CRYSTAL STRUCTURE OF {Ni[(C_4H_9O)_2PS_2](C_(12)H_8N_2)_2} -[(C_4H_9O)_2PS_2]

<正> {Ni C(C4H9O)2PS2] (C12H8N2)2} [C(C4H9O)2PS2], Mr= 795. 60, Monocinic,P2,/n,a=16. 806(2), b=12. 720(2), c=21. 248(2) A. β=98. 454(7)°, V = 4493A3,Z=4,Dc= 1. 18g·cm-3,Mo Ka radiation,A=0. 71069A ,F(000) = 1664, R=0. 102 for 4154 reflections with I≥3σ(I).The crystal structure consists of complex cation {NiC(C4H9O)2PS2](C12H8N2)2}+ and complex anion C(C4H9O)2PS2]-. In the cation, nickel (Ⅱ) atom is coordinated by four nitrogen atoms and two sulfur atoms to form a distorted octahedron.     

STRUCTURE OF { CEu_2 (OOCCH_2NHCOCH_2NH_3)_4 (H_2O)_4]·(C1O_4)_6·4H_2O}_n

<正> {[Eu(OOCCH2NHCOCH2NH3)2(H2O)2]·(ClO4)3·2H2O}2,Mr = 1572,P21/n,a=12. 014(4),b=8. 910(5),c=22. 749(5)A ,β=91. 73(3)°,V = 2034 A3,Z=2,Dx=2. 15g·cm-3,λ(MoKa) = 0. 71073A,R=0. 060 for 3107 unique observed reflections (I≥3σ(I)). The complex cation is of one-dimensional chain structure in which the basic unit is a dinuclear complex and the gly-gly ligands are coordinated to metal atoms in two kinds of forms. The overall structure of the dinuclear unit is dioxo and dicarboxyl-bridged.     

CRYSTAL AND MOLECULAR STRUCTURE OF THE HEXANUCLE-AR DIAZENIDO-OXOMOLYBDATE [(n-C_4H_9)_4N]_3[Mo_6O_(18)-(N_2C_6H_3-2,4-(NO_2)_2]

<正> Crystal of the title complex [(n-C4H9)4N]3[Mo6O18(N2C6H3-2,4-(NO2)2](Mr= 1710. 5) is orthorhombic with space group P21cn (Pna21), a = 17. 304(3), b = 17.580(2), c=24. 355(4) (?), V = 7409(2)(?)3, Z = 4, Dc=1. 60g/ cm3, μ=10. 29cm-1, F (000) = 3647. The structural solutions and refinements based on 3900 reflections (I≥3σ(I)) converged at R = 0. 0575, Rw =0. 0498. The atoms of Mo(3), Mo(4), O(1), O(5), O(9), O(11) and the [N2C6H3-2,4-(NO2)2] unit in the complex anion locate approximately in a plane about which the complex anion is nearly symmetrical.     

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,Crystal Structure and Electrochemical Property of a Dinuclear Manganese（Ⅱ） Complex [Mn_2（C_（12）H_8N_2）_4（C_8H_5O_4）_2]（C_8H_4O_4）·H_2O

One dinuclear manganese(II)complex [Mn2(C12H8N2)4(C8H5O4)2](C8H4O4)·H2O has been synthesized with o-phthalic acid and 1,10-phenanthroline.The crystal structure was determined by X-ray diffraction.The crystal belongs to the triclinic system,space group P1 with a = 1.17767(3),b = 1.22292(2),c = 1.35860(3)nm,α = 110.5300(10),β = 97.6140(10),γ = 93.7300(10)o,V = 1.80307(7)nm3,Dc = 1.404 g/cm3,Z = 2,F(000)= 784,the final GOOF = 1.047,R = 0.0398 and wR = 0.1038.The crystal structure of the title complex consists of one [Mn2(C12H8N2)4(C8H5O4)2]2+ cation,one uncoordinate o-phthalate anion(C8H4O4)2-and one uncoordinate water molecule.In [Mn2(C12H8N2)4(C8H5O4)2]2+,the central Mn(II)ion is coordinated by four nitrogen atoms and two oxygen atoms to give a distorted octahedral coordination geometry.The electrochemical property of the title complex was also studied.     

