α-substituted Phosphoryl Compounds (II). The Crystal and Molecular Structure of Diphenyl-[5,6-dichloro-1, 3-benzodioxol-(2)]-phosphine-oxide,C19H13O3PCl2

The compound crystallizes in the monoclinic space group P 2₁/c with four molecules per unit cell, and with the lattice parameters a = 11.807 Å, b = 13.070 Å, c = 11.312 Å, β = 96.74°. With X-ray diffraction data collected on a four circle diffractometer, the crystal structure has been determined by direct methods and refined to an R-value of 0.061 for 2735 measured and symmetrically independent reflections. The substance is a derivative of acetales of formyl diphenyl phosphine oxides. Correlations between the geometry of the structure and NMR-data are of interest.     

α-substitued phosphoryl compounds (IV). The crystal and molecular structure of diethyl[bis-(p-chlorophenoxy)-methan]-phosphonate,C17H19O5PCl2

Diethyl-[bis-(p-chlorophenoxy)-methan]-phosphonate crystallizes in the triclinic space group P 1 with two molecules per unit cell. The lattice parameters are a = 8.757 Å, b = 10.479 Å, c = 12.878 Å, α = 82.21°, β = 116.27°, γ = 113.80°. With X-ray diffraction data, collected on an automatic four circle diffractometer, the crystal structure was solved by direct methods and refined to an R-value of 0.049 for 3116 measured and symmetrically independent reflections. The substance is a derivative of acetales of formyl phosphonic acid esters. Correlations between the geometry of the structure and NMR-data are of interest.     

α-substituted phosphoryl compounds (III). The crystal and molecular structure of diphenyl[1,3-benzodithiolyl-(2)]-phosphinoxide,C19H15OPS2

Diphenyl[1,3-benzodithiolyl-(2)]-phosphinoxide crystallizes in the monoclinic space group P 2₁/c with four molecules per unit cell. The lattice parameters are a = 9.600 Å, b = 11.270 Å, c = 16.484 Å; β = 99.72°. With X-ray diffraction data collected at an automatic four circle diffractometer, the crystal structure has been solved by direct methods and refined to an R-value of 0.08 for 2690 measured and symmetrically independent reflections. The substance is a derivative of acetales of formyl diphenyl phosphine oxides. Correlations between the geometry of the structure and NMR-data are of interest.     

Synthesis and Single Crystal X-Ray Structure of [Na(H2O)2(C18H15O6SO3)]2

Abstract  [Na(H₂O)₂(C₁₈H₁₅O₆SO₃)]₂ was synthesized by sulfated 5-hydroxy-6,7,4′-trimethoxyisoflavone with concentrated sulfuric acid. Single-crystal X-ray diffraction study indicates that it is a dimeric centrosymmetric species. The coordination polyhedron of each Na(I) atom exhibits a distorted trigonal bipyramidal geometry. The dimeric units are linked by intermolecular hydrogen bonds C–H⋯π, C–H⋯O and O–H⋯O to result in a three-dimensional framework. Graphical Abstract  [Na(H₂O)₂(C₁₈H₁₅O₆SO₃)]₂ was synthesized by sulfated 5-hydroxy-6,7,4′-trimethoxyisoflavone with concentrated sulfuric acid. The coordination polyhedron of each Na(I) atom exhibits a distorted trigonal bipyramidal geometry. The dimeric centrosymmetric units are linked by intermolecular hydrogen bonds C–H⋯π, C–H⋯O and O–H⋯O to result in a three-dimensional framework. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal and molecular structure ofN-[2-phenyl-glyoxylohydroximoyl]-pyridinium bromide,C13H11N2O2Br

The crystal structure of the title compound, C₁₃H₁₁N₂O₂Br, has been determined by three-dimensional X-ray diffraction data. The crystals are monoclinic,P2₁/c:a=8.3029(9),b=12.798(3),c=12.314(2) Å,=105.94(1)°,Z=4. The structure was solved by Patterson and Fourier methods and refined to anR value of 0.044 for 1924 observed reflections. The phenyl ring shows a mean C-C bond length significantly short, 1.375(4) Å; all other bond lengths and angles have normal values, and a -delocalization is evident within the molecule, with the exclusion of the pyridinium. The two rings are in reciprocaltrans-position [=–170.5(2)°], whereas the oxime and the pyridinium are incis-position [=2.0(3)°]. A hydrogen bridge connects the bromide ion and the oxime [Br^–H: 1.91(2) Å] and there are also two short approaches of the bromide ions with carbon atoms, which ensure the crystalline cohesion.     

