Synthesis and Crystal Structure of {(PPh_3)_2CIRuCIRu(PPh_3) B_(10)H_8[OCH(CH_3)_2)]_2}

1INTRODUCTIONAlthoughseveralhundredpolyhedralmetallaboraneshavebeencharacterized,theincidenceofruthenaboranesisparticularlysurprising.(hThefirstpolyhedralruthenaboraneisstructurallytypifiedbythecompound[(PPh,)2RuB,,HS(OEt),j,whichisobtainedin40%yieldsfromthereactionbetweentRuCI,(PPh,),jandcloso-tB,,H,,j'--inCHCI,/EtOH.tZiWithCH,COOH/THFt'iandC,H,COOH/CH,CI,">insteadofCHCI,/EtOH,twocompoundsF{(PPh,)2Ru}~(p-MeCO,)3--(pH)z-{RuB,,H,}jand[(PPh,)2(PhCOO)RuB,,HSCljhav…     

Synthesis and Crystal Structure of Two iso-closo 11-Vertex p-Bromobenzoate Ruthenoborane Clusters： [（PPh3）（p-BrC6H4CO2）2RUB10H8 and [（PPh3）2Ru（p-BrC6H4CO2）-（PPh3）RuB10H9]

The title clusters [（PPh3）（p-BrC6H4CO2）2RuB10H8] （1） and [（PPh3）2Ru（PPh3）（p-BrC6H4CO2）RuB10H9] （2） have been prepared and characterized by elemental analysis, FT-IR, ^1H, ^13C NMR spectra and single-crystal X-ray diffraction analysis. The clusters crystallize in monoclinic system, space group C2/c, with a =2.569（4） nm, b= 1.546（2） nm, c= 1.927（3） nm ,8=95.11（2）°, Z=8, V=7.622（21） nm^3, Dc=1.533 Mg/m^3, F（000）=3472, S= 1.009, R= 0.0418, wR=0.0775 and triclinic system, space group P-l, with a=1.3142（3） nm, b= 1.3761（3） nm, c=1.8503（4） nm, a =90.445（4）°,β=105.950（4）°, γ108.980（4）°, Z=2, V=3.0251（12） nm^3, Dc = 1.434 Mg/m^3, F（000）= 1316, S=1.007, R=0.0464, wR=0.1175, respectively for 1 and 2. In the structures, both of the dusters are based on a closo-type C2v 1： 2 ： 4 ： 2 ： 2 RUB10 stack with the metal occupying the unique six-connected apical position. In cluster 1, the metal center has three exo-polyhedral ligands： one triphenylphosphine and two dative oxygen atoms of p-bromobenzoates. The other oxygen atoms of two p-bromobenzoate are additionally bonded to B（2） and B（3） atoms respectively, resulting in two exo-cyclic five-membered Ru-O-C-O-B rings and engendering a symmetrical conformation. The cluster 2 is a bimetallic species in which the second ruthenium is bound to the {RUB10} center via one Ru-Ru bond and two {RuHμB} bridges resulting in one closo distorted exo-polyhedral Ru（1）-Ru（2）-B（3）-B（6） tetrahedron.     

Synthesis and Crystal Structure of Nido 11-Vertex Platinaborane [ （PPh3）2PtB10H10-9,10-（H0.7Cl0.3）2]

The reaction of PtCl2（PPh3）2 with closo-[B10H10]^2- in t-BuOH under reflux （70 h） unexpectedly afforded the nido 11-vertex platinaborane [（PPh3）2PtB 10H10-9,10-（H0.7Cl0.3）2] 1, which was characterized by single-crystal X-ray diffraction study. Crystallographic data for 1： C36H41.40B10Cl0.60P2Pt, Mr = 860.49, triclinic system, space group P1, a = 11.255（2）, b = 11.623（2）, c = 17.148（3）A, α = 81.012（2）, β = 88.115（3）, γ=64.322（2）°, V= 1995.4（7）A^3, Z= 2, Dc = 1.432 g/cm^3, μ（MoKα） = 3.662 mm^-1, F（000） = 851, R = 0.0358 and wR = 0.0951. Compound 1 has a nido 11-vertex {PtB10} polyhedral skeleton with the Pt atom lying in the open PtB4 face and further ligating to two PPh3 ligands. 1 is partially chlorinated at positions B（9） and B（10）, and for each chlorine atom an occupancy factor of 0.3 is given by crystallography.     

