Syntheses and Crystal Structures of Two New Iron-sulfur Carbonyl Complexes: [Fe_2(SC_6H_4Cl)_2(CO)_6]·0.5(Et_2O) and [Fe_3(SC_6H_4NH_2)_6(CO)_6]·2(MeOH)

Two new iron-sulfur carbonyl complexes, [Fe2（SC6H4Cl）2（CO）6]·0.5（Et2O） 1 and [Fe3（SC6H4NH2）6（CO）6]·2（MeOH） 2, have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. Crystal data for 1： monoclinic, C2/c, a = 18.4439（8）, b = 11.0999（5）, c = 25.1830（10）A°, β = 97.0370（10）°, V = 5116.8（4） A°^3, Z = 8, C20H13Cl2Fe2O6.50S2, Mr = 604.02, Dc = 1.568 g/cm^3, μ = 1.540 mm^-1, F（000） = 2424, the final R = 0.0545 and wR = 0.1454 for 3443 observed reflections with I 〉 2σ（I）; 2： monoclinic, P21/n, a = 12.350, b = 26.3050（11）, c = 16.057A°, β = 97.891 （3）°, V = 5166.9（2）A°^3, Z = 4, C44H44Fe3N6O8S6, Mr = 1144.76, Dc = 1.472 g/cm^3, μ = 1.128 mm^-1, F（000） = 2352, the final R = 0.0442 and wR = 0.1197 for 7978 observed reflections with I 〉 2σ（I）. Complex 1 contains one iron dimer, in which two tricarbonyliron（Ⅰ） fragments are bridged together by two 4-chlorophenylthiolate ligands, whereas complex 2 contains a linear tri-iron cluster, in which two terminal tricarbonyliron（Ⅱ） fragments and the central Fe（Ⅱ） atom are linked together by six 4-aminophenylthiolate bridging ligands.

Crystal Structure of Binuclear Bridging Complex[(dppf)_2Pd_2 (Ⅱ) (μ-Cl)_2] [PF_6]_2

The title complex [(dppf)2Pd2 (Ⅱ) (μ-Cl)2] [PF6]2 (C68H56-Fe2Pd2Cl2P6F12, Mr= 1682. 35) has been synthesized, the crystal and molecular struc-ture of the complex has been determined by X-ray diffraction method. The complex istriclinic space group P1 with a= 10. 453(3), b= 12. 918(4), c= 13. 449(4) A; α=86. 42(3), β=75. 57(2), γ=71. 58(3)°, Z= 1, Dc= 1. 68 g/cm3, μ(MoKα) = 12. 5cm-1, F(000) = 844. Final R= 0. 063 (Rw= 0. 082) for 4944 unique reflections with I≥3σ(I). The molecular configuration is centrosymmetric with symmetric double chlo-rine bridges.

Syntheses and Crystal Structures of Two Cyano-bridged Bimetallic Complexes [Ce(DMSO)_4(H_2O)_3Fe(CN)_6]·H_2O and [La(DMSO)_4(H_2O)_3Co(CN)_6]·H_2O(DMSO = Dimethylsulfoxide)

Two new bimetallic cyano-bridged complexes [Ce（DMSO）4（H2O）3Fe（CN）6]·H2O 1 and [La（DMSO）4（H20）3Co（CN）6].H20 2 have been prepared by the ball milling reaction method and structurally characterized by X-ray single-crystal structure analyses. Crystallographic data for 1： C14H32CeFeN6O8S4, Mr= 736.67, monoclinic, space group P2 1/n, a = 14.952（1）, b = 13.7276（9）, c = 15.392（1） A, β= 108.288（1）°, V = 2999.6（4） A3, Z = 4, Dc= 1.631 g/cm^3, g = 2.304 mm^-1, F（000） = 1480, R = 0.0593 and wR = 0.1611; and those for 2： C14H32CoLaN6O8S4, Mr=738.54, monoclinic, space group P21/n, a = 14.945（3）, b = 13.731（3）, c = 15.300（3） A, β= 107.806（1）°, V= 2989.3（11） A^3, Z= 4, Dc = 1.641 g/cm^3, μ = 2.288 mm^-1, F（000） = 1480, R = 0.0383 and wR = 0.1132. In both complexes the lanthanide ion is eight-coordinated in a square antiprism arrangement, and the Fe（Ⅲ） or Co（Ⅲ） ion in a nearly regular octahedral environment The [LnM（CN）6（DMSO）4（H2O）3]·H2O （Ln = Ce and M = Fe for 1; Ln = La and M = Co for 2） species are held together via hydrogen bonds by coordinated water molecules, lattice water molecules and nitrogen atoms of cyanide groups to form a three-dimensional framework.

