SYNTHESIS AND MOLECULAR STRUCTURE OF NOVEL BINUCLEAR COBALT COMPLEX WITH MIXED VALENCE STATE Co(Ⅰ)Co(Ⅱ) (μ-Ph_2Ppy)_2(μ-CO)_2Cl_3

A novel binuclear cobalt complex with mixed valence state Co(Ⅰ)Co(Ⅱ)(μ-Ph_2Ppy)_2(μ-CO)_2Cl_3 has been prepared, Ph_2Ppy=2-(diphenyl phosphino)pyridine, and its molecular structure determined by using 3569 independent reflections. The complex was crystallized in the orthorhomblc space group P2_1nb with a=13.32(1), b=14.31(1),c=18.94(2) and Z=4. The structure was solved by direct method and full-matrix least squares refinement carried out. The final R value is 0.072.If the Co-Co bond is not taken into account, two cobalt atoms exhibit a five-coordlnate reformed trigonal bipyramid configuration (formal oxidation state +1) and a six-coordinate reformed octahedral configuration (formal oxidation state +2), respectively. The Co-Co distance is 2.685(1). The molecule belongs to the C_(2v), point group. A new W-frame compound with mixed valence state Co(0)Co(Ⅰ)(μ-Ph_2Ppy)_2(μ-CO)(CO)Cl can be formed by reducing this complex.     

THE CRYSTAL STRUCTURE OF [Co(TPPO)_4][Co (NCS)_3TPPO]_2

The title complex [Co(TPPO)_4] [Co(NCS)_2TPPO]_2 (TPPO=triphenylphosphine oside) was prepared by solvent evaporation method. Its crystal structure was determined by x-ray diffraction method. The crystal is rhombohedral with space group R3. The unit cell parameters are presented and the structure has been refined to a final R of 0.064.     

Synthesis and crystal structure of a novel two-dimensional network complex [Mn(O_2CCH_2Cl)_2(phen)]_n

A novel two-dimensional network manganese(Ⅱ) polymer complex [Mn(O2CCH2CI)2-(phen)]n has been synthesized and characterized by elemental analysis and IR spectrum. The crystal structure of title complex has also been determined, which is in monoclinic of a space group P21/c with the following unit cell parameters at 294K: a =1.9738(4) nm, b =1.1384(2) nm, c =0.74915(14) nm, V=1.6795(5) nm3, Z= 2.     

Hydrothermal Synthesis and Crystal Structure of a Novel Dinuclear Co(Ⅱ) Complex:[Co2(2,2'-bpy)_2(μ-L)_2(L)_2(μ-H_2O)](HL=4-Chlorobenzoic Acid)

A new 4-chlorobenzoic acid bridge Co(Ⅱ) complex [Co2(2,2'-bpy)2(μ-L)2(L)2(μ-H2O)] (HL=4-chlorobenzoic acid) has been obtained by hydrothermal synthesis,and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system,space group C2/c with a=22.537(5),b=16.212(3),c=15.306(3) ,β=124.37(3)°,V=4616.1(16) 3,Mr=1070.45,Dc=1.540 g/cm3,Z=4,μ=1.012 mm-1,F(000)=2176,the final R=0.0338 and wR=0.0810. The title complex is composed of dinuclear [Co2(2,2'-bpy)2(μ-L)2(L)2(μ-H2O)] molecules. Each Co(Ⅱ) atom is coordinated by two nitrogen atoms from one 2,2'-bipyridine ligand,three oxygen atoms from three 4-chlorobenzoic ions and another oxygen atom from one water molecule. The two Co(Ⅱ) atoms are connected by two 4-chlorobenzoic ions and one bridged water molecule. The dinuclear molecules are interlinked by hydrogen bond and π-π stacking interactions into a three-dimensional supramolecular network.     

咪唑配合物[Co(C3H4N2)6](PhCHCHCOO)2的合成及晶体结构

The complex [Co(Im)6](Cin)2 (Im=imidazole,Cin=cinnamate) was prepared by reaction of Co(PhCHCHCOO)2 with imidazole in ethanol. It has been determined by single crystal X-ray analyses. The crystals are triclinic, space group P, with a=9.7601(3),b=10.5935(3),c=11.3269(2)(A),α =69.948(1),β =71.027(1),γ =62.803(1)°, and Z=1. The crystal structure of the title complex consists of monomeric [Co(Im)6]2+ cations and cinnamate anions in which the cobalt(Ⅱ) ion assumes a centrosymmetric octahedral geometry with the CoN6 chromophore. In the solid state, the complex forms a three dimensional network through N-H… O hydrogen bonds, the intermolecular hydrogen bonds connect the [Co(Im)6]2+ cations and cinnamate anions.The cinnamate anions are nearly planar.     

