http://journals.iucr.org/c/issues/2013/06/00/isscontsbdy.html Acta Crystallographica Section C: Crystal Structure Communications specializes in the rapid dissemination of high-quality studies of crystal and molecular structures of interest in fields such as chemistry, biochemistry, mineralogy, pharmacology, physics and materials science. The numerical and text descriptions of each structure are submitted to the journal electronically as a Crystallographic Information File (CIF) and are checked and typeset automatically prior to peer review. The journal is well known for its high standards of structural reliability and presentation. Section C publishes approximately 1000 structures per year; readers have access to an archive that includes high-quality structural data for over 10000 compounds. en Copyright (c) 2013 International Union of Crystallography 2013-05-23 International Union of Crystallography International Union of Crystallography http://journals.iucr.org urn:issn:0108-2701 Acta Crystallographica Section C: Crystal Structure Communications specializes in the rapid dissemination of high-quality studies of crystal and molecular structures of interest in fields such as chemistry, biochemistry, mineralogy, pharmacology, physics and materials science. The numerical and text descriptions of each structure are submitted to the journal electronically as a Crystallographic Information File (CIF) and are checked and typeset automatically prior to peer review. The journal is well known for its high standards of structural reliability and presentation. Section C publishes approximately 1000 structures per year; readers have access to an archive that includes high-quality structural data for over 10000 compounds. text/html Acta Crystallographica Section C: Crystal Structure Communications, Volume 69, Part 6, 2013 text monthly 1 2002-01-15T00:00+00:00 6 69 2013-05-23 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications 565 urn:issn:0108-2701 med@iucr.org May 2013 2013-05-23 http://journals.iucr.org/logos/rss10c.gif http://journals.iucr.org/c/issues/2013/06/00/isscontsbdy.html Still image http://scripts.iucr.org/cgi-bin/paper?ku3094 The reaction of N1,N1′-(ethane-1,2-diyl)bis(propane-1,3-diamine) (bapen), K2[Ni(CN)4]·H2O and dimethylformamide in the presence of Gd(NO3)3·6H2O under solvothermal conditions yielded yellow crystals of dicyanido(2,3,4,6,7,9,10,11-octahydropyrimido[2′,1′:3,4]pyrazino[1,2-a]pyrimidine)nickel(II) hemihydrate, [Ni(CN)2(C10H16N4)]·0.5H2O, (I), the crystal structure of which is composed of [Ni(CN)2(pdpm)] molecules (pdpm is 2,3,4,6,7,9,10,11-octahydropyrimido[2′,1′:3,4]pyrazino[1,2-a]pyrimidine) on general positions linked by O—H...N hydrogen bonds to water molecules located on twofold axes. This structural unit is further linked by nonclassical C—H...N interactions to form a warped two-dimensional net perpendicular to the unit-cell b axis. The nets are stacked, with C—H...O contacts joining successive units. The NiII cation is coordinated with square-planar geometry by a chelating pdpm ligand and two cyanide ligands in mutually cis positions. Complex (I) is stable up to 360 K, at which point dehydration takes place; the ligands start to decompose at 558 K. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Stolárová, M. Černák, J. Tomás, M. Falvello, L.R. 2013-05-02 doi:10.1107/S0108270113010585 International Union of Crystallography The reaction of N1,N1′-(ethane-1,2-diyl)bis(propane-1,3-diamine) (bapen), K2[Ni(CN)4]·H2O and dimethylformamide in the presence of Gd(NO3)3·6H2O under solvothermal conditions yielded yellow crystals of dicyanido(2,3,4,6,7,9,10,11-octahydropyrimido[2′,1′:3,4]pyrazino[1,2-a]pyrimidine)nickel(II) hemihydrate, [Ni(CN)2(C10H16N4)]·0.5H2O, (I), the crystal structure of which is composed of [Ni(CN)2(pdpm)] molecules (pdpm is 2,3,4,6,7,9,10,11-octahydropyrimido[2′,1′:3,4]pyrazino[1,2-a]pyrimidine) on general positions linked by O—H...N hydrogen bonds to water molecules located on twofold axes. This structural unit is further linked by nonclassical C—H...N interactions to form a warped two-dimensional net perpendicular to the unit-cell b axis. The nets are stacked, with C—H...O contacts joining successive units. The NiII cation is coordinated with square-planar geometry by a chelating pdpm ligand and two cyanide ligands in mutually cis positions. Complex (I) is stable up to 360 K, at which point dehydration takes place; the ligands start to decompose at 558 K. EN The reaction of N1,N1′-(ethane-1,2-diyl)bis(propane-1,3-diamine) (bapen), K2[Ni(CN)4]·H2O and dimethylformamide in the presence of Gd(NO3)3·6H2O under solvothermal conditions yielded yellow crystals of dicyanido(2,3,4,6,7,9,10,11-octahydropyrimido[2′,1′:3,4]pyrazino[1,2-a]pyrimidine)nickel(II) hemihydrate, [Ni(CN)2(C10H16N4)]·0.5H2O, (I), the crystal structure of which is composed of [Ni(CN)2(pdpm)] molecules (pdpm is 2,3,4,6,7,9,10,11-octahydropyrimido[2′,1′:3,4]pyrazino[1,2-a]pyrimidine) on general positions linked by O—H...N hydrogen bonds to water molecules located on twofold axes. This structural unit is further linked by nonclassical C—H...N interactions to form a warped two-dimensional net perpendicular to the unit-cell b axis. The nets are stacked, with C—H...O contacts joining successive units. The NiII cation is coordinated with square-planar geometry by a chelating pdpm ligand and two cyanide ligands in mutually cis positions. Complex (I) is stable up to 360 K, at which point dehydration takes place; the ligands start to decompose at 558 K. text/html Crystal structure and thermal properties of a square-planar NiII complex of cyanide and a tricyclic bis-amidine ligand formed in situ under solvothermal conditions text 6 69 2013-05-02 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?wq3030 Bis[μ-di-tert-butyl(hydroxy)silanolato]bis[chloridoindium(III)], [In2(C8H19O2Si)2Cl4], (I), is a centrosymmetric two-centre indium complex featuring a system of three annulated four-membered rings; the structure is the first example of an In2O2 ring which is annulated with two Si—O units to form a ring system composed of three rings. The coordination environment of the In centres is a distorted trigonal bipyramid. The crystal packing of (I) is characterized by chains of molecules connected by O—H...Cl hydrogen bonds. The crystal of (I) was a nonmerohedral twin. There is no known example of an In2O2 ring in which the In atoms carry any two halogen ligands. The structure of tetrakis(tetrahydrofuran)lithium tetrakis[(trimethylsilyl)methyl]borate, [Li(C4H8O)4](C16H44BSi4), (II), is composed of discrete cations and anions. The coordination geometries of the Li and B centres is tetrahedral. The cations and anions lie in planes parallel to the ab plane. There are no short contacts between the cations and anions. Compound (II) is the first example of a B centre bonded to four –CH2Si units. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Scholz, S. Vitze, H. Bolte, M. Lerner, H.-W. 2013-05-02 doi:10.1107/S0108270113009311 International Union of Crystallography Bis[μ-di-tert-butyl(hydroxy)silanolato]bis[chloridoindium(III)], [In2(C8H19O2Si)2Cl4], (I), is a centrosymmetric two-centre indium complex featuring a system of three annulated four-membered rings; the structure is the first example of an In2O2 ring which is annulated with two Si—O units to form a ring system composed of three rings. The coordination environment of the In centres is a distorted trigonal bipyramid. The crystal packing of (I) is characterized by chains of molecules connected by O—H...Cl hydrogen bonds. The crystal of (I) was a nonmerohedral twin. There is no known example of an In2O2 ring in which the In atoms carry any two halogen ligands. The structure of tetrakis(tetrahydrofuran)lithium tetrakis[(trimethylsilyl)methyl]borate, [Li(C4H8O)4](C16H44BSi4), (II), is composed of discrete cations and anions. The coordination geometries of the Li and B centres is tetrahedral. The cations and anions lie in planes parallel to the ab plane. There are no short contacts between the cations and anions. Compound (II) is the first example of a B centre bonded to four –CH2Si units. EN Bis[μ-di-tert-butyl(hydroxy)silanolato]bis[chloridoindium(III)], [In2(C8H19O2Si)2Cl4], (I), is a centrosymmetric two-centre indium complex featuring a system of three annulated four-membered rings; the structure is the first example of an In2O2 ring which is annulated with two Si—O units to form a ring system composed of three rings. The coordination environment of the In centres is a distorted trigonal bipyramid. The crystal packing of (I) is characterized by chains of molecules connected by O—H...Cl hydrogen bonds. The crystal of (I) was a nonmerohedral twin. There is no known example of an In2O2 ring in which the In atoms carry any two halogen ligands. The structure of tetrakis(tetrahydrofuran)lithium tetrakis[(trimethylsilyl)methyl]borate, [Li(C4H8O)4](C16H44BSi4), (II), is composed of discrete cations and anions. The coordination geometries of the Li and B centres is tetrahedral. The cations and anions lie in planes parallel to the ab plane. There are no short contacts between the cations and anions. Compound (II) is the first example of a B centre bonded to four –CH2Si units. text/html An approach to creating novel anions: silylated triel compounds with –CH2– and –O– linkers, [InCl2{O(HO)Si(t-Bu)2}]2 and Li[B(CH2SiMe3)4] text 6 69 2013-05-02 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?sk3485 The title compound, [K(C14H23)(C4H8O)]n, comprises zigzag chains of alternating bridging 2,3,4,5-tetramethyl-1-n-pentylcyclopentadienyl ligands and potassium ions, with an ancillary tetrahydrofuran ligand in the coordination environment of potassium. The coordination polymer strands so formed extend by 21 screw symmetry in the b-axis direction. The chemically modified cyclopentadienyl ligand, with a tethered n-pentyl group, was synthesized from 2,3,4,5-tetramethylcyclopent-2-enone by a Grignard reaction. