Synthesis and Structure of a Ruthenium（Ⅱ）-dithiocarbamate Complex [RuH（CO）（PPh_3）_2（4-ClPhNHCS_2）]·C_6H_（14）

The title complex [RuH(CO)(PPh3)2(4-ClPhNHCS2)]·C6H14 has been prepared and characterized by X-ray diffraction analysis.It crystallizes in the triclinic system,space group P1 with a = 11.0817(2),b = 14.3889(2),c = 15.2136(2) ,α = 71.018(1),β = 74.911(1),γ = 85.146(1)°,V = 2214.86(6) 3,Z = 2,Mr = 900.4,Dc = 1.350 g/cm3,Mr = 900.40,μ(MoKα) = 0.616 mm-1,F(000) = 926,S = 1.016,the final R = 0.0478 and wR = 0.0947 for 6828 observed reflections with I > 2σ(I) and 505 variables.The molecular structure of 1 consists of one neutral complex [RuH(CO)(PPh3)2(4-ClPhNHCS2)] and one hexane solvent molecule.The geometry around ruthenium is pseudo-octahedral with two trans-binding PPh3 ligands and one chelating bidentate 4-ClPhNHCS2- ligand via two sulfur atoms.The average Ru-S,Ru-P and Ru-H bond lengths are 2.4824(8),2.3495(8) and 1.71(2),respectively.The electrochemical properties of 1 have been studied in CH2Cl2 solution by cyclic voltammetry.     

Synthesis, Characterization and Crystal Structure of a Diiron Azadithiolate Complex [（μ-SCH2）2NCH2Ph]Fe2（CO）5（PPh3）

Treatment of complex [(μ-SCH 2) 2 NCH 2 Ph]Fe 2 (CO) 6 with PPh 3 in the presence of decarbonylating agent Me 3 NO·2H 2 O afforded the title complex [(μ-SCH 2) 2 NCH 2 Ph]Fe 2 (CO) 5 (PPh 3) in 70% yield.The new complex was characterized by elemental analysis,IR,and 1 H (31 P,13 C) NMR spectroscopic techniques as well as by X-ray crystallography.It crystallizes in triclinic,space group P 1 with a=9.3016(19),b=12.698(3),c=13.904(3),V=1519.8(7)3,Z=2,C 32 H 26 Fe 2 NO 5 PS 2,M r=711.33,D c=1.554 g/cm 3,μ(MoKα)=1.187 mm-1,F(000)=728,T=113(2) K,the final R=0.0288 and wR=0.0680 for 3982 observed reflections (I > 2σ(I)).The PPh 3 ligand resides in an axial position of the square-pyramidal geometry of the neighboring Fe atom and trans to the benzene ring in order to minimize the steric repulsion between PPh 3 and the benzene ring.     

Synthesis and Crystal Structure of the Diiron Azadithiolate Complex [（μ-SCH_2）_2NPh]Fe_2（CO）5（Ph_2PCH_2PPh_2）

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.     

Synthesis, Crystal Structure and Fluorescent Property of One New Complex [Na2（2-benzoylbenzoato）4（Phen）2（H2O）2]·H2O

One binuclear sodium(Ⅰ) complex [Na2(2-benzoylbenzoato)4(Phen)2(H2O)2]·H2O has been synthesized with 2-benzoylbenzoic acid and 1,10-henanthroline as ligands. The crystal structure was determined by X-ray diffraction. The crystal belongs to the triclinic system with space group P , a = 1.08096(8), b = 1.09619(8), c = 1.09740(8) nm, α = 79.0600(1), β = 71.0450(1), γ = 62.0540(1)o, V = 1.08533(1) nm3, Dc = 1.421 g/cm3, Z = 2, F(000) = 484, GOOF = 1.036, the final R = 0.0363 and wR = 0.0961. The crystal structure shows that two neighboring sodium(Ⅰ) ions are linked together by two bridging water molecules, and each end position is coordinated with one 1,10-phenanthroline molecule and one 2-benzoylbenzoato to form a binuclear structure. Each sodium(Ⅰ) ion in the molecule is coordinated with five atoms to give a distorted trigonal bipyramid. The fluorescence property of the title complex is also discussed.     

