Seredyuk M, Gumienna-Kontecka E, Brzuszkiewicz A
… +2 more, Iskenderov TS, Kalibabchuk VA
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484793
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The porphyrin core of the title centrosymmetric compound, C44H26N8O8·2C6H5NO2, is approximately planar, the maximum deviation being 0.069 (3) Å. The planes of the benzene rings of the nitro-phenyl substituents are almost...The porphyrin core of the title centrosymmetric compound, C44H26N8O8·2C6H5NO2, is approximately planar, the maximum deviation being 0.069 (3) Å. The planes of the benzene rings of the nitro-phenyl substituents are almost perpendicular to the porphyrin mean plane, making dihedral angles of 73.89 (9) and 89.24 (9)°. The two pyrrole ring H atoms are equally disordered over the four pyrrole ring N atoms. In the crystal, weak C-H⋯O and C-H⋯N hydrogen bonds link the porphyrin mol-ecules into a three-dimensional supra-molecular network. The nitro-benzene solvent mol-ecules are linked by weak C-H⋯O hydrogen bonds into supra-molecular chains propagating along the a-axis direction.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484792
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In the title compound, C7H9NO2, all non-H atoms are essentially coplanar [r.m.s. deviation = 0.032 Å]. The largest deviation from the plane of the pyridine ring is 0.105 (6) Å for the terminal C atom of the eth-oxy group...In the title compound, C7H9NO2, all non-H atoms are essentially coplanar [r.m.s. deviation = 0.032 Å]. The largest deviation from the plane of the pyridine ring is 0.105 (6) Å for the terminal C atom of the eth-oxy group. In the crystal, mol-ecules are linked by pairs of N-H⋯O hydrogen bonds, forming inversion dimers. These dimers are further linked by C-H⋯π inter-actions and weak π-π inter-actions between pyridine rings [centroid-centroid distance = 4.023 (1) Å].
Haress NG, Ghabbour HA, El-Emam AA
… +2 more, Chidan Kumar CS, Fun HK
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484791
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In the mol-ecule of the title compound, C7H9ClN2O2, the conformation is determined by intra-molecular C-H⋯O and C-H⋯Cl hydrogen bonds, which generate S(6) and S(5) ring motifs. The isopropyl group is almost perpendicular...In the mol-ecule of the title compound, C7H9ClN2O2, the conformation is determined by intra-molecular C-H⋯O and C-H⋯Cl hydrogen bonds, which generate S(6) and S(5) ring motifs. The isopropyl group is almost perpendicular to the pyrimidine ring with torsion angles of -70.8 (3) and 56.0 (3)°. In the crystal, two inversion-related mol-ecules are linked via a pair of N-H⋯O hydrogen bonds into R 2 (2)(8) dimers; these dimers are connected into chains extending along the bc plane via an additional N-H⋯O hydrogen bond and weaker C-H⋯O hydrogen bonds. The crystal structure is further stabilized by a weak π-π inter-action [3.6465 (10) Å] between adjacent pyrimidine-dione rings arranged in a head-to-tail fashion, producing a three-dimensional network.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484790
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In the title compound, [Tm(C6H5Se)3(C4H8O)3], the Tm(III) atom lies on a threefold rotation axis and is coordinated by three phenyl-seleno-late ligands and three tetra-hydro-furan ligands leading to a distorted fac-octa-...In the title compound, [Tm(C6H5Se)3(C4H8O)3], the Tm(III) atom lies on a threefold rotation axis and is coordinated by three phenyl-seleno-late ligands and three tetra-hydro-furan ligands leading to a distorted fac-octa-hedral coordination environment. The Tm-Se and Tm-O bond lengths are 2.7692 (17) and 2.345 (10) Å, respectively, and the bond angles are 91.32 (6)° for Se-Tm-Se, 92.6 (2) and 94.4 (2)° for Se-Tm-O, and 81.2 (3)° for O-Tm-O. In the crystal, the discrete complexes are linked by van der Waals inter-actions only. The crystal was refined as a non-merohedral twin (ratio = 0.65:0.35).
