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1.
SYNTHESIS AND CRYSTAL STRUCTURE OF A TUNGSTEN-COPPER-SULFUR CLUSTER [Et_4N]_2[WCU_3S_4(S_2CNEt_2)_3]
《结构化学》1991,(3)
<正> [Et4N]2 [WCu3S4 (S2CNEt2)3], Mr = 1172. 01, orthorhombic, space group P212121 with a=12. 858(9),b=13. 204(5) ,c=29. 501(9) A ,V=5008. 7 A3, Z = 4, Dc = 1. 55gcm-3, μ(MoKa) = 40. 3cm-1. The final R and Rw are 0. 069 and 0. 075, respectively, for 3072 observed unique reflections. The anion contains a slightly distorted WS42~ tetrahedron coordinated by three CuS2 CNEt2 units,with four metal atoms lying in a plane. 相似文献
2.
《结构化学》1991,(3)
<正> [(Ph3P)3 (Cu3S3MoBr)O] 0. 5CH2C12, Mr = 1308. 00, monoclinic, P21/c,a=11. 831(3),b = 28. 471(8),c=19. 232(5) A ,β= 101. 05(3)°,V = 6358 A3,Z = 4,DC=1.37 g/cm3,F(000) = 2620,μ(MoKa) = 20. 47 cm-1. Final R=0. 085 for 4271 observede reflections. The core [Cu3S3MoBr] has a distorted cubic configuration. Two dichloromethane molecules distribute statistically in a unit cell. 相似文献
3.
《结构化学》1991,(3)
<正> [(C6H5)4P]Cu(S2C6H4)2(Ⅰ),Mr = 683. 39,monoclinic,space group C2/c,a=16. 099 (4),b= 11. 913(3) ,c = 16: 715(9) A ,β=97. 13(4)°, v = 3180. 7 A3,z=4.MoKa radiation,λ= 0. 71069A ,Dc= 1. 427g/cm3,μ= 10. 1cm-1,F(000) = 1400,R=0. 061 and Rw = 0. 068 for 2189 reflections with Ⅰ>3σ(Ⅰ). [(C6H5)4P]Cu (S2C7H6)2(Ⅰ),Mr = 711. 45,monoclinic,space group C2/c,a=16. 501(6),b = 37. 461 (15),c=16. 684(4)A,β=96. 70(4)°, v= 10248. 8(46) A3,z= 12. MoKa radiation, λ= 0. 71069A,Dc=1.383g/cm3,μ=9. 45cm-1,F(000).= 4416,R= 0. 074 and Rw= 0. 078 for 2085 reflections with I>2σ(I)(1). The copper atom in the complexes is surrounded by four sulfur atoms from two dithiolato ligands in an approximate, square-plane. The average Cu-S distances of the copmplexes(Ⅰ) and (Ⅱ) are 2. 179 and 2. 178 A, respectively. 相似文献
4.
Hu Yong-Han Kang Bei-Sheng Chen Xue-TaiState Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure ofMatter Chinese Academy of Sciences Fuzhou Fujian 《结构化学》1993,(5)
<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. 相似文献
5.
《结构化学》1993,(1)
<正> [Cu(C8H4F3O2S)2(C3H7NO)], Mr = 579. 0, monoclinic, P21/c, a = 9. 4851(6), b = 26. 6574(6), c=9.2619(6) A ,β=96.08(3)°, V = 2328.7A3, Z=4, Dc=1. 65gcm-3, μ(MoKa) = 7. 2cm-1, F (000) = 1172, MoKa radiation, final R = 0. 074 and Rw = 0. 068 for 1841 reflections with I≥3σ(Ⅰ). The Cu(Ⅱ) atom is coordinated by five oxygen atoms, one of which from DMF is in the axial position, to form a square pyramidal geometry. That the thenoyl groups in the ligands take the cis-form around the Cu(Ⅱ) atom is explained by the hydrogen bonding effect. 相似文献
6.
