Copper(I) iodide complexes are well known for displaying a diverse array of structural features even when only small changes in ligand design are made. This structural diversity is well displayed by five copper(I) iodide compounds reported here with closely related piperidine-2,6-di-thione (SNS), isoindoline-1,3-di-thione (SNS6), and 6-thioxopiperidin-2-one (SNO) ligands di-μ-iodido-bis-[(aceto-nitrile-κN)(6-sulfanylidenepiperidin-2-one-κS)copper(I)], [Cu2I2(CH3CN)2(C5H7NOS)2] (I), bis-(aceto-nitrile-κN)tetra-μ3-iodido-bis-(6-sulfanylidenepiperidin-2-one-κS)-tetra-hedro-tetra-copper(I), [Cu4I4(CH3CN)4(C5H7NOS)4] (II), catena-poly[[(μ-6-sulfanylidenepiperidin-2-one-κ2OS)copper(I)]-μ3-iodido], [CuI(C5H7NOS)] n (III), poly[[(piperidine-2,6-di-thione-κS)copper(I)]-μ3-iodido], [CuI(C5H7NS2)] n (IV), and poly[[(μ-isoindoline-1,3-di-thione-κ2SS)copper(I)]-μ3-iodido], [CuI(C8H5NS2)] n (V). Compounds I and II crystallize as discrete dimeric and tetra-meric complexes, whereas III, IV, and V crystallize as polymeric twottering effects and to identify the solvent mol-ecules. The given chemical formula and other crystal data do not take into account the solvent mol-ecules.The title compound, C6H11NO2·2H2O2, is the richest (by molar ratio) in hydrogen peroxide among the peroxosolvates of aliphatic α-amino acids. The asymmetric unit contains a zwitterionic pipecolinic acid mol-ecule and two hydrogen peroxide mol-ecules. The two crystallographically independent hydrogen peroxide mol-ecules form a different number of hydrogen bonds one forms two as donor and two as acceptor ([2,2] mode) and the other forms two as donor and one as acceptor ([2,1] mode). The latter hydrogen peroxide mol-ecule forms infinite hydrogen-bonded hydro-peroxo chains running along the c-axis direction, which is unusual for aliphatic α-amino acid peroxosolvates.The title compound, C15H12F3NO, crystallizes with one mol-ecule in the asymmetric unit. The configuration of the C=N bond is E and there is an intra-molecular O-H⋯N hydrogen bond present, forming an S(6) ring motif. The dihedral angle between the mean planes of the phenol and the 4-tri-fluoro-methyl-phenyl rings is 44.77 (3)°. In the crystal, mol-ecules are linked by C-H⋯O inter-actions, forming polymeric chains extending along the a-axis direction. The Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from C⋯H/H⋯C (29.2%), H⋯H (28.6%), F⋯H/H⋯F (25.6%), O⋯H/H⋯O (5.7%) and F⋯F (4.6%) inter-actions. The density functional theory (DFT) optimized structure at the B3LYP/6-311 G(d,p) level is compared with the experimentally determined mol-ecular structure in the solid state. The HOMO-LUMO behaviour was elucidated to determine the energy gap. The crystal studied was refined as an inversion twin.The title compound, C15H14ClNO, was synthesized by condensation reaction of 2-hy-droxy-5-methyl-benzaldehyde and 3-chloro-4-methyl-aniline, and crystallizes in the monoclinic space group P21/c. The 3-chloro-benzene ring is inclined to the phenol ring by 9.38 (11)°. The configuration about the C=N bond is E and an intra-molecular O-H⋯N hydrogen bond forms an S(6) ring motif. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the packing arrangement are from H⋯H (43.8%) and C⋯H/H⋯C (26.7%) inter-actions. The density functional theory (DFT) optimized structure at the B3LYP/ 6-311 G(d,p) level is compared with the experimentally determined mol-ecular structure and the HOMO-LUMO energy gap is provided.The title compound, [Ni(H2O)6][****(C2O4)3(H2O)3]2·4H2O, was obtained in the form of single crystals from the slow evaporation of an aqueous mixture of Ba6(H2O)17[Cr(C2O4)3]4·7H2O and NiSO4·6H2O in the molar ratio 14. Its structure is made up of corrugated anionic (101) layers of formula [****(C2O4)3(H2O)3] n n - that leave voids accommodating the charge-compensating cations, [Ni(H2O)6]2+ (point group symmetry ), as well as the water mol-ecules of crystallization. The anionic layers are built from the connection of barium and chromium atoms through bridging oxalate ligands. The CrIII atom is hexa-coordinated by O atoms of three oxalate ligands while the BaII atom is tenfold coordinated by three O atoms of water mol-ecules and seven O atoms of four oxalate ligands. Each NiII atom sits on an inversion center and is coordinated by six water mol-ecules. https://www.selleckchem.com/products/oseltamivir-phosphate-Tamiflu.html One of the uncoordinated water mol-ecules is disordered over two sites, with a refined occupancy ratio of 0.51 (5)0.49 (5). In the crystal, extensive O-H⋯O hydrogen-bonding inter-actions