CRYSTAL STRUCTURE OF W_4(μ_(3-)S)_4[S_2P(OEt)_2]_6

<正> W4S4 [S2P (OEt)2]6, Mr= 1974. 94, triclinic, P1, a = 14. 063 (5) , b = 16. 289(4), c= 13. 377(3) A ,α=92. 06 (2), β=95. 24(3), γ= 73. 06(2)°, V= 2919(3)A3,Z=2,DC=2. 18g/cm3, Moka radiation,λ =0. 71069A ,μ = 90. 64cm-1, F(000) = 1764,R=0. 053 and Rw = 0. 069 for 5422 reflections with I≥3σ(I).The title compound is comprised of a cubane-like cluster core [W4S4] in which every W atom is coordinated by six S atoms to form a distorted octahedron.     

SYNTHESIS AND STRUCTURE OF CU8S[S2P（OC2H5）2]6

<正> Cu8C24H60O12P6S13,Mt= 1651. 73,trigonal,R3,a=b = c= 12. 667(4) A,α= β=γ=111. 42(1)°.V=1441(2)A3,Z=1,Dc=1. 903g·cm-3,λ(MoKa) = 0. 71073 A ,μ(MoKa) = 35. 671cm-1, F ( 000 ) = 830, 293K. Final R = 0. 066,Rw= 0. 077 for 850 unique intensity data (I≥3σ(I)). Each unit cell of the crystal comprises of a neutral molecule of formula Cu8S(dtp)6[dtp=S2P(OEt)2],wherein the eight copper atoms are arranged at the corners of regular cube,with each dtp ligand μ4-bridged to each face of the cube and a μ8-S in the center bonded to all the eight copper atoms. Each copper atom is coordinated by four sulfur atoms in a tetrahedral configuration. The bond lengths of Cu-(μ8-S) are in the range of 2. 627(2)-2. 543(2) A ,those of Cu-S(dtp)in the range of 2. 251-2. 280A.The adjacent Cu-Cu bond lengths (2. 950(5)-3. 070(2) A) show a weak interaction between the copper atoms     

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.     

OXIDATION DECARBONYLATION OF NH_4[Mo(CO)_5I]: SYNTHE-SES AND CRYSTAL STRUCTURES OF CMo(S_2CNC_4H_8)_4]I_3 · C_7H_8 and Mo_2S_2O_2(S_2CNC4H_8)_2

<正> Both of the title complexes were produced by oxidative decarbony-lation of NH4 CMO (CO)5I]. The complexes CMo(S2CNC4H8)4]I3 ?C7H8(1) and Mo2S2O2 (S2CNC4H8)2(2) both crystallize in triclinic, space group P1 with cell dimensions for (1) : a=13. 554(4), b=13. 620(4), c= 13. 058 (4) A , α=95. 58 (3), β=105. 38(2), γ=115. 49(2)°,V = 2035(1) A3, Z=2, Dc=1. 89 g. cm-3, final R=0. 054 and Rw = 0. 062 for 2926 observed reflections; and for (2): a = 8.730(2), b=16.592(6), c = 6. 688(2)A, α=97. 67(3), β=98. 10(2), γ=80. 26(2)% V = 939. 2(5) A3, Z = 2, Dc = 2. 05 g. cm-3, final R = 0. 038 and Rw = 0. 046 for 2248 observed reflections. The Mo(V) atom is bonded to eight S atoms in distorted dodecahedron for (1). The Mo atoms in compound (2) are bridged by two S atoms and each Mo atom is coordinated by two S atoms from S2CNC4H8 and one O atom to form distorted tetragonal pyramid.     

CRYSTAL STRUCTURE OF A SILVER COMPLEX Ag（PPh3）2（S2P—（OCH3）2）

<正> The crystal structure of the title silver complex has been determined by the single crystal X-ray diffraction method.The white plate crystal is tri-clinic.space group P1 with a=12.289(1),b=13.330(2),c=14.846(1)A.α=59.78(1),β=70.33(1),γ=64.01(1)°,V=1867.9A3,Z=2,Dc=1.404 g/ cm3,Mr=789.6,F(000)=808,MoKa radiation,μ(MoKa)=7.891 cm-1,final R=0.049 and Rw=0.051 for 5753 observed reflections.The silver(I)is surrounded by two P and two S atoms in a distorted tetrahedral coordination.     

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.     