Synthesis,Crystal Structure and Fluorescent and Thermal Stability Properties of the Zinc(Ⅱ) Complex [Zn(C_(15)H_(11)O_3)_2(C_(12)H_8N_2)_2]·5H_2O

A new complex has been synthesized with o-methylbenzoyl-benzoic acid(HL) and 1,10-phenanthroline(phen) in the mixture of water and ethanol. It crystallizes in monoclinic, space group C2/c with a = 13.6328(18), b = 17.7876(18), c = 19.998(2), β = 104.720(4)o, C54H48N4O11Zn, Mr = 994.33, V = 4690.2(9)3, Dc = 1.408 g/cm3, Z = 4, F(000) = 2072, μ(MoKα) = 0.59 mm-1, R = 0.0736 and wR = 0.2029. The crystal structure shows that the zinc ions are coordinated with two oxygen atoms from two HL molecules and four nitrogen atoms from two phen molecules, forming distorted octahedral coordination geometry. The fluorescent and thermal stability properties of the complex are studied. The result shows that it has one fluorescent emission band at around 412 nm. In addition, the complex is stable under 210 ℃.     

CRYSTAL STRUCTURE OF (C_5H_9C_5H_4)_3Er_4(μ_2-Cl)_6(μ_3-Cl)(μ_4-O)-(THF)_3

<正> The crystal of (C5H9C5H4)Er4(μ2-Cl)6(μ3-Cl)(μ4-O)(THF)3 belongs to triclinic space group P1, with a = 11. 909(4), b = 15.343(5), c=15. 619 (4)(?), α=104. 18(2), β=98. 81(3), γ= 111. 06(2)°, V = 2486(1)(?)3, Z = 2, Dc = 2. 07g/cm3, λ(MoKα) = 0.71073(?), μ= 73. 4cm-1, F(000) = 1476, Mr=1549. 25. The structure was solved by Patterson and Fourier techniques and refined by block diagonel least-squares method to final R = 0. 078 and Rw = 0. 084 for 5594 reflections with I≥1. 5σ(I). The results revealed that the complex is composed of four Er atoms bridged by seven Cl and one oxygen atoms with three of the Er atoms bonded each to a cyclopentylcyclopentadienyl group, and one Er atom, bonded to three THF. The Er atoms constitute a pseudo-tetrahedron.     

CRYSTAL STRUCTURE OF CK(C_(12)H_(24)O_6)]_2Pd(SCN)_4(H_2O)

<正> [K(C_12H_24O_6)]_2Pd(SCN)_4(H_2O),MT=963.59,monoclinic, P21/n,a= 11. 075(1),b= 12. 231(1),c= 15. 863(2) A ,β=93. 25(1)°,V=2145. 3A3,Z=2, Dc=1. 492gcm-3,λ(MoKa) = 0. 71073A μ=8. 64cm-1,F(000) = 996,final R=0. 045 for 1835 observable reflections. The Pd2+ ion coordinates with four S atoms from SCN- groups forming a regular square planar configuration. The K+ ion is surrounded by six ether oxygen atoms,one O atom from water molecule coordinated to two K+ions and one N atom from SCN- group to form a distorted hexagonal bipyramid. Two K atoms are linked with one Pd atom by two bridging SCN- groups forming a chain molecular array in the crystal.     

SYNTHESIS AND STRUCTURE OF (Ph_4P)_2[Ni_3(μ-SC_3H_6S)_4]·2CH_3CN

<正> (Ph4P)2[Ni3(u-SC3H6S)4].2CH3CN was obtained from the reaction of NiCl2.6H2O,Na2(1,2-pdt)(pdtH2=CH3CH(SH)CH2SH) and Ph4PBr.Mr=1361. 80, P21/c,a=10.802(2),b=30.111 (7),c=9. 907(3) A ,B=93. 60(3) ;V= 3216. 0 A3;Z=2,Dc=1. 41g/cm3. The three Ni atoms of the anion are linearly arranged and bridged by four sulfur atoms from the four 1 ,2-propyldithiolato ligands.     

