Synthesis and Crystal Structure of an Ionic Compound [Fe(CN)_6(phCH_2NC_5H_5)3]·(H_2O)_4

A novel ionic compound [Fe(CN)6(phCH2NC5H5)3]·(H2O)4(Mr = 794.71) has been synthesized and its structure was characterized by IR, elemental analysis and X-ray diffraction. The compound crystallizes in monoclinic, space group P21/c with a = 10.837(2), b = 16.551(3), c = 23.402(5) , β = 97.531(4)o, V = 4161.0(15) A3, Z = 4, Dc = 1.269 g/cm3, F(000) = 1668, μ = 0.414 mm-1, R = 0.0479 and wR = 0.1232. The building unit of the title compound consists of three (phCH2N+C5H5) ions, one [Fe(CN)6]3- anion and four water molecules. According to the structural analysis, [Fe(CN)6]3- are linked together by O–H···N and O–H···O hydrogen bonds, but [Fe(CN)6]3- and [(phCH2N+C5H5)3] ions are bound by electrostatic force to form an ionic compound.     

Synthesis and Crystal Structure of an Ionic Compound [Fe（CN）6·（PhCHeNC9H7）4]·12H2O

A novel ionic compound [Fe（CN）6·（PhCHeNC9H7）4]·12H2O
（C70H80FeN10O12, Mr = 1309.29） has been synthesized and its structure was characterized by I-R, elemental analysis and X-ray diffraction. The compound crystaUizes in triclinic, space group P1, with a = 10.968（7）, b = 11.466（7）, c = 14.077（8）A, α= 87.014（7）, β= 78.124（7）, γ = 72.708（7）°, V = 1654.1（17）A3, Z = 1, Dc = 1.314 g·cm^-3, F（000） = 692, p = 0.298 mm^-1, the final R = 0.0519 and wR = 0.1355. The building unit of the title compound consists of four （PhCH2N＋C9H7） ions, one [Fe（CN）6]4- anion, and a dozen water molecules. According to the structural analysis, [Fe（CN）6]4- ions are linked together by O-H…O and O-H…N hydrogen bonds, while （PhCH2N＋C9HT） and [Fe（CN）6]4- ions interact with each other by electrostatic force to form an ionic compound.     

Synthesis and Crystal Structure of an Ionic Compound [Fe(CN)_6·(PhCH_2NC_9H_7)_4]·12H_2O

A novel ionic compound [Fe(CN)6(PhCH2NC9H7)4]·12H2O (C70H80FeN10O12, Mr = 1309.29) has been synthesized and its structure was characterized by IR, elemental analysis and X-ray diffraction. The compound crystallizes in triclinic, space group P1, with a = 10.968(7), b = 11.466(7), c = 14.077(8) , α = 87.014(7), β = 78.124(7), γ = 72.708(7)o, V = 1654.1(17) 3, Z = 1, Dc = 1.314 g·cm–3, F(000) = 692, μ = 0.298 mm–1, the final R = 0.0519 and wR = 0.1355. The building unit of the title compound consists of four (PhCH2N+C9H7) ions, one [Fe(CN)6]4– anion, and a dozen water molecules. According to the structural analysis, [Fe(CN)6]4– ions are linked together by O–H···O and O–H···N hydrogen bonds, while (PhCH2N+C9H7) and [Fe(CN)6]4– ions interact with each other by electrostatic force to form an ionic compound.     

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]~(2 )·[SbCl_5]~(2-)}_2

A new supramolecular compound,{[2-(2-pyridyl)benzimidazoleH2]2 ·[SbCl5]2-}2,was synthesized by the hydrothermal reaction of o-diaminobenzene,2-pyridinecarboxylic acid and SbCl3 in 1:1 HCl solution,and characterized by chemical analysis,elemental analysis,IR spectra,thermogravimetric analysis and fluorescence spectra. The crystal structure was deter-mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system,space group P21/c,with a=16.0397(13),b=14.3189(12),c=15.6370(13),β=105.8980(10)°,V=3454.0(5)3,Z=4,C24H22Cl10N6Sb2,Mr=992.48,Dc=1.909 g/cm3,μ=2.366 mm-1,S=1.010,F(000)=1920,R=0.0254 and wR=0.0555. The coordination anion,[SbCl5]2-which is a distorted tetragonal pyramid,is composed by coordinating action with Sb3 ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2-form a biquaternion ring structure through the secondary bonding of Sb···Cl. Moreover,the compound adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-(2-pyridyl)benzimidazole divalent cations. The title compound also shows good fluorescent behaviors.     

