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 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 bis(cyclopentadienyl)tungsten tetrasulphide

The crystal and molecular structure of bis(cyclopentadienyl)tungsten tetrasulphide, (C₅H₅)₂WS₄, has been determined from three-dimensional X-ray data collected by counter techniques. The coordination about the tungsten atom, consisting of the two terminal sulfur atoms of the tetrasulphide chain and the ring centroids of the two cyclopentadienyl rings, may be described as a distorted tetrahedron. The inner S-S bond distance is found to be somewhat shorter than the outer two S-S bond distances in the tetrasulphide chain. The substance crystallizes in the monoclinic space groupP2₁/n witha = 11·242(3),b = 12·154(5),c = 8·790(2) Å and = 92·93(3) °. The structure was refined by least-squares techniques using 1581 independent reflections for whichFsk0/2 > 2(Fsk0/2), and the refinement converged at a conventionalR factor (onF) of 4·5 %.We wish to thank Dr. H. Köpf (Würzburg) for the gift of the crystals and the U.S. Atomic Energy Commission for financial support.     

Crystal and molecular structure of bis(tetrathiafulvalene) bis(maleonitrile-1,2-dithiolato)nickelate(II)

The crystal and molecular structure of the title compound, C₂₀H₈N₄S₁₂Ni, is reported. Crystals are triclinic, space groupP¯1 (No. 2) withz=1 in a cell of dimensionsa=8;482(2),b=7.950(2),c=9.976(2) Å,=95.64(2),=98.60(2), and =87.65(2)°. The structure was solved by Fourier methods and refined by the method of least squares toR=0.033 for 2027 unique reflections. The Ni atom has an approximate square-planar configuration with Ni-S(1)=2.179(1), Ni-S(2)=2.175(1) Å, and the S(1)-Ni-S(2) bite angle of 91.89(4)°. The anions and the cations form a mixed stack (DAD-DAD-) along the diagonal of theab plane, showing the possibility of unusual electrical behavior.     

Crystal and molecular structure of bis(protonated thiamine) tetrachlorodioxouranium(VI)

The crystal and molecular structure of bis(protonated thiamine) tetrachlorodioxouranium(VI), [C₁₂H₁₈ClN₄OS]₂ UO₂Cl₄, has been determined from three-dimensional X-ray diffractometer data. The crystals are monoclinic:P2₁/n,a = 11.199,b = 6.968,c = 23.675 Å, = 97.50°,Z = 2.The structure was determined by Fourier methods and refined by least squares toR = 0.062, using 1675 observed reflections.The structure contains octahedral [UO₂ Cl₄]^2–ions with average U-Cl and U-O distances of 2.67(1) and 1.78(1) Å, respectively.The organic portion of the molecule resembles that of previously reported thiamine structures. The failure to find the hydrogen atoms no doubt prevented our determining either which nitrogen atom is protonated or, with certainty, the hydrogen-bonding distribution.     

Crystal and molecular structure of bis(imazapyr)diaqua copper(II)

The imidazolinone herbicide imazapyr, 2-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)nicotinic acid (H₂imz) interacts with Cu(II) leading to [Cu(Himz)₂(H₂O)₂] which crystallizes in the space group Pbca, with a = 12.5370(3) Å, b = 19.8500(5) Å, c = 22.7720(9) Å, and Z = 8. The Cu(II) atom is octahedrally surrounded by four nitrogen atoms of two Himz^– anions and two water molecules. Each Himz^– acts as a chelating ligand by means of N pyridine and N lactam atoms leading to five-membered chelate rings. The Cu N distances vary from 1.948(4) to 2.299(5) Å while the Cu O are 2.114(5) and 2.256(6) Å. The imidazol N-H are involved in short intramolecular hydrogen bonds with the carboxylate groups. The structure is stabilized by an intermolecular hydrogen-bonded network involving the water molecules and the carboxylate groups.     

