:issn:2414-3146text/htmlA tetradentate ligand, namely, ortho-xylylenebis(pyridyltriazole), o-xpt, was synthesized using the `click' method and complexed with Pd(BF4)2. In the title complex, bis{μ-1,1′-(o-xylylene)bis[4-(pyridin-2-yl)triazole]-κN3:N3′}dipalladium(II) tetrakis(tetrafluoridoborate)–dimethylformamide–diethyl ether (1/2/1), as the BF4 salt, and including dimethylformamide and diethyl ether solvent molecules, with stoichiometry [Pd2(C22H18N8)2](BF4)4·2C3H7NO·C4H10O, the Pd complex and the disordered diethyl ether molecule lie on inversion centers. The ligand coordinates to the PdII centers with square-planar geometry, forming a dimeric macrocycle. The Pd⋯Pd separation in the complex [Pd2(o-xpt)2]4+ cation is 3.6184 (4) Å. In the crystal, the complex molecules are stacked along the b axis, with π–π interactions between the pyridyltriazole ligands of two molecules.doi:10.1107/S24143146230036202023-04-25texthttps://creativecommons.org/licenses/by/4.0/Pokharel, U.Naquin, A.Fronczek, F.8https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-04-25IUCrData2414-3146metal-organic compoundsApril 2023x2303622414-314642-(3-Methyl-2-oxoquinoxalin-1-yl)-N-(4-methylphenyl)acetamide
http://scripts.iucr.org/cgi-bin/paper?vm4060
The quinoxaline moiety in the title molecule, C18H17N3O2, is not quite planar and the p-tolyl group is rotationally disordered over two nearly equally populated sets of sites. In the crystal, N—H⋯O and C—H⋯O hydrogen bonds form chains extending along the b-axis direction. Due to the disorder of the p-tolyl rings, short C⋯C distances are observed between adjacent chains.Chains extending along the b-axis direction are formed through hydrogen bonding between the amide functions of the title quinoxaline derivative.International Union of CrystallographyenCRYSTAL STRUCTURE; HYDROGEN BOND; EDGE-TO-EDGE [PI]-INTERACTION; AMIDE; QUINOXALINE2-(3-Methyl-2-oxoquinoxalin-1-yl)-N-(4-methylphenyl)acetamideurn:issn:2414-3146text/htmlThe quinoxaline moiety in the title molecule, C18H17N3O2, is not quite planar and the p-tolyl group is rotationally disordered over two nearly equally populated sets of sites. In the crystal, N—H⋯O and C—H⋯O hydrogen bonds form chains extending along the b-axis direction. Due to the disorder of the p-tolyl rings, short C⋯C distances are observed between adjacent chains.doi:10.1107/S24143146230035772023-04-21texthttps://creativecommons.org/licenses/by/4.0/Missioui, M.Alsubari, A.Mague, J.T.Essassi, E.M.Ramli, Y.x230357April 202342414-31462414-3146organic compoundsIUCrData82023-04-21med@iucr.orghttps://creativecommons.org/licenses/by/4.0/(N-Benzoyl-N-phenylhydroxylaminato)carbonyl(triphenylarsine)rhodium(I)
http://scripts.iucr.org/cgi-bin/paper?wm4184
The molecule of the title compound, [Rh(C13H10NO2){As(C6H5)3}(CO)] or [Rh(BPHA)(AsPh3)(CO)] (BPHA is the N-benzoyl-N-phenylhydroxylaminate anion), comprises a bidentate N-benzoyl-N-phenylhydroxylaminate anion coordinating through the O atoms to the soft Lewis acid, rhodium(I), and two monodentate ligands, viz. triphenylarsine and carbonyl. The resulting CO2As coordination environment around the central RhI atom is distorted square planar.