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     

STUDY OF THE CRYSTAL STRUCTURE OF AN IRIDIUM COMPLEX WITH A TETRAPHENYLBISMUTH CATION [Ph4Bi]2[(μ2-Br)Br3Ir(CH3CN)]2

Journal of Structural Chemistry - Crystals of complex [Ph4Bi]2[(μ2-Br)Br3Ir(CH3CN)]2 (1) are prepared by the interaction of tetraphenylbismuth nitrate with sodium hexabromoiridate(IV) in water...     

STRUCTURE OF [Et4N]2[Mo2（CO）8（SCH2C6H4CH2SH）]

<正> Mr =1015.05, P21/c, a= 10.912(4), b= 12.088(3), c= 18.807(8) A.β=103.57(3)° ,V= 2411.4 A3, Z = 2, DC = 1.40 g/cm3.λ(MoKα)= 0.71073 A, μ=7.2 cm-1,F(000)=1048.Room temperature, final R=0.069, Rw=0.091. The geometry around the Mo atom is a distorted octahedron. The equatorial Mo-C distances are shorter than the axial ones. The Mo...Mo distance is 3.949A.     

[Cu(C8H4F3O2S)2(C12H8N2)]·C3H6O的合成及其晶体结构

标题配合物 [Cu(C8H4 F3O2 S) 2 (C12 H8N2 ) ]·C3H6 O属于三斜晶系 ,空间群为P1,并测得如下晶胞参数a =10 .5 77(3) ,b =15 .72 2 (4) ,c =10 .133(2 ) ,α =94 .5 3(2 ) ,β =10 0 .81(2 ) ,γ =96 .18(2 )° ,V =16 37.0 3 3,Z =2 ,Mr =74 4.18,Dx =1.5 1× 10 6 g·m- 3,F(0 0 0 ) =5 2 6 ,μ =8 2 4cm- 1,最终偏差因子为R =0 .0 83,Rw=0 .0 74。Cu(II)与 2个 4 ,4 ,4 三氟 1 (2 噻吩基 )丁二酮 1,3中的四个氧原子和菲咯啉中的两个氮原子 ,组成了一个畸变的八面体构型。     

SYNTHESIS AND STRUCTURE OF （Me4N）[Mo（OC6H4S—o）3]

<正> (Me_4N)[Mo(OC_6H_4S-o)_3] ,Mr=542. 57,orthorhombic,space group Pnb21 with a = 22. 708(1),b = 9. 737(4),c=10. 486(2) A;V=2318. 6A3;Z=4,Dc = 1. 55g/cm3,final R=0. 064 and Rw=0. 074.μ=8. 3cm-1, F(000) = 1108,The atom Mo( V ) of the anion issix-coordinated to three oxygen and three sulfur atoms in a distorted octahedral geometry.     

SYNTHESIS AND CRYSTAL STRUCTURE OF [C8H8NdCl（THF）2]2

<正> The title complex was prepared from the reaction of NdClLi0.3 and C8H8, its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P21/c with cell dimensions o = 11. 819(3), 6=12.651(3), c=13. 478(3)A, β=122.99(2)°, Mr = 856. 00, Z = 2, Dc=1. 68g/cm3, F(000) = 636. 89, V = 1690. 33A3. The structure was solved by direct methods and Fourier techniques. Least squares refinement on the basis of 1842 observed reflections led to final R = 0. 038 and Rw = 0. 040. The molecule is a dimer of C3H8NdCl(THF)2 bridged by two Cl atoms with Nd -Cl bond lengths of 2. 832(2) A and 2. 917(3)A.     

SYNTHESIS AND CRYSTAL STRUCTURE OF A POLYMERIC 1,2,4,5-BENZENETETRACARBOXYLATO COMPLEX OF Cu(II) WITH IMIDAZOLE,Cu2(C10H2O8)(C3H4N2)6(H2O)4 · 4H2O

Abstract

The title complex, Cu₂(C₁₀H₂O₈)(C₃H₄O₂)₆(H₂O)₄ · 4H₂O, consists of polymeric copper(II) complex anions and discrete copper(II) complex cations. Benzenetetracarboxyl anions bridge copper(II) atoms coordinated to water and imidazole groups to form the anionic polymeric chains along the a axis, while discrete copper(II) complex cations involving four imidazole and two water ligands are packed between parallel polymeric anionic chains, an extensive H-bonding network linking complex cations and anions.     

聚金属氧酸盐[(C4H9)4N]6[PMo12O40]2·0.5H2O的晶体结构

在乙腈-水混合溶剂中培养得到了聚金属氧酸盐[(C4H9)4N]6[PMo12O40]2.0.5H2O的单晶.X射线衍射结构分析表明,该晶体属于单斜晶系,C2/c空间群,晶胞参数:a=4.996(10)nm,b=1.411(3)nm,c=2.633(5)nm,β=114.804(4)°,V=16.844 nm3,Z=1,R1=0.0843,wR2=0.2546.化合物分子由两个多阴离子[PMo12O40]3-,6个四丁基胺阳离子[n-Bu4N]+和0.5个结晶水组成.     