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Seidel, R.W. Ganesamoorthy, C. Loerke, S. Winter, M.V. Gemel, C. Fischer, R.A. 2013-05-02 doi:10.1107/S0108270113011074 International Union of Crystallography The title compound, [K(C14H23)(C4H8O)]n, comprises zigzag chains of alternating bridging 2,3,4,5-tetramethyl-1-n-pentylcyclopentadienyl ligands and potassium ions, with an ancillary tetrahydrofuran ligand in the coordination environment of potassium. The coordination polymer strands so formed extend by 21 screw symmetry in the b-axis direction. The chemically modified cyclopentadienyl ligand, with a tethered n-pentyl group, was synthesized from 2,3,4,5-tetramethylcyclopent-2-enone by a Grignard reaction. EN The title compound, [K(C14H23)(C4H8O)]n, comprises zigzag chains of alternating bridging 2,3,4,5-tetramethyl-1-n-pentylcyclopentadienyl ligands and potassium ions, with an ancillary tetrahydrofuran ligand in the coordination environment of potassium. The coordination polymer strands so formed extend by 21 screw symmetry in the b-axis direction. The chemically modified cyclopentadienyl ligand, with a tethered n-pentyl group, was synthesized from 2,3,4,5-tetramethylcyclopent-2-enone by a Grignard reaction. text/html catena-Poly[[(tetrahydrofuran-κO)potassium]-μ-(η5:η5)-2,3,4,5-tetramethyl-1-n-pentylcyclopentadienyl] text 6 69 2013-05-02 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?mx3099 A novel metal–organic framework, {[Zn2Cl4(C25H24N4O4)]·4C3H7NO}n, has been synthesized solvothermally by assembling the semi-rigid tetrahedral ligand tetrakis[(pyridin-4-yl)oxymethyl]methane (tpom) and zinc nitrate in dimethylformamide (DMF). The crystal structure is noncentrosymmetric (P\overline{4}21c). Each ZnII cation has a tetrahedral coordination environment (C2 symmetry), which is formed by two chloride ligands and two pyridine N atoms from two tpom ligands. The tetrahedral tetradentate tpom linker has a quaternary C atom located on the crystallographic \overline{4} axis. This linker utilizes all the peripheral pyridine N atoms to connect four ZnII cations, thereby forming a wave-like two-dimensional sheet along the c axis. The two-dimensional layer can be topologically simplified as a typical uninodal 4-connected sql/Shubnikov net, which is represented by the Schläfli symbol {44,62}. Adjacent layers are further packed into a three-dimensional structure by C—H...Cl hydrogen bonds. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Wang, Y.-Q. Xie, F.-Z. Du, L. 2013-05-10 doi:10.1107/S0108270113010937 International Union of Crystallography A novel metal–organic framework, {[Zn2Cl4(C25H24N4O4)]·4C3H7NO}n, has been synthesized solvothermally by assembling the semi-rigid tetrahedral ligand tetrakis[(pyridin-4-yl)oxymethyl]methane (tpom) and zinc nitrate in dimethylformamide (DMF). The crystal structure is noncentrosymmetric (P\overline{4}21c). Each ZnII cation has a tetrahedral coordination environment (C2 symmetry), which is formed by two chloride ligands and two pyridine N atoms from two tpom ligands. The tetrahedral tetradentate tpom linker has a quaternary C atom located on the crystallographic \overline{4} axis. This linker utilizes all the peripheral pyridine N atoms to connect four ZnII cations, thereby forming a wave-like two-dimensional sheet along the c axis. The two-dimensional layer can be topologically simplified as a typical uninodal 4-connected sql/Shubnikov net, which is represented by the Schläfli symbol {44,62}. Adjacent layers are further packed into a three-dimensional structure by C—H...Cl hydrogen bonds. EN A novel metal–organic framework, {[Zn2Cl4(C25H24N4O4)]·4C3H7NO}n, has been synthesized solvothermally by assembling the semi-rigid tetrahedral ligand tetrakis[(pyridin-4-yl)oxymethyl]methane (tpom) and zinc nitrate in dimethylformamide (DMF). The crystal structure is noncentrosymmetric (P\overline{4}21c). Each ZnII cation has a tetrahedral coordination environment (C2 symmetry), which is formed by two chloride ligands and two pyridine N atoms from two tpom ligands. The tetrahedral tetradentate tpom linker has a quaternary C atom located on the crystallographic \overline{4} axis. This linker utilizes all the peripheral pyridine N atoms to connect four ZnII cations, thereby forming a wave-like two-dimensional sheet along the c axis. The two-dimensional layer can be topologically simplified as a typical uninodal 4-connected sql/Shubnikov net, which is represented by the Schläfli symbol {44,62}. Adjacent layers are further packed into a three-dimensional structure by C—H...Cl hydrogen bonds. text/html Poly[[tetrachlorido{μ4-tetrakis[(pyridin-4-yl)oxymethyl]methane-κ4N:N′:N′′:N′′′}dizinc(II)] dimethylformamide tetrasolvate] text 6 69 2013-05-10 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?wq3029 The title compound, hexadecacarbonylbis{μ3-[(diphenylphosphanyl)methanediidyl]sulfanido}-μ4-disulfido(2−)-hexairon(4 Fe—Fe), [Fe6(C13H10PS)2(S2)(CO)16], contains two inversion-related [Fe3(Ph2PCS)(CO)8] subclusters linked by an equatorial disulfide bond [S—S = 2.1490 (9) Å]. Each Ph2PCS3− ligand is coordinated to a triiron core in a μ3-κP:κ2C:κ2S fashion. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Shi, Y.-C. Cheng, H.-R. Cheng, D.-C. 2013-05-10 doi:10.1107/S0108270113009049 International Union of Crystallography The title compound, hexadecacarbonylbis{μ3-[(diphenylphosphanyl)methanediidyl]sulfanido}-μ4-disulfido(2−)-hexairon(4 Fe—Fe), [Fe6(C13H10PS)2(S2)(CO)16], contains two inversion-related [Fe3(Ph2PCS)(CO)8] subclusters linked by an equatorial disulfide bond [S—S = 2.1490 (9) Å]. Each Ph2PCS3− ligand is coordinated to a triiron core in a μ3-κP:κ2C:κ2S fashion. EN The title compound, hexadecacarbonylbis{μ3-[(diphenylphosphanyl)methanediidyl]sulfanido}-μ4-disulfido(2−)-hexairon(4 Fe—Fe), [Fe6(C13H10PS)2(S2)(CO)16], contains two inversion-related [Fe3(Ph2PCS)(CO)8] subclusters linked by an equatorial disulfide bond [S—S = 2.1490 (9) Å]. Each Ph2PCS3− ligand is coordinated to a triiron core in a μ3-κP:κ2C:κ2S fashion. text/html A novel hexairon cluster with one disulfide and two Ph2PCS3− ligands text 6 69 2013-05-10 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?mx3092 The title complex, [Rh(C10H15)Cl(C14H12N2O4)]Cl·2C4H5NO3, has been synthesized by a substitution reaction of the precursor [bis(2,5-dioxopyrrolidin-1-yl) 2,2′-bipyridine-4,4′-dicarboxylate]chlorido(pentamethylcyclopentadienyl)rhodium(III) chloride with NaOCH3. The RhIII cation is located in an RhC5N2Cl eight-coordinated environment. In the crystal, 1-hydroxypyrrolidine-2,5-dione (NHS) solvent molecules form strong hydrogen bonds with the Cl− counter-anions in the lattice and weak hydrogen bonds with the pentamethylcyclopentadienyl (Cp*) ligands. Hydrogen bonding between the Cp* ligands, the NHS solvent molecules and the Cl− counter-anions form links in a V-shaped chain of RhIII complex cations along the c axis. Weak hydrogen bonds between the dimethyl 2,2′-bipyridine-4,4′-dicarboxylate ligands and the Cl− counter-anions connect the components into a supramolecular three-dimensional network. The synthetic route to the dimethyl 2,2′-bipyridine-4,4′-dicarboxylate-containing rhodium complex from the [bis(2,5-dioxopyrrolidin-1-yl) 2,2′-bipyridine-4,4′-dicarboxylate]rhodium(III) precursor may be applied to link Rh catalysts to the surface of electrodes. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Sivanesan, D. Kim, H.M. Sungho, Y. 2013-05-10 doi:10.1107/S0108270113009633 International Union of Crystallography The title complex, [Rh(C10H15)Cl(C14H12N2O4)]Cl·2C4H5NO3, has been synthesized by a substitution reaction of the precursor [bis(2,5-dioxopyrrolidin-1-yl) 2,2′-bipyridine-4,4′-dicarboxylate]chlorido(pentamethylcyclopentadienyl)rhodium(III) chloride with NaOCH3. The RhIII cation is located in an RhC5N2Cl eight-coordinated environment. In the crystal, 1-hydroxypyrrolidine-2,5-dione (NHS) solvent molecules form strong hydrogen bonds with the Cl− counter-anions in the lattice and weak hydrogen bonds with the pentamethylcyclopentadienyl (Cp*) ligands. Hydrogen bonding between the Cp* ligands, the NHS solvent molecules and the Cl− counter-anions form links in a V-shaped chain of RhIII complex cations along the c axis. Weak hydrogen bonds between the dimethyl 2,2′-bipyridine-4,4′-dicarboxylate ligands and the Cl− counter-anions connect the components into a supramolecular three-dimensional network. The synthetic route to the dimethyl 2,2′-bipyridine-4,4′-dicarboxylate-containing rhodium complex from the [bis(2,5-dioxopyrrolidin-1-yl) 2,2′-bipyridine-4,4′-dicarboxylate]rhodium(III) precursor may be applied to link Rh catalysts to the surface of electrodes. EN The title complex, [Rh(C10H15)Cl(C14H12N2O4)]Cl·2C4H5NO3, has been synthesized by a substitution reaction of the precursor [bis(2,5-dioxopyrrolidin-1-yl) 2,2′-bipyridine-4,4′-dicarboxylate]chlorido(pentamethylcyclopentadienyl)rhodium(III) chloride with NaOCH3. The RhIII cation is located in an RhC5N2Cl eight-coordinated environment. In the crystal, 1-hydroxypyrrolidine-2,5-dione (NHS) solvent molecules form strong hydrogen bonds with the Cl− counter-anions in the lattice and weak hydrogen bonds with the pentamethylcyclopentadienyl (Cp*) ligands. Hydrogen bonding between the Cp* ligands, the NHS solvent molecules and the Cl− counter-anions form links in a V-shaped chain of RhIII complex cations along the c axis. Weak hydrogen bonds between the dimethyl 2,2′-bipyridine-4,4′-dicarboxylate ligands and the Cl− counter-anions connect the components into a supramolecular three-dimensional network. The synthetic route to the dimethyl 2,2′-bipyridine-4,4′-dicarboxylate-containing rhodium complex from the [bis(2,5-dioxopyrrolidin-1-yl) 2,2′-bipyridine-4,4′-dicarboxylate]rhodium(III) precursor may be applied to link Rh catalysts to the surface of electrodes. text/html Chlorido(dimethyl 2,2′-bipyridine-4,4′-dicarboxylate-κ2N,N′)(η5-pentamethylcyclopentadienyl)rhodium(III) chloride 1-hydroxypyrrolidine-2,5-dione disolvate text 6 69 2013-05-10 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?yf3031 Two polyoxometallate-based compounds, tris[1,1′-(butane-1,4-diyl)bis(1H-imidazol-3-ium)] bis[tetracosa-μ2-oxido-dodecaoxido-μ12-phosphato-dodecamolybdenum(VI)], (C10H16N4)3[PMo12O40]2, (I), and 1,1′-(butane-1,4-diyl)bis(1H-imidazol-3-ium) 1-[4-(1H-imidazol-1-yl)butyl]-1H-imidazol-3-ium tetracosa-μ2-oxido-dodecaoxido-μ12-phosphato-dodecamolybdenum(VI) dihydrate, (C10H16N4)(C10H15N4)[PMo12O40]·2H2O, (II), were synthesized by hydrothermal techniques at different pH values. The stoichiometric ratio between the polyoxometallate (POM) anions and organic cations is 2:3 in (I), with one of the cations lying on an inversion centre. The doubly protonated 1,1′-(butane-1,4-diyl)diimidazole (BIM) cations are linked to the [PMo12O40]3− anions by hydrogen bonds to form a three-dimensional supramolecular network. The stoichiometric ratio of POM anions and organic cations is 1:2 in (II), and the anion is located about a centre of inversion. The partly protonated BIM cations and solvent water molecules form hydrogen bonds with the [PMo12O40]3− anions, yielding a two-dimensional supramolecular layer. The different lattice architectures of (I) and (II) may be governed by the ratio between the POM anions and organic cations, which, in turn, is determined by the pH value. