THE SYNTHESIS AND CRYSTAL STRUCTURE OF CIS-BIS(1,10-PHENANTHROLINE)GLYCINECOBALT(Ⅲ)

A new coordination compound of cis-bis(1,10-phenanthroline)glycinecobalt(Ⅲ) chloridate tetrahydrate,cis-[Co(phen)_2gly]Cl_2.4H_2O,has been prepared by glycine reacted with cis-[Co(phen)_2Cl_2]Cl,then isolated by SP-Sephadex C-25 H^+ form column. The crystal and molecular structure of the new compound has been determined by RIGAKU AFC5R four circle diffractometer,5032 independent reflections were collected of which 3781 observable reflections were used for structure refinement.The crystal is monoclinic,space group C2/c,with a=35.13(1),b=9.637(3)(,c=17.485(6),β= 115.08(Z)~,V=5362(3),Z=8.The structure was refined by full matrix least-squares procedure to a final R=0.041 and R_=0.060.The molecular formula was CoC_(28)H_(28)N_5O_8Cl_2. with molecular weight M_r=636.38,D_c=1.58g/cm^3,μ=8.88cm^(-1)and F_((000))=2624.

Synthesis and Crystal Structure of a Three-dimensional Mn(Ⅱ) Coordination Polymer with 3-(Pyrazin-2-yloxy)-pyridine and Azide Anion as Mixed Bridge Ligand

A three-dimensional coordination polymer [Mn2（μ1.3-N3）4（μ-PP）2]n （PP = 3-（pyrazin-2-yloxy）-pyridine） has been synthesized with 3-（pyrazin-2-yloxy）-pyridine and azide anion as mixed bridge ligand, and its crystal structure was determined by X-ray crystallography. The crystal data： triclinic system, space group P1, with a = 6.794（4）, b = 9.885（6）, c = 9.947（6） A, α = 64.170（6）, β= 84.190（8）, γ= 85.319（8）°, V = 597.7（6）A^3, Z = 1, C18H14Mn2N18O2, Mr = 624.35, Dc = 1.735 g/cm^3, F（000） = 314 and μ = 1.117 mm^-1. In the crystal, the azide anion acts as a bridge ligand and makes adjacent Mn（Ⅱ） ions connect into a two-dimensional sheet on the ab plane, then 3-（pyrazin-2-yloxy）-pyridine serves as a bidentate bridge ligand to connect neighboring sheets along

HETERONUCLEAR COMPLEX CONTAINING COPPER-LANTHANIDE ARRAYS: THE SYNTHESIS AND CRYSTAL STRUCTURE OF Ln_2Cu_4L_8 (HL)_4(OH)_2(CIO_4)_4(H_2O)_(10)·2CH_3COCH_3 (Ln = Tb (1), Y (2); HL = 2-Pyridone C_5H_5NO)

Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and the structure was determined by four-circle diffractometer. Data showed that the crystal is in space group C2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A^3. The structure was solved by a combination of Patterson method and Fourier technique. The final R value is 0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form an essentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atoms are five-coordinate.

STUDIES ON SOLID STATE REACTIONS OF COORDINATION COMPOUNDS(LXⅡ)Solid state synthesis and crystal structure of the complex ICu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)CIJ·0.5CS_2

[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15cm^(-1),F(000)=1855,R=0.052, R_W=0.045 for 3930 observed reflections with Ⅰ>1.5σ(Ⅰ).The central metal atom has a dis. torted tetrahedral geometry with bond lengths Cu-S=2.384(2) (Au-S=2.389(4)), Cu-Cl=2.481(3)(Au-Cl=2.474(1))and Cu-P=2.269(2)-2.289(2)(Au-P=2.270(4)-2.279(4)) .

