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.

STUDY ON TETRANUCLEAR TRANSITION METAL CLUSTER WITH μ_3-O BRIDGES I . SYNTHESIS AND CRYSTAL STRUCTURE OF [Fe_4O_2(O_2CCH_3)_7(2,2'-bipy)_2]Cl

[Fe4O2(O2CCH3)7(2,2’-bipy)2]Cl,Mr=1016.5,monoclinic,C2/c,a=27.628(5),b=11.882(3),c=16.587(3)A,β=119.03(1)°,V=4761.4A3,Z=4,Dc=1.418 g/cm3,λ(MoKa)=0.71069A,μ=13.13 cm-1,F(000)=2088,R=0.062 and Rw=0.077 for 3116 reflections with I≥3σ(I).The title compound contains a [Fe4O2]8+core with bridging CH3COO-and terminal bipy groups giving the structure with a C2 symmetry.The arrangement of the four metal atoms is not planar but has a butterfly-like structure with a dihedral angle of 141.58°.

CRYSTAL STRUCTURE OF MIXED-METAL CLUSTER (η~5-C_5H_5)_2W_2Fe_2(μ_3-S)_2(CO)_8

(η5-C5H5)W2Fe2(μ3-S)2(CO)8,Mr = 897. 80,monoclinic,C2/c,a= 18. 019 (2),b = 8. 330(1),c= 16. 043(2) A ,β= 114. 30(1)°,v = 2194. 7(6)A3,z= 4, Dx = 2. 717g/cm3, A(MoKa) = 0. 71037 A , μ= 122. 01cm-1, F (000) = 1656, T = 295K,R=0.056,Rw = 0. 059 for 1250 observed reflections. The crystals of the title compound are isomorphous with the analog (η5-C5H5)2Mo2Fe2(μ3-S)2(CO)8.

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.

SYNTHESIS AND CRYSTAL STRUCTURE OF A TRITUNGSTEN CLU-STER COMPOUND H[W_3O_2(O_2CCH_3)_9]·5H_2O

In this paper we report the structure of another new W3 cluster compound H[W3O2(O2CCH3)9]·5H2O prepared by the method reported previously. The title compound crystal lizes in monoctinic system, space group P21 with cell dimensions: a = 8. 237(3),6=13. 273(2),c=14.508(4)A,β=92.97°(3),V=1584A3.Z=2,and Dc=2. 529g/cm3.The average W - W, W -U_3-O,W -Oac and W -Ot distances are 2. 775, 2. 01,2. 09 and 2. 04 A, respectively.

Preparation and Structure of (Ph_3PCH_2Ph)[Ni(OSNC_5H_3)_2]DMF

Compound (Ph3PCH2Ph)[Ni (OSNC5H3)2] . DMF was obtained from the reaction.of NiCl2,Na2(OSNC5H3)and Ph3PCH2PhCl. Mr = 735. 53,monoclinic,P21/ c,a=9. 857(6),b=17. 594(9),c=21. 369(10) A,β=102. 85(4)°,V=3613. 1A3,Z = 4,Dc=1. 35g/cm3,λ(Mo-Ka) = 0.71073A.μ=7. 3cm-1,F(000) = 1532,The nickel (Ⅲ) ion is coordinated by two 2-mercapto-3-pyridinolate ligands to give an approximate square-plannar configuration with cis-geometry.

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 STRUCTURES OF TWO DITHIOLATO-COPPER COMPLEXES (Ph_4P)Cu(BDT)_2 AND (Ph_4P)Cu(TDT)_2

[(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.

SYNTHESIS AND CRYSTAL STRUCTURE OF DINUCLEAR IRON CARBONYL DERIVATIVE (μ-SC_6H_5) (μ-P (SC_6H_5)_2) Fe_2 (CO)_5 (P-(SC_6H_5)_3)

The reaction of Fe3(CO)12 with P(SPh)3 yields the tile compound. C41H30Fe2O5P2S6, Mr = 968. 65, monoclinic, space group, P21/n, a = 14. 449(9), b = 18. 046(11), c=16.871(10)(?), β=98. 76°, V = 4348(?)3, Z = 4, Dc=1. 480g/ cm3, λ(MoKα) = 0. 71073(?) The structure was determined by direct methods and difference Fourier syntheses and refined by full-matrix least-squares procedure to R = 0.084, Rw = 0.144 for 4059 reflections. Fe(1)-Fe(2) = 2. 576(6), Fe(2)-P(2) = 2.194(9)(?). The dihedral angle between the Fe(l)SFe(2) and Fe(1)PFe(2) planes is 81. 9°. The other one (dihedral angle between SFe(1)P and SFe(2)P planes) is 75. 2°.

CRYSTAL AND MOLECULAR STRUCTURE OF [Cu_2(α-C_(10)H_7-CH_2CO_2)_4(DMF)_2](DMF)_2· H_2O

The title complex crystallizes in the triclinic system, space group P1, a =11. 912(4), b = 13. 626(2), c=10. 040(3)(?), a=95. 03(2) ,β= 114. 8 (3), γ = 73. 58(3)°, V = 1418.0(?)3, Z = 1, D,= 1. 37g/cm3, F(000) = 612, R = 0. 064 for 4860 independent reflections [I>3σ(I)]. Each Cu atom is coordinated by the oxygen atoms from the C10H7CH2COO groups and DMF in a square pyramid geometry.

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 CRYSTAL STRUCTURE OF A TRITUNGSTEN CLUS-TER COMPOUND [W_3O_2(O_2CCH_3)_6(H_2O)_3]ZnBr_4·8H_2O

C12H40O25Br4W3Zn, Mr = 1520. 71, monoclinic, space group P1, a = 10. 470(4) b=17. 669(6),c=14. 477(2) A ,α=99. 80(2),αB=101. 51(2),γ=99. 78 (4)°,V=1829A3,Z = 2,DX = 2. 66g/cm3,λ(MoKa) = 0. 71073A,μU= 146. 9cm-1,F (000) = 1408. Final R=0. 038,Rw = 0. 049 for 4088 independent observable reflections.

SYNTHESIS AND CRYSTAL STRUCTURE OF TRINUCLEAR CLUSTER [M_3O_2(O_2CCH_3)_6(H_2O)_3]ZnBr_4·8H_2O(M=0. 33Mo+0. 67W)

C12H40O25Br4MoW2Zn, Mr=1432. 75,Monoclinic,Space group C2/c,a= 13. 239(2),b= 16. 215(3),c= 17. 670(3) A ,β= 105. 53(2) ,V=3654 A3,Z= 4,μ= 64. 0cm-1,λ(MoKa) = 0. 71073 A , F (000) = 2688, Dc = 2. 605g/cm3. Final R = 0. 042,Rw = 0. 057 for 2688 observed independent reflections.

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 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(?).

CRYSTAL STRUCTURE OF [PdCl_2 (DMAF)_2]·C_7H_8

C33H42 Fe2PdCl2N2 (dichloro-bis (dimethylaminomethylferrocene) pal-ladium(Ⅰ) toluene solvate) ,Mr = 755. 72,monoclinic,P21/c,a=7. 521(1),b= 11. 128 (2),c=19. 260(7) A ,β=91. 77(2)°,V=1611. 1A3,Z=2,Dc = 1. 56g·cm-3,D0 = 1. 58g·cm-3,μ=76. 3cm-1, The least-squares refinement gave a final R value of 0. 062 for 2192 observed reflections. The Pd atom is of squareplanar coordination. The ferrocene ligand of in DMAF has an approximately eclipsed conformation.

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].