Synthesis and Crystal Structure of <Emphasis Type="Italic">N</Emphasis>′-(6-Chloropyridin-3-formyl)-<Emphasis Type="Italic">N</Emphasis>-<Emphasis Type="Italic">t</Emphasis>-Butyl Urea

Abstract The crystal structure of N′-(6-chloropyridin-3-formyl)-N-t-butyl urea, C₁₁H₁₄ClN₃O₂, has been established, and which belongs to monoclinic crystal system, space group Pn with unit cell dimensions a = 9.335(3) ?, b = 12.715(3) ?, c = 21.813(6) ?, β = 95.417(6)°, V = 2577.6(12) ?³ and Z = 8. An intramolecular N–H···O hydrogen bond forms a six-membered ring in the central part of the molecule. Both two N–H atoms of single unit participate in intermolecular hydrogen bonds and an intramolecular hydrogen bond, respectively. Index Abstract The crystal structure ofN′-(6-chloropyridin-3-formyl)-N-t-butyl urea, C₁₁H₁₄ClN₃O₂, has been established, and which belongs to monoclinic crystal system withZ = 8, space group Pn.      

Synthesis and Crystal Structure of the Hydrated Nickel(II) Complex of Tartrate

Abstract  A new dinuclear hydrated nickel(II) tartrate has been isolated and structurally characterized by single-crystal X-ray diffraction. The title compound formulated as [Ni₄(C₄H₄O₆)₄(H₂O)₈](EtOH)_0.5(H₂O)_10.25 (C₁₇H_55.5Ni₄O_42.75) crystallizes in monoclinic system, space group P2(1)/c with a = 13.684(5), b = 17.143(6), c = 18.586(6) ?, β = 96.638(6)°, V = 4331(3) ?³, Z = 4. The unit cell contains two crystallographic independent dimeric units of [Ni₂(C₄H₄O₆)₂(H₂O)₄] without significant structural difference, half of menthol molecule and ten and a quarter packing water molecules. In each dimeric unit, one (R,R)-tartrato dianion chelates two Ni(II) ions by the use of two hydroxy oxygen and two carboxyl oxygen atoms as donor atoms, and another tartrato dianion chelates the same pair of Ni(II) cations in the same way. Each Ni(II) atom is six-coordinated by six O atoms from two tartrate units and two water molecules. Index Abstract  The crystal structure of complex [Ni₄(C₄H₄O₆)₄(H₂O)₈](EtOH)_0.5(H₂O)_10.25 contains two crystallographic independent dimeric units of [Ni₂(C₄H₄O₆)₂(H₂O)₄] without significant structural difference. In each dimeric unit, one (R,R)-tartrato dianion chelates two Ni(II) ions by the use of two hydroxy oxygen and two carboxyl oxygen atoms as donor atoms, and another tartrato dianion chelates the same pair of Ni(II) cations in the same way.      

Synthesis,Crystal Structure and Fluorescent Study of Bis(2-(2-hydroxyphenyl)benzimidazolate)zinc with Ethanol Solvate

Abstract  The zinc(II) complex with 2-(2-hydroxyphenyl)benzimidazole, namely [Zn(2-(2-hydroxyphenyl)benzimidazolate)₂]·C₂H₅OH (1 · C₂H₅OH) has been synthesized and characterized by X-ray crystallography and photoluminescent analysis. The complex crystallizes in monoclinic space group P2₁/c with cell parameters a = 10.156(1) ?, b = 25.771(3) ?, c = 9.674(1) ?, α = 90°, β = 103.641(2)°, γ = 90°, Z = 4, V = 2460.4(4) ?³. The central Zn(II) is four-coordinate and has a tetrahedral geometry. The steady-state and time-resolved photoluminescent spectra for the title compound have also been studied. The emission property can be ascribed to ligand-centered charge-transfer transition (LCCT) with π → π* property. Index Abstract   A new co-crystal of Zn(II) complex of 2-(2-hydroxylphenyl)benzimidazole with ethanol solvate has been prepared, characterized by X-ray crystallography and fluorescent studies.      

