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 {(PPh3)2ClRu(μ-Cl)-Ru(PPh3)B10H7[OCH(CH3)2]3}·0.4(H2O)

The title compound has been synthesized by the reaction of [RuCl2(PPh3)3] and closo-[B10H10]2- in (CH3)2CHOH solution. Crystals suitable for a single crystal X-ray diffraction analysis were obtained from n-pentane diffused to CH2Cl2 solution. The crystal {(PPh3)2ClRu(μ-Cl)Ru(PPh3)B10H7[OCH(CH3)2]3}·0.4(H2O) is monoclinic , space group P21/n , Mr=1359.47, with a=19.434(4), b =14.340(4), c=25.865(9)(A), β= 95.48(3)°, V=7175(4)(A)3, Dc=1.258 g/cm3, Z=4, λ(MoKα)=0.71073(A),μ=6.03 cm-1, F(000)=2784, R=0.0631, wR2= 0.1425, S=1.001. The title compound is a bimetallic species in which the second ruthenium center is bound to the cluster {(PPh3)RuB10H7[OCH(CH3)2]3} via an Ru-Cl-Ru and two Ru-H-B-Ru bridges. The third isoproxy group replaces a hydrogen atom on B(10) of the cage, which indicates the activity of the cage.     

[(O)MoCu_3(μ_3-S)_3(μ_3-Cl)(PPh_3)_3]·2THF的合成及其晶体结构

固体化合物(NH_4)_6Mo_7O_(24)·4H_2O和(PPh_3)_2CuCl与饱和液体NH_4HS反应获得桔红针状标题晶体。晶体空间群为P2_1/c,晶胞参数a=11.742(2),b=28.186(7),c=19.304(3),β=100.57(2)°,V=6280.4(?)~3,D_c=1.46g/cm~3,Z=4,F(000)=2816。在3≤2θ≤45°范围内收集到8414个独立衍射强度数据,其中3856个I≥1.5σ(I)强度数据参加结构计算。标题化合物分子是以{MoCu_3S_3Cl}类立方烷型簇为核心的分子,Mo—Cu的平均距离为2.716。     

Synthesis and Crystal Structure of ｛( P Ph_3)_2 Cl Ru( μ- Cl) Ru( P Ph_3) B_(10)H_7〔 O C H( C H_3)_2〕_3｝·0 .4( H_2O)

１　ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅｆｉｒｓｔｐｏｌｙｈｅｄｒａｌｒｕｔｈｅｎａｂｏｒａｎｅｉｓｓｔｒｕｃｔｕｒａｌｌｙｔｙｐｉｆｉｅｄｂｙｔｈｅｃｏｍｐｏｕｎｄ〔（ＰＰｈ３）２ＲｕＢ１０Ｈ８（ＯＥｔ）２〕ｉｎ１９８４〔１〕,ｗｈｉｃｈｉｓｏｂｔａｉｎｅｄｉｎ４０％ｙｉｅｌｄｂｙｔｈｅｒｅａｃｔｉｏｎｏｆｔｈｅｃｌｏｓｏｄｅｃａｂｏｒａｎｅａｎｉｏｎＢ１０Ｈ１０２－ｗｉｔｈ〔ＲｕＣｌ２（ＰＰｈ３）３〕ｉｎｅｔｈａｎｏｌ／ｃｈｌｏｒｏｆｏｒｍｓｏｌｕｔｉｏｎ．Ｒｅｓｅａｒｃｈｅｒｓｈａｖｅｓｙ…     

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, structures and reactions of lithium complexes of [(o-RCHC6H4)PPh2=NSiMe3]-(R = H, SiMe3) ligands

N-Trimethylsilyl o-methylphenyldiphenylphosphinimine, (o-MeC6H4)PPh2=NSiMe3 (1), was prepared by reaction of Ph2P(Br)=NSiMe3 with o-methylphenyllithium. Treatment of 1 with LiBun and then Me3SiCl afforded (o-Me3SiCH2C6H4)PPh2=NSiMe3 (2). Lithiations of both 1 and 2 with LiBu(n) in the presence of tmen gave crystalline lithium complexes [Li{CH(R)C6H4(PPh(2=NSiMe3)-.tmen](3, R = H; 4, R = SiMe3). From the mother liquor of 4, traces of the tmen-bridged complex [Li{CH(SiMe3)C6H4(PPh2=NSiMe3)-2}]2(mu-tmen) (5) were obtained. Reaction of 2 with LiBun in Et2O yielded complex [Li{CH(SiMe3)C6H4(PPh2=NSiMe3)-2}.OEt2] (6). Reaction of lithiated with Me2SiCl2 in a 2:1 molar ratio afforded dimethylsilyl-bridged compound Me2Si[CH2C6H4(PPh2=NSiMe3)-2]2 (7). Lithiation of 7 with two equivalents of LiBun in Et2O yielded [Li2{(CHC6H4(PPh2=NSiMe3)-2)2SiMe2}.0.5OEt2](8.0.5OEt2). Treatment of 4 with PhCN formed a lithium enamide complex [Li{N(SiMe3)C(Ph)CHC6H4(PPh2=NSiMe3)-2}.tmen] (9). Reaction of two equivalents of 5 with 1,4-dicyanobenzene gave a dilithium complex [{Li(OEt2)2}2(1,4-{C(N(SiMe3)CHC6H4(PPh2=NSiMe3)-2}2C6H4)] (10). All compounds were characterised by NMR spectroscopy and elemental analyses. The structures of compounds 2, 3, 5, 6 and 9 have been determined by single crystal X-ray diffraction techniques.     

