Crystal structure of monomethylammonium monochlorodibromomercurate(II)

The crystal structure of monomethylammonium monochlorodibromomercurate (II) was refined from single crystal X-ray data including the fractional contribution of centrosymmetric domains. The refinement converged toR=0.05 in space groupC2. The fraction of structure and its inverse were detected in the refinement. The structure is one-dimensional consisting of distorted tetrahedra (HgCl₂Br₂) connected together by chlorine atoms, The CH₃NH ₃ ⁺ groups are connected to the chains by hydrogen bonds to the halogen atoms contributing to the cohesion of the crystal.     

Crystal structure of monomethylammonium monochlorodibromomercurate(II)

The crystal structure of monomethylammonium monochlorodibromomercurate (II) was refined from single crystal X-ray data including the fractional contribution of centrosymmetric domains. The refinement converged toR=0.05 in space groupC2. The fraction of structure and its inverse were detected in the refinement. The structure is one-dimensional consisting of distorted tetrahedra (HgCl₂Br₂) connected together by chlorine atoms, The CH₃NH ₃ ⁺ groups are connected to the chains by hydrogen bonds to the halogen atoms contributing to the cohesion of the crystal.     

Crystal and molecular structure of [5,10,15,20-tetrakisphenyl-2-ethoxy-3-oxa-chlorinato]Ag(II)

The silver(II) complex of the chlorin-like derivativev [5,10,15,20-tetrakisphenyl-2-ethoxy-3-oxa-chlorinato]Ag(II) (1Ag), formally formed by substitution of one pyrrolic subunit in silvermeso-tetraphenylporphyrin by one ethoxy-substituted hydrooxazole moiety, crystallizes in the tetragonal space groupI4/m witha = 13.4811(10) Å,c = 9.7361(13) Å, andZ = 2. The molecule, which is asymmetric, accommodates the high-symmetry space group by rotational disorder with the silver atom located on the four-fold axis.     

Crystal structure of dicyanatobis(pyridinato)-copper(II)

The crystal structure of dicyanatobis(pyridinato)copper(II), C₁₂H₅CuN₄O₂, was determined from 658 X-ray diffraction data obtained by the -2 scanning technique with MoK radiation on a SYNTEX P2₁ four-circle diffractometer. The blue crystals are tetragonal:I4₁/a,a = 15.649(3),c = 9.917(3) Å, andZ = 8. The structure was determined by the heavy-atom method and refined by full-matrix least squares toR = 7.1%. Nonhydrogen atoms were refined anisotropically, and the positional parameters of hydrogen atoms were calculated from geometrical considerations. The copper atom is planarlytrans coordinated by two nitrogen atoms from the NCO groups and two nitrogen atoms from the pyridine molecules. The oxygen atoms from two of the approximately linear NCO groups complete the Cu(II) coordination as a distorted octahedron. Through their oxygen and nitrogen atoms, the NCO groups link the metal atoms to the skeleton structure. The bond lengths are 1.15 and 1.18 Å for N-C and C-O, respectively, the N-C-O bond angle being 176.8 °. The bond lengths Cu-N in square-planar coordination are 1.95 and 2.05 Å, while the Cu-O bonds are out of plane and 2.61 Å in length.Part XVIII in the seriesCyanatocopper(II) complexes with organic ligands; Part XVII: J. Kohout, A. Malejova and J. Gazo, Chem. Zvesti, in press.     

Crystal structure of chloritopentamminecobalt(III) tetracyanopalladate(II)

The X-ray crystal structure of [(NH₃)₅Co(ClO₂)][Pd(CN)₄]·H₂O consists of two discrete complex ions and a water of hydration. The red crystals are triclinic, P , with lattice parameters a = 7.1992(5), b = 9.4873(7), c = 11.7752(8) Å. = 66.680(1), = 75.784(1), = 82.203(1)°, and Z = 2 giving a cell volume of 715.27(9) ų and a calculated density of 2.043 g/cm³ at 293°. The chlorite ion is O-bonded to the cobalt atom with amine N—Co distances all equal. The chlorite ion is bent with a O—Cl—O angle of 110.8(2)° and the Cl—O distances being 1.601(3) and 1.558(3) Å, the longer value for the O atom also coordinated to Co. The Pd(CN)^–2 ₄ ions are planar, C-coordinated and stack along the x-axis, separated by 3.599(1) Å and alternatively rotated by 29.9(5)°.     

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(2,4-pentanedionato)copper(II)

The structure of bis(acetylacetonato)copper(II) has been redetermined from single crystal X-ray diffraction data. The unit cell parameters area=11.331(9),b=4.697(3),c=10.290(9) Å, and=91.84(7)dg. A finalR=0.056 for 727 observed reflections was obtained. The O-Cu-O chelate (bite) angle is 93.2(2)°. The two Cu-O bond lengths are 1.914(4) and 1.912(4) Å. The complex has a slight chair structure and a step angle of 7.05°.     