=The molecular structure of the title compound, [Rh(BPHA)(CO)(AsPh3)] (where BPHA = N-benzoyl-N-phenylhydroxylaminate), has a distorted square-planar coordination environment around the central RhI atom, defined by a CO2As coordination set.International Union of CrystallographyenCRYSTAL STRUCTURE; RHODIUM; N-BENZOYL-N-PHENYLHYDROXAMIC ACID; TRIPHENYLARSINE(N-Benzoyl-N-phenylhydroxylaminato)carbonyl(triphenylarsine)rhodium(I)urn:issn:2414-3146text/htmlThe molecule of the title compound, [Rh(C13H10NO2){As(C6H5)3}(CO)] or [Rh(BPHA)(AsPh3)(CO)] (BPHA is the N-benzoyl-N-phenylhydroxylaminate anion), comprises a bidentate N-benzoyl-N-phenylhydroxylaminate anion coordinating through the O atoms to the soft Lewis acid, rhodium(I), and two monodentate ligands, viz. triphenylarsine and carbonyl. The resulting CO2As coordination environment around the central RhI atom is distorted square planar.=doi:10.1107/S24143146230035532023-04-25texthttps://creativecommons.org/licenses/by/4.0/Motente, M.A.Venter, J.Brink, A.IUCrData8med@iucr.org2023-04-25https://creativecommons.org/licenses/by/4.0/x230355April 202342414-31462414-3146metal-organic compounds5-[(4-Methylphenyl)sulfonyl]-1-phenylthiopyrano[4,3-b]indole-3(5H)-thione dichloromethane monosolvate
http://scripts.iucr.org/cgi-bin/paper?bt4137
Rhodium-catalyzed [2+2+2] cycloaddition of carbon disulfide to o,N-dialkynyltosylanilines gives two isomeric indolothiopyranthiones, a violet and a red isomer. This is the first crystal structure of a red isomer, which crystallizes with one solvent molecule of dichloromethane in the asymmetric unit, C24H17NO2S3·CH2Cl2. In the extended structure, centrosymmetric pairs of the planar annulated system are arranged in strands and solvent molecules fill the space between the strands.Rhodium-catalyzed [2+2+2] cycloaddition of carbon disulfide to o,N-dialkynyltosylanilines gives two isomeric indolothiopyranthiones as violet and red isomers. This is the first crystal structure of a red isomer, which crystallizes with one molecule of dichloromethane in the asymmetric unit.International Union of CrystallographyenCRYSTAL STRUCTURE; SULFUR; ANNULATED HETEROCYCLES5-[(4-Methylphenyl)sulfonyl]-1-phenylthiopyrano[4,3-b]indole-3(5H)-thione dichloromethane monosolvateurn:issn:2414-3146text/htmlRhodium-catalyzed [2+2+2] cycloaddition of carbon disulfide to o,N-dialkynyltosylanilines gives two isomeric indolothiopyranthiones, a violet and a red isomer. This is the first crystal structure of a red isomer, which crystallizes with one solvent molecule of dichloromethane in the asymmetric unit, C24H17NO2S3·CH2Cl2. In the extended structure, centrosymmetric pairs of the planar annulated system are arranged in strands and solvent molecules fill the space between the strands.doi:10.1107/S24143146230035412023-05-12texthttps://creativecommons.org/licenses/by/4.0/Dassonneville, B.Schollmeyer, D.Detert, H.x230354May 202352414-31462414-3146organic compoundsIUCrData8med@iucr.org2023-05-12https://creativecommons.org/licenses/by/4.0/{μ-2,2′-(Ethane-1,2-diyl)bis[4,6-bis(trimethylsilyl)-1,3-dihydrocyclopenta[c]pyrrol-5-one]}bis[tricarbonyliron(0)]
http://scripts.iucr.org/cgi-bin/paper?bh4073