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Zhang, Q. Liu, J. Lu, J. Gong, S.-W. 2013-05-10 doi:10.1107/S0108270113011554 International Union of Crystallography Two polyoxometallate-based compounds, tris[1,1′-(butane-1,4-diyl)bis(1H-imidazol-3-ium)] bis[tetracosa-μ2-oxido-dodecaoxido-μ12-phosphato-dodecamolybdenum(VI)], (C10H16N4)3[PMo12O40]2, (I), and 1,1′-(butane-1,4-diyl)bis(1H-imidazol-3-ium) 1-[4-(1H-imidazol-1-yl)butyl]-1H-imidazol-3-ium tetracosa-μ2-oxido-dodecaoxido-μ12-phosphato-dodecamolybdenum(VI) dihydrate, (C10H16N4)(C10H15N4)[PMo12O40]·2H2O, (II), were synthesized by hydrothermal techniques at different pH values. The stoichiometric ratio between the polyoxometallate (POM) anions and organic cations is 2:3 in (I), with one of the cations lying on an inversion centre. The doubly protonated 1,1′-(butane-1,4-diyl)diimidazole (BIM) cations are linked to the [PMo12O40]3− anions by hydrogen bonds to form a three-dimensional supramolecular network. The stoichiometric ratio of POM anions and organic cations is 1:2 in (II), and the anion is located about a centre of inversion. The partly protonated BIM cations and solvent water molecules form hydrogen bonds with the [PMo12O40]3− anions, yielding a two-dimensional supramolecular layer. The different lattice architectures of (I) and (II) may be governed by the ratio between the POM anions and organic cations, which, in turn, is determined by the pH value. EN Two polyoxometallate-based compounds, tris[1,1′-(butane-1,4-diyl)bis(1H-imidazol-3-ium)] bis[tetracosa-μ2-oxido-dodecaoxido-μ12-phosphato-dodecamolybdenum(VI)], (C10H16N4)3[PMo12O40]2, (I), and 1,1′-(butane-1,4-diyl)bis(1H-imidazol-3-ium) 1-[4-(1H-imidazol-1-yl)butyl]-1H-imidazol-3-ium tetracosa-μ2-oxido-dodecaoxido-μ12-phosphato-dodecamolybdenum(VI) dihydrate, (C10H16N4)(C10H15N4)[PMo12O40]·2H2O, (II), were synthesized by hydrothermal techniques at different pH values. The stoichiometric ratio between the polyoxometallate (POM) anions and organic cations is 2:3 in (I), with one of the cations lying on an inversion centre. The doubly protonated 1,1′-(butane-1,4-diyl)diimidazole (BIM) cations are linked to the [PMo12O40]3− anions by hydrogen bonds to form a three-dimensional supramolecular network. The stoichiometric ratio of POM anions and organic cations is 1:2 in (II), and the anion is located about a centre of inversion. The partly protonated BIM cations and solvent water molecules form hydrogen bonds with the [PMo12O40]3− anions, yielding a two-dimensional supramolecular layer. The different lattice architectures of (I) and (II) may be governed by the ratio between the POM anions and organic cations, which, in turn, is determined by the pH value. text/html Two polyoxometallate-based supramolecular compounds influenced by the ratio between the polyoxometallate anion and organic cation text 6 69 2013-05-10 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?fn3134 In the title compound, {[Cu(C15H11ClN2O3)(C4H9NO)]n, the CuII cation has square-pyramidal geometry. The morpholine ligand serves as a bridge to link two symmetry-related metal atoms, resulting in an infinite chain structure along the a axis. Adjacent chains are extended into a two-dimensional layered structure via hydrogen bonds formed between morpholine and amide N atoms [N—H...N = 2.971 (3) Å]. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Wang, M. Lian, Z.-X. 2013-05-15 doi:10.1107/S0108270113011967 International Union of Crystallography In the title compound, {[Cu(C15H11ClN2O3)(C4H9NO)]n, the CuII cation has square-pyramidal geometry. The morpholine ligand serves as a bridge to link two symmetry-related metal atoms, resulting in an infinite chain structure along the a axis. Adjacent chains are extended into a two-dimensional layered structure via hydrogen bonds formed between morpholine and amide N atoms [N—H...N = 2.971 (3) Å]. EN In the title compound, {[Cu(C15H11ClN2O3)(C4H9NO)]n, the CuII cation has square-pyramidal geometry. The morpholine ligand serves as a bridge to link two symmetry-related metal atoms, resulting in an infinite chain structure along the a axis. Adjacent chains are extended into a two-dimensional layered structure via hydrogen bonds formed between morpholine and amide N atoms [N—H...N = 2.971 (3) Å]. text/html catena-Poly[[[2-(2-chlorophenoxy)-N′-(2-oxidobenzylidene-κO)acetohydrazidato-κ2N′,O]copper(II)]-μ-morpholine-κ2N:O] text 6 69 2013-05-15 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?wq3033 In the title mixed-ligand metal–organic polymeric complex, {[Co(NCS)2(C8H12N6)2]·2H2O}n, the asymmetric unit contains a divalent CoII cation, which sits on an inversion centre, two halves of two crystallographically distinct and centrosymmetric 1,4-bis(1,2,4-triazol-1-yl)butane (BTB) ligands, one N-bound thiocyanate ligand and one solvent water molecule. The CoII atom possesses a distorted {CoN6} octahedral geometry, with the equatorial positions taken up by triazole N atoms from four different BTB ligands. The axial positions are filled by thiocyanate N atoms. In the crystal, each CoII atom is linked covalently to four others through the distal donors of the tethering BTB ligands, forming a neutral (4,4)-topology two-dimensional rhomboid grid layer motif, which is coincident with the (1\overline{2}1) crystal planes. Magnetic investigations show that weak antiferromagnetic coupling exists between CoII atoms in the complex. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Tao, J.-Q. Mao, D. Wang, J. 2013-05-15 doi:10.1107/S0108270113011153 International Union of Crystallography In the title mixed-ligand metal–organic polymeric complex, {[Co(NCS)2(C8H12N6)2]·2H2O}n, the asymmetric unit contains a divalent CoII cation, which sits on an inversion centre, two halves of two crystallographically distinct and centrosymmetric 1,4-bis(1,2,4-triazol-1-yl)butane (BTB) ligands, one N-bound thiocyanate ligand and one solvent water molecule. The CoII atom possesses a distorted {CoN6} octahedral geometry, with the equatorial positions taken up by triazole N atoms from four different BTB ligands. The axial positions are filled by thiocyanate N atoms. In the crystal, each CoII atom is linked covalently to four others through the distal donors of the tethering BTB ligands, forming a neutral (4,4)-topology two-dimensional rhomboid grid layer motif, which is coincident with the (1\overline{2}1) crystal planes. Magnetic investigations show that weak antiferromagnetic coupling exists between CoII atoms in the complex. EN In the title mixed-ligand metal–organic polymeric complex, {[Co(NCS)2(C8H12N6)2]·2H2O}n, the asymmetric unit contains a divalent CoII cation, which sits on an inversion centre, two halves of two crystallographically distinct and centrosymmetric 1,4-bis(1,2,4-triazol-1-yl)butane (BTB) ligands, one N-bound thiocyanate ligand and one solvent water molecule. The CoII atom possesses a distorted {CoN6} octahedral geometry, with the equatorial positions taken up by triazole N atoms from four different BTB ligands. The axial positions are filled by thiocyanate N atoms. In the crystal, each CoII atom is linked covalently to four others through the distal donors of the tethering BTB ligands, forming a neutral (4,4)-topology two-dimensional rhomboid grid layer motif, which is coincident with the (1\overline{2}1) crystal planes. Magnetic investigations show that weak antiferromagnetic coupling exists between CoII atoms in the complex. text/html Magnetic investigations of a two-dimensional coordination polymer with a three-dimensional supramolecular framework: poly[[bis[μ2-1,4-bis(1,2,4-triazol-1-yl)butane]bis(thiocyanato-κN)cobalt(II)] dihydrate] text 6 69 2013-05-15 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?ov3026 Two new symmetric double-armed oxadiazole-bridged ligands, 4-methyl-{5-[5-methyl-2-(pyridin-3-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-3-carboxylate (L1) and 4-methyl-{5-[5-methyl-2-(pyridin-4-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-4-carboxylate (L2), were prepared by the reaction of 2,5-bis(2-hydroxy-5-methylphenyl)-1,3,4-oxadiazole with nicotinoyl chloride and isonicotinoyl chloride, respectively. Ligand L1 can be used as an organic clip to bind CuII cations and generate a molecular complex, bis(4-methyl-{5-[5-methyl-2-(pyridin-3-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-3-carboxylate)bis(perchlorato)copper(II), [Cu(ClO4)2(C28H20N4O5)2], (I). In compound (I), the CuII cation is located on an inversion centre and is hexacoordinated in a distorted octahedral geometry, with the pyridine N atoms of two L1 ligands in the equatorial positions and two weakly coordinating perchlorate counter-ions in the axial positions. The two arms of the L1 ligands bend inward and converge at the CuII coordination point to give rise to a spirometallocycle. Ligand L2 binds CuI cations to generate a supramolecule, diacetonitriledi-μ3-iodido-di-μ2-iodido-bis(4-methyl-{5-[5-methyl-2-(pyridin-4-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-4-carboxylate)tetracopper(I), [Cu4I4(CH3CN)2(C28H20N4O5)2], (II). The asymmetric unit of (II) indicates that it contains two CuI atoms, one L2 ligand, one acetonitrile ligand and two iodide ligands. Both of the CuI atoms are four-coordinated in an approximately tetrahedral environment. The molecule is centrosymmetric and the four I atoms and four CuI atoms form a rope-ladder-type [Cu4I4] unit. Discrete units are linked into one-dimensional chains through π–π interactions. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Wu, X.-W. Xin, M.-M. Ma, J.-P. Wu, Z.-H. Dong, Y.