Crystal structure of bis(triphenylphosphine)-cyclopentadienyl-ruthenium-phenylacetylide chloro-copper(I) acetone solvate

The product of the reaction of (-C₅ H₅)Ru(PPh₃)₂ Cl and CuC₂Ph has been characterized by single-crystal x-ray diffraction techniques and shown to have stoichiometry (-C₅ H₅)Ru(PPh₃)₂Cu(C₂Ph)Cl-(CH₃)₂CO(I). The compound contains a phenylethynyl group -bonded to the ruthenium atom and simultaneously -bonded to a terminal Cu-Cl bond. Crystals of this compound from acetone are monoclinic,P2₁/c, witha = 12.914, = 22.111,c = 16.534 Å, = 110.77 °, andZ — 4. Full-matrix least-squares refinement constraining the phenyl rings of the triphenylphosphines, the cyclopentadienyl ring, and the solvent of crystallization (acetone) as rigid groups yieldedR and weightedR values of 0.084 and 0.075, respectively.     

Preparation and crystal structure of bis(protonated 2,6-diacetylpyridine bis(phenylhydrazone)) uranyl tetrachloride,CH3CN

The reaction of 2,6-diacetylpyridine-bis(phenylhydrazone),L, with commercial uranyl chloride under a variety of different conditions gave only complexes of the type [2LH]²⁺[UO₂Cl₄]^2?,xCH₃CN (x = 1 or 2). The structure of the title compound was determined by X-ray analysis. The crystals are triclinic, space groupP¯1,a=12.77(1),b= 23.12(2),c= 8.11(1) Å, α = 94.33(3) °, β = 89.43(3) °, γ = 98.22(3) ° andZ= 2. The structure was solved by Fourier methods, and refined by least-squares toR= 0.074 for 5210 reflections which were measured on an automatic diffractometer. The [UO₂Cl₄]^2? anions have approximately^4mm _m (D _4h ) symmetry, with the uranyl group perpendicular to a plane in which the four chlorine atoms occupy the corners of a square. The organic cations are approximately planar. Shortening in the C-N (chain) bond distances suggests the presence of a mesomeric effect extended over the entire organic system.     

Heptacoordination in MnII,NiII, and CuII complexes of 2,6-diacetylpyridine bis (acetylhydrazone)

Manganese(II), nickel(II), and copper(II) complexes of 2,6-diacetylpyridine bis (acetylhydrazone) (H₂dapac) have been synthesized and structurally characterized by X-ray diffraction methods. [Mn(H₂dapac) (OH₂)₂](NO₃)₂ crystallizes in the monoclinic space groupP2₁/c witha=11.145(3),b=10.723(4),c=17.189(2) Å, =92.81(2)° andZ=4; [Ni(H₂dapac)(OH₂)₂] (NO₃)₂·H₂O crystallizes in the monoclinic space groupP2₁ witha=9.994(3),b=14.423(4),c=7.697(2)Å, =100.37(2)°, andZ=2; [Cu(H₂dapac)(OH₂)₂](NO₃)₂·H₂O crystallizes in the orthorhombic space groupPbcn witha=20.986(5),b=14.552(3),c=6.905(1)Å andZ=4. In each case the metal atom has a slightly distorted pentagonal bipyramidal environment, the equatorial positions being occupied by three nitrogen and two oxygen atoms from the hydrazone ligand and the apices by two water molecules. The crystalline cohesion in ensured by a three-dimensional network of hydrogen bonds involving the complex cations, the nitrate anions, and, where present, the uncoordinate water molecules.     

Crystal structure of bis(4-dimethylaminopyridinium) tribromocuprate(I) and bis(4-dimethylaminopyridinium) tetrabromocuprate(II)

The synthesis and crystal structures of two copper bromide salts of the 4-dimethylaminopyridinium (4DMAP⁺) cation are reported. The Cu(I) salt, (4DMAP)₂CuBr₃, crystallizes in the monoclinic space group C2/c, with a = 11.724(2), b = 11.055(3), c = 15.763(3) Å, = 107.64(3)°, and Z = 4. It contains isolated planar 4DMAP⁺ cations and trigonal planar CuBr₃ ^2– anions. Small distortions from idealized D _3h symmetry are observed for the anion. For the Cu(II) salt, (4DMAP)₂CuBr₄, a triclinic cell is observed with a = 8.2373(2), b = 9.2428(2), c = 14.4391(1) Å, = 93.760(1), = 94.576(1), = 105.249(1)°, and Z = 2. This compound contains discrete planar 4DMAP⁺ cations and flattened tetrahedral CuBr₄ ^2– anions. Small distortions are observed for ideal D _2d symmetry.     

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.     