The binuclear title compound, [Fe2(C28H48N2O2Si4)(CO)6], consists of two central iron(0) atoms, each of them surrounded by a cyclopentadienone moiety and three carbonyl ligands in a three-legged piano-stool shape. Furthermore, the bis(cyclopentadienone) ligand acts as a bridge between the two metal atoms.The binuclear title compound consists of two iron(0) centres, each of them surrounded by a cyclopentadienone moiety and three carbonyl ligands in a three-legged piano-stool geometry.International Union of CrystallographyenCRYSTAL STRUCTURE; IRON CARBONYL COMPLEX; CYCLOPENTADIENONE LIGAND; BINUCLEAR COMPLEX{μ-2,2′-(Ethane-1,2-diyl)bis[4,6-bis(trimethylsilyl)-1,3-dihydrocyclopenta[c]pyrrol-5-one]}bis[tricarbonyliron(0)]urn:issn:2414-3146text/htmlThe binuclear title compound, [Fe2(C28H48N2O2Si4)(CO)6], consists of two central iron(0) atoms, each of them surrounded by a cyclopentadienone moiety and three carbonyl ligands in a three-legged piano-stool shape. Furthermore, the bis(cyclopentadienone) ligand acts as a bridge between the two metal atoms.doi:10.1107/S24143146230034622023-04-21texthttps://creativecommons.org/licenses/by/4.0/Huerta-Zerón, H.D.Spannenberg, A.Beller, M.Junge, H.IUCrData82023-04-21med@iucr.orghttps://creativecommons.org/licenses/by/4.0/x230346April 202342414-31462414-3146metal-organic compounds(23R,231S,25S)-231,26-Epoxy-23-ethylfurost-20(22)-en-3β-ol
http://scripts.iucr.org/cgi-bin/paper?bt4138
The title compound, C29H46O3, is a steroid synthesized through a rearrangement of a sarsasapogenin derivative in acidic medium. The newly formed ring F is a tetrahydro-2H-pyran heterocycle substituted by two methyl groups placed in equatorial positions. This ring displays a chair conformation, while dihydrofuran ring E, to which it is bonded, has an envelope conformation. The molecules are associated by weak O—H⋯O hydrogen bonds to form chains running in the [101] direction in the crystal.The title steroid includes a tetrahydro-2H-pyran heterocycle bonded to the steroidal nucleus, resulting from a spirostan rearrangement.International Union of CrystallographyenCRYSTAL STRUCTURE; TETRAHYDROPYRAN; SARSASAPOGENIN; REARRANGEMENT REACTION; HYDROGEN BOND(23R,231S,25S)-231,26-Epoxy-23-ethylfurost-20(22)-en-3β-olurn:issn:2414-3146text/htmlThe title compound, C29H46O3, is a steroid synthesized through a rearrangement of a sarsasapogenin derivative in acidic medium. The newly formed ring F is a tetrahydro-2H-pyran heterocycle substituted by two methyl groups placed in equatorial positions. This ring displays a chair conformation, while dihydrofuran ring E, to which it is bonded, has an envelope conformation. The molecules are associated by weak O—H⋯O hydrogen bonds to form chains running in the [101] direction in the crystal.doi:10.1107/S24143146230034492023-04-21texthttps://creativecommons.org/licenses/by/4.0/Guerrero-Luna, G.Hernández-Linares, M.-G.Cárdenas García, M.Bernès, S.2414-3146organic compoundsx230344April 202342414-314682023-04-21med@iucr.orghttps://creativecommons.org/licenses/by/4.0/IUCrData9-(Pyrrolidinium-1-yl)-9-boranuidabicyclo[3.3.1]nonane
http://scripts.iucr.org/cgi-bin/paper?im4018