Synthesis and Crystal Structure of [Zn(FcCOO)_2(2,2'-bipy)(H_2O)]_2·H_2O

A novel complex [Zn(FcCOO)2(2,2'-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2'-bipy = 2,2'-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) A, α = 90, β = 97.7420(10), γ = 90o, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) A3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I > 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2'-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.     

Synthesis,Structure and Characterization of a New Complex: [Mn(C_6H_(12)N_4)_2(H_2O)_4][Mn(H_2O)_6][SO_4]_2·6H_2O

A novel complex,[Mn(C_6H_(12)N_4)_2(H_2O)_4][Mn(H_2O)_6][SO_4]_2·6H_2O,was synthesized and hexagonal single crystals with centimeter-scale sizes were obtained by the method of solvent evaporation.It was characterized by elemental analysis,infrared spectrum,thermogravimetric analysis and X-ray single-crystal diffraction.The complex belongs to triclinic crystal system,space group P■ with a=9.3390(8),b=13.3520(13),c=16.3207(13)?,α=100.7160(3)°,β=90.1020(10)°,γ=109.9490(5)°,V=1874.9(3)?~3,Z=2,D_c=1.542 g/cm~3,M_r=870.64,μ=0.876 mm~(-1),T=293(2) K,F(000)=916 and S=0.990.The crystal structure determination displayed a distorted octahedral geometry around the manganese atom,which is bound to two nitrogen atoms from hexamethylenetetramine,acting as monodentate ligands,and to four aqua ligands.Variable-temperature magnetic measurements of the complex indicate the presence of weak antiferromagnetic interaction between manganese centers.     

CEYSTAL STRUCTURE OF EXTRACTED COMPLEX OF URANYL CHLORIDE WITH DICYCLOHEXYL-18-CROWN-6(MIXED ISOMERS),UO_2Cl_4]_3 [C_(20)H_(36)O_6- (ISOMER A)-H_3O]_4 [C_(20)H_(36)O_6(ISOMER B)-H_3O]_2

<正> Mr= 3584.7, monoclinic, P21/c, a = 14.647(2), b = 20.333(2), c = 25.759(3) A, β= 91.05(1)°, Z = 2, V = 7670.1 A3, Dc = 1.544 g/cm3,μ=32.629 cm-1, R=0.056 for 4207 observed reflections. Each asymmetric unit consists of two UO2Cl42- complex anions and three C20B36O6-H3O+ complex cations. In two of the complex cations (isosaer A), HaO+ cation is anchored in each crown ether ring by three stronger hydrogen bonds. In another complex cation (isomer B) only two stronger hydronger bonds are formed between the H3O+ cation and crown ether. The third hydrogen bond is very weak.     

Hydrothermal Synthesis and Crystal Structure of a New Zero-dimensional Complex: [Zn(H_2BPTC)(phen)_2]_n·3nH_2O

A new metal-organic coordination complex [Zn(H2BPTC)(phen)2]n·3nH2O (BPTC = 3,3′,4,4′-benzophenone tetracarboxylate, phen = 1,10-phenanthroline) 1 has been obtained from hydrothermal reaction and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. In compound 1, the zinc cation is hexa-coordinated with two carboxylate oxygen atoms from one H2BPTC ligand and four nitrogen atoms from two different phen ligands, showing a slightly distorted octahedral geometry. Crystal data: C41H30N4O12Zn, Mr = 836.06, monoclinic, P21/c, a = 14.2714(9), b = 16.9386(10), c = 15.0151(9) , β = 101.3420(10)o, V = 3558.8(4) 3, Dc = 1.560 g/cm3, μ(MoKα) = 0.766 mm-1, F(000) = 1720, Z = 4, R = 0.0439 and wR = 0.1157 for 4123 observed reflections with I > 2σ(I).     