The Twinned Crystal Structure of Zinc(II) Acetylacetonate Trimer

Abstract  The crystal structure of the title compound, C₃₀H₄₂O₁₂Zn₃, originally determined from untwinned crystals (Bennett et al. Acta Cryst B 24:904, 1968) has been redetermined from twinned crystals. The effect of the twinning is that additional reflections appear in the diffraction pattern leading to a unit cell with a too long c-axis in which the structure cannot be solved. Thus, for a successful structure solution the correct unit cell has to be found and for refinement the twinning has to be taken into account. The central Zn atom is located on a twofold rotation axis. It is hexacoordinated in a distorted octahedral mode, whereas the coordination geometry of the two terminal Zn atoms is distorted trigonal bipyramidal. Index Abstract  The crystal structure of the title compound, Zinc(II) acetylacetonate trimer, has been redetermined from twinned crystals. For a successful structure solution the correct unit cell had to be found and for refinement the twinning had to be taken into account. The central Zn atom is located on a twofold rotation axis. It is hexacoordinated in a distorted octahedral mode, whereas the coordination geometry of the two terminal Zn atoms is distorted trigonal bipyramidal. An erratum to this article can be found at     

Synthesis and Crystal Structure of a Compound with Two Conformational Isomers: <Emphasis Type="Italic">N</Emphasis>-(2-methylbenzoyl)-<Emphasis Type="Italic">N</Emphasis>′-(4-nitrophenyl)thiourea

Abstract  The single crystal of the title compound (C₁₅H₁₃N₃O₃S) with two conformational isomers was obtained from the solution of the title compound dissolved in the N,N-dimethylformamide (DMF) by slow evaporation at room temperature. The crystal is triclinic, space group P-1 with a = 10.418(2), b = 10.758(2), c = 14.494(3) ?, α = 71.07(3), β = 81.56(3), γ = 85.61(3)o, V = 1519.2(5) ?³, Z = 2, C₃₀H₂₆N₆O₆S₂, D _c  = 1.379 g/cm³, μ(MoKα) = 0.229 mm⁻¹, S = 0.994, F(000) = 656, R = 0.0688 and wR = 0.1695. In the unit cell, there are two independent molecules having only slightly different bond lengths and angles, but the corresponding dihedral angles of the two molecules are different. Intermolecular N–H···S and N–H···O hydrogen bonds forming R ² ₂(8) and R ² ₂(12) rings, respectively, link the molecules into ribbons. Index Abstract  In the unit cell, there are two independent molecules having only slightly different bond lengths and angles between them, but different corresponding dihedral angles.      

Crystal Structure of 9α,11-Epoxy-7α-(methoxycarbonyl)-3-oxo-17α-pregn-4-ene-21,17-carbolactone

Abstract  The title compound (common name eplerenone), C₂₄H₃₀O₆, is an aldosterone receptor antagonist. From the isopropyl acetate solution the compound crystallizes in monoclinic space group P 21 with a = 8.811(1) ?, b = 11.250(1) ?, c = 11.079(1) ?, β = 93.822(12)°, Z = 2. The molecule contains three six membered rings, two five membered rings and one three membered ring. Both five membered rings display envelope conformation, whereas three six membered rings show different conformation: chair, half-chair and envelope. In the crystal the eplerenone molecules link to one another via intermolecular weak C–H···O hydrogen bonding to form the smaller cavity of 12.0(1) ?³ between eplerenone molecules, no solvent molecule filled in this cavity. Index Abstract  In the title molecule three six-membered rings show different conformation. Weak C–H···O hydrogen bonding links adjacent molecules to form the small cavity 12.0(1) ?³, no solvent molecule filled in the cavity.      

Synthesis,Isolation and X-ray Crystal Structure Characterization of <Emphasis Type="Italic">Trans</Emphasis>-γ-{(C-<Emphasis Type="Italic">meso</Emphasis>-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)(diisothiocyanato)} Nickel(II) Complex

Abstract  A new isomer of [Ni(tet-a)]²⁺ (assigned as γ-isomer) (tet-a = C-meso-5,5,7,12,12,14−hexamethyl-1,4,8,11-tetraazacyclotetradecane), which is found in the complex of trans-γ-[Ni(tet-a)(NCS)₂], has been isolated from the reaction of β-[Ni(tet-a)](ClO₄)₂ with NaSCN in a mixture of MeOH–H₂O (1:1, v/v) solution and characterized by X-ray crystallography. The complex crystallizes in orthorhombic Pca2(1) space group with the crystal cell parameters of a = 12.5787(10) ?, b = 11.6834(10) ?, c = 15.4019(12) ?, V = 2263.5(3) ?³, and Z = 4. The crystal structure shows that the complex is noncentrosymmetric. The conformations of the six-asymmetric centers are assigned as 1R,4R,8S,11S,7R,14S or 1S,4S,8R,11R,7S,14R (Trans-III). The coordination polyhedron around the nickel atom is axially elongated octahedron with an N₆ chromophore. The association of the complex units through N(3)–H···S(1) (2.665 ?) hydrogen bonding interactions leads one-dimensional hydrogen bonded network along c-axis. Index Abstract  A new isomer of Ni(tet-a)²⁺, which is assigned as γ-isomer, in the complex of trans-γ-[Ni(tet-a)(NCS)₂] has been synthesized, isolated and characterized by X-ray crystallography. The complex units form a one-dimensional self-assembly hydrogen bonded network.      

