SYNTHESIS AND STRUCTURE OF A NEW LINEAR TETRANUCLEAR Mo-Fe-S CLUSTER (Et_4N)_2[(Et_2NCSSMoS_2)_2O_3Fe_2S_2]·DMF

(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).

SYNTHESIS AND CRYSTAL STRUCTURE OF A PLATINUM (Ⅱ) COMPLEX WITH MIXED DIPHOSPHINE AND THIOLATE LIG-ANDS, Pt(dppm)(SPh)_2

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.

SYNTHESIS AND STRUCTURE OF THE PEROXOVANADIUM (V) COMPLEX CONTAINING NITRILOTRIACETATE Na_2[VO (O_2) N-(CH_2COO)_3]·5H_2O

Na2[VO(O2)N(CH2COO)3] · 5H2O, Mr= 423. 11, monoclinic, space group P21/c, a = 6. 283(3), b = 20. 378(6), c=12. 056(4)(?) , β=102. 96 (3)°, V = 1507. 9(?)3, Z = 4, Dc= 1. 864 g/cm3. λ(MoKα) = 0. 71069A , F(000) = 864. Final R = 0. 037 and Rw = 0. 046 for 1658 observed reflections with I>10σ (I). The structure of the anion of the title complex shows that the vanadium atom is coordinated by one vanadyl oxygen atom, two oxygen atoms of the peroxp-group, three oxygen atoms and one nitrogen atom from the NTA ligand to form a distorted pentagonal bipyramid.

CRYSTAL STRUCTURE OF Pt(dppe)(SPh)_2

Anaerobic reaction of Pt (dppe)Cl2 (dppe = Ph2PCH2CH2PPh2) with NaSPh and elemental selenium affords complex Pt(dppe)(SPh)2,which crystallizes in the monoclinic system space group C2/c with a=14. 392(7) ,b=16. 380(7) ,c=14. 266(5) A ,β=86. 44(4)°,V=3342(5) A3,Z = 4,Dc=1. 613g/cm3,and μ(MoKa) = 44. 813 cm-1. The final structural refinement converged with unweighted and weighted R factors of 0. 041 and 0. 057 for 2206 observed reflections (I>3σ(I)). X-ray analysis shows that the Pt atom in Pt(dppe)(SPh)2 is at the center of the approximately planar tetragon of two P atoms and two S atoms.

CRYSTAL STRUCTURE OF A TRINUCLEAR COBALT COMPLEX Co_3(bdt)_3(PBu_3~n)_3 · ~2CH_2C1 (bdt = S_2C_6H_4~2- ) WITH MIXED o-BEN-ZENEDITHIOLATE AND TRIBUTYLPHOSPHINE LIGANDS

Co3(S2C6H4)3{P(C4H9)3}3 ·2CH2Cl2, Mr = 1373. 45, mono-clinic, space group P21/c, a = 16. 110(5), b=36.313(10), c=13. 502(5) A , β= 105. 69(4)% V=7604. 4 A3, Z = 4, Dc = 1. 20 g. cm-3, μ=10. 03 cm-1, and F (000) = 2990. R(Rw) is 0. 086(0. 091) for 4559 observed unique reflections. The three cobalt atoms in the complex form an isosceles triangle with an average Co -Co bond distance of 2. 504(5) A. The average values of Co - S and Co - P bond distances are 2. 271(7) A , and 2. 198(8) A , respectively.

SYNTHESIS AND STRUCTURE OF (Me_4N)[Mo(OC_6H_4S-o)_3]

(Me4N)[Mo(OC6H4S-o)3] ,Mr=542. 57,orthorhombic,space group Pnb21 with a = 22. 708(1),b = 9. 737(4),c=10. 486(2) A;V=2318. 6A3;Z=4,Dc = 1. 55g/cm3,final R=0. 064 and Rw=0. 074.μ=8. 3cm-1, F(000) = 1108,The atom Mo( V ) of the anion issix-coordinated to three oxygen and three sulfur atoms in a distorted octahedral geometry.

SYNTHESIS AND CRYSTAL STRUCTURE OF BIS (TETRAETHY-LAMMONIUM) BIS(TRITHIOCARBONATO) BIS(μ-PHENYLTHIO-LATO)-DI-NICKEL(Ⅱ), (Et_4N)_2[Ni_2(μ-SC_6H_5)_2(S_2CS)_2]

(Et4N)[Ni2(SC6H5)2(S2CS)2],Mr= 844. 68; monoclinic P21/c, a = 16. 951(3), b = 11. 151(3), c=20. 428(2)(?) ,β=99. 03(2)°, V = 3813(3)(?)3, Z = 4, Dm = l. 48, Dx = 1. 471 gem-3, graphite-monochromated MoKa=0. 71073 (?), μ=14. 4cm-1, F(000) = 1776; T' = 295K, R = 0.061, Rw =0.072 for 5586 unique observed reflections, and 211 parameters. The structure of the complex consist of discrete [Ni2(μ-SC6H5)2(S2CS)2]2- complex anions and tetraethylammonium cations. In each anion nickel (Ⅱ) is distorted square planar coordinated with four atoms, two bridging atoms from the benzene-thiolato and two from the trithio-car-bonate, SCS22- ligand. The structure has the synendo conformation[1].

SYNTHESIS AND STRUCTURE OF Ni_2(PBu_3~n)_2(SC_7H_6S)_2

The nickel(Ⅱ) complex Ni2(PBu3n)2(tdt)2(tdt = SC7H6S2-) containing dithiolato and phosphino ligands has been prepared and characterized by X-ray diffraction. The complex crystallizes in triclinic system, space group P1, with a = 14. 423(4), b = 15. 053(3), c=10. 648(3)(?), α=93.,95(2), β=100. 31(3), γ = 84. 16(2)°; V =2259.6 (?)3; Z = 2, Dc= 1. 22 gem-3, Mr = 830. 57; μ = 11. 076cm-1, F (000) = 888. In the complex, the Nickel atoms are linked by two bridging sulfur atoms from the two tdt ligands with the Ni-Ni distance of 2. 679 (?) . and each nickel atom is four coordinated by one phosphorus and three sulfur atoms with a square-planar geometry, the average length of Ni -S bond is 2. 193(?) and that of Ni-P bond 2.186(?).

SOME NOVEL Au-Ag SUPRACLUSTERS: THE SYNTHESES AND CHAR- ACTERIZATION OF 25-ATOM,37-ATOM,AND 38-ATOM CLUSTERS

The reduction of mixtures of mononuclear Au(I)and Ag(I) phosphine halide complexes with sodium,boronhydride in different solvents gave rise to two types of 25-atom clusters,and 37-atom and 38-atom clusters. These clusters were formed by vertex-sharing of Au-centered icosahedral cluster units (Au7Ag6). The nuclearity of these clusters is given by (13n-e) , where n is the number of the cluster units and e is the edges of the polyhedron formed by centers of the icosahedral cluster units . The structures of these novel 25-atom,37-atom and 38-atom clusters can be described as two icosahedra sharing one vertex (2×13-1 = 25)or three icosahedra sharing three vertices in a triangle(3×13-3 = 36)plus capping atom(s).