The title compound, C12H24BN, is an adduct formed from 9-borabicyclo[3.3.1]nonane (9-BBN) and pyrrolidine. It crystallizes in the triclinic space group P\overline{1} with three molecules in the asymmetric unit, one of which has disorder of the pyrrolidine ring. The B—N bond lengths are between 1.631 (2) and 1.641 (2) Å. The boron and nitrogen atoms are bound to one hydrogen atom each. These hydrogen atoms are in antiperiplanar orientation. Both six-membered rings of the 9-BBN unit are in a chair conformation in all three molecules. Differences between the three crystallographic independent molecules are found in the five-membered rings of the pyrrolidine unit. These adopt different twisted and envelope conformations.The title compound, C12H24BN, is an adduct formed from 9-borabicyclo[3.3.1]nonane (9-BBN) and pyrrolidine. It crystallizes in the the triclinic space group P\overline{1} with three molecules in the asymmetric unit.International Union of CrystallographyenCRYSTAL STRUCTURE9-(Pyrrolidinium-1-yl)-9-boranuidabicyclo[3.3.1]nonaneurn:issn:2414-3146text/htmlThe title compound, C12H24BN, is an adduct formed from 9-borabicyclo[3.3.1]nonane (9-BBN) and pyrrolidine. It crystallizes in the triclinic space group P\overline{1} with three molecules in the asymmetric unit, one of which has disorder of the pyrrolidine ring. The B—N bond lengths are between 1.631 (2) and 1.641 (2) Å. The boron and nitrogen atoms are bound to one hydrogen atom each. These hydrogen atoms are in antiperiplanar orientation. Both six-membered rings of the 9-BBN unit are in a chair conformation in all three molecules. Differences between the three crystallographic independent molecules are found in the five-membered rings of the pyrrolidine unit. These adopt different twisted and envelope conformations.doi:10.1107/S24143146230033222023-04-18texthttps://creativecommons.org/licenses/by/4.0/Herbig, M.Böhme, U.2414-31464April 2023x230332organic compounds2414-3146IUCrDatahttps://creativecommons.org/licenses/by/4.0/med@iucr.org2023-04-188Trimethylphosphine oxide dihydrate
http://scripts.iucr.org/cgi-bin/paper?hb4428
The title hydrate, Me3PO·2H2O, crystallizes in the orthorhombic space group Pbca with eight formula units per unit cell. The extended structure displays O—H⋯O hydrogen bonding, with Me3PO molecules as acceptors and water molecules acting as donors and acceptors of hydrogen bonds, forming hydrogen-bonded layers, which propagate in the ac plane.Trimethylphosphine oxide and water molecules form 16-membered hydrogen-bonded rings interconnected into layers.International Union of CrystallographyenPHOSPHINE OXIDE; HYDRATE; HYDROGEN BONDING; CRYSTAL STRUCTURETrimethylphosphine oxide dihydrateurn:issn:2414-3146text/htmlThe title hydrate, Me3PO·2H2O, crystallizes in the orthorhombic space group Pbca with eight formula units per unit cell. The extended structure displays O—H⋯O hydrogen bonding, with Me3PO molecules as acceptors and water molecules acting as donors and acceptors of hydrogen bonds, forming hydrogen-bonded layers, which propagate in the ac plane.doi:10.1107/S24143146230031402023-04-14texthttps://creativecommons.org/licenses/by/4.0/Urlep, M.Cerkovnik, J.Lozinšek, M.2023-04-14med@iucr.orghttps://creativecommons.org/licenses/by/4.0/8IUCrDataorganic compounds2414-314642414-3146x230314April 2023{N-[(4-Methoxy-2-oxidophenyl)(phenyl)methylidene]glycinato}diphenylsilicon(IV)
http://scripts.iucr.org/cgi-bin/paper?pk4039