Synthesis and Crystal Structure of a Dinuclear Cu(II) Complex with Tridentate Schiff Base and Azido Bridge

A new dinuclear copper(II) complex ([Cu(C12H17N2O)(N3)]2, C24H34Cu2N10O2) has been synthesized and characterized by X-ray structure determination. It crystallizes in the monoclinic system, space group P21/c with a = 18.529(4), b = 10.933(2), c = 14.534(3) ?, β = 111.07(3)°, V = 2748(1) ?3, Z = 4, Mr = 621.69, F(000) = 1288, Dc = 1.503 g/cm3 and μ(MoKα) = 1.590 mm?1. The structure was refined to R = 0.0647 and wR = 0.1846 for 4406 observed reflections (I > 2σ(I)). The asymmetric unit comprises two halfmolecules. The complex is a centrosymmetric dimmer in which the copper atoms are penta-coordinated by three coordination atoms from the corresponding tridentate Schiff base ligand and two bridging azide anions. The Cu(II)…Cu(II) average distance is 3.350(1) ?.

Hydrothermal Synthesis, Crystal Structure and Fluorescence Properties of a Three-dimensional Triply-bridged Binuclear Zinc(Ⅱ) Complex [Zn_2(Mba)_3(Phen)_2EtOH)]·ClO_4

The novel complex [Zn2（Mba）3（Phen）2EtOH）]·ClO4 （Hrnba = methoxybenzoic acid, Phen = 1,10-phenanthroline, EtOH = ethanol） was synthesized by hydrothermal reactions, and its structure was determined by X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 1.15362（1）, b = 1.3655（3）, c = 1.61451（1） nm, α= 72.842（2）, β = 83.259（3）, y = 72.083（2）°, V = 2.3112（6） nm3, Z = 2,μ（MoKa） = 11.71 cm-1, F（000） = 1120, R = 0.0552 and wR = 0.1157 （I 〉 2σ（I））. The two centric zinc（H） ions in the complex locate in a distorted octahedral coordination geometry and a distorted trigonal bipyramid coordination geometry, respectively. Two bridging bidentate carboxyl groups and a μ2-O carboxyl group from three methoxybenzoic acids act as the bridge to link two Zn（Ⅱ） ions. The asymmetric units are connected by π-π packing interactions between aromatic rings to form a three-dimensional supramolecular network. The experimental results show a good fluorescence property for the complex.

Hydrothermal Synthesis and Crystal Structure of Binuclear Copper(Ⅱ) Complex Bridged by 1,2,4,5- Benzenetetracarboxylato Trivalent Anion

The title complex [(phen) 2Cu(Htcb)Cu(phen) 2]H 3tcb(tcb=1,2,4,5-benzenetetracarboxylato tetravalent anion; phen=1,10-phenanthroline) was synthesized by the hydrothermal synthesis method. The crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in the triclinic system with space group P1, a=1.04174(8) nm, b=1.07119(8) nm, c=1.26360(10) nm, α=98.169(2)°, β=99.679(10)°, γ=93.658(10)°, V=1.37031(18) nm3, Z=1. The two copper(Ⅱ) cations are bridged by Htcb in the monodentate fashion, and have the same five-coordinated environment completed by the four N atoms from the two phen molecules and one O atom from the carboxylic group of Htcb respectively, which can be best described as distorted trigonal-bipyramid geometry. Moreover, the three dimensional network is formed by H-bonding interactions [O…O distance from 0.2506(10) nm to 0.3176(11) nm] and π-π stacking interactions between the phen rings of adjacent binuclear entities with a face-to-face separation of ca. 0.354 nm.

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 Cyano-bridged Bimetallic Complex[La(betaine)_2(H_2O)_6Fe(CN)_6]·2H_2O

The title complex [La(betaine)2(H2O)6Fe(CN)6]?2H2O (betaine = (CH3)3NCH2CO2) has been synthesized and characterized by X-ray single-crystal structure analysis. The crystal crystallizes in monoclinic, space group P21/n with a = 15.793(5), b = 8.927(3), c = 22.257(7) ?, β = 110.147(5)o, C16H38FeLaN8O12, Mr = 729.31, Z = 4, V = 2946.0(15) ?3, Dc = 1.640 g/m3, μ(MoKα) = 1.988 mm-1, F(000) =1476, R = 0.0388 and wR = 0.0827 for 4237 observed reflections (I > 2σ(I)). The La3+ ion is nine-coordinated by one cyano nitrogen atom and eight oxygen atoms of two betaine and six water molecules. Each complex molecule is connected to form a 3D network structure by some O–H…O and O–H…N hydrogen bonds.