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484789
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In the polymeric title compound, [Cd(C7H4O6S)(C11H6N2O)(H2O)2] n , the Cd(2+) atom is seven-coordinated by two water O atoms, by three O atoms from two 2-hy-droxy-5-sulfonato-benzoate (Hssal(2-)) ligands and by two N ato...In the polymeric title compound, [Cd(C7H4O6S)(C11H6N2O)(H2O)2] n , the Cd(2+) atom is seven-coordinated by two water O atoms, by three O atoms from two 2-hy-droxy-5-sulfonato-benzoate (Hssal(2-)) ligands and by two N atoms from a 4,5-di-aza-fluoren-9-one (Dafo) ligand in a distorted penta-gonal-bipyramidal geometry. The Cd(2+) atoms are monodentately coordinated by the sulfonate group of one Hssal(2-) ligand and bidentately coordinated by the carboxyl-ate group of another Hssal(2-) ligand, generating zigzag chains running parallel to [010]. The chains are linked by O-H⋯O hydrogen bonds into a three-dimensional architecture.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484788
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The title compound [Na3(C11H6NO3)2(C2H3O2)] n , crystallized through diffusion of diethyl ether into methanol as needles. There are three crystallographically independent Na(+) cations present, each exhib-it-ing a distor...The title compound [Na3(C11H6NO3)2(C2H3O2)] n , crystallized through diffusion of diethyl ether into methanol as needles. There are three crystallographically independent Na(+) cations present, each exhib-it-ing a distorted octa-hedral coordination geometry, two through coordination by five O atoms and one N atom, and one through coordination by six O atoms. A series of inter-molecular O⋯Na and N⋯Na contacts leads to the formation of chains along the a-axis direction.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484787
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The mol-ecular structure of the title compound, [ZnCl2(C11H20N2S)2], shows tetra-hedral Zn coordination from two Cl ligands and two thione groups. The Zn-Cl bond lengths differ sligthly at 2.2310 (10) and 2.2396 (11) Å w...The mol-ecular structure of the title compound, [ZnCl2(C11H20N2S)2], shows tetra-hedral Zn coordination from two Cl ligands and two thione groups. The Zn-Cl bond lengths differ sligthly at 2.2310 (10) and 2.2396 (11) Å while the Zn-S bond lengths are equal at 2.3663 (9) and 2.3701 (10) Å. The Cl-Zn-Cl angle is 116.04 (4) and S-Zn-S is 101.98 (3)°. All other angles at the central Zn atom range from 108.108 (3) to 110.21 (4)°. The C-S-Zn angles are 100.75 (10) and 103.68 (11)°, the difference most probably resulting from packing effects, as both the C-S and both the S-Zn bonds are equal in each case. The two imidazole ring planes make a dihedral angle of 67.9 (1)°. The CH3 groups of one isopropyl moiety are disordered over two sets of sites with occupation factors of 0.567 (15) and 0.433 (15). It may be noteworthy that the isomolecular Cu complex shows a different crystal packing (group-subgroup relation) with the Cu atom lying on a twofold rotation axis. In the crystal, the shortest non-bonding contact is a C-H⋯Cl inter-action. This leads to the formation of centrosymmetric dimers that are stacked along the c-axis.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484786
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The crystal structure of the title compound, [ZnCl2(C15H11N3)], was redetermined based on modern CCD data. In comparison with the previous determination from photographic film data [Corbridge & Cox (1956 ▶). J. Chem. Soc...The crystal structure of the title compound, [ZnCl2(C15H11N3)], was redetermined based on modern CCD data. In comparison with the previous determination from photographic film data [Corbridge & Cox (1956 ▶). J. Chem. Soc. 159, 594-603; Einstein & Penfold (1966 ▶). Acta Cryst. 20, 924-926], all non-H atoms were refined with anisotropic displacement parameters, leading to a much higher precision in terms of bond lengths and angles [e.g. Zn-Cl = 2.2684 (8) and 2.2883 (11) compared to 2.25 (1) and 2.27 (1) Å]. In the title mol-ecule, the Zn(II) atom is five-coordinated in a distorted square-pyramidal mode by two Cl atoms and by the three N atoms from the 2,2':6',2''-terpyridine ligand. The latter is not planar and shows dihedral angles between the least-squares planes of the central pyridine ring and the terminal rings of 3.18 (8) and 6.36 (9)°. The mol-ecules in the crystal structure pack with π-π inter-actions [centroid-centroid distance = 3.655 (2) Å] between pyridine rings of neighbouring terpyridine moieties. These, together with inter-molecular C-H⋯Cl inter-actions, stablize the three-dimensional structure.
