CRYSTAL AND MOLECULAR STRUCTURE OF BIS(O,O'-DICYCLOHEXYLDITHIOPHOSPHATO)-NICKEL(Ⅱ)

<正> Ni[(C6H11O)2PS2]2, Mr=627.39, Monoclinic, P21/n, a=11.802(7), b= 9.336(2), c=14.177(5) A,B=96.72(4)°,V=1551.3A3, Z=2, Dc=1.343g·cm-3, MoKα radiation λ=0.71073A, F(000)=648e, R=0.068 for 2642 reflections. Ni(Ⅱ) atom is surrounded by four sulfur atoms, forming a square.     

CRYSTAL AND MOLECULAR STRUCTURE OF THE ADDUCT OF BIS (1,1,1 TRIFLUORO 3-2-2'''' THENOYLACETONATO) COPPER (II) WITH PYRIDINE

<正> Mr=666.12, triclinic, Pl, a=8.868(1), b=9.719(2), c=10.861(1) A,α=58.23(1)°, β =64.06(1)° r =71.63(1)°; V =711.2 A3; 2=1, Dc=1.555 g.cm-3,for 3724 reflections with I≥ 3σ(I). In the title compound, the copper atomhas a distorted octahedral coordination with four Cu-O long bonds and twoCu-N short bonds. ,     

THE CRYSTAL AND MOLECULAR STRUCTURE OF BIS(p-NITROPHENACETURO)DIAQUOCOPPER(II)

Abstract

The crystal and molecular structure of [Cu(p-NO₂C₆ H₅CH₂CONHCH₂CO₂)₂ (H₂O)₂] has been determined by single-crystal, x-ray diffraction techniques. The compound is centrosymmetric crystallizing in a monoclinic unit cell (P2₁/c) with two molecules per unit cell. The cell dimensions are: a = 11.588(1)A, b = 11.405(1)A, c = 8.041(1)Å and β = 93.47 · (1). The structure was solved by Patterson methods and refined to a value of R = 0.063. The coordination about the copper assumes an unexpected square planar geometry in which two phenaceturic moieties are each coordinated through the carboxylic oxygen (Cu—O = 1.933A) and the two waters complete the coordination (Cu—O_w = 1.959Å). The overall conformation of the phenaceturic acid is retained although there is a rotation of 180° about the peptide C—N bond.     

CRYSTAL STRUCTURE OF TETRAMETHLAMMONIUM BIS(TETRATHIOCYANATOVANADYL) MONOHYDRATE

<正> Preliminary informatiom. The title compound [(CH_3)_4N]_4[VO(NCS)_4VO(NCS)_4.H_2O] is a member of a series of vanadyl complexes, currently being investigated. It was prepared by the reaction of VOSO_4 with NH_4SCN in aqueous solution. Crystal data. (from single, crystal diffractometry, MoKα, λ=0.71073) M=945.16, orthogonal, a=23.252(6), b=13.015(2), c=30.621(6), space group Pcab, Z=8, D_m=1.32, D_c=1.34 g.cm~-3     

双邻苯二酚锑二甲基羟乙铵的晶体结构

含锑配合物是治疗血吸虫病、肿瘤等的常用药物,我们曾对双邻苯二酚锑二乙基羟乙胺进行了晶体结构测定,本文简要报导双邻苯二酚锑二甲基羟乙胺的结构.锑化合物的制法与其二乙基羟乙铵衍生物类似.产物为淡黄色晶体,它在水溶液中长时间放置会变成紫黑色,因此,制得的晶体须立即用丙酮溶解进行重结晶.晶体的密度为1.667g/cm~3.按C_(16)H_(20)O_5NSb的元素分析结果(％)如下:Sb 28.3(28.5),C 43.9(44.9),N 3.3(3.3),H 4.7(4.7).括号内为理论值.     