-B. 2013-05-15 doi:10.1107/S0108270113010913 International Union of Crystallography Two new symmetric double-armed oxadiazole-bridged ligands, 4-methyl-{5-[5-methyl-2-(pyridin-3-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-3-carboxylate (L1) and 4-methyl-{5-[5-methyl-2-(pyridin-4-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-4-carboxylate (L2), were prepared by the reaction of 2,5-bis(2-hydroxy-5-methylphenyl)-1,3,4-oxadiazole with nicotinoyl chloride and isonicotinoyl chloride, respectively. Ligand L1 can be used as an organic clip to bind CuII cations and generate a molecular complex, bis(4-methyl-{5-[5-methyl-2-(pyridin-3-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-3-carboxylate)bis(perchlorato)copper(II), [Cu(ClO4)2(C28H20N4O5)2], (I). In compound (I), the CuII cation is located on an inversion centre and is hexacoordinated in a distorted octahedral geometry, with the pyridine N atoms of two L1 ligands in the equatorial positions and two weakly coordinating perchlorate counter-ions in the axial positions. The two arms of the L1 ligands bend inward and converge at the CuII coordination point to give rise to a spirometallocycle. Ligand L2 binds CuI cations to generate a supramolecule, diacetonitriledi-μ3-iodido-di-μ2-iodido-bis(4-methyl-{5-[5-methyl-2-(pyridin-4-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-4-carboxylate)tetracopper(I), [Cu4I4(CH3CN)2(C28H20N4O5)2], (II). The asymmetric unit of (II) indicates that it contains two CuI atoms, one L2 ligand, one acetonitrile ligand and two iodide ligands. Both of the CuI atoms are four-coordinated in an approximately tetrahedral environment. The molecule is centrosymmetric and the four I atoms and four CuI atoms form a rope-ladder-type [Cu4I4] unit. Discrete units are linked into one-dimensional chains through π–π interactions. EN Two new symmetric double-armed oxadiazole-bridged ligands, 4-methyl-{5-[5-methyl-2-(pyridin-3-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-3-carboxylate (L1) and 4-methyl-{5-[5-methyl-2-(pyridin-4-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-4-carboxylate (L2), were prepared by the reaction of 2,5-bis(2-hydroxy-5-methylphenyl)-1,3,4-oxadiazole with nicotinoyl chloride and isonicotinoyl chloride, respectively. Ligand L1 can be used as an organic clip to bind CuII cations and generate a molecular complex, bis(4-methyl-{5-[5-methyl-2-(pyridin-3-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-3-carboxylate)bis(perchlorato)copper(II), [Cu(ClO4)2(C28H20N4O5)2], (I). In compound (I), the CuII cation is located on an inversion centre and is hexacoordinated in a distorted octahedral geometry, with the pyridine N atoms of two L1 ligands in the equatorial positions and two weakly coordinating perchlorate counter-ions in the axial positions. The two arms of the L1 ligands bend inward and converge at the CuII coordination point to give rise to a spirometallocycle. Ligand L2 binds CuI cations to generate a supramolecule, diacetonitriledi-μ3-iodido-di-μ2-iodido-bis(4-methyl-{5-[5-methyl-2-(pyridin-4-ylcarbonyloxy)phenyl]-1,3,4-oxadiazol-2-yl}phenyl pyridine-4-carboxylate)tetracopper(I), [Cu4I4(CH3CN)2(C28H20N4O5)2], (II). The asymmetric unit of (II) indicates that it contains two CuI atoms, one L2 ligand, one acetonitrile ligand and two iodide ligands. Both of the CuI atoms are four-coordinated in an approximately tetrahedral environment. The molecule is centrosymmetric and the four I atoms and four CuI atoms form a rope-ladder-type [Cu4I4] unit. Discrete units are linked into one-dimensional chains through π–π interactions. text/html The coordination chemistry of two symmetric double-armed oxadiazole-bridged organic ligands with copper salts text 6 69 2013-05-15 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?bg3157 In the title complex, [Cu(C16H16Cl3N3O2P)Cl(C12H8N2)], the CuII cation presents a square-pyramidal environment, where the CuO2N2 base is formed by two O atoms from carbonyl and phosphoryl groups, and by two N atoms from a 1,10-phenanthroline molecule. A coordinated Cl atom occupies the apex. N—H...Cl hydrogen bonds link the molecules into one-dimensional chains. The trichloromethyl group is rotationally disordered over two positions, with occupancies of 0.747 (7) and 0.253 (7). Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Gubina, K. Ovchynnikov, V. Amirkhanov, V. Shishkina, S. 2013-05-15 doi:10.1107/S0108270113011943 International Union of Crystallography In the title complex, [Cu(C16H16Cl3N3O2P)Cl(C12H8N2)], the CuII cation presents a square-pyramidal environment, where the CuO2N2 base is formed by two O atoms from carbonyl and phosphoryl groups, and by two N atoms from a 1,10-phenanthroline molecule. A coordinated Cl atom occupies the apex. N—H...Cl hydrogen bonds link the molecules into one-dimensional chains. The trichloromethyl group is rotationally disordered over two positions, with occupancies of 0.747 (7) and 0.253 (7). EN In the title complex, [Cu(C16H16Cl3N3O2P)Cl(C12H8N2)], the CuII cation presents a square-pyramidal environment, where the CuO2N2 base is formed by two O atoms from carbonyl and phosphoryl groups, and by two N atoms from a 1,10-phenanthroline molecule. A coordinated Cl atom occupies the apex. N—H...Cl hydrogen bonds link the molecules into one-dimensional chains. The trichloromethyl group is rotationally disordered over two positions, with occupancies of 0.747 (7) and 0.253 (7). text/html Chlorido[N,N′-dibenzyl-N′′-(trichloroacetyl)phosphoramidato-κ2O,O′](1,10-phenanthroline-κ2N,N′)copper(II) text 6 69 2013-05-15 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?bg3158 The cation-templated self-assembly of 1,4-bis(2-methyl-1H-imidazol-1-yl)butane (bmimb) with CuSCN gives rise to a novel two-dimensional network, namely catena-poly[2,2′-dimethyl-1,1′-(butane-1,4-diyl)bis(1H-imidazol-3-ium) [tetra-μ2-thiocyanato-κ4S:S;κ4S:N-dicopper(I)]], {(C12H20N4)[Cu2(NCS)4]}n. The CuI cation is four-coordinated by one N and three S atoms, giving a tetrahedral geometry. One of the two crystallographically independent SCN− anions acts as a μ2-S:S bridge, binding a pair of CuI cations into a centrosymmetric [Cu2(NCS)2] subunit, which is further extended into a two-dimensional 44-sql net by another kind of SCN− anion with an end-to-end μ2-S:N coordination mode. Interestingly, each H2bmimb dication, lying on an inversion centre, threads through one of the windows of the two-dimensional 44-sql net, giving a pseudorotaxane-like structure. The two-dimensional 44-sql networks are packed into the resultant three-dimensional supramolecular framework through bmimb–SCN N—H...N hydrogen bonds. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Liu, S.-S. Yuan, S. Lu, H.-F. Xu, M.-Z. Sun, D. 2013-05-15 doi:10.1107/S0108270113011992 International Union of Crystallography The cation-templated self-assembly of 1,4-bis(2-methyl-1H-imidazol-1-yl)butane (bmimb) with CuSCN gives rise to a novel two-dimensional network, namely catena-poly[2,2′-dimethyl-1,1′-(butane-1,4-diyl)bis(1H-imidazol-3-ium) [tetra-μ2-thiocyanato-κ4S:S;κ4S:N-dicopper(I)]], {(C12H20N4)[Cu2(NCS)4]}n. The CuI cation is four-coordinated by one N and three S atoms, giving a tetrahedral geometry. One of the two crystallographically independent SCN− anions acts as a μ2-S:S bridge, binding a pair of CuI cations into a centrosymmetric [Cu2(NCS)2] subunit, which is further extended into a two-dimensional 44-sql net by another kind of SCN− anion with an end-to-end μ2-S:N coordination mode. Interestingly, each H2bmimb dication, lying on an inversion centre, threads through one of the windows of the two-dimensional 44-sql net, giving a pseudorotaxane-like structure. The two-dimensional 44-sql networks are packed into the resultant three-dimensional supramolecular framework through bmimb–SCN N—H...N hydrogen bonds. EN The cation-templated self-assembly of 1,4-bis(2-methyl-1H-imidazol-1-yl)butane (bmimb) with CuSCN gives rise to a novel two-dimensional network, namely catena-poly[2,2′-dimethyl-1,1′-(butane-1,4-diyl)bis(1H-imidazol-3-ium) [tetra-μ2-thiocyanato-κ4S:S;κ4S:N-dicopper(I)]], {(C12H20N4)[Cu2(NCS)4]}n. The CuI cation is four-coordinated by one N and three S atoms, giving a tetrahedral geometry. One of the two crystallographically independent SCN− anions acts as a μ2-S:S bridge, binding a pair of CuI cations into a centrosymmetric [Cu2(NCS)2] subunit, which is further extended into a two-dimensional 44-sql net by another kind of SCN− anion with an end-to-end μ2-S:N coordination mode. Interestingly, each H2bmimb dication, lying on an inversion centre, threads through one of the windows of the two-dimensional 44-sql net, giving a pseudorotaxane-like structure. The two-dimensional 44-sql networks are packed into the resultant three-dimensional supramolecular framework through bmimb–SCN N—H...N hydrogen bonds. text/html A novel two-dimensional CuSCN network templated by 2,2′-dimethyl-1,1′-(butane-1,4-diyl)bis(1H-imidazol-3-ium) cations text 6 69 2013-05-15 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?fn3135 The title compound, [Cu8(C15H10N3O3S)4Cl4(C3H7NO)2]·2C3H7NO, consisting of eight CuII cations, four trianionic 1-(2-oxidobenzoyl)-2-(2-oxo-2-phenylethanethioyl)hydrazine-1,2-diide ligands, four chloride ligands and two coordinated and two solvent dimethylformamide molecules, crystallizes with the octanuclear molecule located on an inversion centre. The two halves of the molecule are connected by two bridging Cl atoms. This is the first example of an octanuclear complex based on a thiosemicarbazone-derived ligand. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Liu, J.-J. Liao, J.-Z. Li, Z.-Y. Wang, Y. Huang, C.