二甲基-2'-乙酰基双二茂铁甲烷的晶体和分子结构

二甲基-2′-乙酰基双二茂铁甲烷C_5H_5FeC_5H_4C(CH_3)_2C_5H_4FeC_5H_4COCH_3为深紫色菱形晶体,m.p.115.5～116.5℃。它属单斜晶系,P2_1/c空间群。晶胞参数为:a=11.626(1),b=13.219(1),c=13.078(2)A,β=90.67(1),V=2009.8A~3,Z=4,Dc=1.501g/cm~3。用MULTAN-78直接法程序求解晶体结构,最后偏离因子R=0.040。中心C原子周围的四个基团以变形四面体取向,分子本身不具有任何对称性。     

乙二醇二甲醚三苯基氧化膦三氯合铬Cr[(CH_3OCH_2CH_2OCH_3)(OPPh_3)Cl_3]的合成和晶体结构

标题配合物由Cr(CO)_6和PPh_3在50ml乙二醇二甲醚中回流5小时后过滤,在滤液中加S_2Cl_2,静置后得配合物单晶。晶体属单斜晶系,空间群为P2_1,单胞参数a=9.062(3)(?),b=11.088(3)(?),c=12.153(3)(?),β=97.93(1)°,V=1209.4(1.8)(?)~3,Z=2。 晶体结构是采用Patterson法和差Fourier合成解出。经全矩阵最小2乘法修正,最后偏离因子R=0.046,R_w=0.054,结构中Cr各与三个氧和三个氯原子键联,Cr-O(CH_3OCH_2CH_2OCH_3)平均距离为2.091(?),Cr-O(OPPh_3)距离为2.000(?),Cr-Cl(平均)距离为2.274(?)。它们形成了八面体配位构型。     

一种新颖钒.钨异金属八核簇合物[VW~3~4(O~2CEt)~8]~2Na~2的合成与结构

本文报道了一种钒.钨异金属八核簇合物[VW~3~4(O~2CEt)~8]~2Na~2(1)在恒温液相条件下的合成与结构研究,晶体属三斜晶系,P1空间群,a=1.2973(4),b=1.4063(3),c=1.2396(5)nm,α=1.09.92(2),β=117.32(2),γ=90.53(2)°,V=1.8513nm^3,D~c=2.29g/cm^3,Z=1对5499个可观测反射点[I>3σ(I)] 最终一致性因子为R=0.030.单晶结构分析表明,簇阴离子中两个[W~3O~4]^4^+单元通过两个"桥"金属V原子联接成一个奇特的环状结构,W-W平均键长为0.25328(6)nm,W...V间平均距离为0.3654nm,簇阴离子通过Na^+联成一个一维长链.Na 原子具有少见的五配位,Na-O距离仅为0.2314nm,Na-O间教情的相互作用以及无限长链的晶体结构很好地解释乐簇合物1的稳定性和不溶性.     

{[Gd(DMF)3(DMSO)(H2O)3](μ-CN)[Fe(CN)5]}·2H2O的合成，结构表征和磁性

A new cyano-bridged Gadolinium^Ⅲ-Iron^Ⅲ complex {[Gd(DMF)₃(DMSO)(H₂O)₃](μ-CN)[Fe(CN)₅]}·2H₂O (DMF=N,N-dimethylformamide; DMSO=dimethylsulfoxide) was synthesized by the grinding reaction method. It crysta-llizes in the triclinic, space group P1 with cell parameters: a=0.90363(2) nm, b=1.250 78(3) nm, c=1.41303(1) nm, α=93.174(1)°, β=94.406(1)°, γ=91.817(2)°, and V=1.588 87(5) nm³, D_c=1.582 g·cm^-3, Z=2, M_r=756.72, F(000)=760, μ=2.645 mm^-1. The slightly distorted square-antiprism eightfold-coordinated Gd(Ⅲ) and the approxi-mately oriented octahedrally sixfold-coordinated Fe(Ⅲ) are linked by a cyano-bridge group to construct a dinuclear compound. The {[Gd(DMF)₃(DMSO)(H₂O)₃](μ-CN)[Fe(CN)₅]} species are held together via hydrogen bonds to form a three-dimensional framework. The Gd(Ⅲ)-Fe(Ⅲ) interaction is antiferromagnetic. CCDC: 223430.     

Synthesis and Crystal Structure of [Ca（DMF）6][Mo6Br8Cl6]

1INTRODUCTION Molybdenum(II)halide clusters containing[Mo6-X8]4 cores have been the subject of interest for over five decades[1].This octahedral cluster-type comple-xes comprise an important,and in a sense archetypal,class of higher nuclearity transition metal cluster com-plexes.Their high symmetry,photochemical and pho-tophysical properties as well as structural relation-ships to cluster complexes of other elements exhibit significant interest[2].In addition,there is a structural simila…     

Solvothermal Synthesis and Structure Studies of a Mixed-valence Oxochloromolybdenum Complex