《结构化学》1993,(4)
<正> The crystal of cluster [Co6(μ3-S)8(PPh3)6] 2DMF CH3OH(1)was obtained by the reaction of CoCl(PPh3)3 with Na2pdt(H2pdt=1,2-propanedithiol)in methanol,and grown from DMF.The compound 1,C116H112 Co6N2O2P6S8(Mr=2362.11)is monoclinic,space group C2/c with cell parameters a=27.060(10),b=15.127(2),c=27.017(2)A,β=98.52(2)°,V=10937.0A3,Z=4,Dc=1.434 g/cm3,F(000)=4864,MoKa=11.716cm-1,final R=0.071 for 4134 independent reflections with I>3o(I).The cluster[Co6(μ3-S)8(PPh3)6] possesses crystallographic symmetry C2,and the inner Co6 core is a slightly distorted octahedron with all faces symmetrically capped by triply-bridging sulphur atoms. 相似文献
7.
《结构化学》1986,(2)
<正> (Ph2Ppy)2(μ-Cl)2Cu2Cl2 (C34H28Cl4Cu2N2P2): Mr=795.5, triclinic, Pl, a=13.891(2), b= 13.196(3), c= 20.158(4) A, d= 90.28(1)°, β=110.05(2)°, r= 90.13(1)°, Z=4, V= 3471.04A3, Dx=1.53 gcm-3, R=0.066, Rw= 0.076 for 5486 observed unique reflections. The complex was prepared by the reaction of (Ph2Ppy)2NiCl2 with CuC≡CPh in CH2Cl2 solution. 相似文献
8.
《结构化学》1990,(2)
<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. 相似文献
9.
Chen Qiu-Hua Huang Xiao-Ying Lu Shao-Fang Huang Jian-QuanState Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structureof Matter Chinese Academy of Sciences Fuzhou Department of Chemistry Fuzhou University Fuzhou 《结构化学》1993,(5)
<正> A new mixed-metal sulfido incomplete cubane cluster [(MoCuS3) (O) (μ-dtp) (PPh3)3] Cdtp = S2P (OC2H5)2] has been prepared by reaction of (NH4)2MoOS3 with Cu(dtp) (PPh3)2 in dimethylformamide solution. It crystallizes in the triclinic space group P1, a = 13.810(5), b = 19. 753(5), c=11. 719(4) A. α=99. 42(2), β=107. 24(3),γ=88. 05(3)°, V = 3012(2)A3, Dc = l. 51g/cm3and Z = 2. Final R=0. 046, Rw = 0. 056 for 7700 unique intensity data(I≥3σ(I)). The central unit [MoCu3S3]3+ can be described as a distorted incomplete cube with one missing corner. The Mo atom is tetrahedrally coordinated by three μ3-S atoms and one terminal O atom. Two Cu atoms are tetrahedrally coordinated whereas the third Cu atom has a highly distorted trigonal environment. The mean Mo - Cu bond length is 2. 752A. The Cu...Cu distances are in the range of 3. 200(1) -3. 740(1) A which are too long to form bonds. 相似文献
10.
《结构化学》1991,(1)
<正> (Et4N)2[Et2NCSSMoS2)2O3Fe2S2]·DMF(1) ,Mr= 1174. 10,mono-clinic,space group P21/n,a = 9. 608(3),b=17. 962(2),c=15. 312(3) A ,β=95. 03 (3)°,V=2632. 4 A3,Dc= 1. 48 g/cm3 and Z=2. The structure was solved from 2499 reflections with I>3σ(Ⅰ) and refined by full-matrix least squares method to R(Rw) = 0. 073(0. 087). The anion of 1 has linear Mo -Fe -Fe-Mo array. The oxidation states of metal atoms in this cluster are 2Mo(Ⅵ) + 2Fe(Ⅲ). 相似文献
11.
Reaction of [(μ-SCH2)2NPh]Fe2(CO)6 with Ph2PCH2PPh2 in the presence of Me3NO·2H2O gave the title complex [(μ-SCH2)2NPh]Fe2(CO)5(Ph2PCH2PPh2)(1)in 78% yield.The new complex 1 was characterized by elemental analysis,spectroscopy and X-ray crys-tallography.It crystallizes in triclinic,space group P1 with a = 10.832(2),b = 12.003(2),c = 15.579(3),V = 1785.6(6)3,Z = 2,C32H26Fe2NO5PS2,Mr = 819.40,Dc = 1.524 g/cm3,μ(MoKα)= 1.064 mm-1,F(000)= 840,T = 113(2)K,the final R = 0.0543 and wR = 0.1218 for 6203 observed reflections(I > 2σ(I)).The Ph2PCH2PPh2 ligand resides in an axial position of the square-pyramidal coordination sphere of the Fe atom and trans to the benzene ring in order to reduce the steric repulsion between Ph2PCH2PPh2 and the benzene ring. 相似文献
12.