STRUCTURE OF {Mo4S4（μ—OAc）2[S2P（OC2H5）2]4H}

<正> {Mo4S4(μ-OAc)2(dtp)4H}3,(dtp=S2P(OEt)2),Mr=1371.60,Or-thorhombic, space group Pcab, a = 18. 90 (2) ,b = 21. 678 (4 ) , c = 24. 491 (4 ) A , V = 10031(7)A3,Z=8,Dc=1.818g/cm-3,F(000)=5464,λ(MoKa)=0.71073A,finalR= 0. 069 for 3738 independent reflections. This is a successful example of the formation of [Mo4S4]5+ from[3+1] reaction mode. The results of the structure determination indicate that the configuration of the title compound exhibits a tetranuclear cubane-type core [Mo4S4]5+ with six Mo - Mo distances in the range 2. 685~2. 969A and is very similar to that of the previously characterized compound {Mo4S4(μ-OAc)2(dtp)4}2, [Mo4S4]6+, which was obtained directly by the reaction of MoCl3·3H2O with dtp. Some notable differences, however, can be found when six Mo - Mo bond distances and bonding parameters of the four terminal bidentate ligands (dtp) are compared between these two compounds , That can be attributed to the difference in the oxidation state of these two clusters .     

STRUCTURAL CHEMISTRY OF EIGHT-COORDINATE COMPLEXES OP MNTHANOID WITH BIDBNTATE LIGANDS IV.CRYSTAL STRUCTURES OF [C_4H_8OH] [Eu(S_2CNC_4H_8)_4]·xC_4H_8O(x=2,0)

<正> Compound [C4H3OH][Eu(S2CNC4H3)4].2C4H8O(I), Mr=953,80,monoclinic, P21/n,a = 11,332(3), b= 22,837(5), c= 15.671(2)A,β= 94.93(1)°, V= 4040.2 A3,Z= 4,Dc = 1.567 g/cm3. [C4H8OH][Bu(S2CNC4H8)4] (2),Mr=809.72, monoclinic,P 21/c,a= 12.184(2), b= 15.181(3), c= 18.334(3)A,β=98.57(1)°,V=3353,3 A3,Z = 4, Dc= 1.605 g/cm3. The Eu atom in the anions of 1 and 2 is coordinated by eight S atoms frow four S2CNC4H8 chelate groups in the form of a dodecahedron with approximate D2d symmetry.     

CRYSTAL STRUCTURE OF RhCl(dppm)_2·H_2O

<正> C50H46OP4ClRh, RhCl(dppm)2 · H2O, Mr = 922. 2, monoclinic, P21/2, a=10. 532(3), b=22.574(8), c=18. 641(8) A, β=93. 41(3)°, V = 4424 (3) A3, Z = 4, Dc=1. 386 g. cm-3, λ(MoKα) = 0. 71073A , F(000) = 1904. The structure was determined by direct methods and difference Fourier syntheses and refined by full-matrix least-squares to final R = 0. 037 and Rw = 0. 036 for 3432 (F> 6. 0σ(F) ) observed reflections. The structure of the title compound contains RhCl-(dppm)2 and non-coordinated H2O molecules. The rhodium atom is coordinated by one chlorine atom and four phosphorus atoms of two DPPM ligands forming a tetragonal pyramidal configuration.     

SYNTHESES OF TUNGSTEN COMPLEXES WITH o-MERCAP-TOPHENOL.CRYSTAL STRUCTURE OF (Ph_4P)[WO(OMe)(mp)_2]

<正> Reaction of WCl6, mpH2 o-mercaptophenol) and MeONa in the presence of Ph4PBr gave complexes (Ph4P)[W(mp)3] (1) and (Ph4P) CWO(OMe) (mp)2] (2). Crystal data complex (2), C37H31O4PS2W, Mr = 818. 61, monoclinic, space group P2/a, a=26. 555(3), b=9. 634(1), c=13. 523(7) A. β=94. 68 (2)°, V=3448. 1 A3. A=1. 58 g/cm3, Z = 4. λ(MoKα)=0. 71073 A , μ= 36. 2 cm-1, F(000) = 1624, T=296K, final R(Rw) = 0. 068(0. 070) for 3929 observed reflections. The WO4S2 core is arranged in a distorted octahedral geometry.     