CRYSTAL AND MOLECULAR STRUCTURE OF BIS(TRIPHENYLBENZYLPHOSPHONIUM) TETRABROMOCADMATE

Abstract

The molecular and crystal structure of bis(triphenylbenzylphosphonium)tetrabromocadmate has been determined by x-ray diffractometer data. Crystals are triclinic, space-group Pl with two formula units in a unit-cell of dimensions a = 12.506(6), b = 10.471(5), c = 18.396(13) Å, α = 93.07(4)°, β = 105.75(5)°, γ = 92.58(4)°. The structure was solved by direct and Fourier methods and refined by least-squares techniques to R = 0.061 for 3723 independent observed reflections. The structure consists of tetrabromocadmate (II) anions and triphenylbenzylphosphonium cations, both with a quasi-perfect tetrahedral symmetry around the cadmium and phosphorus atoms. The most significant average bond distances are: Cd-Br, 2.588(2) Å, P[sbnd]C (Phen), 1.794(5) Å and P[sbnd]CH₂, 1.806(6) Å. The P[sbnd]C (Phen) bonds are in slightly distorted staggered conformation (gauche-, gauche +, and trans) in respect of the C (Phen)-CH₂ bonds of the benzyl residues. The interatomic distances between the ions correspond to the usual Van der Waals distances.     

SYNTHESIS AND X-RAY CRYSTAL STRUCTURE OF BIS (2-AMINOMETHYLAZIRIDINE)NICKEL(II) PERCHLORATE

Abstract

The structure of the big (2-aminomethylaziridine = azida)nickel(II) complex was determined by X-ray diffraction methods. The compound, [Ni(azida)₂](C1O₄)2, crystallizes in the triclinic space group P1, Z=l, with a = 7.3545(4), b = 8.5235(5), c = 6.2156(4)Å, α= 101.871(6). β = 103.217(6), γ= 111.283(4)°, and V= 335.07(5) ų. The crystal shows discrete centrosymmetncal [Ni(azida)]²⁺ units in which azida acts as bidentate chelating ligand through N aziridine and N amino atoms. Thus, Ni has a four-coordinate square-planar geometry with four nitrogens of azida. The aziridine ring is almost perpendicular to the coordination plane. The dihedral angle between the aziridine plane and the coordination plane is 75.28°.     

二(三甲硅基环戊二烯基)二氯合锆的合成和晶体结构

在 THF中 ,通过三甲硅基环戊二烯基锂与四氯化锆反应合成了标题化合物 ,经元素分析 ,IR和 1 H NMR谱表征了其结构 ,并用 X-射线衍射测定了晶体结构 ,该晶体属于三斜晶系 ,空间群为 P1 ,晶体学参数 :a=0 .6787(6) ,b=1 .2 92 4 (2 ) ,c=1 .30 34(2 ) nm,α=67.83(1 ) ,β=82 .50 (3) ,γ=75.64 (3)°,V=1 .0 2 5nm3 ,Z=2 ,Dx=1 .41 5 g· cm-3 ,μ=8.989cm-1 ,F (0 0 0 ) =448,R=0 .0 32。质谱研究表明 ,化合物在质谱过程中发生二聚 C*p2 ZrClZr C*P2Cl(C*P=C5H4Si Me3 )。     

SYNTHESIS,CHARACTERIZATION AND CRYSTAL STRUCTURE OF A COMPLEX OF EUROPIUM PERCHLORATE WITH METHYLENE BIS(DIPHENYLPHOSPHINE OXIDE)

Abstract

A complex of europium perchlorate with methylene bis(diphenylphosphine oxide) (HMPPO), [Eu(HMPPO)₄](ClO₄)₃·2H₂O has been synthesized and characterized by X-ray crystallography, infrared spectroscopy and thermal analysis. The X-ray structure of the complex shows Eu(III) is coordinated by eight oxygen atoms from four HMPPO ligands, forming a distorted square antiprism coordination geometry. The complex crystallizes in space group P-1 with cell parameters a = 15.807(3), b = 17.868(4), c = 20.656(4) Å, α = 86.85(3)°, β = 82.33(3)°, γ = 66.75(3)°. The final R_l and R_w are 0.0803 and 0.1994, respectively, for 9540 observed reflections [I > 2[sgrave](I)]. Its luminescent properties have also been studied.     