Synthesis,Structure, and Luminescent Property of a 3-D Strontium Complex [Sr_3(pda)_2(Hpda)_2(H2O)_2]_n·2nH_2O

The title complex [Sr3(pda)2(Hpda)2(H2O)2]n·2nH2O(H2pda = pyridine-2,6-dicar- boxylic acid) has been prepared under solvothermal conditions. It has been characterized by X-ray single-crystal diffraction, IR and elemental analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 10.3795(8), b = 9.2225(7), c = 18.5726(14) , β = 104.377(2)o, V = 1722.2(2) 3, C28H22N4O20Sr3, Mr = 997.36, Z = 2, Dc = 1.923 g/cm3, μ = 4.722 mm-1, F(000) = 984, the final R = 0.0269 and wR = 0.0538. This complex possesses a 3-D structure which is constructed from 1-D chain motifs linked by carboxylate groups. The luminescent property of the title complex has been investigated.     

Synthesis, Crystal Structure and Properties of a Dinuclear Cobalt（II） Complex [Co2（a-furacrylato）4（Phen）2（H2O）]·C2H5OH

A dinuclear cobalt(Ⅱ) complex [Co2(α-furacrylato)4(Phen)2(H2O)]·C2H5OH has been synthesized with α-furacrylic acid and 1,10-phenanthroline as the ligands, and its crystal structure was determined. The crystal is of monoclinic system, space group C2/c with a=1.07388(8), b=2.4300(2), c=1.86708(14)nm, β=104.3830(10)o, V=4.719.4(7) nm3 , Dc=1.503 g/cm3 , Z=2, F(000)=2196, GOOF=1.053, the final R=0.0343 and wR=0.0883. The crystal structure shows that two neighboring cobalt(Ⅱ) ions are linked by the bridging coordination of two α-furacrylic acid anions and one water molecule, and their end positions are respectively coordinated with two 1,10-phenanthroline molecules and two α-furacrylic acid anions, forming a dinuclear structure. Both cobalt(Ⅱ) ions adopt hexa-coordinated distorted octahedral geometry. The electrochemical and fluorescence properties of the title complex are also discussed.     

Synthesis and crystal structure of [Co(mpt)_2{P(OCH_3)_3}_2]BF_4 (Hmpt = 2-mercaptothiazoline)

The monomeric cobalt-phosphite-thiolato complex [ Co (mpt)2 {P (OCH3 )3 }2 ] BF4 (Hmpt = 2-mercaptothiazoline) has been prepared and characterized by X-ray crystallography. The complex crystallizes in the monoclinic space group C2/c with a= 0.8078(5), b=2.6020(18), c=1.2191(7) nm, β= 99.38 (1)°, V= 2.528(3) nm3, and Z = 4. The structure comprises discrete cations [Co(mpt)2{P(OCH3)3}2.] and anions BF4- , in which the cobalt (Ⅲ) atom is coordinated to two chelate mpt- and two as-oriented monodentate P(OCH3)3 ligands in a highly distorted octahedral geometry. The most distorted angles are S(2)-Co(1)-S(2a) of 162.23(10)° and N(1)-Co(1)-S(2) of 71. 47 (13)°, the latter is caused by the geometric constraint of the bidentate ligand mpt- . Cyclic voltammetry has been used to study the electrochemical behavior of the title complex on the R electrode in MeCN solution with 0.1 mol·L-1 of Bun4NBF4 as electrolyte. The results indicate that the title complex is unstable in MeCN.     

Synthesis and Structural Characterization of Co( Ⅱ ) Coordination Polymer [Co(μ-phth)(imi)2]n

A new cobalt( Ⅱ ) complex [Co(μ-phth)(imi)2]n (phth = o-phthalato, imi = imidazole)has been synthesized by the reaction of CoCl2 with disodium o-phthalate and imidazole. The crystal structure of the compound has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group Pn with a = 8.405(1), b = 9.995(1), c = 9.996(2) (A),β= 104.479(2),V= 813.0(2) (A)3, Dc= 1.467 g/cm3, C14H12N4O4Co, Mr= 359.21, F(000) = 366,μ = 1.079 mm-1, Z = 2, R = 0.0483 and wR = 0.1209 for 1583 observed reflections (Ⅰ＞ 2σ(Ⅰ)). In the title complex, the Co(Ⅱ) ions are bridged by o-phthalate ligands in a bidentate mode, producing a zigzag infinite chain structure. Each four-coordinated cobalt( Ⅱ ) center was coordinated by two oxygen atoms and two nitrogen atoms to give a distorted tetrahedral geometry. The chains are linked by hydrogen bonds between oxygen atoms belonging to carboxylate groups and hydrogen atoms of imidazole molecules, forming an unusual two-dimensional coordination polymer.     

