Crystal and molecular structure ofE-mesityl(phenylsulphinyl)sulphine

E-mesityl(phenylsulphinyl)sulphine, C₁₆H₁₆O₂S₂, crystallizes in the monoclinic system: space groupP2₁/c,a = 8.310(2),b = 14.141(3),c = 14.873(4)Å, = 116.67(4) ° andz = 4.The structure has been determined by direct methods and refined by full-matrix least squares toR = 0.060 for 1834 non-zero reflections. The sulphine moiety has bond lengths 1.628(5)Å for C-S, 1.470(5)Å for S-O and a C-S-O angle of 113.8(2) °, values which are consistent with a cumulated double-bond system and sp² hybridization on the sulphur atom. All other bond distances and angles are close to those usually found for such functional groups.     

Crystal and molecular structure of (±)-cyclomethylenomycinA

The structure of (±)-cyclomethylenomycinA, a penultimate synthetic precursor of the antibiotic methylenomycinA, was determined by direct methods from MoK diffractometer data. The crystals of (±)-cyclomethylen-omycinA are orthorhombic, space groupPbca, a=15.5724(1),b=11.4415(1),c=9.5454(1)Å, andZ=8. The structure was refined toR=0.077. The chemically determined structure was confirmed. Bond distances and angles are normal and there are no unusual C-H | | | O intermolecular contacts.IUPAC name: 3-(Hydroxymethyl)-1,5-dimethyl-4-oxo-6-oxabicyclo[3.1.0]hexane-2-carboxylic acid -lactone.     

Crystal and molecular structure ofS-methyl(pentafluorosulfanyl)thiocarbamate

The X-ray structure of S-methyl(pentafluorosulfanyl)thiocarbamate, SF₅NHC(O)SCH₃, has been determined from three-dimensional diffractometer data and refined by full-matrix least-squares techniques. The crystals are monoclinic:P2₁/m,a=5.008 (5),b=7.811 (2),c=9.348 (4) Å, =99.08 (7)°, andZ=2; finalR=0.046 for 517 observed reflections. The structure comprises hydrogen-bonded (NHO) chains with the component monomers in thecis, cis-conformation, i.e., the arrangement of the nonhydrogen and nonfluorine atoms is nearly planar, the SF₅ group and the O are in acis position with respect to the C-NH bond, and the O and the CH₃ group are in acis position with respect to the C(O)-S bond. Theoretical methods including MNDO and molecular modeling were used to study the relative stabilities of the four possible conformations of SF₅NHC(O)SCH₃.     

Crystal and molecular structure ofcis-mesityl(phenylsulphonyl)sulphine

Cis-mesityl(phenylsulphonyl)sulphine, C₁₆H₁₆O₃S₂, crystallizes in the tri-clinic system: space groupP¯1,a = 9.209(2),b = 11.106(2),c = 7.626(1) Å, α = 92.53(1), β = 98.53(3), γ = 89.82(2) °. The structure has been determined by Patterson and direct methods and refined by full-matrix least squares toR = 0.057 for 2724 observed reflections. The sulphine moiety has bond lengths 1.622(2) Å for C-S, 1.466(3) Å for S-O and a C-S-O angle of 115.2(2) °, indicating sp² hybridization on the sulphur atom. All other bond distances and angles are close to normal values. The molecules are held together by van der Waals forces.     

Crystal and molecular structure oftrans-dichlorobis(oxazole)palladium(II)

The crystal and molecular structure oftrans-dichlorobis(oxazole)palladium-(II), Pd(C₃H₃ON)₂Cl₂, has been determined by single-crystal X-ray diffraction techniques using counter methods and has been refined by full-matrix least-squares procedures to a finalR index of 0.022. The complex crystallizes in the triclinic space groupP¯1 with unit cell dimensions ofa = 6.957(1),b = 7.506(1),c = 5.538(1) Å, = 109.22(1), = 91.37(1), and = 115.09(1) °, withZ = 1. The palladium(II) ion, located at an inversion center, is coordinated in a regular square-planar manner to two chloride ions at 2.293(1) Å and, at 2.016(2) Å, to the nitrogen atoms of two oxazole ligands. The planar oxazole rings are tilted 33 ° with respect to the PdN₂Cl₂ plane. Further verification of the presence of oxazole in the complex was obtained by high-resolution mass spectrometry. Crystals of Pd(C₃H₃ON)₂Cl₂ resulted irreproducibly from attempts to prepare single crystals of a previously reported dimeric palladium(II) disulfide complex by treating Pd(CH₃CN)₂Cl₂ with a slight excess of diphenyl disulfide in benzene in the atmosphere. The source of the oxazole is not understood.     