Synthesis, Crystal Structures and Properties of Two Copper (II) Complexes with Pyridazine Derivative Ligand

Abstract  Two new complexes, [Cu(L)₂(CH₃OH)] · (ClO₄)₂ (1) and [Cu(L)₂(H₂O)] · (NO₃)₂ (2), have been synthesized and their crystal structures have been determined by X-ray analysis, where L = 3-(3,5-bimethylpyrazole-yl)-6-chloro-pyridazine]. The complex 1 crystallizes in the monoclinic, space group C2/c, and the coordination configuration of copper (II) is better described as trigonal pyramidal geometry with four N atoms from L and one O_methanol^. The coordination configuration of 2 is quite similar to that of 1 except O_water instead of O_methanol^. The intermolecular hydrogen bonds link the repeat units and extend the molecules to multinuclear structures in both compounds. The spectral properties of the title compounds have been studied and discussed. Furthermore, the antibacterial activities of the title compounds have been detected, the results indicate that the ligands and two copper(II) complexes exhibit certain fungicidal activities again several bacteria. Index Abstract  Two new complexes, [Cu(L)2(CH3OH)]·(ClO4)2 (1) and [Cu(L)2(H2O)]·(NO3)2 (2), have been synthesized and their crystal structures have been determined by X-ray analysis, where L= 3-(3,5-bimethylpyrazole-yl)-6-chloro-pyridazine. The intermolecular hydrogen bonds extend the molecules to multinuclear structures in both compounds.      

Synthesis and Crystal Structure of Diisopropyl Hydroxy(4-methoxyphenyl)methylphosphonate

Abstract  The title compound, C₁₄H₂₃O₅P, was synthesized by the reaction of 4-methoxybenzaldehyde and diisopropyl phosphite. Its structure was determined with X-ray crystallographic, NMR, MS, and elemental analysis (EA) techniques. The crystal belongs to monoclinic, space group P 2_1/n with the following crystallographic parameters: a = 10.529 (2) ?, b = 8.424 (2) ?, c = 19.448 (4) ?, α = 90°, β = 105.2 (3)°, γ = 90°, μ = 0.180 mm⁻¹, V = 1664.1 (6) ?³, Z = 4, Dx = 1.207 mg/mm³, F (000) = 648, T = 293 (2) K, 2.00° ≤ θ ≤ 25.50°. The final residual factor is 0.049 for 1933 reflections with I > 2σ (I). Crystal packing is stabilized by interatomic hydrogen bond interactions between the doubly bonded phosphoryl O atom and the hydroxyl H atom which link the molecules into chains along the [011] plane of the unit cell. Index Abstract   The title compound, diisopropyl hydroxy(4-methoxyphenyl)methylphosphonate, was synthesized by the reaction of 4-methoxybenzaldehyde and diisopropyl phosphite. Its structure was determined with X-ray crystallographic, NMR, MS, and elemental analysis (EA) techniques. Crystal packing is stabilized by interatomic hydrogen bond interactions between the doubly bonded phosphoryl O atom and the hydroxyl H atom which link the molecules into chains along the [011] plane of the unit cell.      

Synthesis and Crystal Structure of <Emphasis Type="Italic">Tris</Emphasis>-(<Emphasis Type="Italic">N</Emphasis>–<Emphasis Type="Italic">N</Emphasis> dimethyl benzylammonium)-hexachlorobismuthate(III)

Abstract  The salt tris-(N–N dimethyl benzylammonium)-hexachlorobismuthate(III) crystallizes in the triclinic system P1 with unit cell parameters: a = 9.0300(12), b = 9.9220(3), c = 19.575(2) ?, α = 79.955(5), β = 89.952(2), γ = 88.108(6)°, V = 1726.0(3) ?³, Z = 2. The examination of the structure shows an alternate stacking of inorganic layers of hexachlorobismuthate(III) anions and organic layers of [C₆H₅CH₂NH(CH₃)₂]⁺ cations parallel to the a-axis. The cohesion forces of the packing of N–N dimethyl benzylammonium units in the layer and between two adjacent layers are provided by hydrogen bonds (N–H⋯Cl) and van der Waals contacts. Index Abstract  The examination of the structure shows a layer arrangement parallel to the a-axis: planes of octahedral anions [BiCl₆]³⁻ alternate with planes of [C₆H₅CH₂NH(CH₃)₂]⁺ cations (Fig. 3). The cohesion forces of the packing of the N–N dimethyl benzylammonium units in the layer and between two adjacent layers are provided by hydrogen bonds (N–H⋯Cl) and van der Waals contacts. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.