Crystal and Molecular Structures of Modified Progestagens (I). 17α-Cyanomethyl-17β-hydroxy-estr-4-en-3-one,C20H27NO2

17α-Cyanomethyl-17β-hydroxy-estr-4-en-3-one is the first member in a series of progestagens investigated systematically by X-ray structure analyses. It crystallizes in the orthorhombic space group P 2₁2₁2₁ with cell parameters α = 8.887(6), b = 11.814(7), and c = 16.263(2) A. The structure was solved by MULTAN-82 and refined to R = 0.045 for 1453 observed reflections. The steroid ring A has an 1β-sofa conformation, the rings B and C adopt chair forms, ring D is intermediate between 13β,14α-half chair and 13β-envelope. All rings are trans-fused. In the present structure, O H… N hydrogen bonds link the molecules into chains parallel to α.     

Molecular iodine catenation in the anionic chains [Pd2I6(I2)]2–

In the easily accessible salt [(H₅O₂)(db24c8)]₂[Pd₂I₆(I₂)], iodine molecules are catenated in linear anionic chains [^…I₂PdI₂PdI₂^…I–I^…]^2– which are separated by bulky cations consisting of two (H₅O₂)⁺ cations sequestered in dibenzo‐24‐crown‐8 (db24c8) molecules. The new compound is obtained as black single crystals (triclinic, P1, a = 1001.8(2), b = 1185.8(2), c = 1503.7(3) pm, α = 102.97(1), β = 107.65(1), γ = 90.85(1)°, V = 1652.3(5) 10⁶·pm³, Z = 1) from a moist 1:1 dichloromethane/ethanol solution of PdCl₂, iodine and db24c8. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and Molecular Structures of Modified Progestagens (IV). 17α-Azidomethyl-17β-hydroxy-estra-4,9-dien-3-one,C19H25N3O2

The crystal and molecular structure of 17α-azidomethyl-17β-hydroxy-estra-4,9-dien-3-one has been determined by X-ray structure analysis. It crystallizes in the orthorhombie space group P 2₁2₁2₁ with cell parameters a = 9.118(1), b = 9.252(1), and c = 20.444(2) Å. The structure was solved by MULTAN-82 and refined to R = 0.042 for 1408 observed reflections. Steroid ring and 17β-side chain conformations are discussed in the paper. Intermolecular hydrogen bridges between hydroxyl groups and carbonyl oxygen atoms link molecules forming chains in c-direction.     

Electronic Structure of [Cu(C7H4NO3S)2(H2O)4] · 2H2O Crystal

The electronic absorption spectrum and ESR spectrum of the crystal of the title compound [Cu(C₇H₄NO₃S)₂(H₂O)₄] · 2 H₂O, are measured. The experimental results are discussed quantitatively by using the ligand field theory and the radial wave function of non-free Cu(II). The electronic structure of the compound is in agreement with its crystal structure.     

Structure of a binuclear silver(I) complex [Ph3PAg(O2CCH2Ph)]2

The reaction of [Ph₃PAgI]₄ with sodium phenylacetate in MeOH and CH₂Cl₂ at room temperature gave rise to a binuclear silver complex with triphenylphosphine and phenylacetate mixed ligands, [Ph₃PAg(O₂CCH₂Ph)]₂. The crystal and molecular structure of the complex has been determined by single crystal X-ray diffraction analysis. The space group is witha=9.198(2),b=9.516(2),c=13.842(3) Å, =102.00(3), =108.34(3), =93.58(3)°,Z=1, andDc=1.506 g cm^–3. The silver atoms are each coordinated by one phosphorus atom from triphenylphosphine and two oxygen atoms from the carboxylate groups in a T-shape. The complex is further characterized by its IR,¹H, and³¹P NMR spectra.     

Crystal and molecular structure ofN-methylphenazinium bis(benzene-1,2-dithiolato)nickelate(III). Structure of (C13H11N2)[Ni(S2C6H4)2]

The crystal and molecular structure of the title compound, (C₁₃H₁₁N₂)[Ni(S₂C₆H₄)₂], is reported. Crystals are triclinic, space groupP¯1(No.2) withZ=2 in a unit cell of dimensionsa=9.363(1),b=10.148(1),c=13.623(1) Å,=85.64(1),=107.33(1), and =113.10(1)°. The structure was solved by the heavy-atom method and refined by the method of full-matrix least squares toR=0.036 for 2874 unique reflections. The metal atom of the anion has an approximate square-planar configuration. The metal atoms occupy the origins and A-face centers of the lattice. The anions with the metal atoms in the origins stack along thec-axis, the interplanar separation being thec-axis lattice repeat of 13.623(1) Å. The anions with the metal atoms in theA-face centers and the cations form a mixed stack along the short diagonal of theab-plane. The short interplanar distances (C–A=A–C=3.43 Å and C-C=3.91 Å) in the mixed stack (CAC-CAC) show the possibility of unusual electrical behavior. There is no evidence of direct or indirect metal-metal interaction.This work was supported by the Department of Science and Technology, Government of India, New Delhi, for which we are grateful. One of the authors (PK) also expresses his thanks to the U.G.C., New Delhi and Pachaiyappas College, Madras, for the award of FIP Fellowship.     