SYNTHESIS AND CRYSTAL STRUCTURE OF Mo_2OS(μ-S)_2[S_2CNC_4H_8]_2

Mo_2OS(μ-S)_2[S_2CNC_4H_8]_2, Mr=612.61, triclinic, PI, a=8.666(2), b=17.366(6), c=6.708(1), α=98.29(2)°, β=97.27(2)°, γ=79.36(2)°, V=976.5(5)~3, Z=2, Dc=2.03g/cm^3, MoKα(λ=0.71069), μ=19.75cm^(-1), F(000)=588, Final R=0.064, Rw=0.073 for 1517 unique intensity data (I>3σ(I)). The binuclear unit of [Mo_2OS_3] has a new asymmetrically terminal coordinated configuration with Mo-Mo distance of 2.807(3).

Synthesis and Crystal Structure of [Pd(NH_3)_4]Cl_2·2[Pd(NH_3)_3Cl]Cl

A new type of ammine palladium(Ⅱ) chloride was prepared by evaporating the solution of [Pd(NH3)]4Cl2 at room temperature. Its crystal structure was refined from single-crystal X-ray data: P42/nmc, a=10.5390(10)A, c=16.905(3)A,, Z=2, and R=0.0357 for 731 structure factors and 52 variable [arameters. The framework of the title compound is composed of three sorts of structural units: [Pd(NH3)4]2+,[Pd(NH3)3Cl]+, and Cl-,of which the first kind of least squares plane exhibits distortion in some degree

SYNTHESIS AND CRYSTAL STRUCTURE OF[Li.4THF][GdCl_4·2THF]

GdCl_3 reacts with CH_3C_6H_4Li at a molar ratio of 2:1 in tetra- hydyofuran(THF)to yield an interesting compound [Li·4THF][GdCl_4·2THF]; its X-ray crystal structure shows the molecule to be an ion-pair.

SYNTHESIS AND CRYSTAL STRUCTURE OF THE FIRST THREE DIMENSIONAL NETWORK CU(Ⅱ) COMPLEX BRIDGED BY BOTH OXAMIDE AND AZIDE

A novel three dimensional network complex polymer [Cu_4(oxen)_2(N_3)_3]_n(ClO_4)_n·2nH_2O, where oxen is N,N' -bis(2-aminoethyl)oxamide dianion, has been synthesized. It crystallizes in triclinic system, space group P, with a=11.486(2), b=11.706(3), c=12.291(3) , α=77.42(2), β=67.59(2), γ=77.96(2)°, and z=2. The least-square refinements converged at R=0.047, with 3416 observed unique reflections. The complex has a pronounced three-dimensional character and can be viewed as the tetranuclear asymmetric repeating units through inversion and translation operations to extend a three-dimensional network. The structure of Cu_4 asymmetric unit consists of two square planar and two square pyramidal Cu central atoms linked by both azide ligands in end-on and end-to-end bonding modes, and oxamidate bridge in trans conformation.

SYNTHESIS AND CRYSTAL STRUCTURE OF A ONE-DIMENSIONAL POLYMERIC CLUSTER[Mo(μ-S)_2Ag(μ-S)_2·α-MePyH]_n

Reaction of (NH_4)_2MoS_4 with AgI in α-MePy gives the title com- pound,an X-ray analysis of which shows that the molecule forms a one-dimensional polymeric chain with continuous metal-metal bonds.

SYNTHESIS AND CRYSTAL STRUCTURE OF 3-PHENYL-3-HYDROXY-9-METHYL-9-AZABICYCLO [4.2.1] NONANE

A new bicyclic alkaloid, 3-phenyl-3-hydroxy-9-methyl-9-azabicyclo [4.2.1] nonane, has been synthesized from tropinone and its structure was determined by single crystal X-ray diffraction.