Crystal and molecular structure oftrans-dichlorobis(N-propylimidazole)palladium(II)

The crystal structure of Pd(N-PropIm)₂Cl₂ has been determined from X-ray data collected by counter methods. The compound crystallizes in the monoclinic space groupP2₁/n with four molecules per unit cell, the dimensions of which area=14.554(5),b=8.204(2),c=14.860(3) Å,=115.63(2)°. Full-matrix least-squares refinement gave a final R value of 0.0263 for 1913 independent observed reflections. The Pd atom is four-coordinated and is surrounded in atrans square planar fashion by two N atoms of the imidazole groups and by two Cl ions.     

Crystal and molecular structure of bis(diphenylmethyl) ether

Bis(diphenyl methyl)ether, C₂₆H₂₂O, crystallizes in the monoclinic system:a = 9.823(2),b = 22.638(5),c = 9.275(2) Å, β = 104.89(1) °,Z = 4,P2₁/n. The structure has been determined by direct methods, using CuKα photographic data, and refined by full-matrix least squares toR = 0.058 with Cu Kα diffractometer data for 1974 observed reflections. The molecules are held together entirely by van der Waals' forces. There is a marked difference in the molecular conformation, as defined by dihedral angles, on each side of the central oxygen atom.     

Crystal and molecular structure of tetrapyridyl-copper(II)-bis-nitrato-bis-pyridine

The crystal and molecular structure of a pyridine complex of anhydrous copper(II)nitrate is described. The structure has been solved by vector search methods and refined by least-squares methods to R₁=0.049 [I>2(I)]. The complex lies on a twofold axis parallel toa, and two solvent pyridine molecules lie on twofold axes parallel toc. The copper atom is coordinated by four pyridyl groups and two monodentate NO₃ groups. Crystal data: C₃₀H₃₀N₈O₆Cu, orthorhombic, space group Pnna(52),a=14.446(7),b=12.154(5),c=16.881(4) Å,V=2964(2) ų,Z=4.     

Crystal and molecular structure of hexahydropyridine (piperidine) hydrochloride

The structure of hexahydro pyridine (piperidine), a compound of psychobiological importance, has been determined in the form of its hydrochloride by the heavy-atom technique, using three-dimensional X-ray data. Hexahydro pyridine hydrochloride, (C₅H₅N)H₆.HC1, crystallizes in the orthorhombic space groupPbcm with four molecules per unit cell of dimensionsa = 9.68(2),b = 7.30(3),c = 9.67(2) Å. The positions of the hydrogen atoms were located from a difference-Fourier synthesis. The structure was refined by the full-matrix least-squares method, using anisotropic temperature factors, leading to the finalR-value of 0.094. The hexahydro pyridine ring has a chair conformation. The crystallographic mirror plane atz = 1/4 coincides with the molecular mirror plane passing through the C1, N and C(3) atoms of the molecule in such a way that C(1)′ and C(2)′ are the mirror images of C(1) and C(2). The dihedral angles which plane I, containing C(1), C(2), C(2)′ and C(1)′, makes with plane II, containing C(2), C(3) and C(2)′, and planeIII, containing C(1), N and C(1)′, are 120.47 and 116∶42 °, respectively. The molecules are held together by a network of hydrogen bonds of type N⁺ —H ... C1^? in thexy-plane, and by van der Waals forces in thez-direction. Both the hydrogen atoms in the NH ₂ ⁺ group of the molecule take part in the formation of hydrogen bonds.     

Crystal and molecular structure of triethanolammonium nitrate (TEAN)

The crystal and molecular structure of crystalline triethanolammonium nitrate (TEAN) was determined. TEAN is monoclinic with space groupP2₁/c and has lattice parametersa=6.592(1),b=16.358(1),c=9.3850(8)Å and=90.87(1)°. Based on four formula weights of TEAN per unit cell, the computed density is 1.393 g/cm^–3. The structure is a three-dimensional hydrogen bonded network of cations and anions. An interesting feature of the cation conformation is the presence of intramolecular trifurcated hydrogen bonding of the proton.     