A New Luminescent Complex Cd（Ⅱ）-xanthene-9-carboxylate: [Cd（L）2（H2O）]n

A new luminescent Cd(Ⅱ) coordination polymer, [Cd(L)2(H2O)]n 1 (HL = xan-thene-9-carboxylic acid), was synthesized hydrothermally and characterized by satisfactory elemental analysis, FT-IR spectra and single-crystal X-ray diffraction. The crystal is of orthorhombic system, space group P212121 with a = 6.4548(4), b = 13.0876(12), c = 27.466(2), V = 2320.3(3)3, C28H20CdO7, Mr = 580.84, Z = 4, Dc = 1.663 g/cm3, F(000) = 1168, μ = 0.990 mm-1, Flack parameter = 0.00(2), the final R = 0.0296 and wR = 0.0691 for 5301 observed reflections (I > 2σ(I)). 1 features a one-dimensional (1D) carboxylate oxygen-bridged inorganic chain, which is further connected by intermolecular hydrogen bonds into a three-dimensional (3D) framework. Moreover, compound 1 exhibits strong photoluminescence in the solid state at room temperature.     

Synthesis and Crystal Structure of[Cu（dppb）（NO_3）]_2（dppb=1,4-Bis（diphenylphosphino）butane）

The synthesis and molecular structure of a new dinuclear copper(Ⅰ) complex [Cu(dppb)(NO 3)] 2 are reported.The compound crystallizes in the monoclinic system,space group P2 1 /n with a=12.830(3),b=10.899(2),c=19.666 (4),β=104.69(3)°,V=2660.1(9)3,Z=4,D c=1.378 g/cm 3,F(000)=1144,the final R=0.0600 and wR=0.0668 for 2951 observed reflections with I > 2σ(Ⅰ).The complex contains a folded Cu 2 P 4 core structure,with two Cu(Ⅰ) atoms being bridged by a pair of dppb ligands to form a 14-membered Cu 2 P 4 C 8 zigzag ring.The ligand sphere of each metal center is completed by a nitrate anion in a chelating fashion.     

Synthesis, Structure and Photo- luminescence of Cu[（PPh3）2]（acac） （PPh3 = Triphenylphosphine, acac = Acetylacetone）

A novel complex Cu(PPh3)2(acac) 1 (PPh3 = triphenylphosphine, acac = acetylacetone) was obtained by a solution reaction and structurally characterized by X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 13.7361(8), b = 12.8204(7), c = 19.7638(13) , β = 95.946(2)°, C41H37CuO2P2, Mr = 687.19, V = 3461.7(4) 3, Z = 4, Dc = 1.319 g/cm3, S = 1.067, μ(MoKα) = 0.758 mm–1, F(000) = 1432, R = 0.0403 and wR = 0.0990. Complex 1 is characterized by an isolated structure. X-ray structure analysis of 1 shows that acac behaves as a chelating ligand and PPh3 coordinates as a monodentate ligand to the Cu(I) atoms. Photoluminescent investigation reveals that the title complex displays a strong green-light emission.     

Crystal Structure and Spectroscopic Properties of a New Ternary Tungstate Li3Ba2Ho3（WO4）8

A single crystal of Li3Ba2Ho3(WO4)8 was obtained from a flux of Li2WO4 under an air atmosphere. The structure of the pure crystal was determined by single-crystal X-ray diffraction method. It crystallizes in the monoclinic system, space group C2/c with a = 5.240(4), b = 12.790(10), c = 19.247(15), β = 91.921(15)°, V = 1289.1(18)3, Z = 2, Mr = 2773.09, Dc = 7.144 g/cm3, μ = 47.732 mm-1, Rint = 0.0693, F(000) = 2340, the final R = 0.0472 and wR = 0.1221 for 1535 observed reflections (I > 2σ(I)). The Li3Ba2Ho3(WO4)8 has a high structure disorder with one 8f site shared by Li(1) and Ho ions with occupancy of 0.25 and 0.75, respectively. The fundamental structure is constituted by distorted square antiprisms Ho/Li(1)O8 with C1 symmetry, distorted Li(2)O6 octahedra and BaO10 polyhedra. The optical properties were investigated by IR and absorption spectroscopy, and the emission cross sections and gain cross sections of 5I7 → 5I8 of Ho3+ were calculated.     