THE SYNTHESIS AND STRUCTURE OF THE IMIDAZOLATE-BRIDGED HETEROTRINUCLEAR COMPLEX (en)_2Ni[(Im)Co-(NH_3)_5]_2(CIO_4)_6·5H_2O

<正> (H2NC2H4NH2)2Ni [(C3H3N2) Co (NH3)5]2 (CIO4)6 · 5H2O,NiCo2Cl6O29N18C10H62, Mr = 1288. 00, monoclinic, C2/c, a = 31. 832(4), b = 9. 691 (1), c=15. 425(4)(?),β=90. 71(2)°, Z = 4, V = 4758. 0(?)3, Dc=1. 798g/cm3, μ (MoKa) = 15. 22cm-1, F(000)=2656. The three metal nuclei, one Ni( Ⅱ ) and two Co( Ⅲ ), bridged by two imidazolyl anions (Im = C3H3N2), form an isosceles triangle. The Ni( Ⅱ ) atom is situated on the two-fold axis and coordinated by six nitrogen atoms to form a distorted octahedron with two nitrogen atoms from two Im in cis-positions. The two Co( Ⅲ ) atoms are related by C2 symmetry and each Co( Ⅲ ) is coordinated by six nitrogen atoms to form an octahedral configuration.     

CRYSTAL AND MOLECULAR STRUCTURE OF TETRANUCLEAR MOLYBDENUM CLUSTER Mo_4(μ_3-O)_2Cl_2(o-CH_3C_6H_4COO)_6

<正> Cluster compound [Mo4(μ3-O)2O4Cl2(o-CH3C6H4COO)6] has been prepared by the reaction of molybdenum pentachloride and o-methylbenzoic acid. It crystllizes in the orthorhombic space group Praia with cell parameters:Mr= 1361. 6,a=13. 792(4), b=17. 957(3),c= 20. 974(9) A ,V=5194(2) A3,Z= 4,Dc= 1. 74g/cm3,F(000) = 2704,μ(MoKa) = 11. 0/cm. The final R=0. 061 and Rw=0. 064 for 1441(I>3oooooooooo(I)) observed unique reflections. The tetranuclear complex molecule, where the molybdenum atoms are bridged by two μ3-O atoms and six bidentate o-methylbenzoato ligands,is located at crystallographic two-fold axis(x,-1/4,1/4) with one Mo-Mo bond of 2. 610A     

Synthesis and Crystal Structure of [Cu_2(DMF)(H_2O)(C_7H_4NO_4)_2(C_7H_3NO_4)]_2·3.5DMF

A new copper(II) complex [Cu2(DMF)(H2O)(C7H4NO4)2(C7H3NO4)]2·3.5DMF has been synthesized and its structure was determined by single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 10.722(3),b = 18.170(4),c = 20.923(7),α = 105.297(9),β = 101.701(10),γ = 105.74(1)°,V = 3615(1) 3,Z = 2,C58.50H64.50Cu4N11.50O31.50,Mr = 1686.90,Dc = 1.550 g/cm3,μ = 1.255 mm-1,F(000) = 1728.00,T = 150(2) K,the final R = 0.0640 and wR = 0.173 for 11310 observed reflections with I > 2σ(I).In the crystal,each formular unit consists of two dinuclear copper(II) compounds,between which the O-H···O hydrogen bonds exist.Each CuII cation is six-coordinated in an octahedral geometry.The intermolecular hydrogen-bonding interaction leads to a 3-D framework of the title compound.     

CRYSTAL STRUCTURE OF (NH_4)_(11)[Na(H_2O)_2P_4W_(14)O_(58)] ·12H_2O

<正> (NH4)11[Na(H2O)2P4W14O58)·12H2O, Mr = 4099. 39, triclinic, space group P1, a = 14. 376(2), b = 19.861(9), c=13. 010(3)(?) , α=104. 68(2), β=91. 37(1), γ= 104. 05(2)°, V = 3471. 1 (?)3, Z = 2, Dc=3. 922g/cm3, μ (MoKα) = 238. 274cm-1, F(000) = 3664, R = 0.0510, Rw = 0. 0665 for 9260 observed reflections with I> 3σ(I). The polyanion [Na(H2O)2P4W14O58]11- consists of two PW7O29 subunits anisostructurally, two linkage phosphorous atoms and one sodium ion with two water ligands as well. The geometries of tungsten atoms within these two subunits are almost the same as those in K12P4W14O58· 21H2O[2]. The four phosphorous atoms are in PO4 coordinations. The sodium ion locates nearly at the center of the polyanion, and is coordinated by two water molecules, five oxygen atoms of the anion and one phosphorous atom with Na-P = 3. 053(3) (?). Due to the presence of the sodium atom, the interactions between oxygen and tungsten atoms in the polyanion are somewhat weakened.     