Synthesis and Crystal Structure of a Bimetallic Cyanide-bridged Complex Derived from Manganese(Ⅲ) Schiff-base Complex and Pentacyanidonitrosylferrate(Ⅱ) Building Blocks

A new cyanide-bridged bimetallic assembly [Mn(3-meosalpn)(H2O)]2[Fe(CN)5NO](1) was obtained by the reaction of [Fe(CN)5NO]2-with [Mn(3-meosalpn)]+,and characterized by elemental analysis,IR and single-crystal X-ray structure analysis.The complex crystallizes in the monoclinic system,space group P21/c with a = 12.992(5),b = 13.274(6),c = 14.644(6) ,β = 115.198(4)o,V = 2285.2(16)3,Z = 2,C43H44FeMn2N10O11,Mr = 1042.61,Dc = 1.515 g/cm3,F(000) = 1072,μ = 0.928 mm-1,S = 1.052,the final R = 0.0347 and wR = 0.0957 for 17377 observed reflections(Ⅰ 2σ(Ⅰ)).X-ray single-crystal diffraction analysis reveals that 1 has a trinuclear molecular structure,in which the two [Mn(3-meosalpn)(H2O)]+ cations are linked by the central [Fe(CN)5NO]2-anion via two trans CN-groups.Furthermore,the two [Mn(3-meo-salpn)(H2O)]+ cations and [Fe(CN)5NO]2-anion are connected into a one-dimensional zigzag chain through hydrogen bonding interactions.     

Hydrothermal Synthesis, Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH2]2+·[SbCl5]2-}2

A new supramolecular compound, {[2-(2-pyridyl)benzimidazoleH2]2 ·[SbCl5]2-}2, was synthesized by the hydrothermal reaction of o-diaminobenzene, 2-pyridinecarboxylic acid and SbCl3 in 1:1 HCl solution, and characterized by chemical analysis, elemental analysis, IR spectra, thermogravimetric analysis and fluorescence spectra. The crystal structure was deter- mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c, with a = 16.0397(13), b = 14.3189(12), c = 15.6370(13) (A), β = 105.8980(10)°, V = 3454.0(5) (A)3, Z = 4, C24H22Cl10N6Sb2, Mr = 992.48, Dc = 1.909 g/cm3, μ = 2.366 mm-1, S = 1.010, F(000) = 1920, R = 0.0254 and wR = 0.0555. The coordination anion, [SbCl5]2- which is a distorted tetragonal pyramid, is composed by coordinating action with Sb3 ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2- form a biquaternion ring structure through the secondary bonding of Sb…C1.Moreover,the compund adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-(2-pyridy1)benzimidazole divalent cations.The title compound also shows godd fluorescent behaviors.     

Synthesis, Crystal Structure and Characterization of α-（1-Benzimidazolyl） -hypnone Cobalt（Ⅱ） Complex： [CoCl （ C7H5N2CH2COPh）4] Br

The crystal structure of [CoCl ( C7H5N2CH2COPh)4] Br has been determined by means of X-ray crystallography. The molecular structure consists of a discrete [CoCl ( C7H5N2CH2COPh)4] ^ cation and one Br^- anion, in the [CoCl ( C7H5N2CH2COPh)4]^ cation, the coordination geometry of the central Co atom is square-pyramidal with four tertiary N atoms of benzimidazole from four α-( benzimidazol-1-yl) -hypnone ligands in the basal position and one chloride anion in the apical position. In the solid state, [CoCl ( C7H5N2CH2COPh)4]^ and Br^- anion possess intermolecular and intramolecular interactions, which stabilize the crystal structure. The characterization of the title compound were also carried out by using elemeutal analysis, FTIR, UV spectrometries and TG-DSC.     