Crystal and molecular structure of bis(acetylacetonato) nickel(II)diethanol

The title compound, Ni(C₅H₇O₂)₂· (C₂H₅OH)₂, crystallizes in the triclinic system with unit cell dimensionsa = 8·923,b = 5·283,c = 9·522 Å, = 81·4, = 106·1 and = 103·3 °;Z= 1, space groupP¯1. The structure was solved by Fourier methods, and the 1557 three-dimensional counter diffraction intensity data (CuK) were used in a least-squares refinement to a conventional unweightedR of 0·053. The nickel atom is surrounded by the four oxygen atoms of the two acetylacetone ligands and the two oxygen atoms of the ethanol molecules, forming a tetragonally-distorted octahedron with acetylacetone oxygen atoms at 1·997 and 2·026 Å and ethanol oxygen atoms at 2·140 Å. Parallel molecules are linked into columns along theb-axis by hydrogen bonds between the ethanol oxygen atom of one molecule and an acetylacetone oxygen atom of a neighboring molecule.Presented at the Amer. Cryst. Ass'n. Summer Meeting, Ames, Iowa, Aug. 1971.Taken in part from the M.S. Thesis in Physics of T. S. Burke, Syracuse University, 1971.     

Crystal and molecular structure of bis(N,N-diethyldithiocarbamato)palladium(II)

The crystal and molecular structure of bis(N,N-diethyldithiocarbamato)palladium(II), Pd(S₂CN(C₂H₅)₂)₂, has been determined by a three-dimensional X-ray analysis. The compound crystallizes in the tetragonal space groupP4₂/n with unit cell dimensionsa = 16·439(8) Å andc = 6·247(3) Å. The crystals are isomorphous with bis(N,N-diethyldithiocarbamato)platinum(II). Intensities were obtained with an automatic diffractometer. The structural parameters were refined by least-squares methods to a conventionalR factor of 0·038 for 600 non-zero observed reflections. The palladium is in planar coordination with four sulphur atoms, the two non-equivalent Pd-S bond lengths being 2·317(3) and 2·315(3) Å.The authors are grateful to Mr J. G. M. van Rens for providing the crystals and measuring the unit cell dimensions, to Professor J.J. Steggerda for his continuous interest and to Mr W.P.J.H. Bosman, Mr J.M.M. Smits and Mr J.A.B.C. Wolf for valuable assistance.     

Crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)copper(III) triiodide

The crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)-copper (III) triiodide, Cu(S₂CN(C₄H₉)₂)₂ ⁺I₃ ^–, has been determined from a single-crystal X-ray diffraction study. The monoclinic unit cell, space groupP2₁/c,a = 14·026(6),b = 8·62(1),c = 25·015(9) Å, = 95·35(5) °, contains four formulaentities. Three-dimensional intensity data were obtained from Weissenberg photographs. Atomic parameters were refined by full-matrix least-squares methods to a conventionalR value of 0·083 for 950 independent non-zero reflexions. The structure contains two symmetry-independent cations. In both cations, the copper atom is in planar coordination with four sulphur atoms, the mean Cu(III)-S bond length being 2·22(2) Å. Cu(III)-S distances are about 0·08 Å less than Cu(II)-S distances in comparable complexes.     

Crystal and molecular structure of trans-bis(dodecylamine) bis(dimethylglyoximato)cobalt(III) nitrite

An octahedral geometry for the molecule of the title complex with very slight distortions around Co(III) is confirmed by single-crystal X-ray diffraction study. The molecular structure of the complex has been shown to contain two dodecylamine moieties in the trans orientations, two N-bonded dimethylglyoximato (DMG) groups and an uncoordinated nitrite ion.     

Crystal and molecular structure of bis(N-ethanol-2-oxy-1-naphthylideneaminato)copper(II)

The crystal structure of the title compound has been determined from single-crystal X-ray diffraction data. The compound crystallizes in the monoclinic space groupp2₁ witha=5.5406(4),b=17.0461(9),c=11.3762(6) Å,=93.99(1)°, andZ=2. The structure was solved by direct methods, and refined by full-matrix least squares toR=0.036 andR _w =0.039 for 2134 intensities above 3(7).The ethanolic O atoms [O(3) and O(4)] are not involved in the Cu coordination. The two bidentate ligands are connected to copper(II) atoms by their phenolic O atoms and imino N atoms in the O-O and N-N trans positions. A tetrahedral distortion of the square coordination is observed. The ethanolic oxygen atoms are involved as donors in intramolecular hydrogen bonds O(4)-H-O(1) and as donors and acceptors in intermolecular O(3)-H-O(4) ones. The molecule is substituent-trans, as the ethanol groups are oriented towards the opposite sides of the mean molecular plane. The molecular structure is compared with the literature data.     