Diammonium μ-oxobis[trichloroferrate(III)] salts. Crystal and molecular structure of bis(benzyldimethylphenylammonium) μ-oxobis(trichloroferrate)

Several alkyl-, aralkyl-, and aryl-substituted diammonium-oxobis[trichloroferrate(III)] salts, of potential interest as model compounds for the study of certain electrophysical and biological processes, are synthesized via the corresponding tetrachloroferrate(III) salts and are characterized by IR and Raman spectroscopy. A structure analysis is performed on the representative bis(benzyldimethylphenylammonium)-oxobis(trichloroferrate). The (tetracoordinate) iron atoms in the oxo-bridged dinuclear anion of the salt each possess an ever so slightly distorted tetrahedral ligand environment; the bridge geometry [Fe-O distances 1.757(5) and 1.775(5) Å, Fe-O-Fe angle 147.7(3)°] compares well with that of other salts containing the [Cl₃Fe-O-FeCl₃]^2- anion. Crystallographic Data:a=26.392(5) Å,b=14.015(3) Å,c=9.638(2) Å,=92.65(2)°, andZ=4; space groupP2₁/n.R(F)=0.070,R _W (F)=0.078 for 4447 observed reflections.     

4-Chloro-2,6-bis(hydroxymethyl)pyridinium Chloride and 4-Dimethylamino-2,6-bis(hydroxymethyl)pyridinium Chloride Hemihydrate

Abstract  Two substituted pyridinium chloride salts, namely 4-chloro-2,6-bis(hydroxymethyl)pyridinium chloride (triclinic, P-1, a = 6.0651(8) ?, b = 8.4393(8) ?, c = 8.6554(9) ?, α = 78.845(1)°, β = 83.156(1)°, γ = 89.047(1)°; V = 431.55(8) ?³; Z = 2) and 4-dimethylamino-2,6-bis(hydroxymethyl)pyridinium chloride hemihydrate (orthorhombic, Aba2, a = 17.2179(14) ?, b = 17.6332(15) ?, c = 7.2068(6) ?; V = 2188.0(3) ?³; Z = 4), have been structurally characterized. Hydrogen bonding and van der Waals contacts are evident in both structures. Furthermore, the 4-dimethylamino derivative features a trigonal planar dimethylamino group with some π interaction between the nitrogen atom and the pyridine ring. Graphical Abstract  Two compounds, namely 4-chloro-2,6-bis(hydroxymethyl)pyridinium chloride and 4-dimethylamino-2,6-bis(hydroxymethyl)pyridinium chloride hemihydrate, have been spectroscopically and structurally characterized.      

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.     

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].     

Crystal structure of bis(2-butyl-4-chloro-imidazole)5-iminoethane

The title compound (C₁₈H₂₆N₆Cl₂) crystallizes in monoclinic space group P2₁/c with a = 14.867(4) Å}, b = 7.758(2) Å}, c = 9.671(3) Å}, = 108.78(1), V = 1056.0(5) Å}³, Z = 2, D_cal = 1.250 Mg/m³ at T = 293 K. The structure was solved by direct methods and refined by full-matrix least-squares procedures to final R = 0.0650 and wR = 0.1719 using 2493 reflections. The imidazole ring is planar and the n-butyl chain adopts an extended conformation. The molecules in the crystal are stabilized by N–H s N type of intermolecular hydrogen bondings in addition to van der Waals forces.     

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(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 structure of (2,2′-bipyrimidine)-dinitratopalladium(II) acetone solvate

(2,2′-bipyrimidine)dinitratopalladium(II) forms a triclinic crystal in space groupP?1 witha=7.605(5) Å,b=8.791(4) Å,c=12.632(5) Å, α=85.11(3)⁰, β=78.79(4)⁰, γ=77.45(4)⁰,V=807.7(7) ų, andZ=2. The Pd atom exhibits square planar coordination geometry with mean Pd?O=2.206(7) Å, Pd?N=1.990(5) Å, O?Pd?O=92.0(2)⁰, and N?Pd?N=81.0(2)⁰. The complexes associate across an inversion center with Pd...Pd=3.190(2) Å. The bipyrimidine ligand is bowed with a 5.9(2)⁰ dihedral angle between the C₄N₂ rings. The nitrate ions are on the same side of the N₂O₂ donor atoms plane and make 60.4(2)⁰ and 66.6(2)⁰ dihedral angles with that plane.     

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 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 4-benzyl piperidinium bis dihydrogenmonophosphate trihydrogenmonophosphate

The salt bis 4-benzyl piperidinium bis dihydrogenmonophosphate trihydrogenmonophosphate (bis 4-BPP bis DPT) is monoclinic with the following unit cell dimensions: a = 13.132(2) Å, b = 8.755(2) Å, c = 13.643(2) Å, β = 92.40(2)°, space group P2₁ with Z = 2. The structure was solved by the Patterson method and refined to final R value of 0.0430. The structure consists of infinite parallel two-dimensional planes built of mutually H₂PO₄ ⁻, H₃PO₄ tetrahedra and cations connected by strong O–H···O and N–H···O hydrogen bonding. There are no contacts other than van der Waals interactions between the layers.     

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 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