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 Structural Characterizations of the Heteronuclear Cubane－like Cluster W_2Ag_2S_4（tdt）_2（PPh_3）_2·CH_2Cl_2

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒａｌＣｈａｒａｃｔｅｒｉｚａｔｉｏｎｓｏｆｔｈｅＨｅｔｅｒｏｎｕｃｌｅａｒＣｕｂａｎｅ－ｌｉｋｅＣｌｕｓｔｅｒＷ_２Ａｇ_２Ｓ_４（ｔｄｔ）_２（ＰＰｈ_３）_２·ＣＨ_２Ｃｌ_２ＹＵＲｏｎｇ－Ｍｉｎ；ＬＵＳｈａｏ－Ｆ...     

Synthesis and Crystal Structure of Dinuclear Copper Cluster Compound ［Cu（dtp）PPh_3］_2

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＤｉｎｕｃｌｅａｒＣｏｐｐｅｒＣｌｕｓｔｅｒＣｏｍｐｏｕｎｄ［Ｃｕ（ｄｔｐ）ＰＰｈ_３］_２ＣｈｅｎＱｉｕ－Ｈｕａ；ＬｕＳｈａｏ－Ｆａｎｇ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ（ＳｔａｔｅｋｅｙＬａｂ...     

Synthesis and Crystallographic Characterization of Complex [(CH_3)_3NCH_2CH_2N(CH_3)_3][HgI_4]·H_2O Containing Novel Cation

1 INTRODUCTION The crystal structures of several tetrahalogeno-mercurates (II) have been reported with a wide va-riety of stereochemical arrangements[1, . These stu- 2]dies have shown that the Hg atom…     

31~P NMR Studies on Quasi-Aromaticity of Mo_3S_3 Core and Structure of {Mo_3(μ_3-S)_3[μ-SOP(OEt)_2][S_2P(OEt)_2]_3(CH3CN)}*CH_3CN

1INTRoDUCTIoNDuringthisdecade,extensivestudieshavebeendoneontheclustercompoundswithMosS`coret1}.Wehavedevelopedanewmethodtosynthesizeaseriesof[Mo,o.S'-.J' ,n=O,l,2,3,inaqueoussolution(2).BythereactionofaqueousclusterionswithHdtp,weobtainedtheircorrespondingcompoundswhichwerefirst-lysynthesizedbythespontaneousself-assemblymethod.Theseaqueousclusterionsandtheirderivativescoordinatedbyorganicligands,bothinaqueousphaseandnon-aqueoussolution,demonstratedreactiveactivitiestowardsmanytransitio…     

CRYSTAL STRUCTURES OF [Bu4N]2[M2Ag3（ μ3—S）2（μ—S）4S2Et2dtc]（M=W,Mo）

<正> The title compounds were prepared from the reation of (NH4)2MS4 (M=W,Mo),AgNO3,NadtcEt2 and Et4NBr in CH3CN-H2O solution. The isomorphous compounds [Bu4N]2[W2Ag3S8Et2du] ( I ) and [Bu4N]2[Mo2Ag3S8Et2dtc] (Ⅱ) crystallize in triclinic space qroup Pi with the following crystal parameters:α=13. 043(4),b = 21. 640(6),c=10. 757(6)A ,α=95. 09(5),β = 91. 90(4),γ = 98. 57(3)°,Z = 2,V = 2987A3,Dc=1. 76g/cm3 for I 5;a= 12. 989(2) ,b=21. 574 (9) ,c= 10. 7/1(1) A .α= 95. 06(7), β=91. 61(4), γ=98. 52(2)°, Z = 2,V = 2961 A3.Dc= 1. 58g/cm3 for Ⅱ . The final R and Rw values are 0. 061 and 0. 072 for Ⅰ ,and 0. 062 and 0. 076 for Ⅱ The M2Ag3 (M = W, Mo) unit in anion M2Ag3S8Et2dtc forms a five-membered ring.     