Synthesis, Crystal Structure and Electrochemical Properties of One-dimensional Chain Coordination Polymer [Co(II)(C_6H_5CH=CHCOOH)_2(4,4′-bipy)(H_2O)_5]_n

A one-dimensional chain coordination polymer [Co(II)(C6H5CH=CHCOOH)2(4,4′- bipy)(H2O)5]n has been synthesized with cinnamylic acid, 4,4′-bipy and cobaltous chloride as raw materials. Crystal data for this complex: monoclinic, space group P21/c, a = 1.1481(3), b = 1.1230(2), c = 1.1759(3) nm, β = 97.054(4)o, V = 1.5046(6) nm3, Mr= 617.50, Dc = 1.363 g/cm3, Z = 2, μ(MoKα) = 0.627 mm-1, F(000) = 646, S = 1.062, R 0.0443 and wR = 0.1178. The crystal structure shows that two neighboring cobalt(II) ions are linked together by one 4,4′-bipy, and the whole complex molecule adopts a one-dimensional chain structure. Each cobalt(II) ion is coordinated with two nitrogen atoms from two 4,4′-bipy molecules and four oxygen atoms from four water molecules, giving a distorted octahedral coordination geometry. The electrochemical properties were analyzed by combining with the crystal structure.     

Synthesis and Crystal Structure of a New Complex {[Co~(Ⅲ)L_2]·[Co~(Ⅱ)(H_2O)_6]_(0.5)·2.25H_2O}_4 (H_2L = N-(2-Hydroxyphenyl)salicylidenimine)

The reaction of Co(OAc)2·4H2O with the Schiff base H2L in a methanol solution affords the red crystals of {[CoIIIL2]·[CoII(H2O)6]0.5·2.25H2O}4 1 (H2L = N-(2-hydroxyphenyl) sali-cylidenimine). The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n, C104H114Co6N8O37, Mr = 2421.61, a = 10.625(3), b = 16.335(4), c = 15.265(4) , β = 102.990(4)o, V = 2581.6(11) 3, Z = 1, Dc = 1.558 g/cm3, μ = 1.034 mm-1, F(000) = 1252, R = 0.0414 and wR = 0.1167 for 5889 reflections. The Co(III) atom is six-coordinated by two nitrogen atoms and four oxygen atoms of two tridentate L ligands. The abundant hydrogen bonding interactions extend the complex into a one-dimensional supra-molecular framework. The uncoordinated water molecules act as space-fillers and consolidate the whole architecture through the hydrogen bonding interactions.     

Synthesis, Crystal Structure and Luminescent Property of a Novel 1-D Cadmium(II) Complex: [Cd_2(C_8H_3NO_6)_2(H_2O)_4]_n·2nH_2O

A novel one-dimensional chain-like coordination polymer constructed from 3-nitro- benzene-1,2-dicarboxylic acid, [Cd2(C8H3NO6)2(H2O)4]n·2nH2O, has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to monoclinic, space group P21/c with a = 6.1252(8), b = 20.706(3), c = 8.8067(11) , β = 95.608(2)°, V = 1111.6(2) 3, Mr = 751.12, Dc = 2.244 g/cm3, F(000) = 736, μ = 2.011 mm-1, Z = 2, the final R = 0.0262 and wR = 0.0692 for 2338 observed reflections with I > 2σ(I). The structure of the title compound presents a 1-D chain-like structure constructed by dimer units, [Cd2(C8H3NO6)2(H2O)4]n, through two carboxylate oxygen atoms. The fluorescence of the title compound has been also discussed in this paper.