Hsuan RE, Hughes JE, Miller TH
… +5 more, Shaikh N, Cunningham PH, O'Connor AE, Tidey JP, Blake AJ
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484785
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Two independent mol-ecules of the title solvated complex, [V(C16H14N2O2)O]·CH3OH, also known as [N,N'-bis-(salicyl-idene)ethyl-enedi-amine]-oxidovanadium(IV) or vanadyl salen, crystallize in the asymmetric unit. Each dis...Two independent mol-ecules of the title solvated complex, [V(C16H14N2O2)O]·CH3OH, also known as [N,N'-bis-(salicyl-idene)ethyl-enedi-amine]-oxidovanadium(IV) or vanadyl salen, crystallize in the asymmetric unit. Each disordered methanol solvent mol-ecule [occupancy ratios 0.678 (4):0.322 (4) and 0.750 (5):0.250 (5)] is linked to a [N,N'-bis-(salicyl-idene)ethyl-enedi-amine]-oxidovanadium(IV) mol-ecule by an O-H⋯O hydrogen bond and to others by C-H⋯O hydrogen bonds. The resulting extended structure consists of a bilayer of mol-ecules parallel to the ab plane. Despite the fact that solvates are common in complexes derived from substituted analogues of the N,N'-bis-(salicyl-idene)ethyl-enedi-amine ligand, the title solvate is the first one of [N,N'-bis-(salicyl-idene)ethyl-enedi-amine]-oxidovanadium(IV) to be structurally characterized. The two vanadyl species have very similar inter-nal geometries, which are best characterized as distorted square-based pyramidal with the vanadium atom displaced from the N2O2 basal plane by 0.5966 (9) Å in the direction of the doubly-bonded oxide ligand.
Kireenko MM, Zaitsev KV, Karlov SS
… +2 more, Egorov MP, Churakov AV
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484784
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The mixed-valence μ-oxide Sn12 cluster, deca-carbonyl-tetra-μ4-oxido-hexa-μ3-oxido-tetra-kis-[μ-2,2'-(pyridine-2,6-di-yl)bis(1,1-di-phenyl-ethano-lato)]deca-tin(II)ditin(IV)dimolyb-denum(O)(2 Mo-Sn) toluene hepta-solvate...The mixed-valence μ-oxide Sn12 cluster, deca-carbonyl-tetra-μ4-oxido-hexa-μ3-oxido-tetra-kis-[μ-2,2'-(pyridine-2,6-di-yl)bis(1,1-di-phenyl-ethano-lato)]deca-tin(II)ditin(IV)dimolyb-denum(O)(2 Mo-Sn) toluene hepta-solvate, [Mo2Sn12(C33H27NO2)4O10(CO)10]·7C7H8, has a crystallographically imposed inversion centre. The asymmetric unit also contains three and a half toluene solvent mol-ecules, one of which is disordered about a centre of symmetry. The complex mol-ecule comprises six distinct Sn atom species with four different coordination numbers, namely 3, 4, 5, and 6. The Sn(II) atoms forming the central Sn10O10 core adopt distorted trigonal-pyramidal, square-pyramidal and octa-hedral coordination geometries provided by the μ-oxide atoms and by the O- and N-donor atoms of two pyridinedi-ethano-late ligands. The terminal Sn(IV) atoms have distorted trigonal-bipyramidal coordination geometries, with a μ4-oxide atom and the N atom of a pyridinedi-ethano-late ligand occupying the axial positions, and the Mo atom of a Mo(CO)5 group and the alk-oxy O atoms of a ligand forming the equatorial plane. In the crystal, weak intra- and inter-molecular C-H⋯O hydrogen bonds are observed.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484783