The title compound, C28H23NO4Si, crystallizes in the monoclinic space group P21/c. The silicon complex consists of a tridentate dinegative Schiff base ligand bound to a diphenylsilyl unit. The coordination geometry of the pentacoordinate silicon atom is a distorted trigonal bipyramid.The silicon title complex consists of a tridentate dinegative Schiff base ligand bound to a diphenylsilyl unit. The coordination geometry of the pentacoordinated silicon atom is a distorted trigonal bipyramid.International Union of CrystallographyenCRYSTAL STRUCTURE; SILICON COMPLEX; SCHIFF-BASE LIGAND; PENTACOORDINATION{N-[(4-Methoxy-2-oxidophenyl)(phenyl)methylidene]glycinato}diphenylsilicon(IV)urn:issn:2414-3146text/htmlThe title compound, C28H23NO4Si, crystallizes in the monoclinic space group P21/c. The silicon complex consists of a tridentate dinegative Schiff base ligand bound to a diphenylsilyl unit. The coordination geometry of the pentacoordinate silicon atom is a distorted trigonal bipyramid.doi:10.1107/S24143146230030612023-04-06texthttps://creativecommons.org/licenses/by/4.0/Böhme, U.Fels, S.IUCrData82023-04-06med@iucr.orghttps://creativecommons.org/licenses/by/4.0/x230306April 202342414-31462414-3146organic compounds[3-Methoxy-5-(methoxycarbonyl)isoxazol-4-yl](4-methoxyphenyl)iodonium 2,2,2-trifluoroacetate
http://scripts.iucr.org/cgi-bin/paper?tk4090
A new isoxazole-based iodonoium salt, C13H13INO5+·C2F3O2−, has been synthesized and structurally characterized. In the crystal, ions are linked by short I⋯O contacts to form a neutral tetra-ion aggregate. These combine with C—H⋯F and C—H⋯O interactions to form double-layered two-dimensional sheets in the (001) plane.The crystal structure of an unsymmetrical diaryl iodonium salt obtained from the nucleophilic coupling of tributyl(4-methoxyphenyl)stannane with a diacetoxyiodo precursor bearing an isoxazole moiety is described.International Union of CrystallographyenCRYSTAL STRUCTURE; ISOXAZOLE; 4-METHOXYPHENYL; IODONIUM; DIMER[3-Methoxy-5-(methoxycarbonyl)isoxazol-4-yl](4-methoxyphenyl)iodonium 2,2,2-trifluoroacetateurn:issn:2414-3146text/htmlA new isoxazole-based iodonoium salt, C13H13INO5+·C2F3O2−, has been synthesized and structurally characterized. In the crystal, ions are linked by short I⋯O contacts to form a neutral tetra-ion aggregate. These combine with C—H⋯F and C—H⋯O interactions to form double-layered two-dimensional sheets in the (001) plane.doi:10.1107/S24143146230030002023-04-06texthttps://creativecommons.org/licenses/by/4.0/Abdul Manan, M.A.F.Cordes, D.B.Slawin, A.M.Z.O'Hagan, D.organic compounds2414-31462414-31464April 2023x230300https://creativecommons.org/licenses/by/4.0/2023-04-06med@iucr.org8IUCrDataN-(4-Methoxy-3-nitrophenyl)acetamide
http://scripts.iucr.org/cgi-bin/paper?hb4429
The title compound, C9H10N2O4, crystallizes with a disordered nitro group in twinned crystals. Both the methoxy group and the acetamide groups are nearly coplanar with the phenyl ring, and the C—N—C—O torsion angle [0.2 (4)°] is also insignificantly different from zero. Overall, the 12-atom methoxyphenylacetamide group is nearly planar, with an r.m.s. deviation of 0.042 Å. The nitro group is twisted out of this plane by about 30°, disordered into two orientations with opposite senses of twist. In the crystal, the N—H group donates a hydrogen bond to a nitro oxygen atom, generating chains propagating in the [101] direction. The amide carbonyl oxygen atom is not involved in the hydrogen bonding.The title compound crystallizes with a disordered nitro group in twinned crystals. In the crystal, the N—H group donates a hydrogen bond to a nitro oxygen atom, generating chains propagating in the [101] direction. The amide