Synthesis and Crystal Structure of a Novel Bimetallic Porphyrin Complex Salt {[MnTPP(CH_3OH)_2]_3Fe(CN)_6}·13H_2O

A novel bimetallic porphyrin complex salt, {[MnTPP(CH3OH)2]3Fe(CN)6}13H2O (TPP = tetraphenylporphyrin), has been synthesized and structurally characterized by X-ray diffraction analysis. The crystal is of trigonal, space group R-3 with a = b = 31.0618(10), c = 11.8366(8) A, Z = 3, V = 9890.3(8) A3, C144H134FeMn3N18O19, Mr = 2641.36, Dc = 1.330 g/cm3, μ(MoΚα) = 0.463 mm-1, F(000) = 4131, R = 0.0525 and wR = 0.1382 for 3045 observed reflections (I > 2σ(I)). The title complex is composed of one [Fe(CN)6]3- anion, three [MnTPP(CH3OH)2]+ cations and thirteen water molecules, which are connected by multiform hydrogen bonds leading to a 3D supramolecular network structure.     

Hydrothermal Synthesis and Crystal Structure of a New Polyoxovanadate: [Mn(en)3]2en0.5[HV8VV8IVO38(Cl)]·4.5H2O (en = Ethylenediamine)

A new compound has been synthesized under hydrothermal conditions and characterized by IR, elemental analysis, XPS and single-crystal X-ray diffraction analysis. The title compound [Mn(en)3]2en0.5[HV16O38(Cl)]·4.5H2O crystallizes in monoclinic, space group C2/c, with a = 17.016(4), b = 18.858(4), c = 18.872(4) (A), β = 93.667(4)°, V = 6043(2) (A)3, Z = 4, Dc = 2.242 g/cm3, Mr = 2040.12, F(000) = 4020, μ = 2.895 mm-1, Rint = 0.0921, R = 0.0649 and wR = 0.1325. Single-crystal X-ray structure analysis indicates that the title compound consists of a polyanion [HV8VV8IVO38(Cl)]4( cage, two [Mn(en)3]22 cations, four and a half lattice waters and a half ethylenediamine. In addition, intermolecular O-H…N,O-H…O and C-H…O and C-H…O hydrogen bonds link the molecules together to form a three-dimensional structure.     

Cyanide-bridged complexes based on dinuclear Cu(II)-M(II) [M = Pb and Cu] building blocks: Synthesis, crystal structures and magnetic properties

Four cyanide-bridged heterometallic complexes {[CuPb(L 1 )][Fe III (bpb)(CN) 2 ]} 2 ·(ClO 4 ) 2 ·2H 2 O·2CH 3 CN (1), {[CuPb(L 1 )] 2 [Fe II (CN) 6 ](H 2 O) 2 }·10H 2 O (2), {[Cu 2 (L 2 )][Fe III (bpb)(CN) 2 ] 2 }·2H 2 O·2CH 3 OH (3) and {[Cu 2 (L 2 )] 3 [Fe III (CN) 6 ] 2 (H 2 O) 2 }·10H 2 O (4) have been synthesized by treating K[Fe III (bpb)(CN) 2 ] [bpb 2-=1,2-bis(pyridine-2-carboxamido)benzenate] and K 3 [Fe III (CN)] 6 with dinuclear compartmental macrocyclic Schiff-base complexes [CuPb(L 1 )] (ClO 4 ) 2 or [Cu 2 (L 2 )]·(ClO 4 ) 2 , in which H 2 L 1 was derived from 2,6-diformyl-4-methyl-phenol, ethylenediamine, and diethylenetriamine in the molar ratio of 2:1:1 and H 2 L 2 from 2,6-diformyl-4-methyl-phenol and propylenediamine in the molar ratio of 1:1. Single crystal X-ray diffraction analysis reveals that compound 1 displays a cyclic hexanuclear heterotrimetallic molecular structure with alternating [FeⅢ (bpb)(CN) 2 ]- and [CuPb(L 1 )] 2+ units. Complex 2 is of a neutral dumb-bell-type pentanuclear molecular configuration consisting of one [Fe(CN)6] 4- anion sandwiched in two [CuPu(L 1 )] 2+ cations, and the pentanuclear moieties are further connected by the hydrogen bonding to give a 2D supramolecular framework. Heterobimetallic complex 3 is a tetranuclear molecule composed of a centrosymmetric [Cu 2 (L2)] 2+ segment and two terminal cyanide-containing blocks [FeⅢ (bpb)(CN)2 ]- . Octanuclear compound 4 is built from two [Fe(CN)6]3- anions sandwiched in the three [Cu 2 L 2 ] 2+ cations. Investigation of their magnetic properties reveals the overall antiferromagnetic behavior in the series of complexes except 2.     