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The title coordination polymer, {[Co2(C15H7O7)(OH)(C14H14N4)]·0.25H2O} n , was synthesized under hydro-thermal conditions. The asymmetric unit contains two Co(2+) ions, one L (3-) anion originating from 5-(4-carb-oxy-phe...The title coordination polymer, {[Co2(C15H7O7)(OH)(C14H14N4)]·0.25H2O} n , was synthesized under hydro-thermal conditions. The asymmetric unit contains two Co(2+) ions, one L (3-) anion originating from 5-(4-carb-oxy-phen-oxy)isophthalic acid (H3 L), one OH(-) ligand, one 1,4-bis-[(1H-imidazol-l-yl)meth-yl]benzene (bix) ligand and one disordered lattice water mol-ecule (occupancy 0.25). The two Co(2+) ions have different environments. One has an octa-hedral O4N2 coordin-ation sphere, defined by four O atoms from three carboxyl-ate groups and one OH(-) ligand, and two N atoms from two symmetry-related bix ligands. The other has a trigonal-bipyramidal O5 coordination sphere resulting from three carboxyl-ate groups and two OH(-) ligands. The dihedral angles between the two benzene rings in the L (3-) ligand and between the benzene ring and the two imidazole rings in the bix ligand are 67.05 (15), 75.27 (17) and 82.05 (17)°, respectively. Four neighbouring Co(2+) ions are linked by six carboxyl-ate groups and two μ 3-OH ligands, forming a butterfly-shaped secondary building unit (SBU). These SBUs are connected by L (3-) anions into layers parallel to (1-10). Adjacent layers are cross-linked by the bix ligands, forming a three-dimensional framework that has a bimodal (3,8)-connected tfz-d topology. The disordered lattice water mol-ecule is located in the voids of the framework and has O⋯O and O⋯N contacts of 2.81 (2) and 2.95 (2) Å, suggesting medium-strength hydrogen bonds. The title compound may be a good candidate for artificial eye lenses.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484782
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The title compound, {[Mn(C24H14N2O4)(C24H16N2O4)]·0.5H2O} n , was obtained by the reaction of manganese nitrate with the ligand 4,4'-(4,4'-bi-pyridine-2,6-di-yl) di-benzoic acid under hydro-thermal conditions. The water...The title compound, {[Mn(C24H14N2O4)(C24H16N2O4)]·0.5H2O} n , was obtained by the reaction of manganese nitrate with the ligand 4,4'-(4,4'-bi-pyridine-2,6-di-yl) di-benzoic acid under hydro-thermal conditions. The water O atom is located on a twofold rotation axis. The Mn(2+) ion is hepta-coordinated by six O atoms and one N atom from the ligands. In this structure, the ligands adopts two different forms, one completely deprotonated and one with a protonated N atom (pyridinium) and a carboxylic acid function. In the crystal, N-H⋯O and O-H⋯O hydrogen bonds consolidate the packing, forming a three-dimensional framework.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484781
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The mol-ecular components of the title salt, [Cu(C4H11NO2)2](C8H4O4), are one Cu(II) cation O,N,O'-chelated by two tridentate 2-[(2-hy-droxy-eth-yl)amino]-ethanol ligands, and a terephthalate counter-dianion, located abo...The mol-ecular components of the title salt, [Cu(C4H11NO2)2](C8H4O4), are one Cu(II) cation O,N,O'-chelated by two tridentate 2-[(2-hy-droxy-eth-yl)amino]-ethanol ligands, and a terephthalate counter-dianion, located about a centre of inversion. The complex Cu(II) cation is located about a centre of inversion and shows typical Jahn-Teller distortion, with two short Cu-O and two short Cu-N bonds in the equatorial plane and two long Cu-O bonds to the axial atoms. The cations are arranged in sheets parallel to (100), with the centrosymmetric terephthalate anions located between the sheets. Each anion is the acceptor of four O-H⋯O and two N-H⋯O hydrogen bonds, forming a three-dimensional network structure.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484780