link the anionic layers, the charge-balancing cations as well as the water mol-ecules of crystallization into a three-dimensional supra-molecular network.The syntheses and crystal structures of the two title compounds, C11H10O3 (I) and C17H14BrNO2 (II), both containing the bi-cyclo-[2.2.2]octene ring system, are reported here [the structure of I has been reported previously White & Goh (2014 ▸). Private Communication (refcode HOKRIK). CCDC, Cambridge, England]. The bond lengths and angles of the bi-cyclo-[2.2.2]octene ring system are similar for both structures. The imide functional group of II features carbonyl C=O bond lengths of 1.209 (2) and 1.210 (2) Å, with C-N bond lengths of 1.393 (2) and 1.397 (2) Å. The five-membered imide ring is nearly planar, and it is positioned exo relative to the alkene bridgehead carbon atoms of the bi-cyclo-[2.2.2]octene ring system. Non-covalent inter-actions present in the crystal structure of II include a number of C-H⋯O inter-actions. The extended structure of II also features C-H⋯O hydrogen bonds as well as C-H⋯π and lone pair-π inter-actions, which combine together to create supra-molecular sheets.Caesium propano-ate monohydrate, Cs+·C3H5O2-·H2O, is composed of two symmetry-independent Cs+ cations, which are situated on the special position 4e of space group P 21m, one symmetry-independent propano-ate mol-ecule in a general position and a pair of water mol-ecules also situated on special position 4e. Two pairs of these symmetry-independent cations, four propano-ate mol-ecules and two pairs of symmetry-independent water mol-ecules form a repeat unit. These units form columns that are directed along the c axis and possess symmetry mm2. There are four such columns passing through each unit cell. Each column is inter-connected to its neighbours by four bifurcated three-centred Ow-H⋯Op (w = water, p = propano-ate) hydrogen bonds of moderate strength. There are also four intra-molecular Ow-H⋯Op hydrogen bonds of moderate strength within each column. One Cs+ cation is coordinated by six oxygen atoms (two water and four carboxyl-ate) in a trigonal-prismatic geometry, while the other Cs+ cation is coordinated by four water and four carboxyl-ate O atoms in a tetra-gonal-prismatic arrangement.
Copper(I) iodide complexes are well known for displaying a diverse array of structural features even when only small changes in ligand design are made. This structural diversity is well displayed by five copper(I) iodide compounds reported here with closely related piperidine-2,6-di-thione (SNS), isoindoline-1,3-di-thione (SNS6), and 6-thioxopiperidin-2-one (SNO) ligands di-μ-iodido-bis-[(aceto-nitrile-κN)(6-sulfanylidenepiperidin-2-one-κS)copper(I)], [Cu2I2(CH3CN)2(C5H7NOS)2] (I), bis-(aceto-nitrile-κN)tetra-μ3-iodido-bis-(6-sulfanylidenepiperidin-2-one-κS)-tetra-hedro-tetra-copper(I), [Cu4I4(CH3CN)4(C5H7NOS)4] (II), catena-poly[[(μ-6-sulfanylidenepiperidin-2-one-κ2OS)copper(I)]-μ3-iodido], [CuI(C5H7NOS)] n (III), poly[[(piperidine-2,6-di-thione-κS)copper(I)]-μ3-iodido], [CuI(C5H7NS2)] n (IV), and poly[[(μ-isoindoline-1,3-di-thione-κ2SS)copper(I)]-μ3-iodido], [CuI(C8H5NS2)] n (V). Compounds I and II crystallize as discrete dimeric and tetra-meric complexes, whereas III, IV, and V crystallize as polymeric twottering effects and to identify the solvent mol-ecules. The given chemical formula and other crystal data do not take into account the solvent mol-ecules.The title compound, C6H11NO2·2H2O2, is the richest (by molar ratio) in hydrogen peroxide among the peroxosolvates of aliphatic α-amino acids. The asymmetric unit contains a zwitterionic pipecolinic acid mol-ecule and two hydrogen peroxide mol-ecules. The two crystallographically independent hydrogen peroxide mol-ecules form a different number of hydrogen bonds one forms two as donor and two as acceptor ([2,2] mode) and the other forms two as donor and one as acceptor ([2,1] mode). The latter hydrogen peroxide mol-ecule forms infinite hydrogen-bonded hydro-peroxo chains running along the c-axis direction, which is unusual for aliphatic α-amino acid peroxosolvates.The title compound, C15H12F3NO, crystallizes with one mol-ecule in the asymmetric unit. The configuration of the C=N bond is E and there is an intra-molecular O-H⋯N hydrogen bond present, forming an S(6) ring motif. The dihedral angle between the mean planes of the phenol and the 4-tri-fluoro-methyl-phenyl rings is 44.77 (3)°. In the crystal, mol-ecules are linked by C-H⋯O inter-actions, forming polymeric chains extending along the a-axis