THE CRYSTAL STRUCTURE OF BIS(N-METHYLIMIDAZOL)- PALLADIUM OXALATE MONOHYDRATE

<正> INTRODUCTION. In recent years, Zhang Liangfu et al. were successful in using complexes composed of chelate ligand of diphosphine, dinitrogen and transition metal elements of lower valence multi-electrons to activate C-H bond. Recently, we synthesized complexes of bis(N-methylimidazol) ligand with palladium(Ⅱ) or platinum(Ⅱ) oxalate. These compounds activate also     

CRYSTAL AND MOLECULAR STRUCTURE OF BIS(2-ME-THOXYETHYL-CYCLOPENTADIENYL) ERBIUM CHLORIDE

<正> Complex Cp'2 ErCl(Cp'=2-methoxyethylcyelopentadienyl)(I)has been synthesized by the reaction of Cp' Na and ErCl3 in THF It crystallizes in space group Pnma with a=12.269(0),b=11.742(6),c=11.197(2)A,V=1613.1A3,Dc=1.849 g/cm3,Z=4,A=0.71073 A,μ(MoKa)=54.38 cm-1,F(000)=876,R=0.043,Rw=0.046.The Er atom is formally nine-coordinated with a pseudo-trigonal bipyramidal geometry with the "equatorial" plane composed of the Er atom,the Cl atom and the centers(1)and(2)of the two Cp rings(Cp=cy-clopentadienyl).The molecule is located at the crystallographic mirror plane through the atom C(3),C(4),C(S),Er,O(1)and C(6).The atom Cl and the atoms of Cp'(2)(except C(16)and C(16'))are disordered with an occupancy of 0.5 each.     

OPEN METALLOCENE(X)CRYSTAL STRUCTURE OF BIS(2,4-DIMETHYLPENTADIENYL)-MONOCARBONYLTITANUIM

<正> The crystal structure of the complex [2,4-(CH3)2C5H5)2TiCO has been determined by X-ray analysis, belonging to orthorhombic systen, space group P212121 with lattice parameters a = 10.078(2), b = 11,907(2), c = 11.946(3) A, V = 1433.7 A3 and Z = 4. Several cycles of block matrix least-squares refinement gave the final R = 0.054. The results of the X-ray diffraction study confirm the open sandwich configuration of the compound with two ligand planes nearly parallel and eclipsed.     

CRYSTAL AND MOLECULAR STRUCTURE OF THE ADDUCT OF BIS [4,4,4-TRIFLUOR-1-(2-THIENYL) Butandion-1,3] COPPER (Ⅱ) WITH DIMETHYLFORMAMIDE, [Cu(TTA)_2(DMF)]

<正> [Cu(C8H4F3O2S)2(C3H7NO)], Mr = 579. 0, monoclinic, P21/c, a = 9. 4851(6), b = 26. 6574(6), c=9.2619(6) A ,β=96.08(3)°, V = 2328.7A3, Z=4, Dc=1. 65gcm-3, μ(MoKa) = 7. 2cm-1, F (000) = 1172, MoKa radiation, final R = 0. 074 and Rw = 0. 068 for 1841 reflections with I≥3σ(Ⅰ). The Cu(Ⅱ) atom is coordinated by five oxygen atoms, one of which from DMF is in the axial position, to form a square pyramidal geometry. That the thenoyl groups in the ligands take the cis-form around the Cu(Ⅱ) atom is explained by the hydrogen bonding effect.     

CRYSTAL STRUCTURE OF BIS(μ-SULFIDO)-BIS[OXO-DIETHYL-DITHIOCARBAMATO-MOLYBDENUM(V)]

<正> INTRODUCTION. Reaction of MoCl_3·3H_2O with dithio-carbamate to synthesize dinuclear or trinuclear molybdenum complexes is an interesting topic. We have obtained sulfido-bridged molybdenum(V) complex Mo_2(μ-S)_2O_2(S_2CNEt_2)_2 by reacting MoCl_3·3H_2O with NadtcEt_2 in MeOH solvent. The molecular structure of the title compound was characterized by, X-ray structure determination. We report the result of the structure determination in this paper.     