carbonyl oxygen atom is not involved in the hydrogen bonding.International Union of CrystallographyenN-ALKOXYACETANILIDES; PHENACETIN CONGENERS; NITRO PRODUCTS; CRYSTAL STRUCTURE; HYDROGEN BONDINGN-(4-Methoxy-3-nitrophenyl)acetamideurn:issn:2414-3146text/htmlThe title compound, C9H10N2O4, crystallizes with a disordered nitro group in twinned crystals. Both the methoxy group and the acetamide groups are nearly coplanar with the phenyl ring, and the C—N—C—O torsion angle [0.2 (4)°] is also insignificantly different from zero. Overall, the 12-atom methoxyphenylacetamide group is nearly planar, with an r.m.s. deviation of 0.042 Å. The nitro group is twisted out of this plane by about 30°, disordered into two orientations with opposite senses of twist. In the crystal, the N—H group donates a hydrogen bond to a nitro oxygen atom, generating chains propagating in the [101] direction. The amide carbonyl oxygen atom is not involved in the hydrogen bonding.doi:10.1107/S24143146230029852023-04-04texthttps://creativecommons.org/licenses/by/4.0/Hines III, J.E.Agu, O.A.Deere, C.J.Fronczek, F.R.Uppu, R.M.8med@iucr.org2023-04-04https://creativecommons.org/licenses/by/4.0/IUCrData2414-3146organic compoundsx230298April 202342414-3146Bis[5-methyl-2,3-bis(thiophen-2-yl)quinoxaline-κN1](nitrato-κ2O,O′)silver(I)
http://scripts.iucr.org/cgi-bin/paper?bt4136
The crystal structure of the title silver(I) complex, [Ag(NO3)(C17H12N2S2)2], has monoclinic (C2/c) symmetry, with the silver(I) atom and the nitrate group sitting on a twofold rotation axis. The complex also exhibits a thienyl-ring flip disorder, which is common for unsubstituted thiophene rings.In the title compound, the silver(I) metal center sits on a twofold rotation axis, as does the coordinated nitrato anion. The two 2-thienyl groups of the ligand make dihedral angles of 17.14 (9) and 77.55 (6)° with respect to the quinoxaline plane. The thienyl group that is less planar with the quinoxaline ring exhibits ring-flip disorder.International Union of CrystallographyenCRYSTAL STRUCTURE; THIENYLQUINOXALINE; SILVER NITRATEBis[5-methyl-2,3-bis(thiophen-2-yl)quinoxaline-κN1](nitrato-κ2O,O′)silver(I)urn:issn:2414-3146text/htmlThe crystal structure of the title silver(I) complex, [Ag(NO3)(C17H12N2S2)2], has monoclinic (C2/c) symmetry, with the silver(I) atom and the nitrate group sitting on a twofold rotation axis. The complex also exhibits a thienyl-ring flip disorder, which is common for unsubstituted thiophene rings.doi:10.1107/S24143146230026512023-03-23texthttps://creativecommons.org/licenses/by/4.0/Crundwell, G.Ellis, K.M.8med@iucr.org2023-03-23https://creativecommons.org/licenses/by/4.0/IUCrData2414-3146metal-organic compoundsx230265March 202332414-3146Bis[2-(thiophen-2-yl)quinoxaline-κN4]silver(I) perchlorate
http://scripts.iucr.org/cgi-bin/paper?bt4134