REN Yu-Shu CHEN Yang LI Duan-Xiu GUO Cheng-Xin QIAO Shan-Bao LI Hong-Xi REN Zhi-Gang LANG Jian-Ping 《结构化学》2010,29(6):861-868
The reaction of [Et4N]2WOS3 with three equiv.of CuI and dmpzm in MeCN afforded [WOS3Cu3I(dmpzm)2]·2(MeCN)0.5(1·2(MeCN)0.5) while that of [PPh4]2WS4 with four equiv.of CuI in DMF/MeCN followed by the addition of two equiv.of dmpzm in MeOH gave rise to [WS4Cu4I2(dmpzm)2]·DMF(2·DMF).Both compounds were characterized by elemental analysis,IR,and single-crystal X-ray diffraction analysis.1·2(MeCN)0.5 crystallizes in triclinic,space group P1-with a = 11.4552(5),b = 11.6735(3),c = 16.2278(9) ,α = 99.537(9),β = 101.986(2),γ = 118.464(13)o,V = 1775.5(3)3,Z = 2,μ = 6.080 mm-1,Dc = 1.983 Mg/m3,T = 193(2) K,C24H35Cu3IN9OS3W,Mr = 1063.22,F(000) = 1018,S = 1.060,R = 0.0376 and wR = 0.0870.2·DMF belongs to the orthorhombic system,space group Pmn21 with a = 22.145(4),b = 11.464(2),c = 7.7370(15) ,V = 1964.2(6)3,Z = 2,μ = 6.865 mm-1,Dc = 2.189 Mg/m3,T = 193(2) K,C25H39Cu4I2N9OS4W,Mr = 1301.72,F(000) = 1226,R = 0.0632,wR = 0.1706 and S = 1.130.1·2(MeCN)0.5 consists of one CuI and two [Cu(dmpzm)]+ fragments that are linked by [WOS3]2-species via six Cu-S bonds,forming a nido-like [WS3Cu3] core.2·DMF contains a saddle-shaped [WS4Cu4] core with two iodides coordinated at two Cu centers in a cis position and two dmpzm ligands being chelated at another two Cu centers in a cis position. 相似文献
13.
《结构化学》1993,(4)
<正> C80H76Cl6Cu2P6,Mr=1563.13,monoclinic,P21/n,a=12.608(9),b=21.729(7),c=14.473(8)A.,β=105.34(5)°,V=3823.6A3,Z=2,Dc=1.28 g.cm-3,F(000)=1528,μ=8.6 cm-1,The final R and Rw are 0.076 and 0.083 respectively for 4418 observed reflections with I≥3σ(I).There is a center of inversion in the molecule. 相似文献
14.
《中国化学快报》1992,(12)
(PPh_3)_2Ni(i-mnt),(i-mnt=S_2C=C(CN)_2),Mr=613.43,monoclinic,Pn,a=9.167(3),b=10.872(3),c=18.209(7) ,β=101.46(3)°,V=1779(1) ,Z=2,Dc=1.15 g/cm~3,λ(Moka)=0.71069 ,μ=7.67 cm~(-1),F(000)=648,T=296K,final R=0.060,Rw=0.073 for 1909 observed reflections with Ⅰ≥3σ(Ⅰ).The complexadopts a square planar geometry as its coordination unit,the mean Ni-S and Ni-P distances are 2.216and 2.221 ,respectivety. 相似文献
15.
《结构化学》1992,(5)
<正> The reaction of [Et4N][Mo(CO)4(S2CNEt2)] with tetraethylam-monium tetrathiomolybdate affords a new mixed-valence dinuclear molybdenum complex [Et4N]2[(CO)4MoS2MoS2] (1). 1 crystallizes in the orthorhombic space group Pbom with a = 18.403(2), b = 11.963(1), c= 13. 482(1)(?) , Z = 4, V = 2986(?)3, Dc=1. 55g/cm3, Mr = 6S2. 69. R =0. 042 and Rw =0. 057 for 1975 independent reflections with I≥3σ(I), F(000) = 1416, μ =11. 2cm-1. The structure of the anion of 1 consists of an octahedron for the lowvalent Mo atom and a tetrahedron for the high-valent Mo atom sharing an S - S edge. The Mo - Mo bond distance is 2. 992 (2) (?) and the bimetallic center MoS2Mo is planar with Mo-S of 2. 517 and 2. 231 A and MoSMo angles of 78. 04° and 77. 67°. The electron delocalization between the two Mo atoms with wide separated oxidation states is also discussed. 相似文献
16.