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In the title salt, [Cd(C6H15NO3)2](C8H4O4), the Cd(2+) cation is coordinated by six O atoms and two N atoms from two tetra-dentate 2-[bis-(2-hy-droxy-eth-yl)amino]-ethanol ligands, displaying a distorted square-anti-pris...In the title salt, [Cd(C6H15NO3)2](C8H4O4), the Cd(2+) cation is coordinated by six O atoms and two N atoms from two tetra-dentate 2-[bis-(2-hy-droxy-eth-yl)amino]-ethanol ligands, displaying a distorted square-anti-prismatic coordination. The terephthalate dianion does not coordinate to the cation but is connected through O⋯H-O hydrogen bonds of medium strength to the complex cations, leading to a layered structure extending parallel to (100).
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484779
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The title mol-ecule, [Fe(C5H5)(C16H11O4)], consists of a ferrocenyl moiety and a 4-methyl-coumarin group linked through an ester unit to one of the cyclo-penta-dienyl (Cp) rings. The two Cp rings are virually parallel, w...The title mol-ecule, [Fe(C5H5)(C16H11O4)], consists of a ferrocenyl moiety and a 4-methyl-coumarin group linked through an ester unit to one of the cyclo-penta-dienyl (Cp) rings. The two Cp rings are virually parallel, with an angle between the two least-squares planes of 0.74 (16)°. The distances between the Fe(II) atom and the centroids of the two Cp rings are 1.639 (2) and 1.652 (2) Å. The conformation of the ferrocenyl moiety is slightly away from eclipsed. The dihedral angle between the coumarin ring system and the ferrocenyl ester moiety is 69.17 (19)°. π-π stacking inter-actions involving the benzene rings of neighbouring coumarin moieties, with centroid-centroid distances of 3.739 (2) Å, consolidate the crystal packing.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484778
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The title salt, [Co(C8H4F3O3)(C12H8N2)(H2O)3](C8H4F3O3), was obtained under solvothermal conditions by the reaction of 2,4,5-tri-fluoro-3-meth-oxy-benzoic acid with CoCl2 in the presence of 1,10-phenanthroline (phen). Th...The title salt, [Co(C8H4F3O3)(C12H8N2)(H2O)3](C8H4F3O3), was obtained under solvothermal conditions by the reaction of 2,4,5-tri-fluoro-3-meth-oxy-benzoic acid with CoCl2 in the presence of 1,10-phenanthroline (phen). The Co(II) ion is octa-hedrally coordinated by two N atoms [Co-N = 2.165 (2) and 2.129 (2) Å] from the phen ligand, by one carboxyl-ate O atom [Co-O = 2.107 (1) Å] and by three O atoms from water mol-ecules [Co-O = 2.093 (1), 2.102 (1) and 2.114 (1) Å]. The equatorial positions of the slightly distorted octa-hedron are occupied by the N atoms, the carboxyl-ate O and one water O atom. An intra- and inter-molecular O-H⋯O hydrogen-bonding network between the water-containing complex cation and the organic anion leads to the formation of ribbons parallel to [010].