Hydrothermal Synthesis,Crystal Structure and Thermal Stability Properties of the Complex [Cd_2(phen)_2(C_(14)H_(11)O_3)_4(CH_3CH_2OH)]·(CH_3OH)·(H_2O)

A dinuclear cadmium complex [Cd2(phen)2(C14H11O3)4(CH3CH2OH)]·(CH3OH)·(H2O) has been synthesized with benzilic acid and 1,10-phenanthroline by hydrothermal method.The crystal structure was determined by X-ray diffraction with crystal parameters as follows:triclinic system with space group P1,a = 1.21298(10),b = 1.32586(11),c = 2.4815(2) nm,α = 76.2630(10),β = 81.4500(10),γ = 69.1700(10)o,V = 3.6143(5) nm3,Dc = 1.438 g/cm3,Z = 1,F(000) = 1600,the final GOOF = 0.937,R = 0.0521 and wR = 0.1328.In the title complex,the dinuclear structure is defined by carboxyl oxygen atoms adopting a monodentate bridged coordination mode.The coordination environment of Cd(Ⅱ) ion is CdO4N2,giving a distorted octahedral coordination geometry.TG analysis shows that the title complex is stable under 140 ℃.     

Antitumor Metallothiosemicarbazonate:Synthesis,Crystal Structure,Spectra and Antitumor Studies of Co(Ⅲ) Complex with Thiosemicarbazone Derivative of 2-Benzoylpyridine

The title complex Co(L)2Cl·4H2O I has been achieved via self-assembly by incorporating cobalt into 2-benzoylpyridine thiosemicarbazonate ligand, and characterized by elemental analysis, infrared spectra, mass spectra and single-crystal X-ray diffraction study. The crystal crystallizes in monoclinic, space group P21/n, with a=10.227(3), b=17.363(4), c=17.459(4), β=100.408(4)o, V=3049.2(13)3, Z=4, Mr=677.08, Dc=1.475 g/cm3, μ(MoKα)=0.834 mm-1, F(000)=1400, the final R=0.0747 and wR=0.0896 for 1663 observed reflections with I > 2σ(I). The complex contains one six-coordinated cobalt ion connected by two thiosemicarbazone ligands which act as a tridentate ligand to coordinate with the center metal atoms via two pyridyl nitrogen atoms, two imine nitrogen atoms and two sulfur atoms giving rise to a mononuclear structure. Hydrogen bonds existing in the complex link the different com-ponents to stabilize the crystal structure. The antitumor activity of the title complex was tested against A549 lung cancer cell line. Complex I exhibits antitumor activity.     

SYNTHESIS, CHARACTERIZATION AND STRUCTURE OF [Co(DBP)_2·3Py]_2·2CHCl_3

The mixed ligand complex of cobalt with dibutylphosphate (HDBP) and pyridine has been synthesized. Elemental analysis yields the result that the formula of this compound is Co(DBP)_2·3Py·CHCl_3 (Py=pyridine). The thermal analsyis, visible spectra and magnetic properties of it have been studied as well. Single crystal structural analysis shows that the crystal is triclinic with space group P and the unit cell parameters are as follows:a=14.490(10), α=90.37(4)°,b=15.721(7), β=96.04(5)°,c=20.109(12), γ=105.63(4)°.The final R factor is 0.0773. Two Co atoms are connected by two bridging DBP groups to form a dinuclear molecule [Co(DBP)_2·3Py]_2 which has a C_s, symmetry. Each cell contains two dinuclear molecules and four chloroform molecules. The cobalt is coordinated in an octahedral arrangement by three oxygen atoms and three nitrogen atoms, of which one oxygen atom comes from a monodentate DBP group, two oxygen atoms from two bridging DBP groups, and the three nitrogen atoms from the three pyridi     