Syntheses and Crystal Structures of Two Cyano-bridged Bimetallic Complexes [Ln(DMSO)_2(H_2O)(μ-CN)_4Fe(CN)_2] (Ln = Ce and Eu, DMSO = Dimethylsulfoxide) with Layered Structure

Two new bimetallic cyano-bridged complexes [Ln（DMSO）2（H2O）（μ-CN）4Fe（CN）2] （Ln = Ce 1, Eu 2） have been prepared by the grinding reaction method and structurally characterized by X-ray single-crystal structure analysis. Crystallographic data for 1： C10H14CeFeN6O3S2, Mr = 526.36, monoclinic, P2/n, a = 7.852（4）, b = 10.729（5）, c = 11.181（5）A,β = 96.992（8）°, V = 935.0（7） A^3, Z = 2, Dc = 1.870 g/cm^3,/1 = 3.421 mm^-1, F（000） = 512, R = 0.0363 and wR = 0.0971; and those for 2： C10H14EuFeN6O3S2, Mr = 538.20, monoclinic, P21n, a = 7.739（5）, b = 10.668（7）, c = 11.008（7） A,β = 96.943（3）°, V = 902.1（11） A^3, Z = 2, Dc = 1.981 g/cm^3,/1 = 4.499 mm^-1, F（000） = 522, R = 0.0345 and wR = 0.0855. In each complex the lanthanide ion is seven-coordinated in a pentagonal bipyramidal arrangement, and the Fe（Ⅲ） ion is in a nearly regular octahedral environment. The title complexes can be described as two- dimensional （2-D） stair-like structures, which are further connected by hydrogen bonds to form three-dimensional （3-D） frameworks.

Synthesis and Crystal Structure of Mercury BridgedBiferrocene Trinuclear Complex Hg(FcL)_2,Bis(S-methyl-N-(1-ferrocenyl-1-methyl)methylenedithiocarbazate)mercury(Ⅱ)

The title complex, mercury bridged biferrocene trinuclear complex Hg(FcL)2. Bis (S-methyl-N- (1-ferrocenyl-1-methyl) methylenedithiocarbazate) mercury,Crystallizes in space group Pbca with a =19. 510 (4), b=19. 921 (5), c=15. 581 (3)A. V=6095(3) A, Z=8,M.=863. 12, Dc=1.881 g/cm3; u=19. 24 cm-1 and F(000) = 3376. The final refinement of 2455 observed reflections is converged with R= 0. 043 and Rw=0.047. X-ray crystal structure analysis revealed that the coordinationgeometry of Hg atom is a distorted tetrahedron with two Hg-N bonds and two Hg- S bonds. The Schiff-base ligand loses a proton from its tautomeric thiol form and is cryordianted to the Hg aotm uia the mercapto sulphur and the β-nitrogen atoms.

Crystal Structure of Bridged Dimer Complex of [Yb (H_2O)) (acac)_2 (Ac)]_2

The title complex C24H38O14Yb2(Mr=896. 62 ) crystallized in orthorhombic system, space group Pbcn with unit cell dimensions a=13. 478 (4), b=16. 161(7), c=15. 110(5); V=3291. 2(2); Z=4; F(000) = 1736; Dc=1. 810g. cm-3;μ= 17. 5 cm-1 (MoKa). The final R and Rw are 0.061 and 0.058 respectively. The title complex is a bridged dimer. The ligands that bridge two Yb(Ⅲ) centerions are the two acetatos in the complex and every Yb(Ⅲ) ion is eight-coordinated, being bonded to one O atom of one H,O molecule, four O atoms of two acetylacetonatos,two O atoms of an acetato and one O atom of another acetato. The coordination polyhedron of the Yb(Ⅲ) ion in the title complex is a dodecahedron.