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-（2-Pyridyl）benzimidazoleH2]2＋ ·[SbCls]2-}2

A new supramolecular compound, { [2-（2-pyridyl）benzimidazoleH2]2＋.[SBC15]2-}2, was synthesized by the hydrothermal reaction of o-diaminobenzene, 2-pyridinecarboxylie acid and SbCl3 in 1：1 HC1 solution, and characterized by chemical analysis, elemental analysis, IR spectra, thermogravimetfic analysis and fluorescence spectra. The crystal structure was deter- mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P211c, with a = 16.0397（13）, b = 14.3189（12）, c = 15.6370（13） A, β = 105.8980（10）°, V = 3454.0（5） A3, Z = 4, C24H22Cl10N6Sb2, Mr = 992.48, Dc = 1.909 g/cm3,/z = 2.366 mm-1, S = 1.010, F（000） = 1920, R = 0.0254 and wR = 0.0555. The coordination anion, [SbCl5]2- which is a distorted tetragonal pyramid, is composed by coordinating action with Sb3＋ ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2- form a biquaternion ring structure through the secondary bonding of Sb...Cl. Moreover, the compound adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-（2-pyridyl）benzimidazole divalent cations. The title compound also shows good fluorescent behaviors.     

Hydrothermal Synthesis and Crystal Structure of a New Polyoxovanadate： [Mn（en）3]2en0.5[HV8VV8IVO38（CI）]·4.5H2O （en = Ethylenediamine）

A new compound has been synthesized under hydrothermal conditions and characterized by IR, elemental analysis, XPS and single-crystal X-ray diffraction analysis. The title compound [Mn（en）3]2en0.5[HV8VV8IVO38（CI）]·4.5H2O crystallizes in monoclinic, space group C2/c, with a = 17.016（4）, b = 18.858（4）, c = 18.872（4） A, β = 93.667（4）°, V = 6043（2）A3, Z = 4, Dc = 2.242 g/cm3, Mr = 2040.12, F（000） = 4020,μ = 2.895 mm-1, Rint = 0.0921, R = 0.0649 and wR = 0.1325. Single-crystal X-ray structure analysis indicates that the title compound consists of a polyanion [HV8VV8IVO38（CI）]4- cage, two [Mn（en）3]2^2＋ cations, four and a half lattice waters and a half ethylenediamine. In addition, intermolecular O-H...N, O-H...O, N-H...O and C-H...O hydrogen bonds link the molecules together to form a three-dimensional structure.     

Crystal structure of a novel two-dimensional supramolecular network based on polyoxoanion and yttrium~Ⅲcoordination cation

A novel compound (NH4)2Y(H2O)8[PMo10V2O40]·10H2O has been prepared in an aqueous solution and characterized by elemental analysis, IR, and TG-DTG analysis. X-ray diffraction analysis was carried out on (NH4)2Y(H2O)8 [PMo10V2O40]·10H2O single crystal, which crystallizes in the monoclinic system of a space group P21/C with a=0.9871(3) nm,b=1.5424(5) nm,c=2.7924(9) nm,β=94.183(5)°and Z=2. In the compound, a two-dimensional network is constructed by the PMo10V2O405- anion and the Y(H2O)83 cation building blocks via hydrogen bonding exhibiting the porous structure.     