SYNTHESIS AND CRYSTAL STRUCTURE OF [(η~5-C_5H_5)_2NdCl·OC_4H_8]_2

All attempts to prepare light lanthanide dicyclopeutadienyt chloride failed,due to the disproportionation reaction. The crystal complex of [（η5-C5H5）2NdCl.OC4H8]2 was successfully prepared by the reaction of NdCl3·2C4H8O with cyclopentadienyl sodium （molar ratio 1:1.8）in tetrahydrofuran at room temperatureThe composition of the title compound was determined by the methods of elemental analysis, infrared spectroscopy and photoelectron spectroscopy. The crystal structure of [（η5-C5H5）2NdCl·OC4H8]2 was determined from single crystal X-ray diffraction. Data were collected at-60℃ under dry nitrogen atmosphere.The complex crystallizes in the monoclinic space group P21/c,with Z=2. Lattice parameters are: a=8.201（3）, b=21.589（6）,c=8.596（3）,β=109.10（3）°.The structure was solved by Patterson and Fourier techniques and refined by least-squares to a final conventional R=0.0636 for 1680 reflections. There are two Nd atoms in the dimeric unit which are bridged asymmetrically by the two

The Synthesis and Crystal Structure of the First Trinuclear Molybdenum Complex Containing PyS Ligands [Mo_3(CO)_6(μ-PyS)_2(μ_3-PyS)_2]

The deprotonated derivative pyridine-2-thiolato （PyS-） of pyridine-2-thione （PySH）is a potentially amibidentate or multi-functional donor which coordinates toward transitionmetals with either the exocyclic S or heterocyclic N atom or both atoms to form differentcoordination modes. We have recently reported the synthesis and crystal structure ofthe first dinuclear molybdenum complex with doubly-bridging PyS ligands [Mo2（CO）4（μ-PyS）2（PPh3）2]which was obtained from the reaction of [Mo（CO）3（CH3CN）3]

Structural comparison to the molybdenumsite of nitrogenase Synthesis and crystal structure of binuclear oxomolybdenum(V)complex with both omercaptophenolate and alkoxide ligands

Complex(n-Bu_4N)[Mo_2O_2(OMe)(mp)_3][1,mp=(o-OC_(?)H_4S)^(2-)]was synthesized by the reaction of MoOCl_3(THF)_2 and Na_2mp in EtOH and crystallized in monoclinic space group P2_(?)/n with crystal data:a=13.910(3),b=23.554(3),c=12.558(2)(?),β=105.20(2)°,Z=4,D_o=1.455g/ cm^3,final R=0.077 for 5325 reflections[I>3σ(I)].The two[Mo(O)mp]^+ moicties are bridged by one 1,2-bidentate ligand mp^(2-) with exceedingly small bite angle(69.0°)and bite distance (2.70(?))and by a methoxy group.The structure can be interpreted as two distorted octahedra around the Mo atoms sharing a face.Attempts have been made to provide structural informa- tions for the syntheses of modelling compounds of FeMoco by comparing the Mo—O and Mo—S bond distances of o-mercaptophenolate ligated compounds to those of the molybdenum site of nitrogenase.

Synthesis and crystal structure of a new polpouclear complex with a monomer of (3,4,9,10-dibenzo-1, 12-diaza-5, 8-dioxacyclopentadecane)-copper(Ⅱ) (μ-Cl)_2 zinc(Ⅱ) chloride

A polynuclear complex containing a monomer of Cu(Ⅱ)-Zn(Ⅱ) heterobinuclear unit was synthesized and characterized by IR spectra and magnetic moment. The crystal and molecular structure of the complex, CuZnC_(19)H_(24)Cl_4N_2O_2, was determined by X-ray diffraction, it crystallized in monoclinic, P2_1 / m, a = 8.812 (2), b = 15.972(3), c = 8.831(1) A, β = 114.33(1)°, V = 1132.4A^3, Z=2, D_c= 1.710 g / cm^3, λ(Mo K_α) = 0.71073A, μ = 25.227 cm^(-1), R = 0.051. R_w = 0.063 for 1130 ob- served reflections with I> 3σ(I) . The coordinated octahedra of Cu(Ⅱ) and tetrahedra of Zn(Ⅱ) via bridging Cl atoms form a single chain polynuclear complex. The Cu, Zn and bridging Cl atoms are located on the crystallographic symmetry plane m which is perpendicular to 2N and 2O donor plane.