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 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 structure of cesium aquanickelo(II)undecatungstophosphate dihydrate

The title compound, Cs₅[PNi(H₂O)W₁₁O₃₉]·2H₂O, is tetragonal with space groupP4₂/ncm and cell dimensionsa=20.908(5),c=10.391(6) Å. The single-crystal structure determination (diffractometer data, Mo radiation,R=0.054 for 1484 unique reflexions) shows that two types of disorder are present: the Ni atom substituting for W in the parent-PW₁₂O ₄₀ ^3– anion is distributed equally over all twelve W sites and, in addition, the anion lies at a crystal site of symmetry 2/m in two equally weighted orientations related by the two-fold axis. The dimensions of the anion are normal.     

Crystal structure of 1,4,8,12-tetraazacyclopentadecane copper(II) tribromocuprate(I)

The title compound is a mixed valence compound obtained as one of the products of the reaction of Cu(15-ane N₄)Br₂ with CoBr₂·6H₂O in water/acetone solvent (15-ane N₄=1,4,8,12-tetraazacyclopentadecane). The compound is tetragonal, space group P4₂/mbc witha=16.675(2)Å,c=13.185(3)Å,V=3666(1)ų, withZ=8, for p_calc=2.106 g/cc. Refinement of 674 unique observed reflection yielded final values ofR=0.088 andR _w=0.083. The compound contains chains of alternating Cu(15-ane N₄)²⁺ cations and CuBr ₃ ^2– anions. The chains run perpendicular to thec axis, and are arranged in alternate layers running parallel toa andb. The chains lie athwart the mirror planes atz=0 andz=1/2, with disorder observed for both the (15-ane N₄) rings and the CuBr ₃ ^2– anions. The Cu(II) ion is coordinated by the tetradentate macrocycle to yield an approximate square planar coordination. The CuBr ₃ ^2– anions are nearly planar with Cu–Br(ave.)=2.37Å. Long semi-coordinate Cu(II)...Br bonds of 3.0Å link the cations and anions.     

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 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 structure of dichlorobis(pyridine-1-oxide)copper(II)

The crystal and molecular structure of dichlorobis(pyridine-1-oxide) copper(II), C₁₀H₁₀N₂O₂Cl₂Cu, has been determined from 3931 reflections measured on a Picker four-circle diffractometer, using the /2 scan technique and MoK radiation. The crystals are monoclinic, space groupP2₁/c,a = 6.900(4),b = 15.065(7),c = 12.065(5) Å, = 97.00(4) ° andZ = 4. The structure was solved by Fourier methods and refined by full-matrix least-squares. The final conventionalR-factor was 0.033. The compound is dimeric, and the units of the dimer are held together by oxygen bridges. The coordination polyhedron for Cu is a tetragonal pyramid, with two bridging oxygens and two chlorines in the basal plane. The apical position is occupied by oxygen in the non-bridging ligand. The Cu–Cu distance in the dimer is 3.306(1) Å.     

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.     

Crystal and molecular structure of bromo-bis(bis-diphenylphosphino-ethylene)-nickel(II)-tetraphenylborate

The Ni(II) complex of the ligandcis-1,2[bis(diphenylphosphino)ethylene] (VPP), [Ni(VPP)₂Br]BPh₄, crystallizes in the orthorhombic space groupP2₁2₁,2, witha=25.971(6),b=24.508 (6),c=19.642(5) Å,Z=8. The structure was determined by the procedure DIRDIF from Cu K automatic diffractometer X-ray data and refined by block-diagonal least-squares toR=11% for 5572 reflections. A question on the space group assignment betweenP2₁2₁2 andP2₁2₁2₁ was resolved only after the complete structure had been determined. The detailed crystal and molecular structure is presented.     

Crystal structure and vibrational spectra of polyamine-copper(II) complexes

The structures of [Cu(en)(H₂O)₂]SO₄ (I), [Cu(en)₂](NO₃)₂ (II) and [Cu(trien)I]I (III) have been determined by single crystal X-ray diffraction. ComplexI is monoclinic, space group C2/c, with unit cell parametera=7.232(1),b=11.725(2),c=9.768(1), =105.50(1)°, andZ=4. ComplexII is also monoclinic, space group P2₁/a, witha=7.978(2),b=9.982(4),c=8.218(3), =111.11(2)°, andZ=2. ComplexIII is orthorhombic, space group P2₁2₁2₁, witha=8.098(1),b=11.902(1),c=13.682(2), andZ=4. The structures were solved by direct methods and refined by full-matrix least-squares to finalR values of 0.031, 0.043 and 0.036 for complexesI, II, andIII, respectively. ComplexesI andII show an octahedral coordination geometry. ComplexIII shows a square pyramidal coordination geometry. ComplexI forms infinite monodimensional chains where the SO ₄ ^2– ions acts as a bridge between two neighboringen molecules. The vibrational spectra of these complexes agree well with their crystal structures. Structure and stability of seven other related Cu(II) complexes of (trien), (dien)₂, (en)₂ and (en) are inferred in this study.     

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.