Synthesis and Crystal Structure of [(PPh3)(CH3COS)2NiB10H10]·0.4(C5H12)

The title compound [(PPh3)(CH3COS)2NiB10H10]·0.4(C5H12) has been synthesized by the reaction of [NiCl2(PPh3)2], closo-[B10H10]2- and CH3COSH in CH2Cl2 solution. It was recrystallized from n-pentane/CH2Cl2 solution and its structure was determined by X-ray diffraction analysis. The crystal is triclinic, space group P1, Mr=618.23, with a=10.049(1), b=12.638(2), c=14.077(2) , α=110.13(1), β=87.65(1), γ=96.01(1)°, V=1669.3(4)(A)3, Dc=1.230 g/cm3, Z=2, λ(MoKα)=0.71073(A), μ=7.76 cm-1, F(000)=642. The final refinement is converged with R=0.042 (5986 observed reflections with I≥2σ(I)), wR2 =0.151. The cluster is a nido eleven-vertex {NiB10} cage with the Ni atom in the open NiB4 face. Cyclizations resulting in two five-membered rings, Ni(7)-S(1)-C(1)-O(1)-B(2) and Ni(7)-S(2)-C(2)-O(2)-B(3), have occurred.     

HRh[(C_6H_5)_2PCH_2CH_2P(C_6H_5)_2]_2的晶体和分子结构

HRh[(C_6H_5)_2PCH_2CH_2P(C_6H_5)_2]_2(分子量900.8)晶体属单斜晶系,空间群P21/n,晶胞参数a=21.319(2),b=20.844(2),c=10.130(3),β=91.255(2)°,V=4500.4,Z=4,D_c=1.15g·cm~(-3),F(000)=1864,μ(CuKα)=44.97cm~(-1)。共收集独立衍射点数7636个,其I>3σ(1)的衍射点数6810个。最终的R=0.045,R_w=0.050(W=1/σ~2(F)+(F)+g|F|~2)。其分子结构呈畸变的三角双锥构型。     

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…     

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 {4-[2-（9- Hexyl-9H-carbazol-3-yl）vinyl]phenyl} Dimethylamine

The title compound {4-[2-(9-hexyl-9H-carbazol-3-yl)vinyl]phenyl} dimethylamine has been synthesized by the well known Wittig reaction, and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 47.87(2), b = 10.222(4), c = 9.612(4) , β = 92.401(9)o, V = 4699(3) 3, Z = 8, C28H32N2, Mr = 396.56, Dc = 1.121 g/cm3, F(000) = 1712 and μ(MoKa) = 0.065 mm-1. The final R and wR are 0.0793 and 0.1983, respectively for 3524 observed reflections with I > 2σ(I). In the title compound, the bond lengths are normal, and the crystal is stabilized by Van der Waals’ forces.     

盖帽三核钴羰基簇合物(μ_3-CH_3C)Co_3(CO)_7(μ-PPh_2CH_2PPh_2)和(μ_3-CH_3C)Co_3(CO)_9的质谱研究

本文从结构化学角度,阐述了标题化合物的EI质谱断裂行为。这些化合物的分子离子基本上按分步断裂分别失去羰基,直至获得[CH_3CCo_3(PPh_2CH_2PPh_2)]~+和[CH_3CCo_3]~+。然后,这些残基和含膦配体继续断裂,失去Ph、PhP、Ph_3P、C_7H_7、C_6H_6、C_2H_2、H_2和Co等,生成各种相应的三核、二核和单核钴的碎片离子。     

Synthesis and Crystal Structure of 2-Ethoxy-3-n-butyl-benzofuro[2,3-d]pyrimidin-4（3H）-one

The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4（3H）-one （C16H18N2O3, Mr = 286.32） has been prepared and determined by singlecrystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 13.7167（14）, b = 13.113（1）, c = 8.378（1） A, β = 98.992（2）^o, V = 1488.4（3） A^3, Z = 4, Dc = 1.278, F（000） = 608, μ = 0.089 mm^-1, MoKa radiation （2 = 0.71073）, R = 0.0498, wR = 0.1238 for 2336 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that all ring atoms in the benzo[4, 5]furo [2,3-d] pyrimi- dinone moieties are almost coplanar.     

A Novel 3D Extended Network Cobalt Paradodecatungstate:Synthesis,Characterization and Crystal Structure of [Co(H_2O)_5]_2[Co(H_2O)_4]_3[H_2W_(12)O_(42)]·11H_2O

1 INTRODUCTION Polyoxometalates are the unique metal-oxygen clusters composed of transition metals in groups V and VI (Mo, W, V, Nb, Ta) in a high oxidation state showing a large structural varieties as well as inte- resting physical and chemical properties in diverse fields including catalysis, analytical chemistry, nanotechnology, chemical sensing, biochemical and geochemical processes, medicine and materials science[1～5]. Recently, there has been increasing interest in the synthesis…