《结构化学》1993,(2)
<正> The reaction of Ru(DMSO)4Cl2 and Ph2PN (i-Bu)Ph2(1:2) gave the title compound, trans-RuCPh2PN(i-Bu)PPh2]2Cl2. Crystallographic data for C56 H58Cl2N2P4Ru: triclinic, space group P1, a = 11. 575(1), b = 12. 193(3), c = 20. 297(4)A, α=75. 30(2),β=76.28(1),γ= 72. 08(2)°, V = 2596. 6(8)A3, Z = 2, Mr = 1054. 97, Dc=1. 35g/cm3,μ(MoKa) = 5. 58cm-1, F (000) = 1092; R = 0. 046 and Rw = 0. 056 for 3411 observed reflections. The Ru atom is coordinated by four P atoms and two Cl atoms, forming an octahedral configuration. 相似文献
17.
《结构化学》1990,(1)
<正> The title compound crystallizes in orthogonal space group P212121with α= 12. 848 (5), b =13. 227 (3), c = 29. 519(8) A ,Z = 4 , V= 5016. 5 A3 and Dc = 1. 483g/cm3. 4940 independent reflcctiions were collected on a CAD4 diffractometer with MoKa radiation in the range of 1°<0<25°,of which 3559 reflections having intensities I >3σ(I) were used for structure determination. The structure was solved by direct methods and refined by the least-squares method to final discrepancy factors R=0. 071 and Rw - 0. 075. The anion of the title compound can be described as a slightly distorted MoS42-tetrahedron coordinated by three [CuS2CNEt2] units ,with the four metal atoms lying approximately in a plane. 相似文献
18.
《结构化学》1991,(3)
<正> trans-PtH(PCy3)2[S2CN(CH2C6H5)2] crystallizes in triclinic space group P1 with a=10. 961 (9),b= 13. 247 (6), c= 18. 331(4) A ,α=82. 97(2) ,β= 103. 89(5),γ=103. 79(7)°,Mr=1029. 39,V = 2503(4)A3,Z = 2,Dc = 1. 366g/cm3, μ= 30. 06cm-1,F(000) = 1068,R=0. 033 and Rw = 0. 039 for 6940 unique observed reflections. The platinum atom is coordinated by one hydrogen,one sulfur and two phosphorus atoms to form a distorted square plane. 相似文献
19.
The crystal structure of .[Et4N][Sm(S2CNEt2)4] was determined by X-ray diffraction technique. The crystal crystallizes in monoclinic system, space group P21/n with a= 1. 1695(3), b=2.0821(6), c=1.7420(7) nm, β=99. 79(3)°? Z=4, Dc= 1. 39 g/ cm3, μ(Mo/KTσ) = 18. 4 cm-1, F(000) = 1812. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R of 0. 053 for 3116 (Ⅰ> 3σ- (Ⅰ)) reflections. Each asymmetric unit contains two ions [Sm (S2CNEt2)4]-1 and [Et4N] +1, having distance between central atoms N5 and Sm3+ to be 0. 6522 nm. The atom Sm is coordinated by eight sulphur atoms. The Sm-S distance lies in the range of 0. 285-0. 290 nm with an average of 0. 288 nm. 相似文献
20.
《结构化学》1992,(5)
<正> The reaction of H2PtC14, Ph2PCH2PPh2(dppm) , NaSPh, and element selenium in DMF gives rise to a mononuclear complex Pt (dppm ) (SPh)2, PtS2P2C37H32, Mr = 797. 83, triclinic, space group P1, a = 10. 051(2), b = 11. 805 (3), c=15. 499(4)(?). α=109.41(3), β=90. 94(3), γ=107. 80°, V = 1636.3 (?)3. Z = 2, Dc= 1. 619gcm-3, * = 45. 749cm-1, and F(000) = 788. The final structural refinement converged with unweighted and weighted R factors of 0. 029 and 0. 044, respectively, for 4832 observed unique reflections with I>3σ(I). The complex is an asymmetric molecule with a four-coordinated Pt atom. The average of Pt -S and Pt-P bond distances are 2. 334(3) and 2. 260(3) (?), respectively. 相似文献