Hydrothermal Synthesis and Crystal Structure of a Novel Dinuclear Co(Ⅱ) Complex: [Co2(2,2(')-bpy)2((-L)2(L)2(μ-H2O)] (HL = 4-Chlorobenzoic Acid)

A new 4-chlorobenzoic acid bridge Co(Ⅱ) complex [Co2(2,2(')-bpy)2(μ-L)2(L)2(μ- H2O)] (HL = 4-chlorobenzoic acid) has been obtained by hydrothermal synthesis, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group C2/c with a = 22.537(5), b = 16.212(3),c = 15.306(3)(A), β= 124.37(3)°, V = 4616.1(16) (A)3, Mr = 1070.45, Dc = 1.540 g/cm3, Z = 4, μ = 1.012 mm-1, F(000) = 2176, the final R = 0.0338 and Wr = 0.0810. The title complex is composed of dinuclear [Co2(2,2(')-bpy)2(μ-L)2(L)2(μ-H2O)] molecules. Each Co(Ⅱ) atom is coordinated by two nitrogen atoms from one 2,2'-bipyridine ligand, three oxygen atoms from three 4-chlorobenzoic ions and another oxygen atom from one water molecule. The two Co(Ⅱ) atoms are connected by two 4-chlorobenzoic ions and one bridged water molecule. The dinuclear molecules are interlinked by hydrogen bond and π-π stacking interactions into a three-dimensional supramolecular network.     

Crystal structure and fluorescence spectrum of the complex [Eu(Ⅲ)(TTA)_3(phen)]

The title complex Eu(Ⅲ)(TTA)3(phen) (where TTA= thenoyltrifluoroacetone monoanion; phen = 1,10-phenanthroline) has been synthesized in mixed solvents of acetone and ethanol (1:1 volume ratio) and its crystal structure has been determined by X-ray diffraction. The complex crystals are triclinic, space group P1(#2) with cell dimensions of a = 1.3241 (2) nm, 6 = 1.5278(4) nm, c = 0.9755(3) nm, α = 92.49 (2)°, β=102.57(2)°, γ = 91.62(2)°, V=1.9268(8) nm3, Z = 2, μ(Mo Kα) = 18.77 cm-1, Dx = 1.720 g/cm3. The coordination geometry of Eu atom is a distorted square antiprism, and the encapsulated structure that can meet the structural requirement of the typical europium luminescent sensor. The fluorescence spectrum suggests that the complex is a strong photoluminescent material.     

阶梯状配位聚合物[Cu(μ_3-I)INH]_n的合成、晶体结构及其热稳定性研究

The complex [Cu( μ3-I)INH]n has been synthesized in DMF solution with INH, CuI, where INH=isoniazid. The crystal structure of the complex has been determined by X-ray diffraction single crystal structure analysis. The crystal belong to monoclinic system, space group P21/c. The cell parameters are: a=1.009 48(10) nm, b=0.467 51(5) nm, c=1.992 62(19) nm, β=101.413 0(10)°, and V= 0.921 81(16) nm3, Z=4, μ(Mo Kα)=5.674 mm-1, F(000)=616.0, R1=0.031 6, wR2=0.082 5 [I2σ(I)]. The copper(Ⅰ) atom locates in a distorted coordination tetrahedron. The copper(Ⅰ) atoms bridged by μ3-I to form a band stair-like chain, and INH occupying the remaining coordination site of the approximately tetrahedral. The stair-like chains extend along b axis. The results of TG analysis show the title complex was stable under 200℃.     

杂-双核配合物[CaCu(C3H2O4)2(H2O)4]n的合成、晶体结构及热稳定性

The title complex, [CaCu(C3H2O4)2(H2O)4]n, with a formula of C6H12CaCuO12 and Mr=379.78 has been sy-nthesized and characterized by single crystal X-ray diffraction structure analysis, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is Orthorhombic, space group Pbcn with a=0.669 21(5) nm, b=1.370 23(5) nm, c=1.322 39(10) nm, V=1.212 59(16) nm3, Dc=2.080 g·cm-3, μ=2.288 mm-1, F(000)=772 and Z=4. The final R=0.054 0 and wR=0.112 8 for 1 189 observed reflections with I>2σ(I). The structure of the title complex consists of CaO8 polyhedra and CuO6 elongated octahedra linked together by malonate ligands. The Ca(Ⅱ) cation, on a twofold axis, is coordinated by two water molecules and six malonate O atoms. The Cu(Ⅱ) cation, which lies in a centre of symmetry in an octahedral arrangement, is coordinated by four malonate O atoms and two water molecules. The structure comprises alternating layers along the [101] plane, with the shortest Cu…Cu distance of 0.762 46(6) nm. The whole 3D structure is maintained and stabilized by the presence of hydrogen bonds. Its thermo gravimetric analysis was determined by TG-DTG techniques. CCDC:663184.     