Crystal structure of bis(morpholino)-disulphide

The crystal structure of bis(morpholino)-disulphide C₈H₁₆N₂O₂S₂, has been solved by the symbolic addition procedure using three-dimensional CuK diffractometer data. The system is monoclinic,a = 5·717(4),b = 8·880(7),c = 23·080(20) Å, = 107·8(1) ° andZ = 4. The structure was refined by fullmatrix least-squares methods to a conventional, unweightedR of 0·039 for 1441 observed reflexions. All hydrogen positions have been determined. The molecule possesses a pseudo-diad axis, the morpholine rings being in the chair conformation. Bonds at nitrogen are distorted pyramidal with the attached sulphur equatorial.     

Crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)gold(III) dibromoargentate(I)

The crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)gold(III)dibromoargentate(I), Au(S₂CN(C₄H₉)₂)₂AgBr₂, has been determined by three-dimensional X-ray methods. The compound crystallizes in the monoclinic space groupC2/c with unit cell dimensions:a= 17·39(1)b = 18·65(1);c = 9·199(6) Å; = 93·9(1)°;Z=4. Intensities were collected on an automatic diffractometer. The structural parameters were refined by least-squares methods to a conventionalR factor of 0·048 for 854 non-zero observed reflexions. The structure consists of Au(S₂CN(C₄H₉)₂)2⁺ and AgBr₂ ^– ions. The gold is in planar coordination with four sulphur atoms, the two crystallographically non-equivalent Au-S bond lengths being 2·357(8) and 2·324(8) Å. The silver is linearly coordinated, the Ag-Br bond lengths being 2·450(5) Å. The ionic packing in the structure differs from that in the analogous Au(S₂CN(C₄H₉)₂)₂AuBr₂ complex.The authors are grateful to Professor J. J. Steggerda for his continuous interest and to Mr. W. P. J. Bosman and Mr J. M. M. Smits for valuable assistance. Authors of contributions from the Department of Inorganic Chemistry and Crystallography of this University will no longer be listed in alphabetical order.     

Crystal and molecular structure of the ethanol adduct of tris(oxinato)indium(III)

The ethanol adduct of tris(oxinato)indium(III), prepared in aqueous ethanol, crystallizes in the monoclinic space groupP2₁/n (Nr.14) witha=11.343(2),b=13.477(3),c=16.845(2)Å, -94.71(1)°,V=2566.4(8)ų andZ=4. The structure was solved by direct methods and refined by full-matrix least-squares methods toR=0.032 for 3374 observed reflections withI>2 (I). Three bidentate oxinato ligands (or 8-quinolinolato) coordinate to indium atom leading to an approximately octahedral coordination of the metal(III) ion. One ethanol molecule per mole of metal complex is occluded in the crystal lattice and forms a hydrogen bond with the O(3) oxygen atom of one oxinato ligand [O(3) ... O(4) =2.715(3) Å]. The two other oxinato ligands of the same unit are not involved in hydrogen bonding.     

Crystal and molecular structure of bis(2,2,6,6-tetramethylheptane-5-thiolo-3-onato)nickel(II)

The crystal structure of the nickel(II) chelate of the monothio derivative of 2,2,6,6-tetramethyl-heptane-3, 5-dione has been studied at room temperature by X-ray diffraction methods. The space group isP2₁/c and the crystal data area = 19·96(2),b = 10·25(1),c = 12·45(1) Å, = 102·17(5) °Z = 4,D _m = 1·22,D _c = 1·23 g cm^–3. Full-matrix least-squares refinement of atomic and anisotropic thermal parameters, using 2109 non-zero intensities obtained by counter methods, terminated with a conventionalR of 0·105. The nickel was found to be surrounded by acis arrangement of two oxygen and two sulphur atoms which is almost planar, but slightly distorted towards a tetrahedron. All the evidence obtained supports extensive delocalization in the chelate rings, and the entire molecule has pseudomm symmetry. Thecis, rather thantrans relationship of the ligand atoms may indicate weak S-S interaction.     