The crystal of the title salt, [Ag(C12H8N2S)2]ClO4, has C2/c symmetry whereby the silver(I) atom sits on a twofold rotation axis, as does the perchlorate anion, which is disordered about this axis. The thienylquinoxaline ligand is nearly planar with the thienyl ring making a dihedral angle of 10.88 (8)° with respect to the quinoxaline moiety.The structure of bis[2-(thiophen-2-yl)quinoxaline-κN4]silver(I) perchlorate, [Ag(C12H8N2S)2]ClO4, has a silver(I) metal center that sits on a twofold symmetry axis, as does a disordered perchlorate anion. The thienylquinoxaline ligand is nearly planar with the thienyl ring making a dihedral angle of 10.88 (8)° with respect to the quinoxaline moiety.International Union of CrystallographyenCRYSTAL STRUCTURE; SILVER(I); QUINOXALINES; THIENYL RINGSBis[2-(thiophen-2-yl)quinoxaline-κN4]silver(I) perchlorateurn:issn:2414-3146text/htmlThe crystal of the title salt, [Ag(C12H8N2S)2]ClO4, has C2/c symmetry whereby the silver(I) atom sits on a twofold rotation axis, as does the perchlorate anion, which is disordered about this axis. The thienylquinoxaline ligand is nearly planar with the thienyl ring making a dihedral angle of 10.88 (8)° with respect to the quinoxaline moiety.doi:10.1107/S24143146230024682023-03-21texthttps://creativecommons.org/licenses/by/4.0/Crundwell, G.https://creativecommons.org/licenses/by/4.0/med@iucr.org2023-03-218IUCrDatametal-organic compounds2414-31462414-31463March 2023x2302465-([(Z)-Methoxyimino]{2-[(2-methylphenoxy)methyl]phenyl}methyl)-1,3,4-oxadiazole-2(3H)-thione dimethyl sulfoxide monosolvate
http://scripts.iucr.org/cgi-bin/paper?bt4133
The title compound, C18H17N3O3S·C2H6OS, crystallizes in the monoclinic space group P21/c. In the crystal, C11(9) chains of C—H⋯O interactions are formed, propogating in the c-axis direction. The N—H hydrogen atom forms a strong hydrogen bond with the oxygen atom of a DMSO solvate molecule.The title compound crystallizes in the monoclinic space group P21/c with one molecule in the asymmetric unit. In the crystal, C_{1}^{1}(9) chains of C—H⋯O interactions are formed, propogating in the c-axis direction. The N—H hydrogen atom forms a strong hydrogen bond with the oxygen atom of a DMSO solvate molecule.International Union of CrystallographyenCRYSTAL STRUCTURE; DMSO; FUNGICIDES; STROBILURIN5-([(Z)-Methoxyimino]{2-[(2-methylphenoxy)methyl]phenyl}methyl)-1,3,4-oxadiazole-2(3H)-thione dimethyl sulfoxide monosolvateurn:issn:2414-3146text/htmlThe title compound, C18H17N3O3S·C2H6OS, crystallizes in the monoclinic space group P21/c. In the crystal, C11(9) chains of C—H⋯O interactions are formed, propogating in the c-axis direction. The N—H hydrogen atom forms a strong hydrogen bond with the oxygen atom of a DMSO solvate molecule.doi:10.1107/S24143146230023772023-03-28texthttps://creativecommons.org/licenses/by/4.0/Shripanavar, C.S.Balerao, R.Butcher, R.J.x230237March 202332414-31462414-3146organic compoundsIUCrData8med@iucr.org2023-03-28https://creativecommons.org/licenses/by/4.0/rac-N-(4-Ethoxyphenyl)-3-hydroxybutanamide
http://scripts.iucr.org/cgi-bin/paper?vm4059
In the title compound, racemic bucetin [systematic name: N-(4-ethoxyphenyl)-3-hydroxybutanamide], C12H17NO3, the molecule is in an extended conformation as illustrated by the C—O—C—C torsion angle [170.14 (15)°] in the ethoxy group and the subsequent C—N—C—C [−177.24 (16)°], N—C—C—C [170.08 (15)°] and C—C—C—C [171.41 (15)°] torsion angles in the butanamide chain. In the crystal, the O—H group donates an intermolecular O—H⋯O hydrogen bond to the amide carbonyl oxygen atom and also accepts an intermolecular N—H⋯O hydrogen bond from an adjacent N—H group. The former forms 12-membered dimeric rings about inversion centers, and the latter form chains in the [001] direction. The overall hydrogen-bonded network is two-dimensional, with