Synthesis,Structure and Reaction of a New Bitungsten Compound:(Et_4N)_2W_2S_4 (tdt)_2

1INTRODUCTION'TheclusterscontainingMo--SorW--Shavebeenstudiedextensivelyfortheirimportantapplicationsinmanyfieldsll~43.Alongwith.thedevelopmentofrationaldesignedsynthesissuchasthe"UnitConstruction"utilizingwell-definedactivecom-poundsasbuildingblocks,binuclearsulfidecompoundsusedtodesignnewclustershavebeenpaidattentiontots'6itandalotofcompoundscontainingiM,S.O.--.J' (M=MoorW)coreshavebeenprepared['i.Inthispaper,thefirstexamplpofbitung-stencompoundwithtdtZ--ligands(Et.N),W,S.(tdt),,…     

二核钼化合物Mo_2S_4(S_2P(iprO)_2)_2的合成、反应和结构表征

二核钼化合物Mo2S4（S2P（iprO）2）2（Ⅰ）（ipr=（CH3）2CH）由（NH4）2MoS4和HS2P（iprO）2反应生成，含有1个[Mo2S4]2+簇芯。Mo-Mo键长为2．8201（8）A。除了簇芯的配位外，每个钼原子上都有1个双齿的二异丙基二硫代磷酸酯配体形成钼的四方单锥配位环境。晶体学结构数据：单科晶系，空间群P21／c，晶胞参数a=12．869（2），b=13．90（3），c=16.262（5）A，β＝101.92（3）°，V＝2856（2）A3，Z=4，R=0．044，Rw=0．057。还报道该化合物作为润滑油添加剂的性能测试结果。     

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

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Solvothermal Syntheses of (H_2en)_2Sn_2S_6·en and[(H_2hmda)_3(Hhmda)_2](Sn_2S_6)_2Using SnCl_4 and S_8 as Starting Materials

1 INTRODUCTION Since Bedard et al. reported microporous tin(IV) sulfides synthesized by hydrothermal method in the presence of organic amine in 1989[1, 2], a number of thiostannates have been synthesized using hydro- or solvothermal techniques with organic amines as tem- plates. The structures of the resulting tin(IV) sulfi- des are related to the types of organic amines. Two- dimensional polyanions of the types of [Sn3S7]2- and [Sn4S9]2-, which are denoted as SnS-1 and SnS-3, respe…     

Synthesis and Crystal Structure of Mixed Mo－W Cubane－type Cluster Compound ［Mo_2W_2S_4（μ－OAc）_2（dtp）_3（dtpH）］·CH_2Cl_2

Ｓｙｎｔｈｅｓｉｓ　ａｎｄ　Ｃｒｙｓｔａｌ　Ｓｔｒｕｃｔｕｒｅ　ｏｆ　Ｍｉｘｅｄ　Ｍｏ－Ｗ　Ｃｕｂａｎｅ－ｔｙｐｅ　Ｃｌｕｓｔｅｒ　Ｃｏｍｐｏｕｎｄ　［Ｍｏ_２Ｗ_２Ｓ_４（μ－ＯＡｃ）_２（ｄｔｐ）_３（ｄｔｐＨ）］·ＣＨ_２Ｃｌ_２ＣｈｅｎＱｉｕ－Ｈｕ?..     

APPLICATION OF DITHIO - MOLYBDATE IN THE SYNTHESES OF Mo-Cu CLUSTERS: SYNTHESES AND CRYSTAL STRUC-TURES OF MoOS_3(CuPPh_3)(Cu(PPh_3)_2 AND (Ph_4P)_2[Mo_2Cu_5S_6O_2-(S_2CNEt_2)_3] ·DMF

<正> The reactions of (NH4)2MoO2S2 with Cu(PPh3)3Cl in CH3CN in the air, or with CuCl, Ph4PBr, and NaS2CNEt2 in DMF under anaerobic condition, afforded the cluster complexes MoS3OCu2 (PPh3)3 (Ⅰ) and (Ph4P)2 CMo2Cu5S6O2-(S2CNEt2)33 · DMF (Ⅱ), respectively. Compound (Ⅰ), MoOS3Cu2P3C54H45(Mr = 1121. 0) , crystallizes in the triclinic, space group P1 with cell parameters a = 14. 103 (3), b = 17.906(3), c=11.503(2)(?), α=107. 76(1), β=111.81(2), γ = 74.93 (2)°, F = 2532. 9(?)3 and Z=2, Dc=1. 471 g/cm3, F (000) = 1140, μ(MoKα) = 13. 215 cm-1, final R = 0. 060 (Rw = 0.064) for 5959 independent reflections with I >3σ(Ⅰ). Complex (IⅡ), Mo2O3S12Cu5P2N4C66H77 (Mr = 1930. 67) , crystallizes in monoclinic, space group P2/c with cell parameters a = 25. 325(19) , 6 = 22. 506(9) , c =14. 066(8)(?) , β =100. 96(6)°, V =7871. 16 (?)3, Z = 4, D,= 1. 629 g/cm3, F(000) = 3904, μ(MoKα) = 20. 216 cm-1, R = 0. 097 (Rw = 0. 095) for 5677 reflections with I>3σ(Ⅰ). The core structure of complex (Ⅰ) is defective cub