CRYSTAL AND MOLECULAR STRUCTURE OF THE ADDUCT OF BIS [4, 4, 4-TRIFLUORO-1-(2-THIENYL) BUTANEDIONE-1, 3] NICKEL (Ⅱ) WITH DIMETHYLSULFOXIDE, [Ni(TTA)_2(DMSO)]

<正> The title complex [Ni(TTA)2(DMSO)] (TTA = thenoyl trifluo-roacetone, DMSO=dimethyl sufloxide) belongs to triclinic, space group P1, parameters of crystal cell: a = 9.447(l), b = 10.505(1), c=11. 912(1)(?) , α=97. 42(1), β= 84. 00(1), γ = 102. 08(1)°, V = 1143. 3(?)3, Z = 2, Mr = 581. 22 [Ni (C8H4O2F3S)2(CH3)2SO)], Dc=1. 688g. cm-3, F(000) = 588, final R = 0. 065 and Rw = 0. 072 for 2873 reflections with I≥3σ(I). In the title complex the nickel atom has a square pyramidal geometry with four short Ni-O bonds and one long Ni -O (DMSO) bond.     

CRYSTAL STRUCTURE OF (μ-OXO)-BIS[BIS(DIETHYLDITHIOCARBAMATO)- OXO-MOLYBDENUM]

<正> INTRODUCTION. The reaction oF MoCl_3·3H_2O with dithiocarbamate in organic solvents is a interesting research area. Thus, several dinuclear and trinuclear molybdenum complexes have been synthesized The dinuclear oxo-dridged molybdenum compound was obtained by this reaction in acetonmethanol mixed solvent. The molecular configuration has been characterized     

THE CRYSTAL AND MOLECULAR STRUCTURE OF RUBIDIUM BIS(PYRIDINE-2,6-DICARBOXYLATO)-CHROMATE(III)

Abstract

A three dimensional X-ray structural analysis of rubidium bis (pyridine-2,6-dicarboxylato)chromate(III), Rb[Cr(dipic)₂], has been carried out. The structure was refined by full matrix least-squares methods, using 713 observed independent reflections recorded at room temperature, to a conventional weighted R of 0.034. The crystals are tetragonal with a=b=6.950(3) Å, c=29.47(1) Å, space group 14 1/a and Z=4. The point group symmetry of the [Cr(dipic)₂]^? ion is S₄. The Cr–N and Cr–O distances (1.974(4) and 2.000(3) Å respectively) noticeably differ from the usual values in aminoacid chromium(III) complexes. The π bonding effect of the pyridine nitrogen atom corroborates the previous spectral studies on the sodium salt of this complex. The lability of [Cr(dipic)₂]^? in acid solution has been tentatively explained on the basis of the relatively severe strain within the complex ion.     

SPECTRAL AND MAGNETIC STUDY OF COPPER(II) MEFANAMATES: CRYSTAL AND MOLECULAR STRUCTURE OF BIS(MEFANAMATO)DI(N,N-DIETHYLNICOTINAMIDE)DI(AQUA)COPPER(II)

Abstract

The synthesis and characterization of Cu(II) mefanamate (mef) compounds of composition Cu(mef)₂L (L = water, caffeine, or methyl-3-pyridylcarbamate) and Cu(mef)₂L₂ (L = 3-pyridylcarbinol, nicotinamide, N,N-diethylnicotinamide, 2,6-dimethanol pyridine or nicotine) is reported. Characterizations of the compounds were based on elemental analyses, electronic, infrared and EPR spectra and magnetic susceptibility measurements over a temperature range (80–290 K). The spectral and magnetic properties of Cu(mef)₂L indicate the presence of Cu(II) dimers structurally similar to that of Cu(II) acetate monohydrate. All the Cu(mef)₂L₂ compounds possess octahedral stereochemistry about Cu(II) with differing tetragonal distortion.

An X-ray analysis of Cu(mef)₂(Et₂nia)₂(H₂O)₂was carried out, and it featured tetragonal bipyramidal geometry around the Cu(II) atom. The tetragonal plane is created by mefanamate anions bonded to the Cu(II) atom via the unidentate carboxylate oxygen atoms [Cu-0(2) = 1.936(3)Å] and the pyridine ring nitrogen atoms of the neutral ligand N, N-diethylnicotinamide [Cu-N(l) = 2.027(3)Å] in frans-positions. Axial water molecules [Cu-O(4) = 2.557(3)Å] complete the coordination sphere.