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484777
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In the title compound, [Cu2(C7HF4O2)4(C12H8N2)2]·2H2O, the Cu(II) ion has a square-pyramidal coordination sphere. The basal plane consists of two N atoms [Cu-N = 2.008 (3) and 2.032 (3) Å] from the phenanthroline ligand,...In the title compound, [Cu2(C7HF4O2)4(C12H8N2)2]·2H2O, the Cu(II) ion has a square-pyramidal coordination sphere. The basal plane consists of two N atoms [Cu-N = 2.008 (3) and 2.032 (3) Å] from the phenanthroline ligand, and of two carboxyl-ate O atoms [Cu-O = 1.942 (3) and 1.948 (3) Å] from two 2,3,4,5-tetra-fluoro-benzoate anions. Another 2,3,4,5-tetra-fluoro-benzoate anion provides the apical carboxyl-ate O atom [Cu-O = 2.262 (3) Å] and bridges two Cu(II) ions into a binuclear centrosymmetric dimer. Intra-molecular π-π inter-actions between one of the tetra-fluoro-benzene rings and the middle of the phenenanthroline rings [3.617 (3) Å] stabilize the mol-ecular configuration. O-H⋯O hydrogen bonds between the lattice water mol-ecules and the unbound carboxyl-ate O atoms of the metal complexes leads to the formation of a chain structure parallel to [100].
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484776
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The asymmetric unit of the title Co(II) complex, [Co(C13H8BrN2O)2], contains two independent mol-ecules (A and B). In both mol-ecules, the Co(II) cation is N,O-chelated by two 2-(1H-benzimidazol-2-yl)-4-bromo-phenolate a...The asymmetric unit of the title Co(II) complex, [Co(C13H8BrN2O)2], contains two independent mol-ecules (A and B). In both mol-ecules, the Co(II) cation is N,O-chelated by two 2-(1H-benzimidazol-2-yl)-4-bromo-phenolate anions in a distorted tetra-hedral geometry. In mol-ecule A, both chelating rings display an envelope conformation, with the flap Co atom lying 0.614 (6) and 0.483 (6) Å from the mean planes of the remaining atoms. In mol-ecule B, both chelating rings are approximately planar, the maximum deviations being 0.039 (4) and 0.076 (3) Å. In the crystal, mol-ecules are linked by classical N-H⋯O hydrogen bonds and weak C-H⋯O and C-H⋯Br hydrogen bonds into a three-dimensional supra-molecular network. Extensive π-π stacking is observed between nearly parallel aromatic rings of adjacent mol-ecules with centroid-centroid distances in the range 3.407 (3)-3.850 (4) Å.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484775
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In the title salt, [Zn(C6H15NO3)2](C8H4O4), the Zn(II) cation, located on a centre of inversion, is coordinated by four O atoms and two N atoms from two tridentate 2-[bis-(2-hy-droxy-eth-yl)amino]-ethanol (BHEA) ligands,...In the title salt, [Zn(C6H15NO3)2](C8H4O4), the Zn(II) cation, located on a centre of inversion, is coordinated by four O atoms and two N atoms from two tridentate 2-[bis-(2-hy-droxy-eth-yl)amino]-ethanol (BHEA) ligands, giving rise to a slightly distorted octa-hedral geometry. The terephthalate dianion, located about a centre of inversion, is not coordinated to Zn(II) but is connected through O-H⋯O contacts with [Zn(BHEA)2](2+) cations, leading to a three-dimensional crystal structure.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484774
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Reaction of Co(BF4)2·6H2O with tris-[(6-methyl-pyridin-2-yl)meth-yl]amiine in methanol results in a fluoride abstraction from BF4 (-), yielding the unexpected title compound, [Co2F2(C21H24N4)2](BF4)2. The complex cation...Reaction of Co(BF4)2·6H2O with tris-[(6-methyl-pyridin-2-yl)meth-yl]amiine in methanol results in a fluoride abstraction from BF4 (-), yielding the unexpected title compound, [Co2F2(C21H24N4)2](BF4)2. The complex cation consists of two inversion-related [Co(C21H24N4)](2+) moieties bridged by a pair of fluoride ligands. The Co(II) cation is six-coordinated in a distorted octa-hedral geometry and forms a +II high-spin state. In the crystal, the complex cation and the BF4 (-) anion are connected by C-H⋯F hydrogen bonds, forming a three-dimensional network. An intra-molecular C-H⋯F hydrogen bond is also observed.