SYNTHESIS AND CRYSTAL STRUCTURE OF THE TRI-(μ2-METHOXY)-BRIDGED 'DOUBLE-CUBANE' CLUSTER COMPLEX (Et_4N)_3[Mo_2Fe_6S_8(OMe)_3(SPh)_6]

<正> The title compound was synthesized and crystal structure was solved. (Et4N)3[Mo2Fe6S8(OMe)3(SPh)6], Mr=1922.39, hexagonal, PGs/m, a = 17.750(3), c=15.880(2) A, V=4332.7(26) A3, Z-2, Dx=1.477 g/cm3, MoKα, λ= 0.71069 A, R = 0.059, Rw = 0.065, for 814 observed reflexions. The complex anion contains two Fe3MoS4 cubane-like units linked throug their molybdenum atoms by three ,μ2-methoxy-groups, and the overall structure of the anion has C3b symmetry.     

Synthesis and Crystal Structure of a Novel Ion-pair Compound Consisting of 1,3-Bis（4-cynobenzyl） Imidazole Cation and 7,7,8,8-Tetracyanoquinodimethanide Anion

A novel compound [(CNBz)2Im]2(TCNQ)3(CH3CN)((CNBz)2Im = 1,3-bis(4-cyano-benzyl) imidazole cation,TCNQ-1 = 7,7,8,8-tetracyanoquinodimethanide anion) was synthesized by the reaction of [(CNBz)2Im]Br and LiTCNQ in water and its structure was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21/c with a = 10.1823(17),b = 20.292(3),c = 16.952(3) ,β = 104.73(0)°,V = 3387.6(10)3,Z = 4,C39H24N11,Mr = 646.69,Dc = 1.268 g/cm3,μ = 0.080 mm-1 and F(000) = 1340.The structure was solved by direct methods and refined to R = 0.0596 and wR = 0.0911 for 2690 observed reflections(Ⅰ 2σ(Ⅰ)).The most prominent structural feature is that there are two types of TCNQ entries(TCNQ-1 and TCNQ0) in agreement with the IR spectra analysis of the compound.     

STRUCTURE STUDIES OF [Et_4N]_4[Cu_8(i-mnt)_6] (i-mnt=S_2C=C(CN)_2) AND [Me_4N]_4[Cu_5Ag_3(i-mnt)_6]·H_2O

<正> [Me4N]6[Ag6(i-mnt)6].H2O(1),[Et4N]4[Cu8(i-mnt)6](2) and [Me4N]4-[Cu5Ag3(i-mnt)6].H2O(3)(i-mnt=S2C=C(CN)2) were synthesized. The crystal and molecular structure of the complex 1 was reported by us.The structure of the complex 2 was determined from single crystal X-ray diffraction data. [Et4N]4[Cu8(i-mnt)s] 2, Mr=1870.46, monoclinic, P21/n, a=14.724(6), b = 17.228(3), c=15.59(1)A,β= 100.75(7)°,V=3886.3A3;Z = 2,Dc= 1.598 g/cm3. Complex 3 has been characterized by ICP elemental analyses and IR spectrum.     

Synthesis,Structure,Fluorescent Property and Natural Bond Orbital（NBO） Analysis of a One-dimensional Cobalt（III） Complex Containing 1,3-Benzenedicarboxylate and 2-Methyldipyrido[3,2-f：2＇,3＇-h]quinoxaline Ligand