Crystal and molecular structure of trans-(tricarbonyl)bis(trans-2,2,3,4,4-pentamethyl-1-phenylphosphetane)iron

The title compound crystallizes in the monoclinic space groupP2₁/a witha=13.092(2) Å,b=15.853(2) Å,c=15.406(3) Å,=103.00(1)°,V=3116(1) ų, andD _calc=1.237 g cm^–3 forZ=4. The structure was solved by direct methods, and refined to a finalR value of 0.057. The phosphetane ligands adopt a nonlinear trans relationship. The four-membered rings are non-planar and have different flap angles of 6.1 and 20.3°. Virtual coupling is evident in the¹³C NMR spectrum of the title compound. Comparison of the¹³C NMR spectral data of this molecule with the parent phosphine ligand, the ligand oxide, and the mono-phosphine iron complex is provided.     

Crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)-gold(III) bis(1,2-dicyanoethene-1,2-dithiolato)aurate(III)

The crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)gold(III) bis(1,2-dicyanoethene-1,2-dithiolato)aurate(III), Au[S₂CN(C₄H₉)₂]₂Au[S₂C₂(CN)₂]₂, has been determined from a single-crystal X-ray diffraction study. The monoclinic cell, space groupP2₁,/c, witha = 9·930(3),b = 12·517(3),c = 15·632(3) Å and = 110·46(3) °, contains two formula units. Three-dimensional intensity data, up to = 35 ° were collected on an automatic diffractometer. Atomic parameters were refined by full-matrix least-squares methods to a conventionalR value of 0·04 for 1874 independent non-zero reflections. The structure consists of bis(di-n-butyldithiocarbamato)gold(III) cations and bis(l,2-dicyanoethene-l,2-dithiolato)aurate(III) anions. In both ions, the gold atom is in planar coordination with four sulphur atoms, the Au-S bond lengths being 2·333(4) and 2·337(4) Å in the cation and 2·312(4) and 2·306(5) Å in the anion.     

Crystal structure of bis(benzimidazolium) tetrabromocuprate(II)

Stable, dark-violet crystals of (C₇H₇N₂)₂CuBr₄ were obtained from an aqueous solution of CuBr₂, HBr, and benzimidazole. The crystal structure was determined by three-dimensional X-ray analysis. The crystals are monoclinic:C2/c, a=15.651(4),b=7.945(1),c=15.775(4) Å,=91.44(2)°,Z=4,V _c=1960.96 ų,D _x=2.105 g cm^–3. The structure was refined by full-matrix least squares to giveR=0.042 andR _w=0.048 for 1254 intensities above 3(I). The copper(II) ions are four-coordinated in the form of a distorted tetrahedron CuBr₄ ofC ₂ symmetry. Two different Cu-Br bond lengths are observed: Cu-Br(1)=2.426(2), Cu-Br(2)=2.330(2) Å. Only one flattened angle [Br(2)-Cu-Br(2)=132.71(9)°] in the CuBr₄ tetrahedron is noted. The angles Br(1)-Cu-Br(1)=108.83(7), Br(2)-Cu-Br(1)=99.92(5) and Br(2)-Cu-Br(1)=107.13(5)° have been found. Hydrogen bonds explain the deformation of the CuBr ₄ ^2– coordination polyhedron. The structure is compared with other CuX ₄ ^2– complexes.     

Crystal structure of bis(p-phenoxyphenyl) tellurium dichloride

Crystals of (p-PhOC₆H₄)₂TeCl₂ are monoclinic with space groupP2₁/c,a=8.063(2),b=21.695(5),c=12.622(2) Å,=101.57(2)°, andZ=4. The structure refined to a finalR value of 0.055 for 2135 unique observed reflections. The compound adopts a primary four-coordinate geometry based on a distorted trigonal bipyramid with an equatorial lone pair. A weak Te-Cl secondary interaction links the molecules into centrosymmetric dimers.     

Crystal structure and spectroscopic characterization of bis(N-phenylthiourea)

Bis(N-phenylthiourea) (BPTU) has been synthesized and characterized by means of X-ray, IR, Raman, UV-Vis, ¹H NMR, and FAB mass spectra. The BPTU crystal belongs to the monoclinic C2/c space group with the cell constants a = 26.992(8) Å, b = 6.336(3) Å, c = 9.463(3) Å, = = 90°, = 105.97(7)°, Z = 4. The compound has been found to exist in the thione form, with cis configuration of the thiosemicarbazone moiety and skew conformation of the molecule.