SYNTHESIS AND CRYSTAL STRUCTURE OF THE LANTHANIDE COMPLEX WITH MIXED LIGANDS [Pr (CH_3COO)_2(NO_3)(Phen)]_2

<正> [Pr(CH3COO)2(NO3)(Phen)]2, Mr = 1002. 41. The crystal is monoclinic, space group I2/m, with a = 11. 725(5), b = 12. 269(5), c=12. 732(4) A, V = 1792(2)A3,β=101. 88(0)°. Z = 2, Dc=1. 86g/cm3,μ(MoKa) = 27. 5cm-1, F (000) = 984. The structure was solved by Patterson method and Fourier syntheses, and refined by full matrix least-squares method to R = 0. 033 for 1660 observed reflections with I>3σ(I). The molecule of the complex is a dimer and each praseodymium atom is eight-coordinated in a distorted square antiprism geometry.     

CRYSTAL STRUCTURE OF SEVEN-COORDINATE ZIRCONOCENE COMPLEX (CH_3C_5H_4) Zr(S_2CNBz_2)_3 (Bz=CH_2C_6H_5)

(CH_3C_5H_4)Zr(S_2CNBz_2)_3, Mr=987.55, space group P1, a=13.002(4), b=13.659(3), c=29.685(8); α=100.72(2)~o,β=97.23(2)~o, γ=105.36(2)~o; V=4909(2)~3, Z=4, Dc=1.34gcm~(-3), Mo-K(λ=0.71073A) radiation, μ=5.0cm~(-1), R=0.069, Rw=0.078 for 6100 reflections. The title complex has pentagonal bipyramid configuration in which the zirconium atom is coordinated by one CH_3C_5H_4 group and three bidentate dibenzyldithiocarbamate ligands.     

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

<正> 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(?).     

SYNTHESIS AND STRUCTURE OF COMPLEX(PPh3)_2Ni[S_2C=C(CN)_2]

(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.     

CRYSTAL STRUCTURE OF Na[Nd(S_2CN(C_2H_5)_2)_4]·CH_3CN

<正> Triclinic, PI, a=10.204(3), b=ll.384(2), c=18.399(4) X, a=84.19 (2), 6=106.15(2), Y=116.71(2)? V=1833.1(6)S3, Z=2, y=18.76cm, A=0.71069&, F(OOO)=809.91, room temperature, .R=0.059. In, the title compound the neodym-ium ion is coordinated by eight sulphur atoms from S2CNEt2ligands with the average distances of 2.88A and 2.<.Et2N桟桟\(:S桸Et2-Nb-\\C 桸Et2     

CRYSTAL STRUCTURE OF CsHsFeC_5H_4CH_2N(CH_3)_2BH_3

<正> INTRODUCTION. We have studied the structures of some compounds which contain the cyclependadienyl-aromatic sandwich complexes of metal and boronhydride. The present work is a continuation of our previous work.     

CRYSTAL STRUCTURE OF MOLYBDENUM-CARBENE COMPLEX (CO)_5Mo=C(OC_2H_5)C_6H_4-p-CH_3

<正> INTRODUCTION. Recently, researches on carbene metal complexes are very active, as they are of great importance in both theoretical study and catalytic activity. In a systematic research, the crystal structure of the title complex was analyzed and reported here to the advantage of understanding the catalytic action and searching for new and better carbene catalysts of novel kinds.     

STRUCTURE OF PLATINUM HYDRIDE WITH BULKY PHOSPHINE LIGANDS trans-PtH (PCy_3)_2 {S_2CN (CH_2C_6H_5)_2}

<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.     

SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [Cu_2(CH_3COO)_4(C_8H_(11)NO)_2] · (C_6H_(11)NO)_2 · (C_8H_(12))

<正> SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [Cu_2(CH_3COO)_4(C_8H_(11)NO)_2] · (C_6H_(11)NO)_2 · (C_8H_(12)), where C6H11 = caprolactam, Mr = 900. 07, triclinic,space group P1, a = 11. 103(4), b= 11. 865(6), c=9. 912(3)(?), α=94. 85(4), β=115.20(2), γ=103. 25(4)°, V = 1125(2)(?)3, Z = l, Dx = 1. 33g. cm-3, λ(MoKa) = 0. 71069(?), T = 295K , μ = 10. 45cm-1, F(000) = 478, final R=0. 063 for 2098 observed reflections with I>3σ (I). The two Cu atoms in the molecule are held together by four carboxylate groups. Each Cu atom is bound in a square-pyramidal configuration to four carboxyl oxygen atoms and to the O atom of a caprolactam molecule.     