新型四核铜配合物{[Cu4L2（N3）2（μ2-N3）2]·CH3OH}的合成及其晶体结构

多吡啶配体H2L[N,N’-二(3-甲基吡啶基)-2,6-吡啶二酰胺]与Cu(OAc)2.H2O反应合成了一种新型的四核铜配合物——[Cu4L2(N3)2(μ2-N3)2].CH3OH(1),其结构经IR,XRD和元素分析表征。1属单斜晶系,空间群C2/m,晶胞参数a=15.774(3),b=15.062(3),c=10.724(2),β=114.91(3)°,V=2 344.0(8)3,Z=4,Dc=1.736 mg.cm-3,μ=1.869 mm-1,R1=0.120 1,ωR2=0.298 4。1中四个金属铜原子通过两个L2-配体,四个N3-基团连接在一起,形成了一个新颖的四核铜结构。     

A Lanthanide-transition Metal Coordination Polymer：{[CuEu（Hbidc）_2（H_2O）_4]·H_2O}_n（H_3bidc=1H-benzimidazole-5,6-dicarboxylic Acid）

The title complex 1,{[CuEu(Hbidc)2(H2O)4]·H2O}n(H3bidc = 1H-benzimidazole-5,6-dicarboxylic acid),has been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex 1 crystallizes in triclinic,space group P1,with a = 7.791(2),b = 12.058(3),c = 12.109(3),α = 82.189(5),β = 72.407(5),γ = 89.184(4)°,V = 1073.7(5)3,C18H18CuEuN4O13,Mr = 713.86,Dc = 2.208 g/cm3,μ(MoKα) = 3.967 mm-1,F(000) = 700,GOOF = 0.950,Z = 2,the final R = 0.0531 and wR = 0.1068 for I > 2σ(I).Complex 1 possess a tape-like chain structure consisting of Eu2C8O4 and Cu2Eu2C18N4O4 metallic rings alternatively arranged and is the first 3d-4f heterometallic complex based on the 1H-ben-zimidazole-5,6-dicarboxylato ligand(Hbidc).Plenty of hydrogen-bonding and π...π stacking interactions connect the 1D chains to construct a 3D supramolecular architecture.     

Hydrothermal Synthesis and Crystal Structure of An Iron（Ⅱ） Formate [H3CO3] [Fe（HCO2）3]

An iron(Ⅱ) formate [H 3 CO 3 ][Fe(HCO 2) 3 ] (1) has been synthesized under hydro-thermal conditions and characterized by single-crystal X-ray diffraction analysis.Complex 1 crystallizes in the orthorhombic system,space group Pnna with a=8.4130(4),b=11.8306(6),c=8.9468(4),α=106.527(4),β=105.876(4),γ=103.173(4) o,M r=253.94,V=890.48(7)3,Z=4,D c=1.894 g/cm 3,μ=1.721 mm-1,F(000)=512,R int=0.0164,the final R=0.0323 and wR=0.0998 for 979 observed reflections (I > 2σ(I)).1 exhibits a 3D open microporous framework formed by formate anions bridging Fe(Ⅱ) ions.     

THE MOLECULAR AND CRYSTAL STRUCTURE OF [Et4N]2[Fe2S2（NO）4]

<正> The compound [Et_4N]_2[Fe_2S_2(NO)_4] (M_r=556.36) crystallizes in the monoclinic,space group P 2_1/n with a=9. 688(3), b=10. 882(2), c=12. 625(2), β=97. 86(3)°, Z=2, V=1318. 4, D_c=1. 40g/cm~3, ;μ(MoK_a)=12. 8cm~(-1) and F(000)=588. The final R=0. 028 and R_w=0. 029 for 2041 reflections (I≥3σ(I)).The crystals of [Et_4N]_2[Fe_2S_2(NO)_4] consist of discrete cations [Et_4N]~+ and anions     