Synthesis and Crystal Structures of Two Di-Cu(Ⅱ) Complexes Based on an Asymmetric Dinucleating Ligand

Two new dicopper（II） complexes [Cu2L（OAc）2]（ClO4）·H2O （1） and [Cu2L（BPP）2]-（ClO4） （2） using an asymmetric dinucleating ligand HL and auxiliary ligands such as acetate （OAc） and bisphenyl phosphate （BPP） have been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. Complex 1 crystallizes as blue single crystals that belong to the triclinic crystal system and Pī space group, while complex 2 crystallizes in a monoclinic P21/c space group. Single-crystal X-ray diffraction analysis reveals that the two copper ions in complexes 1 and 2 reside within the adjacent ligand compartments and are bridged by the endogenous phenoxo-O from ligand L and the introduction of two desired exogenous carboxylates or phosphates in the bidentate μ-1,3-bridged mode. The coordination geometries of Cu（1） and Cu（2） are both distorted square pyramids.

Synthesis and Crystal Structure of the First Example of a Tris-Chelated Co(II) Complex Based on Oxamide Dioxime Ligand

A new cobalt(II) complex, [Co(H2 oxado)3 ]C2 O4 H2 oxado·2H2 O (H2 oxado = oxamide dioxime), has been synthesized in aqueous solution and characterized by elemental analysis and single crystal X-ray structure determination. The complex crystallizes in the triclinic space group P-1, with the parameters a = 9.46(4), b = 11.84(5), c = 12. 81(5)?&Aring, α = 104.94(6), β = 99.29(5), γ = 106.73(5), V = 1284(9) &Aring3, Z = 2. The central cobalt(II) cation is pseudo-octahedrally coordinated by six imino N atoms of the neutral oxamide dioxime ligand. In the solid state, each of the following bricks, namely the cationic complexes, the oxalate dianions as well as the oxamide dioxime crystallization molecules, pile up parallel to the a axis. The bulk structure is consolidated by an extended three-dimensional network of hydrogen bridgings—that link the ionic partners, oxamide dioxime and water molecules to one another—and by coulombic interactions.

The Assembly and Molecular Structure of a Novel One-dimensionalCyanide-bridged [Ni(pn)_2Ni(CN)_4]_n·nH_2 O Complex

The synthesis, structure and characterization of a new one-dimensional cyanide-bridgedcomplex [Ni(pn)_2Ni(CN)4]n'nH2O (where pn = 1,2-diaminopropane) are described. The structure ofthis complex consists of a one-dimensional polymeric chain-Ni(pn)2-NC-Ni(CN)2-CN-Ni(pn)2- inwhich the Ni(II) centers are linked by two CN groups.

Synthesis and Crystal Structure of an Azide Bridged Binuclear Zinc(Ⅱ) Dimer Containing Taurine Schiff Base [Zn_2(C_8H_9N_2O_3S)_2·(N_3)_2·(H_2O)_2]_2·_2H_2O

The title complex [Zn2L2（N3）2（H2O）2]·2H2O （L = N-（2-pyridylmethylidene） taurine） has been synthesized in a methanol-water solution. The crystal belongs to monoclinic, space group P2 1/C with a = 15.8064（10）, b = 10.5015（5）, c = 17.3193（11） ,A, β= 111.314（2）°, V = 2678.2 （3） ,A ^3 C16H26N10O10S2Zn2, Mr = 713.33, Z = 4, DC = 1.769 g/cm^3, μ = 2.017 mm^-1 and F（000） = 1456. The asymmetric unit consists of two half-molecules of the complex and two water molecules. Four N and two O atoms form the coordination environment of each Zn atom, resulting in a distorted octahedral configuration. The two halves of each independent dimer are related by a crystallographic inversion centre, which lies at the centre of the ring formed by two Zn atoms and the coordinating atoms of the two azide anions. The average separation of Zn（Ⅱ）...Zn（Ⅱ） is 3.322 A. The molecules are linked by O-H...O hydrogen bonds, generating an interesting zigzag infinite chain structure in the ac plane.

One and Two-dimensional Structures of a New Oxamido Copper(II) Complex with Phthalato Bridged

A new o-phthalato-bridged oxamide copper（Ⅱ） complex 1, {[Cu2（oxap）]（pht）. 4H2O}n （oxap=N, N＇-bis（2-aminopropyl）oxamide, pht= phthalate dianion）, has been prepared and structurally characterized. It crystallizes in monoclinic, space group C2/c with a=23.424（4）, h=7.9696（14）, c=15.727（3）A°,β=129.617（2）°, C16H28Cu2N4O10, Mr=563.50, V=2261.6（7） A°, Z=4, Dc=1.655 g/cm^3, μ（MoKα）=1.939 mm^-1, F（000） = 1160, the final R=0.0393 and wR=0.0928 for 1707 observed reflections with I〉2σ（1）. Single-crystal X-ray analysis reveals that 1 displays a one-dimensional zigzag chain structure, in which each Cu（oxap） moiety adopting trans-conformation is connected by ,μ1,6-phthalate anion bridges, and these zigzag chains are further linked by another ,μ1,6-phthalate anion bridge to form a 2D sheet structure. The polar guest water molecules reside in the inter-and intrasheets to stabilize the whole crystal structure.

