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 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 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) 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 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 structure of bis(isothiocyanato)[2,6-diacetylpyridine bis(4-hydroxybenzoylhydrazone)]Fe(III) Chloride bis(dimethylformamide) solvate

The crystal structure of title compound (Fe[(C₂₅H₂₁N₇O₄S₂)] · 4(C₃NOH₇), where C₃NOH₇ is dimethylformamide, DMF) was determined by the X-ray diffraction method. This compound crystallizes in the monoclinic C2/c space group, Z = 4. Unit cell parameters are: a = 13.6080(5), b = 17.6375(7), c = 19.5571(6) Å, β = 108.753(2)°. The N-H...O and O-H...O interactions stabilize the molecules in the lattice. The structure contains also the solvent dimethylformamide molecules, which are connected with intermoleculer hydrogen bond. The O atoms of DMF molecules take place as acceptor atoms.     

Crystal and molecular structure of bis(tetramethylammonium) di(π-(1)-2-thiollyl)iron(II)

The crystal and molecular structure of bis(tetramethylammonium)di(-(1)-2-thiollyl)iron(II), C₈H₄₄B₂₀FeN₂S₂, has been determined from three-dimensional X-ray data collected by counter techniques. The material crystallizes in the orthorhombic system: space groupIbam, z=4, a=15·585(5), b=12·324(4), and c=14·806(6) Å. The B₁₀H₁₀S^2– moiety is an icosahedron with the sulphur atom and four boron atoms forming that part of the cage which is within bonding distance of the iron. The sulphur atom and one boron atom are disordered. The structure was solved by standard techniques and the least squares refinement, using 969 independent reflexions for whichF ₀ ² 3(F ₀ ²), converged to a conventionalR factor (onF) of 4·2%.No part of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying, microfilming, recording or otherwise, without written permission of Plenum Publishing Company Limited.National Lending Library Supplementary Publication No. 60063 contains 2 pages of structure tables on 1 microfiche.     

Crystal structure of 3-methylrhodaninecopper(I) iodide

The crystal structure of the copper(I) complex has been determined by a three-dimensional X-ray analysis. The monoclinic unit cell, space groupP2₁/c,a = 4·195(1),b = 15·581(2),c = 13·885(2) Å and = 114·9(1) °, contains four formula-units. Intensities were collected on an automatic diffractometer. The structural parameters were refined by full-matrix least-squares methods to a conventionalR value of 0·07 for 1809 non-zero observed reflexions.In this complex, the copper atom is in tetrahedral coordination with three iodine atoms and the sulphur atom of the thiocarbonyl group of the ligand. The iodine atom is coordinated with three copper atoms. The distances are 2·683(2), 2·627(2) and 2·665(2) Å. The distances between neighbouring copper atoms are 3·008(3) and 2·960(3) Å and the corresponding angles are 68·44(6) and 68·02(6) °, suggesting weak copper-copper interactions in this complex.     

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 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 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(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 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.     

Crystal structure of copper bis(tenuazonate) monohydrate

The crystal structure of copper bis(tenuazonate) monohydrate has been determined by X-ray diffraction from 968 counter-measured intensities. The thin flat crystals are monoclinic,P2₁, witha = 13.77(1),b = 15.51(1),c = 11.14(1) Å, = 109.5(2) °, and two formula units, C₂₀H₂₆CuN₂O₆·H₂O, per asymmetric unit. The structure was refined by full-matrix least squares toR = 0.056. Because of the dimerization one copper ion is four- and the other five-coordinate. The dimers are hydrogenbonded into sheets by water molecules.NIM Applied Structural Chemistry Research Group     

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 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.     

Quaternary salts of oxo-sparteines: Crystal structure of N(1)-methyl-15-oxosparteine iodide and N(1)-methyl-17-oxosparteine iodide monohydrate

The crystal structures of twoN-methiodides, derivatives of the alkaloid sparteine, have been determined by single-crystal X-ray analysis. Diffraction data were collected on a diffractometer using MoK radiation (=0.71073 Å). The finalR factors were 0.043 and 0.031 forN(1)-methyl-15-oxosparteine iodide andN(1)-methyl-17-oxosparteine iodide monohydrate, respectively. The geometry of theN-methyl cations explains the differences in reactivities of the free bases with methyl iodide in the quaternization reaction. The axial hydrogen atoms of the methylene groups C(3), C(5), C(11) (in both compounds), and C(17) (in 15-oxosparteine only) shield the N(1) nitrogen electron pair. Three of the four piperidine rings in both cations exhibits similar conformations: ringsA andB-distorted chair, ringC-distorted sofa. The oxo substituent at the C(15) atom in the fourth ring,D, inN(1)-methyl-15-oxosparteine causes the 1,3-diplanar form, while that ring inN(1)-methyl-17-oxosparteine cation adopts the chair conformation. The formation of quaternary cation requires an adjustment in the ringC conformation of the parent 15-oxosparteine skeleton from a distorted boat to a distorted sofa; the max. difference in equivalent torsion angle values is 31.4°.     

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.     

Substituted phenols as ligands III: Crystal and molecular structure of bis(4-formyl-2-methoxyphenolato)bis(pyridine)copper(II) monohydrate

Bis(4-formyl-2-methoxyphenolato)bis(pyridine)copper(II) monohydrate crystallizes in the triclinic system:a = 10·432,b = 9·342,c = 13·799 Å, = 103·75, = 100·53, = 100·81 °,Z = 2, space groupP¯1.The structure was determined by Fourier methods with Cuk diffractometer data, and refined by a combination of block-diagonal and full-matrix least squares toR = 0·068 for 2430 observed reflexions.The copper atoms occupy the special positions 0, 0, 0 and 0,1/2, 1/2; hence, both molecules are centrosymmetric. Both the methoxy and phenolic oxygen atoms of the phenolate ions coordinate to the metal. These, together with coordinated nitrogen atoms from the pyridine molecules, give the copper atoms a six-fold coordination.Hydrogen bonding between a water molecule and the phenolic oxygen atoms of adjacent molecules results in chains of molecules linked approximately along [011].