含双蝶状[2Fe2S]骨架的新型[FeFe]氢化酶模型物{（μ-FcS2）[Fe2（CO）6]2（μ-SMe）2}的合成及其晶体结构

利用1,1’-双锂二茂铁与(μ-S2)Fe2(CO)6和MeI反应,合成了一种新型的含二茂铁基[FeFe]氢化酶活性中心模型化合物——(μ-FcS2)[Fe2(CO)6]2(μ-SMe)2(1),其结构经1H NMR,IR和X-射线单晶衍射表征。1属于斜方晶系,Pbca空间群,晶胞参数a=10.705 8(13),b=21.721 0(3),c=21.721 0(3),V=6 533.2(14)3,Z=8,Dc=1.834 g·cm-3,μ=2.480 mm-1,F(000)=3 584,R1=0.038 8,wR2=0.085 6。     

Synthesis, Crystal Structure and Photoluminescent Property of a Three-dimensional Zinc（Ⅱ） Coordination Polymer: [Zn1.5（PDB）（bix）0.5（μ2-OH）]2n

A new metal-organic coordination polymer [Zn1.5(PDB)(bix)0.5(μ2-OH)]2n 1 (H2PDB = pyridine-3,4-dicarboxylic acid, bix = 1,4-bis(imidazol-1-ylmethyl)-benzene) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P2/c with a = 7.411(2), b = 7.848(3), c = 25.048(8), V = 1451.8(8)3, C28H22N6O10Zn3, Mr = 798.63, Dc = 1.827 g/cm3, μ(MoKα) = 2.529 mm-1, F(000) = 804, Z = 2, the final R = 0.0440 and wR = 0.1035 for 1952 observed reflections (I > 2σ(I)). It exhibits a three-dimensional framework structure. Moreover, its luminescent property has been investigated in the solid state.     

Synthesis and Crystal Structure of N-[2-（4-Chlorophenyl）-1-（1-methylcarbamoyl-2-phenyl-ethylcarbamoyl）-3-phenyl-cyclopropyl]-benzamide

N-[2-(4-chlorophenyl)-1-(1-methylcarbamoyl-2-phenyl-ethylcarbamoyl)-3-phenyl-cyclopropyl]benzamide,C33H30ClN3O3,has been synthesized and characterized by IR,1H NMR,13C NMR and single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 11.646(2),b = 13.795(3),c = 14.559(3),α = 76.422(4),β = 78.028(4),γ = 74.500(4)°,V = 2164.6(7)3,Z = 3,Mr = 552.05,Dc = 1.270 g/cm3,λ = 0.71073 ,μ(MoKα)= 0.171 mm–1,F(000)= 870,the final R = 0.0469 and wR = 0.0805 for 5554 observed reflections with I > 2σ(I).The N–H and oxygen atoms are involved in one-dimensional intermolecular hydrogen bonds,which further stabilize the structure.     

Hydrothermal Synthesis,Crystal Structure and Magnetic Property of a New Co（Ⅱ） Complex：[Co（4,4＇-bpy）_2（H_2O）_2（4-FBA）_2]·（4,4＇-bpy）

A new complex [Co(4,4'-bpy)2(H2O)2(4-FBA)2]·(4,4'-bpy)(1) has been hydro-thermally synthesized using cobalt,4,4'-bipyridyl(4,4'-bpy) and 4-fluorobenzoic acid(4-HFBA),and characterized by thermal analysis,single-crystal X-ray diffraction and magnetic property.The complex crystallizes in the triclinic system,space group P,Z = 1.Crystal data:C54H44CoF2N8O6,Mr = 997.90,a = 9.134(2),b = 11.555(2),c = 12.867(3) ,α = 66.02(3),β = 77.96(3),= 73.11(3)°,V = 1180.9(4) 3,Dc = 1.403 g/cm3,μ(MoKα) = 0.433 mm-1,F(000) = 517,the final R = 0.0633 and wR = 0.1171 for 2152 observed reflections(I > 2σ(I)).The title complex is assembled into 1D supramolecular chains parallel to [001] based on the adjacent molecular ··· stacking interactions and hydrogen bonds.The variable temperature magnetic measurements show a weak ferromagnetic behavior over 300-160 K followed by antiferromagnetic behavior below 160 K for the title complex.     