Crystal structure of samarium hexamolybdoaluminate Sm[Al(OH)6Mo6O18] · 11H2O

The structure of a new complex of samarium(III) with a hexamolybdoaluminate ion, Sm[Al(OH)₆Mo₆O₁₈] · 11H₂O, was established by the methods of X-ray diffraction analysis. The crystallographic data are as follows: sp. gr. Pbc2₁, a = 10.927(4) Å, b = 11.757(5) Å, c = 22.327(9) Å, V = 2868(1) ų, Z = 4, ρ _calcd = 3.040 g/cm³, R = 0.084, R _W = 0.198. In the [Al(OH)₆Mo₆O₁₈ ^3? anion, an Al atom is surrounded by six Mo atoms with distorted octahedral coordination. The anions are linked into chains via Sm atoms. The coordination polyhedron of a Sm atom is a tricapped trigonal prism with the vertices being occupied by two terminal oxygen atoms of two adjacent anions and seven water molecules.     

Crystal and Molecular Structure of Bis(pyridine)N,N′-o-phenylen-bis[2-cyan-2-ethoxycarbonyl-vinyl-amido(–)]-iron(II)-Pyridine

The crystal and molecular structure of bis(pyridine)N,N′-o-phenylen-bis[2-cyan-2-ethoxycarbonyl-vinyl-amido(–)]iron(II)-pyridine were determined by X-ray structure analysis. It crystallizes in the monoclinic space group P 2₁/c with cell parameters a = 9.866(23), b = 19.491(46), c = 16.992(22) Å, and β = 95.19(1)°. The structure was solved by the heavy atom method and refined to R = 0.125. The coordination geometry around the iron atom is octahedrally distorted with the two pyridine molecules in the axial positions.     

Crystal and Molecular Structure of 3-Methoxy-estra-1,3,5(10)-trien-17β-ol

The crystal structure determination of the title compound was undertaken to determine the conformational flexibility of the steroid skeleton. 3-Methoxy-estra-1,3,5(10)-trien-17β-ol (C₁₉H₂₆O₂) crystallizes in the space group P2₁2₁2₁ with Z = 12, a = 12.589(2), b = 16.274(5), and c = 23.535(6) Å. The structure was solved by direct methods and refined to R = 0.056. Three symmetry independent molecules having different molecular conformations were observed in the crystal. The most flexible region of the molecules is the B ring which adopts following conformations: 7α,8β-half-chair, 8β-sofa, and an intermediate form between half-chair and sofa.     

Synthesis and Crystal Structure of 5,7,12,13b,13c,14-Hexahydro-1,4,-dibromo-8,11-dimethoxy-13b,13c-bis(ethoxycarbonyl)-6H,13H-5a,6a,12a,13a-tetra azbenz[5,6]azuleno[2,1,8-ija]benz[f]azulene-6,13-dione

The title compound has been synthesized by the reaction of 4 with 1,4-dimethoxybenzene. The yielded product 5 was investigated with X-ray crystallographic, NMR, EI-MS, and IR techniques. The crystal belongs to a monoclinic system, space group P2₁/c with unit cell parameters a = 12.7790(17) Å, b = 21.565(3) Å, c = 12.2544(16) Å, α = 90°, β = 107.014(2)°, γ = 90°, V = 3229.3(7) Å³, Z = 4, D_c = 1.661, M_r = 807.32, μ = 2.732 mm^?1, F(000) = 1632, R₁ = 0.0540 and wR₂ = 0.0989.     

Three‐Dimensional Structure Constructed via Hydrogen Bonds and π‐π Stacking Interaction. Crystal Structure of [Cu(AFO)2(H2O)2](ClO4)2.2(AFO).2H2O (AFO = 4,5‐Diazafluoren‐9‐one)

The structure of the title complexes [Cu(AFO)₂(H₂O)₂](ClO₄)₂.2(AFO).2H₂O (AFO = 4,5‐Diazafluoren‐9‐one)has been established by single‐crystal X‐ray diffraction. The complex crystallizes in the triclinic space group P‐1 with cell constants a = 7.659(3) Å, b = 11.066(3) Å, c = 14.203(5) Å, alpha = 75.16(3)°, β = 79.87(3)°, gamma = 85.71(3)°, Z = 1. The structure was solved by direct methods and refined to R₁ = 0.0595 (wR₂ = 0.1164). The X‐ray analysis reveals that a pair of AFO ligands chelate to a Cu(II) atom in an asymmetric fashion with one Cu‐N bond being much longer than the other, the Cu(II) atom is further coordinated by a pair of aqua ligands to form an elongated octahedral geometry. In the crystal of the complex, the mononuclear complex cations [Cu(AFO)₂(H₂O)₂]²⁺, uncoordinated AFO molecules, lattice water molecules and perchlorate anions are assembled into 3‐D structure via hydrogen bonds and π‐π stacking interaction.