Emerald green crystals of a new mixed-valence oxochloromolybdenum complex,Mo(OH)2(2,2′-bipy)Cl2.[MoO(2,2′-bipy)Cl3]2, were obtained in an attempt to synthesize the Mo-S cluster compounds under solvothermal conditions. The title compound was characterized by EPR and X-ray single-crystal diffraction techniques. Crystallographic data: orthorhombic, space group Fdd2, a = 12.684(1), b = 21.518(2), c = 29.096(3)A, Mr = 1103.97, V= 7941(1)A^3, Z= 8, Dc =1.843 g/cm^3,μ= 1.514 mm^-1, F(000) = 4304, R = 0.0654 and wR = 0.1544 for 1944 observed reflections with 1 ≥/ 2σ(I). The compound consists of two different neutral molecules, Mo^IV-(OH)2(2,2′-bipy)Cl2 and MoVO(2,2′-bipy)Cl3. Both Mo^IV and Mo^V ions are in a distorted octahedral environment. The Mo(1)^IV atom is surrounded by two Cl^- ions and two O atoms from OH^- and two N atoms from a 2,2′-bipy ligand. The Mo(2) atom is surrounded by three Cl^- ions, one O^2- anion and two N atoms from another 2,2“-bipy ligand. The bipyridine occupies two cis-equatorial sites, while the Cl^- ions are located at the axial and equatorial positions.     

Syntheses and Crystal Structure of [Cu（pyr）3].Hg2I6

1INTRODUCTIONThepolynucleard10metalcomplexesarepotentialluminescentsensormaterialsduetotheirattractivephotochemicalandphotophysicalpro-perties[1,2].Lowdimensionalmetal-organichalidecomplexeshavereceivedever-interestingattentioninrecentyearsfortheirpotentialapplicationsaselectronicandcatalyticmaterials[3,4].RecentlyHomo-metaloligomersandthechainsofcopperhavebeenreportedbyZubietaandthecoworkersviahydrothermalsyntheses[5,6].Theexistingexamplesofcopperwithmercuryareextremelyrare[7].Intherece…     

——>——>双核钴簇合物(C6H5CO2CH2C)2Co2(CO)6的合成与结构

The cluster (C_6H_5CO_2CH_2C)_2Co_2(CO)_6 has been synthesized and characterized by element analysis, IR, ~1H NMR etc. Its crystal structure has been determined by X-ray diffraction analysis with R=0.060. The crystal is triclinic, space group P_1 with a=0.8933(3) nm, b=1.1830(6) nm, c=1.3199(3) nm, α=65.64(3)°, β=84.55(3)°, γ=72.03(4)°, z=2, D_x=1.584 g cm~(-1) The C≡C and Co-Co form a tetrahedron with appoximate C_(2V) symmetry. The Co-Co bond is metl singal bond. The hybrid state of carbon atoms in the acetylene is between sp and sp~2.     

苯并-15-冠-5四溴合铟(Ⅲ)酸钾配合物的晶体结构

苯并-15-冠-5四溴合铟(III)酸钾,KInBr_4(C_(14)H_(20)O_5)_2,晶体属单斜晶系,空间群为C_(2h)~5-P2_1/n,晶胞参数α=14.402(3),b=15.082(3),c=17.262(5)A,β=93.42(2)°,Z=4.非氢原子的位置由Patterson函数及Fourier合成法找出,经全矩阵最小二乘法修正R=0.057.结构分析表明K~+和两个苯并-15-冠-5(B-15-C-5)分子直接配位,对阴离子为InBr_4~-,具有四面体构型.InBr_4~-与配阳离子K(B-15-C-5)_2~+依靠静电引力结合为离子对.由此说明,In(III)在过量KBr存在下可以被B-15-C-5定量地萃取至有机相中.     

过渡金属配合物为模板合成两个新的硫代锡酸盐(英)

利用溶剂热方法在温和的条件下合成了二个新的硫代锡酸盐[Mn(en)₃]₂Sn₂S₆·2H₂O(en=H₂NC₂H₄NH₂) (1)和[Mn(dien)₂]₂Sn₂S₆ (dien=H₂NC₂H₄NHC₂H₄NH₂) (2)，通过X-射线衍射分析表征其晶体结构。化合物1的晶体学参数：C₁₂H₄₈Mn₂N₁₂S₆Sn₂·2H₂O，M_r=936.28，单斜晶系，P2₁/c，a=1.012 9(3)，b=1.574 6(4)，c=1.152 4(3) nm，β=102.36(1)°，V=1.795 5(8) nm³，Z=2，D_c=1.732 g·cm^-3，μ(MoKα)=2.442 mm^-1，F(000)=940，R=0.063 3，wR=0.081 4；化合物2的晶体学参数：C₁₆H₅₂Mn₂N₁₂S₆Sn₂，M_r=952.32，单斜晶系，P2₁/c，a=1.248 12(3)，b=0.937 60(4), c=1.776 17 (7) nm，β=121.752(2)°，V=1.767 5(1) nm³，Z=2，D_c=1.789 g·cm^-3，μ(MoKα)=2.479 mm^-1，F(000)=956，R=0.057 9，wR=0.137 4。在两个化合物中存在的[Sn₂S₆]^4-阴离子均由共边的两个SnS₄四面体构成。在1中，锰离子螯合3个乙二胺做为阳离子模板，而在2中锰离子螯合2个二乙烯三胺做为阳离子模板。金属配合物作为模板对阴离子[Sn₂S₆]^4-在晶体结构中的排列产生重要的影响。