CRYSTAL STRUCTURE OF [(C_4H_9)_4N][O_2Mo~(VI)S_2Cu~Itu](tu=(NH_2)_2CS)

<正> Crystal and molecular structure of [(C4H9)4N][O2MoS2Cutu] (tu-thiourea) has been determined by X-ray diffraction technique. The crystal is monoclinic, space group P21/n, with a = 11.871(4), b=13.920(2), c= 15.814(11)A;β= 90.22(4)°,V=2613.2A3,Z = 4, DC= 1.459, Do = 1.46g/cm3. The final R and Rw are 0.049 and 0.056, respectively. The title complex has a rhombic planar MoCu(μ-S)2 core with Mo-Cu distance of 2.647A.The Ho atom is tetrahedrally coordinated by two 0 atoms and two u-S atoms. The Cu-S(tu) bond length of 2.191 A is significantly shorter than the Cu-S(bridge) in analogues.     

CRYSTAL STRUCTURE OF A HETERONUCLEAR LANTHANIDE COMPLEX OF ERBIUM-YTTRIUM AND GLYCINE[ErY(GlY)_6(H_2O)_4](ClO_4)_65H_2O

The title complex [ErY(Gly)_6(H_2O)_4](ClO_4)_6 5H_2O has been synthesized.Its crystalstructure has been determined by X-ray diffraction method.The crystal is triclinic with space groupP1.The unit cell parameters are as follows:a=11.518(4),b=14.105(7),c=15.530(6) ,α=96.61(3),β=102.74(3),γ=105.70(3)°,V=2327.7(17) ~3,Z=2,Dc=2.091g/cm~3.The structure has been refinedto a final R of 0.0785.The crystal is an infinite chain complex,in which four carboxyl groups fromglycine molecules bridge the Er(Ⅲ)and Y(Ⅲ)ion,other two carboxyl groups bridge two adjacentEr(Ⅲ)or two Y(Ⅲ)ions.     

Synthesis and Crystal Structure of a New Charge-assisted Hydrogen-bonded Host Framework [Co(en)_3]_2[Zr_2(C_2O_4)_7]·2H_2O

Using the deep eutectic solvent formed of oxalic acid and choline chloride, a new charge-assisted hydrogen-bonded host framework [Co(en)3]2[Zr2(C2O4)7]·2H2O(1) has been obtained. The title complex crystallizes in the monoclinic, space group P21/n(No. 14) with a = 7.7448(10), b = 14.5683(19), c = 19.375(3), β = 92.124(2)o, V = 2184.5(5) 3, Z = 4, Dc = 1.996 g.cm-3, F(000) = 1332, μ = 1.328 mm-1, R = 0.0353 and w R = 0.0718(Ⅰ 2σ(Ⅰ)). Single-crystal structure analysis reveals that the title complex possesses a 3D network assembled through a multitude of charge-assisted hydrogen bonds between the in situ generated anionic coordination complexes [Zr2(C2O4)7]6- and metal complexes Co(en)33+.     

Synthesis,Crystal Structure and Photoluminescence of [Gd(C_6NO_2H_5)_3-(H_2O)_2]_(2n)·(nH_5O_2)(nHgCl_5)(2nHgCl_4)·(2nH_2O)

A heterometallic 4f-5d inorganic-organic metal-isonicotinato hybrid Gd(C6NO2H5)3-(H2O)22n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O) 1 has been synthesized via hydrothermal reaction and structurally characterized.Complex 1 crystallizes in the space group C2/c of monoclinic system with four formula units in a cell:a=24.234(8)=b=20.816(7)=c=15.333(3)=β=128.091(8)°=V=6088(3)3=C36H47Cl13Gd2Hg3N6O20=Mr=2260.92=Dc=2.467 g/cm3=S=0.896=μ(MoKα)=10.331 mm-1=F(000)=4216=R=0.0344 and wR=0.0629.The crystal structure analysis reveals that the title complex is characteristic of a one-dimensional chain-like structure.Photoluminescent investigation reveals that the title complex displays a broad and intense emission in the green region.