[(C_5H_4CH_3)_2HoN_4CPh]_2·[(C_5H_4CH_3)(C_5H_5)HoN_4CPh]_2的合成和晶体结构

（C5H4CH3）3Ho和（C5H4CH3）2Ho（C5H5）与5-苯基四唑（HN4CPh）在THF中反应，得到复合产物[（C5H4CH3）2HoN4CPh]2·[（C5H4CH3）（C5H5）HoN4CPh]2，该晶体属三斜晶系，P1空间群，晶胞参数为a=9．386（3），b=13．071（3），c=16.571（2）A，a=86．90（1），β=74．61（2），γ=77.30（2）°，V=1912．2（8）A3，Z=1，Dc=1.602g／cm3，Mr=922．61，μ=41．92cm－1，F（000）=896，最终偏离因子R=0．041，Rw=0．056．晶体数据显示，在同一个晶胞里有两个组成不同的分子，每一个分子都是具有对称中心的四唑基桥二聚体结构，其桥环单元-HoN3HoN3-是平面型的。每个钬原子分别被两个茂基和3个四唑基氮原子配位，形成1个边桥变形四面体构型。     

Synthesis and Crystal Structure of[(CH_3)_4N]_4,H_2[ZnW_(11)SnO_(39)]·9H_2O

1INTRODUCTIONThepseudoliquidcharacterofheteropolycompoundsascatalystisdeterminedbytheircrystallographicproperties"3.Thedeterminationofthecrystalstructureofhet-eropolycompoundhasbecomeanimportantmethodtocharacterizeandidentifythesecompounds,atthesametimeitalsoprovidesinterestinginformationtoenrichhet-eropolyacidandcatalyticchemistry.Inthispaper,wereportthesynthesisandcrys-talstructureof[(CH,).Nj.H,[ZnW,,SnO,,j.gH,O.2EXPERIMENTAL2.1SynthesisNa,WO..ZH,O(18.2g,55mmol)wasdissolvedin…     

{Cu[H_2NC(CH_2OH)_3]_2}{Pic}_2·H_2O的合成与晶体结构

三羟甲基氨基甲烷与苦味酸(Pic)铜在乙醇水混合液中反应,制得少见的不对称氢键连接的超分子化合物{Cu[H2NC(CH2OH)3]2}{Pic}2?H2O。晶体属三斜晶系,空间群为P ,晶胞参数为a = 6.894(1),b = 8.219(1),c = 13.543(3) ? ?= 79.290(1),?= 8 3.36(2), ?= 84.590(1)埃轿狢20H30CuN8O22,V = 746.9(2) 3,Z = 1,Dc = 1.774 g/cm3,F(000) = 411,?= 0.844 mm-1,R = 0.0334,Rw = 0.0863。在配合物的结构单元中, Cu2+位于对称中心,分别与2个四齿配体(三羟甲基氨基甲烷)中的2个OH,1个NH2,三齿配位,呈笼状螯合。而另一个OH,因配体和中心离子构型的限制,不参与配位。     

双（二苯基膦）丁烷的双核银配合物晶体结构

报导了双（二苯基膦）丁烷的双核银配合物－［Ａｇ（Ｐｈ_２ＰＣＨ_２ＣＨ_２ＣＨ_２ＣＨ_２ＰＰｈ_２）－（ＮＯ_３）］_２的合成及晶体结构分析。晶体属于单斜晶系，空间群为Ｐ２_１／ｎ，晶胞参数为：ａ＝１２．８２１（３），ｂ＝１１．２４４（９），ｃ＝１９．３８６（９），β＝１０５．９４（３）°，Ｖ＝２６８７．２~３，Ｚ＝２，Ｄ_ｃ＝１．４７４ｇ／ｃｍ~３，Ｍ_ｒ＝１１９２．７，Ｆ（０００）＝１２１６，μ＝８．８７３ｃｍ~（－１）。晶体结构由直接法和Ｆｏｕｒｉｅｒ合成解出，使用对角块矩阵和全矩阵最小二乘法对原子参数进行修正，最后偏离因子Ｒ＝０．０５６，Ｒ_ｗ＝０．０６８，其中２６３４个Ｉ＞３σ（Ⅰ）的可观察点参加了结构修正，单晶结构分析结果表明，在该配合物中，配体双（二苯基膦）丁烷（ｄｐｐｂ）中的磷原子直接与银离子配位，硝酸根也以双齿配位形式存在，中心银离子的配位采用畸变的四面体构型，整个分子是一个二聚物。     