A novel metal-organic coordination polymer [Co(m-BDC)(Medpq)·2H2O]n(m-H2BDC = benzene-1,3-dicarboxyalic acid,Medpq = 2-methyldipyrido[3,2-f:2',3'-h]quinoxaline) has been hydrothermally synthesized and structurally characterized by elemental analysis,IR spectrum and single-crystal X-ray diffraction.The title compound crystallizes in monoclinic,space group C2/c with a = 19.986(4),b = 15.789(3),c = 16.292(3),β = 126.54(3)°,V = 4130.3(14)3,C23H18N4O6Co,Mr = 505.34,Dc = 1.625 g·cm-3,Z = 8,μ = 0.883 mm-1,F(000) = 2072,the final R = 0.0772 and wR = 0.1428.The crystal structure of complex 1 is an infinite zigzag-like chain of hexacoordinate Co3+ ions,in which the Co3+ ions are bridged in two coordination modes by m-BDC2+ ligands and decorated by Medpq ligands,showing a slightly distorted octahedral geometry.Additionally,the compound shows strong fluorescence in the solid state at room temperature.Natural bond orbital(NBO) analysis is performed by using the NBO method built in Gaussian 03 Program.The calculation results show a covalent interaction between the coordinated atoms and Co3+ ions.     

SYNTHESIS AND STRUCTURE OF[Et_4N]_3[FE_3(SPh)_3Br_3Cl_3]

<正> The title compound was synthesized and its structure solved. The formula is [Et4N]3[Fe3(SPh)3Br3Cl3]. M=1231.95, monoclinic, space group C2/c, a=24.569(4), b=13.504(2), c=18.348.(3)A, β=110.78(1)°, V=5691(3)A3, Z=4, Dm= 1.41, Dc=1.44-g/cm3. The flat structure of the anion has. a planar [Fe3S3] ring and three phenyl groups. Statistical distribution of chlorine and bromine atoms on two sides of the [Fe3S3] plane results in a C2 symmetry of the anion.     

Synthesis and Structural Characterization of a Cyano-bridged 1-D Lanthanum(Ⅲ)-iron(Ⅲ)Complex [La(DMSO)5(H2O)](μ-CN)2[Fe(CN)4]·H2O

A new lanthanumⅢ-ironⅢ complex [La(DMSO)5(H2O)](μ-CN)2[Fe(CN)4]·H2O 1 (DMSO=dimethylsulfoxide) has been prepared by a facile approach, ball-milling method, and characterized by X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a=9.7125(3), b=21.5336(7), c=14.3804(5) (A), β=93.242(3)°, C16H34FeLaN6O7S5, Mr=777.55, V=3002.8(2)(A)3, Z=4, Dc=1.720 g/cm3, S=1.053, μ(MoKα)=2.278 mm-1, F(000)=1564, R=0.0490 and wR=0.1270. The crystal structure analysis of 1 reveals a slightly distorted squareantiprism eightfold-coordinated La(Ⅲ) ion and a 1-D zigzag chain structure extending through the Fe-CN-La-NC-Fe linkages. The [La(DMSO)5(H2O)](μ-CN)2[Fe(CN)4] species are held together via hydrogen bonds to form a three-dimensional framework.     

Synthesis, crystal structure and properties of a new organic-inorganic hybrid Dawson-like polyoxotungstate [Co(2,2′-bpy)_3]_2[Co(2,2′-bpy)_2Cl][Co(2,2′-bpy)_2]H_2- [SbW_(18)O_(60)]·4H_2O

A new organic-inorganic hybrid polyoxometalate based on Dawson-like polyoxotungstate anion [SbW18O60]9, formulated [Co(2,2′-bpy)3]2[Co(2,2′-bpy)2Cl][Co(2,2′-bpy)2]H2[SbW18O60]·4H2O (2,2′-bpy= 2,2′-bipyridine) has been synthesized from Sb2O3, Na2WO4, CoCl2, and 2,2′-bipyridine materials by hydrothermal method, and which was characterized by elemental analyses, IR, XPS, EPR, TG, and X-ray single crystal diffraction. Structure analysis shows that the polyoxoanion self-assembled under hydrothermal conditions consists of a Dawson-like polyoxotungstate cluster anion [SbW18O60]9 en- capsulating a pyramidal {SbO3} group within the {W18} cluster cage. EPR spectra show that the high-spin octahedral CoII and low-spin CoII ions coexist in the title compound. Magnetic properties in- dicate that the compound is antiferromagnetic.