STRUCTURE OF NEODYMIUM TRINITRATE WITH DIPHENYL SULFOXIDE LIGANDS, Nd(N0_3)_3·[(C_6H_5SO]_4

<正> Mr=2278, triclinic, Pl, a=11.154(1), b=14.310(2), c=17.295(2) A, α=84.09(1)°, β=72.97(1)°, r=69:37(1)°, V=2470.2(5)A3, Z=2; 2(MoKα)=12.9cm-1 F(000)=1154, Dx=1.53 g/cm3, room temperature. The final R=0.039, Rw=0.039 with wt=1, S=2.57 for 5710 independent reflections with | Fα|≥2.5σ(F0). The molecular configuration of the Nd-complex is similar to those of the Sm-complex and Pr-complex except for the difference in distances between central metal and the coordinated oxygen atoms.     

THE CRYSTAL STRUCTURE OF BIS(TETRAETHYLAMMONIUM)(μ-OXO)BIS[TRIPHENYL-THIOLATO-IRON(Ⅲ)],(Et_4N)_2[Fe_2O(SPh)_6]

<正> Fe_2OSsN_2C_(52)H_(70),Mr=1043.23,monoclinic, P21/a, a=18.121(3), b=15.249(3), c=20.369(4)A,β=102.49(8)°,V=5495(1)A3, Z=4, Dc=1.261g.cm-3,MoKα(λ =0.710691), μ=17.816mm-1, F(000)=2208. R=0.073 for 4374 observed reflections with I≥3.0σ(I). The structure of the anion contains a linear Fe-O-Fe unit, with mean Fe-O distance of 1.766(2)A. The coordination geometry about each iron atom is close to tetrahedral with the angles O-Fe-S and S-Fe-S being 115.3° and 103.1°, respectively.     

PREPARATION AND STRUCTURE OF TETRAMETHYLAMMONIUM HYDROGEN TRIPEROXOTRIMOLYBDODISULFATE TRIHYDRATE, [N(CH3)4]3[H(SO4)2-(MoO2(O2))3]· 3H2O

Abstract

A novel peroxopolyoxomolybdate compound, [N(CH₃)₄]₃ [H(SO₄)₂ (MoO₂(O₂))₃] · 3H₂O, has been obtained from a strongly acidic aqueous solution of a molybdate-sulfate system as the monoclinic crystal of P2/n, a = 13.497(3), b = 15.231(4), c = 32.603(2) Å, β = 103.113(9)°, and V = 6577(2) ų. The final R-value was 0.0986 for 395 parameters using 7162 reflections. Each of the two crystallographically independent polyanions contains three molybdenum atoms with five O^2?, one O₂ ^2?, and two sulfate groups, one of which is a tripod ligand apical to the molybdenum plane, and the other is a bipod ligand equatorial to the Mo plane.     

SYNTHESIS AND STRUCTURE OF[Et_4N]_3[FE_3(SPh)_3Br_3Cl_3]

<正> The title compound was synthesized and its structure solved. The formula is [Et4N]3[Fe3(SPh)3Br3Cl3]. M=1231.95, monoclinic, space group C2/c, a=24.569(4), b=13.504(2), c=18.348.(3)A, β=110.78(1)°, V=5691(3)A3, Z=4, Dm= 1.41, Dc=1.44-g/cm3. The flat structure of the anion has. a planar [Fe3S3] ring and three phenyl groups. Statistical distribution of chlorine and bromine atoms on two sides of the [Fe3S3] plane results in a C2 symmetry of the anion.     

CRYSTAL STRUCTURE OF（Bu4N）2[Pt（C3S5）2]

<正> The title compound C38H72N2PtS10(Mr=1072.74)crystallizes in triclinic system,space group P1 with cell constants a=11.994(4),b=18.117(7),c=11.855(6)A,α=95.55(4),β=99.14(3),γ=75.71(3)°,V=2460.0A3,Z=2 and Dc=1.45 gcm-3.The structure is solved by direct methods and refined by full-matrix least-squares technique to final R=0.046 and Rw=0.045 based on 5919 independent reflections with I≥3.0(I).The anion [Pt(C3S5)2]2-is approximately planar,of which the platinum-sulfur coordination polyhedron takes a square form with mean Pt-S bond length of 2.310(4)A.     

SYNTHESIS AND STRUCTURE OF A PENTAMETHYLCYCLOPENTADIENYL THULIUMCHLORIDE COMPLEX, [(C5ME5)2Tm(μ3-CL)2K(THF)]N

Abstract

The first structural data on a pentamethylcyclopentadienyl complex ofthulium, [(C₅Me₅)₂Tm(μ₃-C1)₂K(THF)]_n,1, are reported. TmCl₃ reacts with 2 equivalents ofKC₅Me₅ in THF to form 1 in <80% yield. 1 crystallizes from THF/hexanes in thespace group Cc with a = 11.1491(13) Å, b= 28.107(2) Å, c = 8.5921(8) Å, β= 102.485(8)°, V = 2628.8(4) ų, and D_calcd = 1.570 Mg/m³ for Z= 4. Least-squares refinement of the model based on 3114reflections (F² > 3.0 [sgrave] (F²))converged to a final R_F = 1.9%. Thepolymeric structure of 1 is generated by triply bridgingchlorides, each of which is connected to one(C₅Me₅)₂Tm bentmetallocene unit and two K(THF) moieties in a T-shaped geometryaround the chloride.