Synthesis and crystal structure of [V_2(μ-S_2)_2(S_2CNEt_2)_4]·2CH_3Cl

[V_2(μ-S_2)_2(S_2CNEt_2)_4].2CH_3Cl was synthesized by the reaction of NaS_2CNEt_2,Li_2S and VOCl_3 at room temperature.Crystal data:M=1061.3,space group Pbca,with the orthorhombic parameters:a=20.123(3),b=20.485(4),c=10.911(3),V=4497.7,Z=4,D_c=1.57g/cm^3,Mo Kσ radiation(λ=0.71069()?),μ=13.2 cm^(-1),F(000)=2168.Final R=0.041 and R_w=0.047 for 2288 ob- served reflections with I>3σ(1).The coordination sphere of each V atom in title compound is a dis- torted tetragonal prism composed of two bidentate dithiocarbamate and two S_(2^((2-)) ligands.The V—V distance is 2.890 while the V—S distances fall in the range of 2.422—2.505.

Synthesis and crystal structure of azafulgides

Two azafulgides were synthesized and their crystal struetures determined by a single crystal X-ray diffraction analysis. The substances crystallized in the following symmerries and cell parameters. C_(23)H_(19)NO_3(2): triclinic space group P with a=7.243(2), b=10 . 981(6) and c=12. 672(8), a= 80.40(5) °,β=75.58(4)° and γ= 77.32(3)°, Z=2; C_(19)H_(19)NO_3(1): orthogonal space group C_(2v)~9-Pmc2_1 with a=8.079(8), b=12.752(9) and c=15.752(13), Z=4. The calculated densities are 1.26 and 1.27 g/cm^3 respectively for 2 and 1. The crystal structures were determined by direct methods. The least-squares refinement led to R values of 0.044 and 0.058 for 2 and I for 2738 and 952 reflections with I>3σ(1) respectively.

SYNTHESIS,CHARACTERIZATION AND CRYSTAL STRUCTURES OF η~5-CH_3C_5H_4)M(CO)_2NO AND(η~5-CH_3C_5H_4)M(μ_3-NH)(μ_2-NO)(μ_2-CO)Fe_2(CO)_6(M=Mo or W)

Synthesis of complexes（η;-CH;C;H;）M（CO）;NO（M=Mo,I;M=W,II）and clusters（η;-CH;C;H;）M（μ;-NH）(μ;-NO) （μ;-CO）Fe;（CO）;（M=Mo,III:M=W,IV）,based on the reaction of （η;-C5;）M（CO）;Cl with Na[Fe（CO）;NO] at room tem-perature,have been demonstrated,The crystal structures of II and IV arealso presented.

Syntheses and Structural Characterizations of a Series of Capped Keggin Derivatives

Hydrothermal reactions of Na2MoO2·2H2O and NH4VO3（or V2O5） with appropriate reducing agents such as organic amines, NH2OH·HCl and Mo（CO）6 gave rise to the formation of a series of capped Keggin derivatives, [N（CH3）4]2Na3（NH4）2[（V^VO4）Mo^VI8V^IV4O36（V^IVO）2]·-13H2O（1）, [NH4]7[（V^VO4）Mo^VI8V^IV4O36（V^IVO）2]·7H2O（2）, [HN（CH2CH2）3NH][（PO4）Mo^V3Mo^VI9O36（V^IVO）2]·-3[N（CH2CH2）3N]·（en）·4.5H2O（3） and [HNH2OH][NH4]2[（V^VO4）Mo^VI8V^IV4O36（V^IVO）4]·24H2O（4）. Single-crystal X-ray diffraction analysis revealed that the anions in 1-3 are two-capped Keggin derivatives with characteristic trans vanadium-oxygen caps, whereas the heteropoly anion in 4 is a tetra-capped α-Keggin derivative with characteristic vanadium-oxygen caps on the equatorial plane.