Crystal and molecular structure of hydridodinitratobis(triphenylphosphine)iridium(III)

Crystals of hydridodinitratobis(triphenylphosphine) iridium(III), IrH(NO₃)2(PPh₃)₂, belong to the trigonal system, space groupP¯3e1, with hexagonal unit-cell dimensionsa = 16.33(1),c = 22.85(2) Å, andZ = 6. The six Ir atoms lie in special positions. Two (of molecule 1) have site symmetry 32 and four (of molecule 2) have site symmetry 3. Both types of molecule have trigonal bipyramidal coordination with phosphorus atoms axial but do not have sufficient nitrate groups (two instead of three) to satisfy the site symmetry. Thus both types of molecule have disordered nitrate groups and the mode of coordination appears to be somewhat different at the two sites.     

Crystal and molecular structure of bis(aminomethylphosphonate)copper(II)

The crystal and molecular structure of bis(aminomethylphosphonate)-copper(II), C₂H₁₀N₂O₆P₂Cu, has been determined from MoK diffractometer data. The compound crystallizes in the monoclinic space groupP2₁/n witha =7.571(2),b = 4.943(1),c = 11.212(3) Å, = 105.84(2) °, andZ = 2. The structure was solved by the heavy-atom technique and refined by full-matrix least-squares methods toR = 0.041, using 1084 reflections for which ¦F _o¦ > 3.92 (¦F _o¦). In this complex, the Cu atom is square-planar coordinated by four O atoms from four phosphonic groups, and not by the amino group. The Cu-O bond lengths are 1.928(3) and 1.937(3) Å, and the phosphonic groups bridge adjacent Cu atoms in polymeric chains. The infrared spectrum of this complex is reported.     

Crystal and molecular structure of tris-(O-isopropylxanthato)-chromium(III)

The title compound has been synthesized by the reaction of CrCl₃6H₂O with K{S₂COCH(CH₃)₂} in a 13 molar ratio in an aqueous medium. It has been characterized by elemental analysis and IR spectral studies. Crystals of Cr{S₂COCH(CH₃)₂}₃ are monoclinic, space group P2₁/n witha=10.002(2),b=10.973(1),c=18.961(6) Å,=91.78(2)°,V=2079.9 ų,Z=4,D _calc=1.46 g cm^–3, monochromatic radiation (Mo-K), =0.71069 Å,=11.2 cm^–1,F(0 0 0)=948,T=295K, finalR=0.0320 for 2641 reflections. The environment of the chromium atom is based on an octahedral geometry having six sulfur donor atoms from three symmetrically chelated ligands with average distances: Cr-S=2.396(9) Å, C-S=1.690(3) Å and C-O=1.315(3) Å. The bond distance between oxygen atom and the carbon atom of the isopropyl group (O-C_av=1.478(4) Å) suggests that the form –S ₂ ^(–) C=O⁽⁺⁾CH(CH₃)₂ contributes significantly to the structure of the isopropyl group.     

Crystal and molecular structure of dibromobis(benzimidazole)copper(II)

The reaction of CuBr₂ with benzimidazole and HBr in aqueous solution leads to the formation of Cu(C₇H₆N₂)₂Br₂ as dark-brown, stable monoclinic crystals. Space groupP2₁/c witha=13.794(5),b=7.875(2),c=14.510(6) Å;=105.82(5)°;V _c =1516(5) ų;D _x =2.010(3) Mg m^–3. The structure was refined by a full-matrix least-squares procedure to giveR=R _w =0.045 for 1932 intensities above 3(I). The copper (II) ions are four coordinates in the form of a distorted flattened tetrahedron CuN₂Br₂, with the bond lengths Cu-Br(1)=2.402(1), Cu-Br(2)=2.446(1), Cu-N(1)=1.976(7), and Cu-N(11)=1.946(7) Å. The flattened angles are Br-Cu-Br=139.0(1) and N-Cu-N=154.6(3)°. The geometry of intermolecular and intramolecular hydrogen bonds is discussed.     