direction. The Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from C⋯H/H⋯C (29.2%), H⋯H (28.6%), F⋯H/H⋯F (25.6%), O⋯H/H⋯O (5.7%) and F⋯F (4.6%) inter-actions. The density functional theory (DFT) optimized structure at the B3LYP/6-311 G(d,p) level is compared with the experimentally determined mol-ecular structure in the solid state. The HOMO-LUMO behaviour was elucidated to determine the energy gap. The crystal studied was refined as an inversion twin.The title compound, C15H14ClNO, was synthesized by condensation reaction of 2-hy-droxy-5-methyl-benzaldehyde and 3-chloro-4-methyl-aniline, and crystallizes in the monoclinic space group P21/c. The 3-chloro-benzene ring is inclined to the phenol ring by 9.38 (11)°. The configuration about the C=N bond is E and an intra-molecular O-H⋯N hydrogen bond forms an S(6) ring motif. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the packing arrangement are from H⋯H (43.8%) and C⋯H/H⋯C (26.7%) inter-actions. The density functional theory (DFT) optimized structure at the B3LYP/ 6-311 G(d,p) level is compared with the experimentally determined mol-ecular structure and the HOMO-LUMO energy gap is provided.The title compound, [Ni(H2O)6][BaCr(C2O4)3(H2O)3]2·4H2O, was obtained in the form of single crystals from the slow evaporation of an aqueous mixture of Ba6(H2O)17[Cr(C2O4)3]4·7H2O and NiSO4·6H2O in the molar ratio 14. Its structure is made up of corrugated anionic (101) layers of formula [BaCr(C2O4)3(H2O)3] n n - that leave voids accommodating the charge-compensating cations, [Ni(H2O)6]2+ (point group symmetry ), as well as the water mol-ecules of crystallization. The anionic layers are built from the connection of barium and chromium atoms through bridging oxalate ligands. The CrIII atom is hexa-coordinated by O atoms of three oxalate ligands while the BaII atom is tenfold coordinated by three O atoms of water mol-ecules and seven O atoms of four oxalate ligands. Each NiII atom sits on an inversion center and is coordinated by six water mol-ecules. https://www.selleckchem.com/products/oseltamivir-phosphate-Tamiflu.html One of the uncoordinated water mol-ecules is disordered over two sites, with a refined occupancy ratio of 0.51 (5)0.49 (5). In the crystal, extensive O-H⋯O hydrogen-bonding inter-actions link the anionic layers, the charge-balancing cations as well as the water mol-ecules of crystallization into a three-dimensional supra-molecular network.The syntheses and crystal structures of the two title compounds, C11H10O3 (I) and C17H14BrNO2 (II), both containing the bi-cyclo-[2.2.2]octene ring system, are reported here [the structure of I has been reported previously White & Goh (2014 ▸). Private Communication (refcode HOKRIK). CCDC, Cambridge, England]. The bond lengths and angles of the bi-cyclo-[2.2.2]octene ring system are similar for both structures. The imide functional group of II features carbonyl C=O bond lengths of 1.209 (2) and 1.210 (2) Å, with C-N bond lengths of 1.393 (2) and 1.397 (2) Å. The five-membered imide ring is nearly planar, and it is positioned exo relative to the alkene bridgehead carbon atoms of the bi-cyclo-[2.2.2]octene ring system. Non-covalent inter-actions present in the crystal structure of II include a number of C-H⋯O inter-actions. The extended structure of II also features C-H⋯O hydrogen bonds as well as C-H⋯π and lone pair-π inter-actions, which combine together to create supra-molecular sheets.Caesium propano-ate monohydrate, Cs+·C3H5O2-·H2O, is composed of two symmetry-independent Cs+ cations, which are situated on the special position 4e of space group P 21m, one symmetry-independent propano-ate mol-ecule in a general position and a pair of water mol-ecules also situated on special position 4e. Two pairs of these symmetry-independent cations, four propano-ate mol-ecules and two pairs of symmetry-independent water mol-ecules form a repeat unit. These units form columns that are directed along the c axis and possess symmetry mm2. There are four such columns passing through each unit cell. Each column is inter-connected to its neighbours by four bifurcated three-centred Ow-H⋯Op (w = water, p = propano-ate) hydrogen bonds of moderate strength. There are also four intra-molecular Ow-H⋯Op hydrogen bonds of moderate strength within each column. One Cs+ cation is coordinated by six oxygen atoms (two water and four carboxyl-ate) in a trigonal-prismatic geometry, while the other Cs+ cation is coordinated by four water and four carboxyl-ate O atoms in a tetra-gonal-prismatic arrangement.
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