A New 3D Supramolecular Network Formed by [Zn_3（2,6-Pyridinedicarboxylate）_3Cl_4]~（4-）and 4-Carboxypyridinium

A new compound [Zn3(C7NO4H3)3Cl4]·[C6NO2H6]4·4H2O (I) has been synthesized and structurally characterized by X-ray crystallography.It crystallizes in monoclinic,space group C2/c with a=16.9018(14),b=12.6902(10),c=25.1170(2),β=90.54°,V=5387.0(8)3,Z=4,Zn3C45H41Cl4N7O24,Mr=1401.76,Dc=1.728 g/cm3,F(000)=2840,μ(MoKa)=1.615 mm-1,the R= 0.0758 and wR=0.2060 for 3468 observed reflections (I 2σ(I)).Analysis of single-crystal X-ray diffraction data shows that compound I displays an interesting example of 3D supramolecular networks with perfect neutral and ionic hydrogen bonding array.     

[Cu(HIm)2(PPh3)2](BF4)的合成与晶体结构

A Cu(Ⅰ) complex with mix ligands [Cu(HIm)₂(PPh₃)₂](BF₄) was synthesized and characterized by elemental analysis, IRspectroscopy and X-ray diffraction crystallography. The crystal belongs to monoclinic system and P2₁/c space group, with cell parameters, a=1.2836(3)nm, b=1.5089(3)nm, c=2.0661(4)nm, α=90°, β=101.464(4)°,γ=90°, V=3.9219(13)nm³, Z=4 and D_c=1.374mg·m^-3. The Cu(Ⅰ) is coordinated by two Patoms from triphenylphosphine and two Natoms from imidazole to form the distorted tetrahedral geometry.     

Synthesis and Crystal Structure of （E）-ethyl 6-benzyl-2-[（cyclopropylmethylamino）（4-fluorophenylamino）-methyleneamino]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate ethanol monosolvate

The crystal structure of the new title compound (E)-ethyl 6-benzyl-2-[(cyclopropylmethylamino)(4-fluorophenylamino)methyleneamino]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate ethanol monosolvate (C28H31FN 4O2S·C2H6O, Mr=552.70) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a=13.806(10), b=10.850(7), c=19.938(14), β=98.842(9)° , V=2951(4)3 , Z=4, Dc=1.244g/cm 3 , F(000)=1176, μ=0.153 mm-1 , MoKα radiation (λ=0.71073), R=0.0758 and wR=0.2234 for 4262 observed reflections with I > 2σ(I). Intramolecular N-H…S and C-H…N interactions as well as intermolecular N-H…O and O-H…N hydrogen bonds help to stabilize the crystal structure. X-ray diffraction analysis reveals that the asymmetric unit contains one title molecule and one ethanol molecule.     

CRYSTAL STRUCTURES OF [Bu4N]2[M2Ag3（ μ3—S）2（μ—S）4S2Et2dtc]（M=W,Mo）

<正> The title compounds were prepared from the reation of (NH4)2MS4 (M=W,Mo),AgNO3,NadtcEt2 and Et4NBr in CH3CN-H2O solution. The isomorphous compounds [Bu4N]2[W2Ag3S8Et2du] ( I ) and [Bu4N]2[Mo2Ag3S8Et2dtc] (Ⅱ) crystallize in triclinic space qroup Pi with the following crystal parameters:α=13. 043(4),b = 21. 640(6),c=10. 757(6)A ,α=95. 09(5),β = 91. 90(4),γ = 98. 57(3)°,Z = 2,V = 2987A3,Dc=1. 76g/cm3 for I 5;a= 12. 989(2) ,b=21. 574 (9) ,c= 10. 7/1(1) A .α= 95. 06(7), β=91. 61(4), γ=98. 52(2)°, Z = 2,V = 2961 A3.Dc= 1. 58g/cm3 for Ⅱ . The final R and Rw values are 0. 061 and 0. 072 for Ⅰ ,and 0. 062 and 0. 076 for Ⅱ The M2Ag3 (M = W, Mo) unit in anion M2Ag3S8Et2dtc forms a five-membered ring.