Crystal and molecular structure of tetra-n-butylammoniumbis(stilbenedithiolato)-nickelate(III)

The crystal and molecular structure of the title compound, C₄₄H₅₆NS₄Ni, are reported. Crystals are triclinic, space groupP¯1 (No. 2) withZ=2 in a unit cell of dimensionsa=8.874(2) Å,b=9.549(5) Å,c=26.025(7) Å,=97.22(3)°,=95.06(2)°, and=98.75(3)°. The structure was solved by Patterson and Fourier methods and refined by full-matrix least squares toR=0.062 for 2910 unique diffractometer data. The metal atom of the anion has an approximate square-planar configuration and the nitrogen atom of the cation an approximate tetrahedral configuration. The anions as well as the cations are well separated, the closest NiNi and NN approaches being the lattice repeat of 8.874(2) Å.     

Crystal and molecular structure of chlorotris(monomethylthiourea)silver(I)

The crystal and molecular structure of chlorotris(monomethylthiourea)silver(I) has been solved and refined by full-matrix least-squares methods to a finalR of 0·039 from 1150 reflections measured by counter techniques at ambient room temperature. The crystals are orthorhombic:Pmcn, a = 14·824(2),b = 8·524(1),c = 12·671(1) Å,Z = 4,D _m = 1·68,D _c = 1·72 gcm^–3. The structure consists of independent, distorted tetrahedral Ag(I) moieties with only weak hydrogen bonds and/or van der Waals interactions between molecules. These molecules are packed in such a way that Ag, Cl and one entire monomethylthiourea ligand all lie in a crystallographic mirror plane, and the other two ligands are related by this mirror. This arrangement, plus the alternation of the Ag-Cl bond direction, leads to a non-polar sheet of Ag, Cl and monomethylthiourea groups with other monomethylthiourea groups protruding from either side of the sheet. Only N-HCl hydrogen bonds and van der Waals interactions exist between sheets. The Ag-S distance is somewhat long at 2·649(3) Å, as is one of the Ag-S distances at 2·665(3) Å. The other two Ag-S distances are 2·520(2) Å. The geometry of the complex makes it clear that the Ag-S bond is formed by donation of an electron pair from a sulfur sp² orbital.     

Crystal and molecular structures oftrans-dichloro-(ethylene) (4-methylpyridine)platinum(II) andtrans-dichloro(ethylene) (2,4,6-trimethylpyridine)platinum(II)

The crystal and molecular structures oftrans-[PtCl₂(C₂H₄)(4-MeC₅H₄N)] (I) andtrans-[PtCl₂(C₂H₄)(2,4,6-Me₃C₅H₂N)] (II) have been determined by single-crystal x-ray methods.I crystallizes in space groupP2₁/c witha= 4.991(1), b=21.658(3), c=10.675(3) Å, =110.17(2) °,Z=4;II is orthorhombic (Pbca) witha=10.295(6),b=12.393(8),c=20.370(10) Å,Z=8.Full-matrix least-squares refinements have given finalR factors of 0.053 (1520 reflections) forI and 0.042. (1412 reflections) forII. The intensities were recorded by counter methods, and only those reflections havingI>3(I) were used in the analyses.In both complexes, platinum is four-coordinate with the two chlorine atoms, the double bond of the ethylene, and the nitrogen atom of the substituted pyridine. The two structures are discussed in terms of the arrangement of the pyridine ligand with respect to the PtCl₂(C₂H₄) moiety.     

Crystal and molecular structure of nickel(II) dicyanothiosemicarbazide monohydrate

The structure of the title compound (Ni(CN)₂(CH₅N₃S)·H₂O) has been determined, from X-ray diffractometer data, by the heavy-atom method and refined by least-squares. The finalR-values, based on 3109 observed reflections, areR=0.035 andR _w =0.039. The complex has square-planar geometry with two adjacent cyano carbon atoms (Ni-C, 1.838(2) Å and 1.862(2) Å)and thiosemicarbazide sulfur and nitrogen atoms (Ni-S, 2.169(1) Å and Ni-N, 1.923(2) Å). The water molecule does not enter the inner coordination sphere of the nickel atom; however, it plays a very important role in the crystal structure. Water is coordinated by hydrogen bonds to four adjacent complex units.