H_(10)[NiMo~Ⅴ_(12)O_(40){Ni(H_2O)_3}_4]的水热合成和晶体结构

在水热的条件下合成了1个标题的Mo-Ni-O异核簇合物,化学式为H34Ni5Mo12O52 (Mr = 2311.10),用单晶X射线衍射方法测定了它的结构,该晶体属四方晶系,I41/amd空间群,晶胞参数为a = 15.319(2),c = 30.645(3) ,V = 7191.2(16) 3,Z = 4,Dc = 2.135 g/cm3,μ= 3.369 mm-1, F(000) = 4376, 1036个可观察衍射点(I > 2s(I)),最终结构偏离因子R = 0.0560,wR = 0.1632,S = 1.002。该化合物簇阴离子笼中心是Ni2+,由12个MoO6八面体和4个NiO6八面体通过共角和共边构成。     

Synthesis and Crystal Structure of［（n－Bu）_4N］_2［Mo_4O_（10）（OC_（10）H_6O）_2（OCH_3）_2］

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［（ｎ－Ｂｕ）_４Ｎ］_２［Ｍｏ_４Ｏ_（１０）（ＯＣ_（１０）Ｈ_６Ｏ）_２（ＯＣＨ_３）_２］￥ＬｕＸｉａｏ－Ｍｉｎｇ；ＺｈｕＨｕｉ－Ｊｕ；ＹａｎｇＮｉｎｇ；ＬｉｕＳｈｕｎ－Ｃｈｅｎｇ；ＪｉｎＸ?..     

Synthesis and Crystal Structure of the Organotin Complex [(o-Cl-PhCH_2)_3SnOCOC_(10)H_8N]·0.5C_6H_6

1 INTRODUCTION There is increasing interest in the study of orga-notin carboxylic ester compounds due to their insec-ticidal, fungicidal and antibiotic activities[1, as well 2]as structure diversity. In recent years many organo-tin carboxylic ester compounds with good biologi-cal activity have been synthesized[3, . Previous stu- 4]dies show that the coordination geometry of centralatom Sn …     

Preparation and Crystal Structure of a Charge-transfer Complex between an Organic Substrate and Molybdosilicic Acid [(CH_3)_2NH(CH_2)C_6H_5]_4SiMo_(12)O_(40)·2CH_3CN·H_2O

1 INTRODUCTION Photochromism of intermolecular complexes based on polyoxometalates has received increasing attention due to their potential applications in ma- terial science[1～3]. However, most studies of photo- chromism have been made in solution[4～7], and those in solid state are relatively less and only a few with photosenstivity properties have been studied crystal- lographically. The title compound has a light yellow color in the darkness and turns greenish when exposed to sunligh…     

一价铜配合物〔Cu（C_8H_4F_3O_2S）（PPh_3）_2〕的合成和晶体

室温下，铜粉和２－噻吩甲酰三氟丙酮、三苯基膦在甲醇和四氢呋喃混合溶剂中反应，生成一价铜的配合物［Ｃｕ（Ｃ_８Ｈ_４Ｆ_３Ｏ_２Ｓ）（ＰＰｈ_３）_２］，测定了该配合物的晶体结构，结果表明，晶体属单斜晶系，Ｐ２_１／ｎ空间群，晶胞参数：ａ＝１０．５８４（１），ｂ＝１６．７３８（１），ｃ＝２２．７２８（９）Ａ；β＝９４．２２（２）°，Ｖ＝４０１５．２Ａ３，Ｍｒ＝７８５．２９，Ｚ＝４，Ｄｃ＝１０２９９ｇ／ｃｍ３，μ＝９．８６ｃｍ－１。晶体结构由直接法解出，使用块对角矩阵和全矩阵最小二乘法对原子参数进行修正，最后偏离因子Ｒ＝０．０４８，Ｒｗ＝０．０５４，其中４３９１个Ｉ＞３σ（Ｉ）的可观察衍射点参加了结构修正，结果表明，Ｃｕ原子由２个Ｏ原子和２个Ｐ原子配位，形成畸变四面体构型。     

主体分子六次甲基四胺与客体分子二氯化六水合钴(Ⅱ)和结晶水包结物的研究

用X射线单晶衍射分析法研究主体分子六次甲基四胺与客体分子二氯化六水合钴（Ⅱ）和结晶水包结物晶体结构。其分子式为［（CH2）6N4］2·［（Co（H2O）6］Cl2·4H2O，Mr＝59038。晶体属三斜晶系，空间群为P1。晶胞参数：3341个衍射点，其中3148个独立衍射点，2754（F0＞6σ（F0））为可观察反射点。在晶胞内，客体分子和结晶水形成氢键：，客体分子与主体分子形成氢键晶胞之间形成氢键晶胞之内和晶胞之间主体分子和客体分子以及结晶水以氢键和范德华力相联系形成稳定的晶格。     

Synthesis and Crystal Structure of a Novel Bimetallic Porphyrin Complex Salt {[MnTPP(CH_3OH)_2]_3Fe(CN)_6}·13H_2O