-C. 2013-05-17 doi:10.1107/S0108270113012547 International Union of Crystallography The title compound, [Cu8(C15H10N3O3S)4Cl4(C3H7NO)2]·2C3H7NO, consisting of eight CuII cations, four trianionic 1-(2-oxidobenzoyl)-2-(2-oxo-2-phenylethanethioyl)hydrazine-1,2-diide ligands, four chloride ligands and two coordinated and two solvent dimethylformamide molecules, crystallizes with the octanuclear molecule located on an inversion centre. The two halves of the molecule are connected by two bridging Cl atoms. This is the first example of an octanuclear complex based on a thiosemicarbazone-derived ligand. EN The title compound, [Cu8(C15H10N3O3S)4Cl4(C3H7NO)2]·2C3H7NO, consisting of eight CuII cations, four trianionic 1-(2-oxidobenzoyl)-2-(2-oxo-2-phenylethanethioyl)hydrazine-1,2-diide ligands, four chloride ligands and two coordinated and two solvent dimethylformamide molecules, crystallizes with the octanuclear molecule located on an inversion centre. The two halves of the molecule are connected by two bridging Cl atoms. This is the first example of an octanuclear complex based on a thiosemicarbazone-derived ligand. text/html Di-μ2-chlorido-dichloridobis(dimethylformamide)tetrakis[μ3-1-(2-oxidobenzoyl)-2-(2-oxo-2-phenylethanethioyl)hydrazine-1,2-diido]octacopper(II) dimethylformamide disolvate text 6 69 2013-05-17 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?lg3108 A new metal–formate framework, poly[1H-imidazol-3-ium [tri-μ2-formato-manganese(II)]], {(C3H5N2)[Mn(HCOO)3]}n, was synthesized and its structural phase transition was studied by thermal analysis and variable-temperature X-ray diffraction analysis. The transition temperature is around 435 K. The high-temperature phase is tetragonal and the low-temperature phase is monoclinic, with a β angle close to 90°. The relationship of the unit cells between the two phases can be described as: aHT = 0.5aLT + 0.5bLT; bHT = −0.5aLT + 0.5bLT; cHT = 0.5cLT. In the high-temperature phase, both the framework and the guest 1H-imidazol-3-ium (HIm) cations are disordered; the HIm cations are located about 2mm sites and were modelled as fourfold disordered. The Mn and a formate C atom are located on fourfold rotary inversion axes, while another formate C atom is on a mirror plane. The low-temperature structure is ordered and consists of two crystallographically independent HIm cations and two crystallographically independent Mn2+ ions. The phase transition is attributable to the order–disorder transition of the HIm cations. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Wang, B.-Q. Yan, H.-B. Huang, Z.-Q. Zhang, Z. 2013-05-17 doi:10.1107/S0108270113012638 International Union of Crystallography A new metal–formate framework, poly[1H-imidazol-3-ium [tri-μ2-formato-manganese(II)]], {(C3H5N2)[Mn(HCOO)3]}n, was synthesized and its structural phase transition was studied by thermal analysis and variable-temperature X-ray diffraction analysis. The transition temperature is around 435 K. The high-temperature phase is tetragonal and the low-temperature phase is monoclinic, with a β angle close to 90°. The relationship of the unit cells between the two phases can be described as: aHT = 0.5aLT + 0.5bLT; bHT = −0.5aLT + 0.5bLT; cHT = 0.5cLT. In the high-temperature phase, both the framework and the guest 1H-imidazol-3-ium (HIm) cations are disordered; the HIm cations are located about 2mm sites and were modelled as fourfold disordered. The Mn and a formate C atom are located on fourfold rotary inversion axes, while another formate C atom is on a mirror plane. The low-temperature structure is ordered and consists of two crystallographically independent HIm cations and two crystallographically independent Mn2+ ions. The phase transition is attributable to the order–disorder transition of the HIm cations. EN A new metal–formate framework, poly[1H-imidazol-3-ium [tri-μ2-formato-manganese(II)]], {(C3H5N2)[Mn(HCOO)3]}n, was synthesized and its structural phase transition was studied by thermal analysis and variable-temperature X-ray diffraction analysis. The transition temperature is around 435 K. The high-temperature phase is tetragonal and the low-temperature phase is monoclinic, with a β angle close to 90°. The relationship of the unit cells between the two phases can be described as: aHT = 0.5aLT + 0.5bLT; bHT = −0.5aLT + 0.5bLT; cHT = 0.5cLT. In the high-temperature phase, both the framework and the guest 1H-imidazol-3-ium (HIm) cations are disordered; the HIm cations are located about 2mm sites and were modelled as fourfold disordered. The Mn and a formate C atom are located on fourfold rotary inversion axes, while another formate C atom is on a mirror plane. The low-temperature structure is ordered and consists of two crystallographically independent HIm cations and two crystallographically independent Mn2+ ions. The phase transition is attributable to the order–disorder transition of the HIm cations. text/html Reversible high-temperature phase transition of a manganese(II) formate framework with imidazolium cations text 6 69 2013-05-17 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?wq3034 In the crystal structure of the title two-dimensional metal–organic polymeric complex, [Cd2Cl4(C8H14N2O4)(H2O)2]n, the asymmetric unit contains a crystallographically independent CdII cation, two chloride ligands, an aqua ligand and half a 2,2′-(piperazine-1,4-diium-1,4-diyl)diacetate (H2PDA) ligand, the piperazine ring centroid of which is located on a crystallographic inversion centre. Each CdII centre is six-coordinated in an octahedral environment by an O atom from an H2PDA ligand and an O atom from an aqua ligand in a trans disposition, and by four chloride ligands arranged in the plane perpendicular to the O—Cd—O axis. The complex forms a two-dimensional layer polymer containing [CdCl2]n chains, which are interconnected into an extensive three-dimensional hydrogen-bonded network by C—H...O, C—H...Cl and O—H...O hydrogen bonds. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Xu, X.-J. Miao, J.-Y. Wang, J. 2013-05-18 doi:10.1107/S0108270113013000 International Union of Crystallography In the crystal structure of the title two-dimensional metal–organic polymeric complex, [Cd2Cl4(C8H14N2O4)(H2O)2]n, the asymmetric unit contains a crystallographically independent CdII cation, two chloride ligands, an aqua ligand and half a 2,2′-(piperazine-1,4-diium-1,4-diyl)diacetate (H2PDA) ligand, the piperazine ring centroid of which is located on a crystallographic inversion centre. Each CdII centre is six-coordinated in an octahedral environment by an O atom from an H2PDA ligand and an O atom from an aqua ligand in a trans disposition, and by four chloride ligands arranged in the plane perpendicular to the O—Cd—O axis. The complex forms a two-dimensional layer polymer containing [CdCl2]n chains, which are interconnected into an extensive three-dimensional hydrogen-bonded network by C—H...O, C—H...Cl and O—H...O hydrogen bonds. EN In the crystal structure of the title two-dimensional metal–organic polymeric complex, [Cd2Cl4(C8H14N2O4)(H2O)2]n, the asymmetric unit contains a crystallographically independent CdII cation, two chloride ligands, an aqua ligand and half a 2,2′-(piperazine-1,4-diium-1,4-diyl)diacetate (H2PDA) ligand, the piperazine ring centroid of which is located on a crystallographic inversion centre. Each CdII centre is six-coordinated in an octahedral environment by an O atom from an H2PDA ligand and an O atom from an aqua ligand in a trans disposition, and by four chloride ligands arranged in the plane perpendicular to the O—Cd—O axis. The complex forms a two-dimensional layer polymer containing [CdCl2]n chains, which are interconnected into an extensive three-dimensional hydrogen-bonded network by C—H...O, C—H...Cl and O—H...O hydrogen bonds. text/html A novel two-dimensional coordination polymer: poly[diaquatetra-μ2-chlorido-[μ2-2,2′-(piperazine-1,4-diium-1,4-diyl)diacetate]dicadmium(II)] text 6 69 2013-05-18 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?sk3487 The title compound, [CuBr(C6H7NO)2]Br·H2O, is an ionic mononuclear complex in which the [CuBr(C6H7NO)2]+ cation possesses distorted square-pyramidal geometry. The CuII centre is coordinated by two neutral 2-(pyridin-2-yl)methanol (2-pyMeOH) ligands and a terminal bromide ligand. The 2-pyMeOH ligands are coordinated in a bidentate chelating manner through the pyridine N and hydroxy O atoms, forming a five-membered chelate ring with the CuII centre. The planes of the pyridine rings are twisted by 58.71 (14)° with respect to each other. The charge is balanced by a noncoordinating bromide anion which, together with a solvent water molecule, links the components through hydrogen bonds into infinite chains propagating along the a axis. The mononuclear cations appear to associate in pairs through weak interactions between the metal atom of one cation and the halogen atom of an adjacent cation. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Lah, N. Lapanje, K. 2013-05-24 doi:10.1107/S0108270113013437 International Union of Crystallography The title compound, [CuBr(C6H7NO)2]Br·H2O, is an ionic mononuclear complex in which the [CuBr(C6H7NO)2]+ cation possesses distorted square-pyramidal geometry. The CuII centre is coordinated by two neutral 2-(pyridin-2-yl)methanol (2-pyMeOH) ligands and a terminal bromide ligand. The 2-pyMeOH ligands are coordinated in a bidentate chelating manner through the pyridine N and hydroxy O atoms, forming a five-membered chelate ring with the CuII centre. The planes of the pyridine rings are twisted by 58.71 (14)° with respect to each other. The charge is balanced by a noncoordinating bromide anion which, together with a solvent water molecule, links the components through hydrogen bonds into infinite chains propagating along the a axis. The mononuclear cations appear to associate in pairs through weak interactions between the metal atom of one cation and the halogen atom of an adjacent cation. EN The title compound, [CuBr(C6H7NO)2]Br·H2O, is an ionic mononuclear complex in which the [CuBr(C6H7NO)2]+ cation possesses distorted square-pyramidal geometry. The CuII centre is coordinated by two neutral 2-(pyridin-2-yl)methanol (2-pyMeOH) ligands and a terminal bromide ligand. The 2-pyMeOH ligands are coordinated in a bidentate chelating manner through the pyridine N and hydroxy O atoms, forming a five-membered chelate ring with the CuII centre. The planes of the pyridine rings are twisted by 58.71 (14)° with respect to each other. The charge is balanced by a noncoordinating bromide anion which, together with a solvent water molecule, links the components through hydrogen bonds into infinite chains propagating along the a axis. The mononuclear cations appear to associate in pairs through weak interactions between the metal atom of one cation and the halogen atom of an adjacent cation. text/html Bromidobis[2-(pyridin-2-yl)methanol-κ2N,O]copper(II) bromide monohydrate text 6 69 2013-05-24 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications metal-organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?gz3236 The title compound, C8H12Br4, displays crystallographic inversion symmetry, so that the cyclobutane ring is exactly planar. The ring C—C bond with eclipsed substituents is lengthened somewhat to 1.572 (5) Å. The packing can be described in terms of three Br...Br contacts; two of these combine to form layers of molecules parallel to the ac plane, while the third crosslinks the layers in the third dimension. A simple topological descriptor for systems involving Br...Br contacts is proposed. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Kelch, A. Dix, I. Hopf, H. Jones, P.G. 2013-05-02 doi:10.1107/S0108270113010597 International Union of Crystallography The title compound, C8H12Br4, displays crystallographic inversion symmetry, so that the cyclobutane ring is exactly planar. The ring C—C bond with eclipsed substituents is lengthened somewhat to 1.572 (5) Å. The packing can be described in terms of three Br...Br contacts; two of these combine to form layers of molecules parallel to the ac plane, while the third crosslinks the layers in the third dimension. A simple topological descriptor for systems involving Br...Br contacts is proposed. EN The title compound, C8H12Br4, displays crystallographic inversion symmetry, so that the cyclobutane ring is exactly planar. The ring C—C bond with eclipsed substituents is lengthened somewhat to 1.572 (5) Å. The packing can be described in terms of three Br...Br contacts; two of these combine to form layers of molecules parallel to the ac plane, while the third crosslinks the layers in the third dimension. A simple topological descriptor for systems involving Br...Br contacts is proposed. text/html Bromine–bromine interactions in the packing of cis,trans,cis-1,2,3,4-tetrakis(bromomethyl)cyclobutane text 6 69 2013-05-02 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?tp3019 Low-temperature X-ray diffraction experiments were employed to investigate the crystal structures of an orthorhombic polymorph of the intramolecular cyclization product of perindopril, a popular angiotensive-converting enzyme (ACE) inhibitor, namely ethyl (2S)-2-[(3S,5aS,9aS,10aS)-3-methyl-1,4-dioxo-5a,6,7,8,9,9a,10,10a-octahydro-3H-pyrazino[1,2-a]indol-2-yl]pentanoate, C19H30N2O4, (Io), and its tetragonal equivalent, (It), which was previously reported at ambient temperature [Bojarska et al. (2013). J. Chil. Chem. Soc. 58, 1415–1417]. Polymorph (Io) crystallizes in the orthorhombic space group P212121 with two molecules in the asymmetric unit, while tetragonal form (It) crystallizes in the space group P41212 with one molecule in the asymmetric unit. The geometric parameters of (Io) are very similar to those of (It). The six-membered rings in both polymorphs adopt a slightly deformed chair conformation and the piperazinedione rings are in a boat conformation. However, the proline rings adopt an envelope conformation in (Io), while in (It) the ring exists in a slightly deformed half-chair conformation. The most significant difference between the two structures is the orientation of the ethyl pentanoate chain. Molecules associate in pairs in a head-to-tail manner forming infinite columns. In (Io), molecules are related by a twofold screw axis forming identical columns, while in (It), molecules in successive neighbouring columns are related by alternating twofold screw axes and fourfold screw axes. In both cases, the crystal packing is stabilized by weak intermolecular C—H...O interactions only. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Bojarska, J. Maniukiewicz, W. Sieroń, L. Remko, M. 2013-05-02 doi:10.1107/S0108270113011025 International Union of Crystallography Low-temperature X-ray diffraction experiments were employed to investigate the crystal structures of an orthorhombic polymorph of the intramolecular cyclization product of perindopril, a popular angiotensive-converting enzyme (ACE) inhibitor, namely ethyl (2S)-2-[(3S,5aS,9aS,10aS)-3-methyl-1,4-dioxo-5a,6,7,8,9,9a,10,10a-octahydro-3H-pyrazino[1,2-a]indol-2-yl]pentanoate, C19H30N2O4, (Io), and its tetragonal equivalent, (It), which was previously reported at ambient temperature [Bojarska et al. (2013). J. Chil. Chem. Soc. 58, 1415–1417]. Polymorph (Io) crystallizes in the orthorhombic space group P212121 with two molecules in the asymmetric unit, while tetragonal form (It) crystallizes in the space group P41212 with one molecule in the asymmetric unit. The geometric parameters of (Io) are very similar to those of (It). The six-membered rings in both polymorphs adopt a slightly deformed chair conformation and the piperazinedione rings are in a boat conformation. However, the proline rings adopt an envelope conformation in (Io), while in (It) the ring exists in a slightly deformed half-chair conformation. The most significant difference between the two structures is the orientation of the ethyl pentanoate chain. Molecules associate in pairs in a head-to-tail manner forming infinite columns. In (Io), molecules are related by a twofold screw axis forming identical columns, while in (It), molecules in successive neighbouring columns are related by alternating twofold screw axes and fourfold screw axes. In both cases, the crystal packing is stabilized by weak intermolecular C—H...O interactions only. EN Low-temperature X-ray diffraction experiments were employed to investigate the crystal structures of an orthorhombic polymorph of the intramolecular cyclization product of perindopril, a popular angiotensive-converting enzyme (ACE) inhibitor, namely ethyl (2S)-2-[(3S,5aS,9aS,10aS)-3-methyl-1,4-dioxo-5a,6,7,8,9,9a,10,10a-octahydro-3H-pyrazino[1,2-a]indol-2-yl]pentanoate, C19H30N2O4, (Io), and its tetragonal equivalent, (It), which was previously reported at ambient temperature [Bojarska et al. (2013). J. Chil. Chem. Soc. 58, 1415–1417]. Polymorph (Io) crystallizes in the orthorhombic space group P212121 with two molecules in the asymmetric unit, while tetragonal form (It) crystallizes in the space group P41212 with one molecule in the asymmetric unit. The geometric parameters of (Io) are very similar to those of (It). The six-membered rings in both polymorphs adopt a slightly deformed chair conformation and the piperazinedione rings are in a boat conformation. However, the proline rings adopt an envelope conformation in (Io), while in (It) the ring exists in a slightly deformed half-chair conformation. The most significant difference between the two structures is the orientation of the ethyl pentanoate chain. Molecules associate in pairs in a head-to-tail manner forming infinite columns. In (Io), molecules are related by a twofold screw axis forming identical columns, while in (It), molecules in successive neighbouring columns are related by alternating twofold screw axes and fourfold screw axes. In both cases, the crystal packing is stabilized by weak intermolecular C—H...O interactions only. text/html An orthorhombic polymorph of a cyclization product of perindopril text 6 69 2013-05-02 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?wq3031 The title compound, C58H64S8, has been prepared by Pd-catalysed direct C—H arylation of tetrathienonaphthalene (TTN) with 5-hexyl-2-iodothiophene and recrystallized by slow evaporation from dichloromethane. The crystal structure shows a completely planar geometry of the TTN core, crystallizing in the monoclinic space group P21/c. The structure consists of slipped π-stacks and the interfacial distance between the mean planes of the TTN cores is 3.456 (5) Å, which is slightly larger than that of the comparable derivative of tetrathienoanthracene (TTA) with 2-hexylthiophene groups. The packing in the two structures is greatly influenced by both the aromatic core of the structure and the alkyl side chains. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Gao, L. 2013-05-02 doi:10.1107/S0108270113010895 International Union of Crystallography The title compound, C58H64S8, has been prepared by Pd-catalysed direct C—H arylation of tetrathienonaphthalene (TTN) with 5-hexyl-2-iodothiophene and recrystallized by slow evaporation from dichloromethane. The crystal structure shows a completely planar geometry of the TTN core, crystallizing in the monoclinic space group P21/c. The structure consists of slipped π-stacks and the interfacial distance between the mean planes of the TTN cores is 3.456 (5) Å, which is slightly larger than that of the comparable derivative of tetrathienoanthracene (TTA) with 2-hexylthiophene groups. The packing in the two structures is greatly influenced by both the aromatic core of the structure and the alkyl side chains. EN The title compound, C58H64S8, has been prepared by Pd-catalysed direct C—H arylation of tetrathienonaphthalene (TTN) with 5-hexyl-2-iodothiophene and recrystallized by slow evaporation from dichloromethane. The crystal structure shows a completely planar geometry of the TTN core, crystallizing in the monoclinic space group P21/c. The structure consists of slipped π-stacks and the interfacial distance between the mean planes of the TTN cores is 3.456 (5) Å, which is slightly larger than that of the comparable derivative of tetrathienoanthracene (TTA) with 2-hexylthiophene groups. The packing in the two structures is greatly influenced by both the aromatic core of the structure and the alkyl side chains. text/html Synthesis and photophysical properties of 2,5,8,11-tetrakis(5-hexylthiophen-2-yl)tetrathieno[2,3-a:3′,2′-c:2′′,3′′-f:3′′′,2′′′-h]naphthalene text 6 69 2013-05-02 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?sf3191 The crystal structures of 3,4,6a,7,10,10a-hexahydro-7,10-epoxypyrimido[2,1-a]isoindol-6(2H)-one, C11H12N2O2, and 2-(2-aminoethyl)-3a,4,7,7a-tetrahydro-1H-4,7-epoxyisoindole-1,3(2H)-dione, C10H12N2O3, two tricyclic imides, show one and two molecules in the asymmetric unit, respectively. Intermolecular hydrogen-bonding interactions are observed in both compounds. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Mitchell, L.A. Stanley, J.M. Espinosa De Hoyos, L. Holliday, B.J. 2013-05-02 doi:10.1107/S0108270113010706 International Union of Crystallography The crystal structures of 3,4,6a,7,10,10a-hexahydro-7,10-epoxypyrimido[2,1-a]isoindol-6(2H)-one, C11H12N2O2, and 2-(2-aminoethyl)-3a,4,7,7a-tetrahydro-1H-4,7-epoxyisoindole-1,3(2H)-dione, C10H12N2O3, two tricyclic imides, show one and two molecules in the asymmetric unit, respectively. Intermolecular hydrogen-bonding interactions are observed in both compounds. EN The crystal structures of 3,4,6a,7,10,10a-hexahydro-7,10-epoxypyrimido[2,1-a]isoindol-6(2H)-one, C11H12N2O2, and 2-(2-aminoethyl)-3a,4,7,7a-tetrahydro-1H-4,7-epoxyisoindole-1,3(2H)-dione, C10H12N2O3, two tricyclic imides, show one and two molecules in the asymmetric unit, respectively. Intermolecular hydrogen-bonding interactions are observed in both compounds. text/html A comparison of 3,4,6a,7,10,10a-hexahydro-7,10-epoxypyrimido[2,1-a]isoindol-6(2H)-one and 2-(2-aminoethyl)-3a,4,7,7a-tetrahydro-1H-4,7-epoxyisoindole-1,3(2H)-dione: structural and reactivity differences of two homologous tricyclic imides text 6 69 2013-05-02 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?ov3028 The three pyran structures 6-methylamino-5-nitro-2,4-diphenyl-4H-pyran-3-carbonitrile, C19H15N3O3, (I), 4-(3-fluorophenyl)-6-methylamino-5-nitro-2-phenyl-4H-pyran-3-carbonitrile, C19H14FN3O3, (II), and 4-(4-chlorophenyl)-6-methylamino-5-nitro-2-phenyl-4H-pyran-3-carbonitrile, C19H14ClN3O3, (III), differ in the nature of the aryl group at the 4-position. The heterocyclic ring in all three structures adopts a flattened boat conformation. The dihedral angle between the pseudo-axial phenyl substituent and the flat part of the pyran ring is 89.97 (1)° in (I), 80.11 (1)° in (II) and 87.77 (1)° in (III). In all three crystal structures, a strong intramolecular N—H...O hydrogen bond links the flat conjugated H—N—C=C—N—O fragment into a six-membered ring. In (II), molecules are linked into dimeric aggregates by N—H... O(nitro) hydrogen bonds, generating an R22(12) graph-set motif. In (III), intermolecular N—H...N and C—H...N hydrogen bonds link the molecules into a linear chain pattern generating C(8) and C(9) graph-set motifs, respectively. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Vishnupriya, R. Suresh, J. Sivakumar, S. Kumar, R.R. 2013-05-02 doi:10.1107/S0108270113010676 International Union of Crystallography The three pyran structures 6-methylamino-5-nitro-2,4-diphenyl-4H-pyran-3-carbonitrile, C19H15N3O3, (I), 4-(3-fluorophenyl)-6-methylamino-5-nitro-2-phenyl-4H-pyran-3-carbonitrile, C19H14FN3O3, (II), and 4-(4-chlorophenyl)-6-methylamino-5-nitro-2-phenyl-4H-pyran-3-carbonitrile, C19H14ClN3O3, (III), differ in the nature of the aryl group at the 4-position. The heterocyclic ring in all three structures adopts a flattened boat conformation. The dihedral angle between the pseudo-axial phenyl substituent and the flat part of the pyran ring is 89.97 (1)° in (I), 80.11 (1)° in (II) and 87.77 (1)° in (III). In all three crystal structures, a strong intramolecular N—H...O hydrogen bond links the flat conjugated H—N—C=C—N—O fragment into a six-membered ring. In (II), molecules are linked into dimeric aggregates by N—H... O(nitro) hydrogen bonds, generating an R22(12) graph-set motif. In (III), intermolecular N—H...N and C—H...N hydrogen bonds link the molecules into a linear chain pattern generating C(8) and C(9) graph-set motifs, respectively. EN The three pyran structures 6-methylamino-5-nitro-2,4-diphenyl-4H-pyran-3-carbonitrile, C19H15N3O3, (I), 4-(3-fluorophenyl)-6-methylamino-5-nitro-2-phenyl-4H-pyran-3-carbonitrile, C19H14FN3O3, (II), and 4-(4-chlorophenyl)-6-methylamino-5-nitro-2-phenyl-4H-pyran-3-carbonitrile, C19H14ClN3O3, (III), differ in the nature of the aryl group at the 4-position. The heterocyclic ring in all three structures adopts a flattened boat conformation. The dihedral angle between the pseudo-axial phenyl substituent and the flat part of the pyran ring is 89.97 (1)° in (I), 80.11 (1)° in (II) and 87.77 (1)° in (III). In all three crystal structures, a strong intramolecular N—H...O hydrogen bond links the flat conjugated H—N—C=C—N—O fragment into a six-membered ring. In (II), molecules are linked into dimeric aggregates by N—H... O(nitro) hydrogen bonds, generating an R22(12) graph-set motif. In (III), intermolecular N—H...N and C—H...N hydrogen bonds link the molecules into a linear chain pattern generating C(8) and C(9) graph-set motifs, respectively. text/html N—H...O and N—H...N interactions in three pyran derivatives text 6 69 2013-05-02 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?gz3232 (2S,3S)-2,6-Dimethylheptane-1,3-diol, C9H20O2, (I), was synthesized from the ketone (R)-4-benzyl-3-[(2R,3S)-3-hydroxy-2,6-dimethylheptanoyl]-1,3-oxazolidin-2-one, C19H27NO4, (II), containing C atoms of known chirality. In both structures, strong hydrogen bonds between the hydroxy groups form tape motifs. The contribution from weaker C—H...O hydrogen bonds is much more evident in the structure of (II), which furthermore contains an example of a direct short Osp3...Csp2 contact that represents a usually unrecognized type of intermolecular interaction. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Høgmoen Åstrand, O.A. Iqbal, Z. Sandberg, M. Kase, E.T. Görbitz, C.H. Rongved, P. 2013-05-15 doi:10.1107/S0108270113011852 International Union of Crystallography (2S,3S)-2,6-Dimethylheptane-1,3-diol, C9H20O2, (I), was synthesized from the ketone (R)-4-benzyl-3-[(2R,3S)-3-hydroxy-2,6-dimethylheptanoyl]-1,3-oxazolidin-2-one, C19H27NO4, (II), containing C atoms of known chirality. In both structures, strong hydrogen bonds between the hydroxy groups form tape motifs. The contribution from weaker C—H...O hydrogen bonds is much more evident in the structure of (II), which furthermore contains an example of a direct short Osp3...Csp2 contact that represents a usually unrecognized type of intermolecular interaction. EN (2S,3S)-2,6-Dimethylheptane-1,3-diol, C9H20O2, (I), was synthesized from the ketone (R)-4-benzyl-3-[(2R,3S)-3-hydroxy-2,6-dimethylheptanoyl]-1,3-oxazolidin-2-one, C19H27NO4, (II), containing C atoms of known chirality. In both structures, strong hydrogen bonds between the hydroxy groups form tape motifs. The contribution from weaker C—H...O hydrogen bonds is much more evident in the structure of (II), which furthermore contains an example of a direct short Osp3...Csp2 contact that represents a usually unrecognized type of intermolecular interaction. text/html (2S,3S)-2,6-Dimethylheptane-1,3-diol, the oxygenated side chain of 22(S)-hydroxycholestrol, and its synthetic precursor (R)-4-benzyl-3-[(2R,3S)-3-hydroxy-2,6-dimethylheptanoyl]-1,3-oxazolidin-2-one text 6 69 2013-05-15 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?mx3095 The core of the novel title centrosymmetric porphyrin derivative, C72H86N4O4, with long flexible hexyloxy substituents, is almost planar, which is anticipated to facilitate π-electron delocalization and lead to a significant deviation between the planes of the benzene rings and the molecular plane. The two N-bound H atoms on the pyrrole rings are disordered and the occupancy factors refined to a ratio of 0.28 (2):0.72 (2). Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Zhao, H.-B. Chen, L. Wang, B.-Y. Liao, J.-X. Xu, Y.-J. 2013-05-15 doi:10.1107/S0108270113011232 International Union of Crystallography The core of the novel title centrosymmetric porphyrin derivative, C72H86N4O4, with long flexible hexyloxy substituents, is almost planar, which is anticipated to facilitate π-electron delocalization and lead to a significant deviation between the planes of the benzene rings and the molecular plane. The two N-bound H atoms on the pyrrole rings are disordered and the occupancy factors refined to a ratio of 0.28 (2):0.72 (2). EN The core of the novel title centrosymmetric porphyrin derivative, C72H86N4O4, with long flexible hexyloxy substituents, is almost planar, which is anticipated to facilitate π-electron delocalization and lead to a significant deviation between the planes of the benzene rings and the molecular plane. The two N-bound H atoms on the pyrrole rings are disordered and the occupancy factors refined to a ratio of 0.28 (2):0.72 (2). text/html meso-Tetrakis[4-(heptyloxy)phenyl]porphyrin text 6 69 2013-05-15 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?uk3066 Levulinic acid derivatives are potential `green chemistry' renewably sourced molecules with utility in industrial coatings applications. Suitable single crystals of the centrosymmetric title compounds, C14H22O6 and C16H26O6, respectively, were obtained with difficulty. The data for the latter hexane-1,6-diyl compound were extracted from the major fragment of a three-component twinned crystal. Both compounds crystallize in similar-sized unit cells with identical symmetry, utilizing the same weak nonconventional attractive C—H...O(ketone) hydrogen bonds via C(4) and C(5) motifs, which expand to R22(30) ring and C22(14) chain motifs. Their different packing orientations in similar-sized unit cells suggest that crystal growth involving packing mixes could lead to intergrowths or twins. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Gainsford, G.J. Hinkley, S. 2013-05-17 doi:10.1107/S0108270113011980 International Union of Crystallography Levulinic acid derivatives are potential `green chemistry' renewably sourced molecules with utility in industrial coatings applications. Suitable single crystals of the centrosymmetric title compounds, C14H22O6 and C16H26O6, respectively, were obtained with difficulty. The data for the latter hexane-1,6-diyl compound were extracted from the major fragment of a three-component twinned crystal. Both compounds crystallize in similar-sized unit cells with identical symmetry, utilizing the same weak nonconventional attractive C—H...O(ketone) hydrogen bonds via C(4) and C(5) motifs, which expand to R22(30) ring and C22(14) chain motifs. Their different packing orientations in similar-sized unit cells suggest that crystal growth involving packing mixes could lead to intergrowths or twins. EN Levulinic acid derivatives are potential `green chemistry' renewably sourced molecules with utility in industrial coatings applications. Suitable single crystals of the centrosymmetric title compounds, C14H22O6 and C16H26O6, respectively, were obtained with difficulty. The data for the latter hexane-1,6-diyl compound were extracted from the major fragment of a three-component twinned crystal. Both compounds crystallize in similar-sized unit cells with identical symmetry, utilizing the same weak nonconventional attractive C—H...O(ketone) hydrogen bonds via C(4) and C(5) motifs, which expand to R22(30) ring and C22(14) chain motifs. Their different packing orientations in similar-sized unit cells suggest that crystal growth involving packing mixes could lead to intergrowths or twins. text/html Alkyl levulinates as `green chemistry' precursors: butane-1,4-diyl bis(4-oxopentanoate) and hexane-1,6-diyl bis(4-oxopentanoate) text 6 69 2013-05-17 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?yp3029 Reaction between cysteamine (systematic name: 2-aminoethanethiol, C2H7NS) and l-(+)-tartaric acid [systematic name: (2R,3R)-2,3-dihydroxybutanedioic acid, C4H6O6] results in a mixture of cysteamine tartrate(1−) monohydrate, C2H8NS+·C4H5O6−·H2O, (I), and cystamine bis[tartrate(1−)] dihydrate, C4H14N2S22+·2C4H5O6−·2H2O, (III). Cystamine [systematic name: 2,2′-dithiobis(ethylamine), C4H12N2S2], reacts with l-(+)-tartaric acid to produce a mixture of cystamine tartrate(2−), C4H14N2S22+·C4H4O62−, (II), and (III). In each crystal structure, the anions are linked by O—H...O hydrogen bonds that run parallel to the a axis. In addition, hydrogen bonding involving protonated amino groups in all three salts, and water molecules in (I) and (III), leads to extensive three-dimensional hydrogen-bonding networks. All three salts crystallize in the orthorhombic space group P212121. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Benylles, A. Cairns, D. Cox, P.J. Kay, G. 2013-05-17 doi:10.1107/S0108270113012377 International Union of Crystallography Reaction between cysteamine (systematic name: 2-aminoethanethiol, C2H7NS) and l-(+)-tartaric acid [systematic name: (2R,3R)-2,3-dihydroxybutanedioic acid, C4H6O6] results in a mixture of cysteamine tartrate(1−) monohydrate, C2H8NS+·C4H5O6−·H2O, (I), and cystamine bis[tartrate(1−)] dihydrate, C4H14N2S22+·2C4H5O6−·2H2O, (III). Cystamine [systematic name: 2,2′-dithiobis(ethylamine), C4H12N2S2], reacts with l-(+)-tartaric acid to produce a mixture of cystamine tartrate(2−), C4H14N2S22+·C4H4O62−, (II), and (III). In each crystal structure, the anions are linked by O—H...O hydrogen bonds that run parallel to the a axis. In addition, hydrogen bonding involving protonated amino groups in all three salts, and water molecules in (I) and (III), leads to extensive three-dimensional hydrogen-bonding networks. All three salts crystallize in the orthorhombic space group P212121. EN Reaction between cysteamine (systematic name: 2-aminoethanethiol, C2H7NS) and l-(+)-tartaric acid [systematic name: (2R,3R)-2,3-dihydroxybutanedioic acid, C4H6O6] results in a mixture of cysteamine tartrate(1−) monohydrate, C2H8NS+·C4H5O6−·H2O, (I), and cystamine bis[tartrate(1−)] dihydrate, C4H14N2S22+·2C4H5O6−·2H2O, (III). Cystamine [systematic name: 2,2′-dithiobis(ethylamine), C4H12N2S2], reacts with l-(+)-tartaric acid to produce a mixture of cystamine tartrate(2−), C4H14N2S22+·C4H4O62−, (II), and (III). In each crystal structure, the anions are linked by O—H...O hydrogen bonds that run parallel to the a axis. In addition, hydrogen bonding involving protonated amino groups in all three salts, and water molecules in (I) and (III), leads to extensive three-dimensional hydrogen-bonding networks. All three salts crystallize in the orthorhombic space group P212121. text/html Three salts from the reactions of cysteamine and cystamine with l-(+)-tartaric acid text 6 69 2013-05-17 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?tp3021 In the crystal structure of 6-methoxyquinoline N-oxide dihydrate, C10H9NO2·2H2O, (I), the presence of two-dimensional water networks is analysed. The water molecules form unusual water channels, as well as two intersecting mutually perpendicular columns. In one of these channels, the O atom of the N-oxide group acts as a bridge between the water molecules. The other channel is formed exclusively by water molecules. Confirmation of the molecular packing was performed through the analysis of Hirshfeld surfaces, and (I) is compared with other similar isoquinoline systems. Calculations of bond lengths and angles by the Hartree–Fock method or by density functional theory B3LYP, both with 6-311++G(d,p) basis sets, are reported, together with the results of additional IR, UV–Vis and theoretical studies. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Moreno-Fuquen, R. Hernandez, G. Kennedy, A.R. Morrison, C.A. 2013-05-17 doi:10.1107/S0108270113011979 International Union of Crystallography In the crystal structure of 6-methoxyquinoline N-oxide dihydrate, C10H9NO2·2H2O, (I), the presence of two-dimensional water networks is analysed. The water molecules form unusual water channels, as well as two intersecting mutually perpendicular columns. In one of these channels, the O atom of the N-oxide group acts as a bridge between the water molecules. The other channel is formed exclusively by water molecules. Confirmation of the molecular packing was performed through the analysis of Hirshfeld surfaces, and (I) is compared with other similar isoquinoline systems. Calculations of bond lengths and angles by the Hartree–Fock method or by density functional theory B3LYP, both with 6-311++G(d,p) basis sets, are reported, together with the results of additional IR, UV–Vis and theoretical studies. EN In the crystal structure of 6-methoxyquinoline N-oxide dihydrate, C10H9NO2·2H2O, (I), the presence of two-dimensional water networks is analysed. The water molecules form unusual water channels, as well as two intersecting mutually perpendicular columns. In one of these channels, the O atom of the N-oxide group acts as a bridge between the water molecules. The other channel is formed exclusively by water molecules. Confirmation of the molecular packing was performed through the analysis of Hirshfeld surfaces, and (I) is compared with other similar isoquinoline systems. Calculations of bond lengths and angles by the Hartree–Fock method or by density functional theory B3LYP, both with 6-311++G(d,p) basis sets, are reported, together with the results of additional IR, UV–Vis and theoretical studies. text/html Supramolecular study, Hirshfeld analysis and theoretical study of 6-methoxyquinoline N-oxide dihydrate text 6 69 2013-05-17 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?sk3489 The title compound, C16H9FN2S, crystallizes as a nonmerohedral twin with twin rotation about the reciprocal-lattice vector [10\overline{1}]*. The molecules are nearly planar and the dihedral angle between the planes of the two aryl rings is only 4.4 (2)°. The molecules are linked by pairs of C—H...N hydrogen bonds to form cyclic centrosymmetric R22(18) dimers, which are linked into chains by an aromatic π–π stacking interaction. Comparisons are made with some related 3-aryl-2-thienylacrylonitriles. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Trilleras, J. Velásquez, K. Cobo, J. Glidewell, C. 2013-05-17 doi:10.1107/S0108270113013267 International Union of Crystallography The title compound, C16H9FN2S, crystallizes as a nonmerohedral twin with twin rotation about the reciprocal-lattice vector [10\overline{1}]*. The molecules are nearly planar and the dihedral angle between the planes of the two aryl rings is only 4.4 (2)°. The molecules are linked by pairs of C—H...N hydrogen bonds to form cyclic centrosymmetric R22(18) dimers, which are linked into chains by an aromatic π–π stacking interaction. Comparisons are made with some related 3-aryl-2-thienylacrylonitriles. EN The title compound, C16H9FN2S, crystallizes as a nonmerohedral twin with twin rotation about the reciprocal-lattice vector [10\overline{1}]*. The molecules are nearly planar and the dihedral angle between the planes of the two aryl rings is only 4.4 (2)°. The molecules are linked by pairs of C—H...N hydrogen bonds to form cyclic centrosymmetric R22(18) dimers, which are linked into chains by an aromatic π–π stacking interaction. Comparisons are made with some related 3-aryl-2-thienylacrylonitriles. text/html (E)-2-(1,3-Benzothiazol-2-yl)-3-(4-fluorophenyl)acrylonitrile: a chain of π-stacked hydrogen-bonded rings text 6 69 2013-05-17 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0 http://scripts.iucr.org/cgi-bin/paper?gz3235 The crystal structure of the free base of the antidiabetic drug alogliptin [systematic name: 2-({6-[(3R)-3-aminopiperidin-1-yl]-3-methyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-1-yl}methyl)benzonitrile], C18H21N5O2, displays a two-dimensional N—H...O hydrogen-bonded network. It contains two independent molecules, which have the same conformation but differ in their hydrogen-bond connectivity. In the crystal structure of the benzoate salt (systematic name: (3R)-1-{3-[(2-cyanophenyl)methyl]-1-methyl-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-yl}piperidin-3-aminium benzoate), C18H22N5O2+·C7H5O2−, the NH3+ group of the cation is engaged in three intermolecular N—H...O hydrogen bonds to yield a hydrogen-bonded layer structure. The benzoate salt and the free base differ fundamentally in the conformations of their alogliptin moieties. Copyright (c) 2013 International Union of Crystallography urn:issn:0108-2701 Gelbrich, T. Kahlenberg, V. Griesser, U.J. 2013-05-18 doi:10.1107/S0108270113012560 International Union of Crystallography The crystal structure of the free base of the antidiabetic drug alogliptin [systematic name: 2-({6-[(3R)-3-aminopiperidin-1-yl]-3-methyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-1-yl}methyl)benzonitrile], C18H21N5O2, displays a two-dimensional N—H...O hydrogen-bonded network. It contains two independent molecules, which have the same conformation but differ in their hydrogen-bond connectivity. In the crystal structure of the benzoate salt (systematic name: (3R)-1-{3-[(2-cyanophenyl)methyl]-1-methyl-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-yl}piperidin-3-aminium benzoate), C18H22N5O2+·C7H5O2−, the NH3+ group of the cation is engaged in three intermolecular N—H...O hydrogen bonds to yield a hydrogen-bonded layer structure. The benzoate salt and the free base differ fundamentally in the conformations of their alogliptin moieties. EN The crystal structure of the free base of the antidiabetic drug alogliptin [systematic name: 2-({6-[(3R)-3-aminopiperidin-1-yl]-3-methyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-1-yl}methyl)benzonitrile], C18H21N5O2, displays a two-dimensional N—H...O hydrogen-bonded network. It contains two independent molecules, which have the same conformation but differ in their hydrogen-bond connectivity. In the crystal structure of the benzoate salt (systematic name: (3R)-1-{3-[(2-cyanophenyl)methyl]-1-methyl-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-yl}piperidin-3-aminium benzoate), C18H22N5O2+·C7H5O2−, the NH3+ group of the cation is engaged in three intermolecular N—H...O hydrogen bonds to yield a hydrogen-bonded layer structure. The benzoate salt and the free base differ fundamentally in the conformations of their alogliptin moieties. text/html Alogliptin and its benzoate salt text 6 69 2013-05-18 Copyright (c) 2013 International Union of Crystallography Acta Crystallographica Section C: Crystal Structure Communications organic compounds 0 0