SYNTHESIS AND CRYSTAL STRUCTURE OF A MOLYBDENUM-COPPER-SULFUR CLUSTER COMPLEX WITH DITHIOBENZOATE LIGAND [Bu_4N]_2[MoCu_2S_4(C_6H_5CS_2)_2]

<正> The title compound has been synthesized by the reaction of (Bu4N)2MoS4, CuCl and (C6H5CS2)(Bu4N) in DMF and recrystallized from DMF/ Et2O. The red black crystal belongs to the triclinic space group P1 with a = 12. 021 (6), b = 17.045(8), c=17. 136(7)(?) , α=110.05(3), β=108.64(4), γ=103.87 (4)°, V = 2873(3)(?)3, Dc=1. 321gcm-3, Z = 2. The structure was refined to R = 0. 065 for .4783 reflections. The anion of the title compound can be described as a MoS42- tetrahedron coordinated by two [Cu(C6H5CS2)] units with the three metal atoms lying on a line. The coordination number of each Cu atom is three.     

SUBSTITUTION REACTION OF LIGANDS IN TRINUCLEAR Mo CLUSTERS WITH "LOOSE COORDINATION SITE" AS WELL AS SYN-THESIS AND CRYSTAL STRUCTURE OF Mo_3(μ_3-S) (μ-S)_3(dtp)_3(C_3H_4N_2)_3 (dtp)·(CH_3)_2CO

When trinuclear molybdenum cluster compound with "loose coordination site", Mo_3(μ_3-S)(μ-S)_3(μ-dtp)(dtp)_3·H_2O(A) (dtp=diethyldithiophos-phinato anion), is reacted with an excess of imidazole, the H_2O ligand and the bidentate bridging ligand μ-dtp are found to be simultaneously substituted by the imidazole to form the title compound. The title crystal belongs to the space group P(?), Z =2, with the following unit cell parameters: a=14.465(2), b=14.653(4), c=14.886(6), α=99.36(3),β=93.11(2),γ=114.29(2),V=2812(3). The crystalline compound consists of an ordered array of the cluster cation and dtp anion with acetone as packed molecule. The cation possesses a symmetry of C_3. Three Mo atoms form basically an equilateral triangle with three Mo—Mo bond lengths of 2.763 (1), 2.762(1), 2.756(1) respectively.     

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

<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.     

CRYSTAL STRUCTURE OF Ce(ClO_4)_3 COMPLEX WITH 3,3-R,R''''-16-C-5(R=CH_3;R''''=CH_3O(CH_2)_2OCH~-_2)

<正> The title compound C18H37O20NCeCl3, Mr = 834. 25, orthorhom-bic, P212121, a = 11.836(4), b = 13.899(6), c= 19. 401(6) A ; V=3192(2)A3; Z = 4; Dc=1. 74gcm-3, F (000) = 1684,μ= 17. 8cm-1 (MoKa). The final R = 0. 080, Rw = 0. 081. The Ce(Ⅲ) ion is coordinated to one O atom of one C1O4- ion, a CH3CN molecule, a water molecule and seven O atoms from a crown ether molecule. The other two C1O4- ions are not coordinated to the metal. The bond lengths of Ce-N(CH3CN), Ce -O(ClO4-), Ce -O(H2O) and Ce-O(crown) are 2. 61,2. 82,2. 53, and 2. 56A, respectively.     

CRYSTAL AND MOLECULAR STRUCTURE OF MOLYBDENUM COM-PLEX MoO_2Cl_2(C_4H_3OCOOH)_2

<正> The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction method. The complex crystallizes in the mono-clinic space group P21/n with a = 10. 306 ( 3) , b = 10. 161 (2), c = 14. 798 ( 4) A . β= 108. 52(2)°, V= 1469. 4(6)A3,Z= 4. The structure was solved by direct methods. Least-squares refinement converged to a final value of R = 0. 043 and Rw= 0. 040 for 1237 reflections. The molybdenum (Ⅵ) ion is bonded to two chlorine atoms, two oxo atoms and two oxygen atoms from two monodentately and weakly coordinated carboxyl groups of molecules C4H3OCOOH, forming a octahedron. The Mo-O distances are in the range 1. 66 - 2. 39A ,the Mo-Cl distances fall in the range 2. 33-2. 34A.     