A novel bimetallic porphyrin complex salt, {[MnTPP(CH3OH)2]3Fe(CN)6}13H2O (TPP = tetraphenylporphyrin), has been synthesized and structurally characterized by X-ray diffraction analysis. The crystal is of trigonal, space group R-3 with a = b = 31.0618(10), c = 11.8366(8) A, Z = 3, V = 9890.3(8) A3, C144H134FeMn3N18O19, Mr = 2641.36, Dc = 1.330 g/cm3, μ(MoΚα) = 0.463 mm-1, F(000) = 4131, R = 0.0525 and wR = 0.1382 for 3045 observed reflections (I > 2σ(I)). The title complex is composed of one [Fe(CN)6]3- anion, three [MnTPP(CH3OH)2]+ cations and thirteen water molecules, which are connected by multiform hydrogen bonds leading to a 3D supramolecular network structure.     

Synthesis and Crystal Structure of a Novel Heptanuclear Ruthenium- and Sodium-containing Polyoxomolybdate [{Na(H_2O)_3}_2{Ru(dmso)_3}_2(MoO_4)_3]·_3H_2O

1 INTRODUCTION Polyoxomolybdates have been of great interest due to their unique structural varieties, associated multitude of properties and applications as catalysis, medicine and material[1, 2]. One of the most impor- tant aspects is the synthesis and investigation of the materials on polyoxomolybdates containing organo- metallic groups[3～5]. Such materials can provide molecular models for heterogeneous catalysis and display cooperative effects or bifunctional catalytic activity[6]. O…     

Synthesis and Crystal Structure of K_3[HO{VO(O_2)_2}_2]·H_2O

1 INTRODUCTION Though the investigation on chemistry of tran- sition metal-peroxy complexes has been extensively carried out, up to now, only four structures of purely inorganic dimeric peroxovanadates have been deter- mined by single-crystal X-ray meth…     

Synthesis and Structureof［（C_2H_5）_4N］［Mo_3（μ_3－O）（μ－Cl）_3（μ－CH_3CH_2COO）_3Cl_3］

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆ［（Ｃ_２Ｈ_５）_４Ｎ］［Ｍｏ_３（μ_３－Ｏ）（μ－Ｃｌ）_３（μ－ＣＨ_３ＣＨ_２ＣＯＯ）_３Ｃｌ_３］ＺｈｕａｎｇＨｏｎｇ－Ｈｕｉ；ＷｕＤｉｎｇ－Ｍｉｎｇ；ＨｕａｎｇＪｉａｎ－Ｑｕａｎ；ＨｕａｎｇＪｉｎ－Ｌ...     

Synthesis and Crystal Structure of [{Cd(hmbdc)(H_2O)_3}·2H_2O]_n

A novel coordination polymer [{Cd(hmbdc)(H2O)3}·2H2O]n (hmbdc = 5-hydroxy- isophthalic acid) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a = 9.599(3), b = 18.699(5), c = 7.557(2) , β = 108.198(4)°, V = 1288.6(6) 3, Z = 4, Mr = 382.60, Dc = 1.972 g/cm3, F(000) = 760, μ = 1.740, the final R = 0.0555 and wR = 0.0995 for 1732 observed reflections with I > 2σ(I). The structural analysis shows that the intermolecular hydrogen bonds and π-π interactions result in a three-dimensional supramolecular framework.     

Synthesis and Structural Characterization of a New Polyoxovanadium Borate: (H_3NCH_2CH_2NH_3)_4[(VO)_6(B_(10)O_(22))_2]·(H_3O)_7

1 INTRODUCTION Transition metal oxide clusters and their deriva- tives offer an unmatched variety of structural motifs and wide ranging applications in several areas, such as analytical chemistry, materials science and cataly- sis, nanotechnology, chemical sensing, environmental decontamination, biochemical and geochemical pro- cesses, and medicine[1～3]. Polyoxovanadates or vana- dium oxide clusters constitute an important subclass of polyoxometalates and have been studied exten- sively.…     

Synthesis and Crystal Structure of （Et4N）3[{V（o—C6H4OS）3}2Na]

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ（Ｅｔ_４Ｎ）_３［｛Ｖ（ｏ－Ｃ_６Ｈ_４ＯＳ）_３｝_２Ｎａ］￥ＷｅｎＴｉｎｇ－Ｂｉｎ；ＸｕＹｏｎｇ－Ｊｉｎ；ＳｈｉＪｉ－Ｃｈｅｎｇ；ＤｅｎｇＹｕ－Ｈｅｎｇ；ＣｈｅｎＣｈａｎｇ－Ｎｅｎｇ；Ｌｉｕ...