A Novel 3D Heterobimetallic Cyano-bridged Coor- dination Polymer {(NH_4)_2[Cd(H_2O)Fe(CN)_6]}_n:Synthesis and Crystal Structure

A novel heterobimetaUic coordination polymer, {（NH4）2[Cd（H20）Fe（CN）6]}n 1, has been synthesized by using the slow diffusion method and structurally characterized by elemental analysis, 1R spectroscopy and single-crystal X-ray diffraction. The crystal crystallizes in the monoclinic system, space group P21/n, a = 7.4202（16）, b = 14.939（3）, c = 10.868（2） A and ,8 = 91.660（3）°. For 1, five CN groups of Fe（CN）6]4- are involved in bridging. The polymer displays a 3D open microporous framework with 5-connected uninodal （46.64） topology.

Synthesis and Structural Characterization of a Cyano-bridged Dinuclear Neodymium(III)-iron(III) Complex [Nd(DMSO)_5(H_2O)_2](μ-CN)[Fe(CN)_5]

A new neodymiumIII-ironIII complex [Nd(DMSO)5(H2O)2](μ-CN)[Fe(CN)5] (DMSO = dimethyl sulfoxide) has been synthesized by the grinding reaction method. The crystal belongs to monoclinic, space group P21/m with a = 8.859(4), b = 13.684(5), c = 12.290(4) ?, ?= 91.85(2)o, C16H34FeN6NdO7S5, Mr= 782.88, V = 1489(1) ?3, Z = 2, Dc = 1.746 g/cm3, S = 0.906, μ(MoKa) = 2.606 mm-1, F(000) = 788, R = 0.0646 and wR = 0.1654. The slightly distorted square-antiprism eightfold-coordinated Nd(III) and approximately oriented octahedrally sixfold- coordinated Fe(III) are linked by a cyano-bridge group to construct a dinuclear compound. The [Nd(DMSO)5(H2O)2](μ-CN)[Fe(CN)5] species are held together via hydrogen bonds to form a three-dimensional framework.

Synethesis and Crystal Structure of Bi(ethylenediamine)copper Tetracyanonickelate(II)

The crystal structure of the title compound C 8H 16 CuN 8Ni has been determined by single crystal X ray diffraction. The crystal is triclinic with space group P1, a=6.494(3), b=7.270(4), c=7.936(5) , α=106.67(3), β=91.33(4), γ=106.80(6)°, V=341.3(3) 3, Z=1, M r=346.54, F(000)=177, μ =2\^933mm -1 , D c =1.686 Mg/m 3. The final R factor is 0.0603 for 1214 unique observed reflections 〔 I≥2σ(I) 〕. The structure consists of 〔Cu(en) 2〕 2+ (en=ethylenediamine) cations and 〔Ni(CN) 4〕 2- anions linked together by two of the CN groups (the remaining two act as unidentate ligands) to form infinite chains, in the chain, the hydrogen bonds of N(4)…H-N(5) exist,with distance 3.148 , at the same time the hydrogen bonds of N(4)…H-N(7a) and N(5)-H…N(1a) (a: x-1,y-1,z-1 ) between the interchains also exist, with distances of 3.160 and 3.124 , so it forms a three\|dimensional structure of the title compound.

Synthesis and Crystal Structure of 1D Chloride Bridged Cadmium(Ⅱ) Chain

Hydrothermal reaction of 1,10-phenanthroline with CdCl2·2.5H2O in aqueous solution leads to the complex of [Cd(μ-Cl)2(phen)]n (phen = 1-10-phenanthroline). The crystal structure has been determined by X-ray analysis. It crystallizes in monoclinic with space group C2/c, a = 16.947(3), b = 10.529(2), c = 7.235(1) , β = 110.795(3)°, V = 1208.8(3) 3, Z = 4, Dc = 1.997 g.cm-3, μ= 2.22 mm-1, F(000) = 704, R = 0.0231, Rw = 0.0626 for 1194 reflections with I > 2σ (I). In the crystal structure, the [Cd(phen)]2+ units are bridged by chloride ions to form 1D chain. The 1D chains combine through π……π interactions of phen groups to form 2D infinite molecular zipper.