SYNTHESIS AND CRYSTAL STRUCTURE OFμ-TEREPHTHALATO BINUCLEAR COBALT(Ⅱ) COMPLEX [Co_2(tpha)(bpy)_4](ClO_4)_2

<正> The structure of μ-terephthalato binuclear cobalt (Ⅱ) complex CCo2(tpha)(bpy)4](ClO4)2(tpha=μ-terephthalato, bpy=2,2' -bipyridine) has been determined by X-ray method. Crystals of title complex are monoelinic, space group P21/c, with a = 13. 086(2), b = 9. 428(2), c=20. 237(4) A. β= 108. 83(1)°, Mr = 1105.61, Z = 2, Dx = 1. 55g/cm3, μ= 8. 09cm-1 and F(000)= 1128. The structure has been solved by direct methods and refined to R=0. 053, The title cation has Ct symmetry in which the terephthalato group acts as bridging ligand between the two metal atoms. Each cobalt(Ⅱ)ion is in a distorted octahedral environment. The Co.....Co distance is 10. 35A.     

SYNTHESIS AND CRYSTAL STRUCTURE OF MgCl_2(CH_3COOC_2H_5)_2

The crystal of the title compound was prepared and its structure determined by X-ray diffraction method.1672 independent reflections were collected. The crystal is orthogonal with space group P2_12_12, and a=7.353(3),b=25.111(10), c=8.631(2), Z=8. The structure was solved by using Patterson method and modified with LSM program.The final R= 0.0795. The structural features of the title compound are:Mg(Ⅱ) is octahedral and ethyl acetate is located on trans-position.Mg atoms are connected by double chloro-bridge and form polychains.     

THE STUDY OF SPECTRA AND X-RAY CRYSTAL STRUCTURE OF A NOVEL BIONICS INSECTICIDE——(CH_3)_2NHCH(CH_2S_2O_3)_2Na·H_2O

IR and NMR spectra of novel bionics insecticide—C_5NS_4O_6H_(12)Na·H_2O have been studied. The molecular and crystal structures of the compound also have been determined. The compound crystallizes in the monoclinic space group C_(2h)~5, - P2_1/n with α= 8.0972. (9) , b =16.262(4), c = 10.370(3), β= 94.26(2)° and z = 4.The result shows that N atom in this compound captures a proton to form HN~ group, Na~ is in statistical disorder. Therefore, the structural formula of tho compound is (CH_3)_2HN~ —CH(CH_2S_2O_3~-)_2·1/2 (Na~ )_2·H_2O.     

CRYSTAL STRUCTURE OF BINUCLEAR Y(Ⅲ) COMPLEX WITH p-METHYLBENZOIC ACID, Y_2(p-CH_3C_6H_4COO)_6(C_(12)H_8N_2)_2

Y_2(p-CH_3C_6H_4COO)_6(C_(12)H_8N_2)_2, Mr=1349.08, triclinic, space group P, a=13.00(3), b=19.743(2), c=12.754(3)A, α=97.94(1), β=106.24(2), γ=91.66(1)°, V=3177(1)~3, Z=2, Dc=1.41gcm~(-3), λ(MoKα)=0.71069, μ=18.92 cm~(-1), F(ooo)=1384, T=295K, final R=0.073 for 6504 observed reflections with Ⅰ>36(Ⅰ). There are two nonidentical binuclear molecules with different bridging connection patterns in a cell. One has four bridging carboxyl groups bound two Y(Ⅲ) ions and another only has two. The Y-Y distance is 4.196 for the former and 5.302 for the latter respectively.     

STUDIES ON SYNTHESIS, STRUCTURE AND PROPERTIES OF THE CRYSTAL OF TRIADIC COMPLEX {Mo[S_2CN(C_2H_5)_2]_4}~( 1){FeCl_4}~(-1){C_6H_5CH_2SSCH_2C_6H_5}

In this paper, a new complex {Mo[S_2CN(C_2H_5)_2]_4}~( 1){FeCl}~(-1){C_6H_5CH_2SSCH_2C_6H_5} is syn-thesized by the reaction of MoCl_5, FeCl_3, PhCH_2SH and diethyldithiocarbamate (DTC)in MeOH. The complex is characterized by X-ray, IR, UV-visible, reflection spectra, themeasurements of magnetic susceptibility, differential thermal and elemental analyses. The crystal of triadic complex containing multi-bond species is quite stable and rare.