no propagation in the [100] direction.The crystal structure of bucetin, an analgesic and antipyric similar to phenacetin, is presented.International Union of CrystallographyenBUCETIN; NON-OPIOID ANALGESICS; CRYSTAL STRUCTURE; HYDROGEN BONDINGrac-N-(4-Ethoxyphenyl)-3-hydroxybutanamideurn:issn:2414-3146text/htmlIn the title compound, racemic bucetin [systematic name: N-(4-ethoxyphenyl)-3-hydroxybutanamide], C12H17NO3, the molecule is in an extended conformation as illustrated by the C—O—C—C torsion angle [170.14 (15)°] in the ethoxy group and the subsequent C—N—C—C [−177.24 (16)°], N—C—C—C [170.08 (15)°] and C—C—C—C [171.41 (15)°] torsion angles in the butanamide chain. In the crystal, the O—H group donates an intermolecular O—H⋯O hydrogen bond to the amide carbonyl oxygen atom and also accepts an intermolecular N—H⋯O hydrogen bond from an adjacent N—H group. The former forms 12-membered dimeric rings about inversion centers, and the latter form chains in the [001] direction. The overall hydrogen-bonded network is two-dimensional, with no propagation in the [100] direction.doi:10.1107/S24143146230023162023-03-15texthttps://creativecommons.org/licenses/by/4.0/Hines III, J.E.Myles, Z.Breaux, G.Fronczek, F.R.Uppu, R.M.IUCrDatamed@iucr.org2023-03-15https://creativecommons.org/licenses/by/4.0/832414-3146x230231March 2023organic compounds2414-3146(1S,2S)-2-[(S)-2,2,2-Trifluoro-1-hydroxyethyl]-1-tetralol
http://scripts.iucr.org/cgi-bin/paper?tk4089
The crystal structure of the title enantiopure tetralol derivative {systematic name: (1S,2S)-2-[(S)-2,2,2-trifluoro-1-hydroxyethyl]-1,2,3,4-tetrahydronaphthalen-1-ol}, C12H13F3O2, synthesized by asymmetric transfer hydrogenation, was elucidated by low-temperature single-crystal X-ray diffraction. The enantiopure compound crystallizes in the Sohncke space group P212121 with one molecule in the asymmetric unit and features intramolecular as well as intermolecular O—H⋯O hydrogen bonding. The absolute configuration was established from anomalous dispersion effects.The title enantiopure tetralol derivative synthesized by asymmetric transfer hydrogenation crystallizes in the Sohncke space group P212121 and features one molecule in the asymmetric unit. In the crystal, molecules are hydrogen-bonded into chains running parallel to [010].International Union of CrystallographyenTETRALOL; CRYSTAL STRUCTURE; ASYMMETRIC TRANSFER HYDROGENATION; TRIFLUOROMETHYL GROUP(1S,2S)-2-[(S)-2,2,2-Trifluoro-1-hydroxyethyl]-1-tetralolurn:issn:2414-3146text/htmlThe crystal structure of the title enantiopure tetralol derivative {systematic name: (1S,2S)-2-[(S)-2,2,2-trifluoro-1-hydroxyethyl]-1,2,3,4-tetrahydronaphthalen-1-ol}, C12H13F3O2, synthesized by asymmetric transfer hydrogenation, was elucidated by low-temperature single-crystal X-ray diffraction. The enantiopure compound crystallizes in the Sohncke space group P212121 with one molecule in the asymmetric unit and features intramolecular as well as intermolecular O—H⋯O hydrogen bonding. The absolute configuration was established from anomalous dispersion effects.doi:10.1107/S24143146230021712023-03-15texthttps://creativecommons.org/licenses/by/4.0/Radan, K.Cotman, A.E.Lozinšek, M.2414-31463March 2023x230217organic compounds2414-3146IUCrDatahttps://creativecommons.org/licenses/by/4.0/2023-03-15med@iucr.org8