A binuclear vanadium complex NH4[(VⅣO)2( Ⅲ(H2O)9] wa s synthesized by reaction of NH3VO3, nitrilotriacetic acid and EuCl3 in one aque ous solution. The crystal X-ray analysis shows that the complex contains one bin ...A binuclear vanadium complex NH4[(VⅣO)2( Ⅲ(H2O)9] wa s synthesized by reaction of NH3VO3, nitrilotriacetic acid and EuCl3 in one aque ous solution. The crystal X-ray analysis shows that the complex contains one bin uclear vanadium anion [(VⅣO)2( -and one [EuⅢ(H2O)9]3+ cation. T he molecules are built up to a three-dimensional supramolecular structure throug h hydrogen bonding. CCDC: 238716.展开更多
The reactions of Co（C1O4）2·6H2O and Co（NO3）2.6H2O with the di-Schiff base ligand N,N＇-bis-（1-benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine （LA） in ethanol have been investigated. The reactions of LA wi...The reactions of Co（C1O4）2·6H2O and Co（NO3）2.6H2O with the di-Schiff base ligand N,N＇-bis-（1-benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine （LA） in ethanol have been investigated. The reactions of LA with excess amount of cobalt salts yield the six-coordinate complexes [CoL2]（ClO4）E·H2O 1 and [CoL2]（NO3）E·H2O 2 as isolatable products （L= N-（1- benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine）, where L is a tri-dentate mono-Schiff base ligand, resulting from the hydrolysis of the precursor di-Schiff base LA. Both complexes were characterized by X-ray crystallography. Crystal data for complex 1： monoclinic, space group P21/c, a = 11.9214（10）, b = 23.5828（17）, c = 14.0387（12）A, β = 135.219（4）°, C22H30Cl2CoN8O9, Mr = 680.37, V = 2780.1（4） A^3 ,Z = 4, Dc = 1.625 g/cm^3,μ（MoKa） = 0.876 mm^-1, F（000） = 1404, the final R = 0.0725 and wR = 0.1530 for 5726 observed reflections （I 〉 2σ（I））. Crystal data for complex 2： monoclinic, space group P21/c, a = 18.2162（16）, b = 10.0610（6）, c = 18.593（2）A, β = 130.099（3）°, C22H30CoN10O7, Mr = 605.49, V = 2606.5（4） A3 Z = 4, Dc = 1.543 g/cm^3,μ（MoKa） = 0.722 mm^-1, F（000） = 1260, the final R = 0.0619 and wR = 0.1429 for 5194 observed reflections （I 〉 2σ（I））. X-ray diffraction analysis reveals that each cobalt atom in the two complexes is chelated by six nitrogen atoms from two tridentate iigands L, exhibiting a slightly distorted octahedral coordination sphere. In both complexes, the strong hydrogen-bonding interactions between the lattice waters and N-H groups of the ligands result in 1D chains which are further connected by ClO4^- （or NO3^-） groups to form a 3D framework. In complex 2, the strong π-π interactions increase the stability of the structure.展开更多
The reactions of SbCl3 and HgCl2 with 2-（3-pyridyl）benzimidazole （PyBIm） in solution acidified with HCl have been investigated. The PyBIm ligands are protonated into 2-（3-pyridinio）benzimidazolium （H2PyBIm） ca...The reactions of SbCl3 and HgCl2 with 2-（3-pyridyl）benzimidazole （PyBIm） in solution acidified with HCl have been investigated. The PyBIm ligands are protonated into 2-（3-pyridinio）benzimidazolium （H2PyBIm） cations and the corresponding metal ions are bonded with chloride atoms into coordination anions, forming two new coordination compounds, namely, （H2PyBIm）（SbCl5） 1 and （H2PyBIm）2（Hg2Cl8） 2. Both compounds were characterized by X-ray crystallography. Crystal data for 1： triclinic, space group P1^- with a = 5.7030（7）, b = 9.0625（11）, c = 16.5929（18） A, α = 91.808（7）°, β = 93.234（6）, γ = 99.216（7）°, C12H11N3SbCl5, Mr = 496.24, V = 844.44（17） A^3, Z = 2, Dc = 1.952 g/cm^3, μ（MoKα） = 2.419 mm^-1, F（000） = 480, the final R = 0.0496 and wR = 0.1382 for 3433 observed reflections （I 〉 2σ（I））. Crystal data for 2： monoclinic, space group P21/c with a = 7.8061（5）, b = 15.8127（9）, c = 12.2435（9） , β = 91.955（4）o, C24H22N6Hg2Cl8, Mr = 1079.26, V = 1510.40（17） 3, Z = 2, Dc = 2.373 g/cm3, μ（MoKα） = 10.889 mm-1, F（000） = 1008, the final R = 0.0293 and wR = 0.0562 for 2854 observed reflections （I 〉 2σ（I））. X-ray diffraction analysis reveals that the antimony（III） is five-coordinated, exhibiting a slightly distorted square-pyramidal coordination geometry; while in 2, a dimeric [Hg2Cl8]^4-anion consists of two trigonal bipyramids sharing two common edges. The organic cations and coordination anions are connected into a one-dimensional belt and a two-dimensional sheet through N-H···Cl hydrogen bonding interactions in compounds 1 and 2, respectively; both are further aggregated into 3D frameworks by strong π-π contacts.展开更多
The title complex, [Cd（MeHbibzim）（1,4-bdc）]n （1, MelToibzim = 1-methyl-2,2＇- bibenzimidazole, 1,4-bdc = terephthalate）, was synthesized with hydrothermal reactions. The compound crystallizes in monoclinic, spac...The title complex, [Cd（MeHbibzim）（1,4-bdc）]n （1, MelToibzim = 1-methyl-2,2＇- bibenzimidazole, 1,4-bdc = terephthalate）, was synthesized with hydrothermal reactions. The compound crystallizes in monoclinic, space group C2/c with a = 9.822（4）, b = 18.510（7）, c = 22.372（9） A, β = 98.359（6）°, C23H16CdN4O4, Mr = 524.81, V= 4024（3） A3, Z = 8, Dc. = 1.733 g/cm3, μ（MoKa） = 1.126 mm-1, F（000） = 2096, the final R = 0.0597 and wR = 0.1374 for 3906 observed reflections （1 〉 2σ（I））. X-ray diffraction analysis reveals that the Cd atom is coordinated by two nitrogen atoms from the chelating MeHbibzim and three carboxyl oxygen atoms from three terephthalate ligands, thus forming a distorted square pyramidal coordination sphere, [CdN2O3]. Every two Cd atoms are linked together via two carboxyl groups into a dinuclear unit with Cd...Cd separation of 3.806（4） A. The dinuclear building units are linked by terephthalate ligands into two-dimensional layers, which are further aggregated into a 3D framework via hydrogen bonding interactions.展开更多
The title complex, [Co2（bibzim）（H2bibzim）4]·Co2（H2bibzim）2（Hbibzim）（HL）]2- 2H2O （1） （HEbibzim = 2,2＇-bibenzimidazole, H5L = N,N-bis（phosphonomethyl）aminoacetic acid （HO2CCH2N（CH2PO3H2）2））, wa...The title complex, [Co2（bibzim）（H2bibzim）4]·Co2（H2bibzim）2（Hbibzim）（HL）]2- 2H2O （1） （HEbibzim = 2,2＇-bibenzimidazole, H5L = N,N-bis（phosphonomethyl）aminoacetic acid （HO2CCH2N（CH2PO3H2）2））, was synthesized with hydrothermal reactions. The compound crystallizes in triclinic, space group P1 with a = 13.71020（10）, b = 14.9165（5）, c = 20.9924（5） A, a = 86.344（9）, β = 71.214（8）, γ = 73.757（7）°, C162HI24Co6N46O18P4, Mr = 3478.52, V = 3900.55（16） A3, Z = 2, Dc = 1.482 g/cm3,μ（MoKa） = 0.747 mm^-1, F（000） = 1784, the final R = 0.0777 and wR = 0.2091 for 13598 observed reflections （I 〉 2σ（I））. X-ray diffraction analysis reveals that there are three crystallographically independent Co（II） atoms in the complex. The complex consists of binuclear coordination cation, binuclear coordination anion, as well as lattice water molecules, which further aggregate into a 3D framework via hydrogen bonding as well as π-π interactions.展开更多
The reactions of imidazoquinoxaline and 1,3,5-H3 btc acid under different condition have been investigated. The different degree of hydrolysis reaction leads to two different adducts being produced, namely, [（Hdiam Q...The reactions of imidazoquinoxaline and 1,3,5-H3 btc acid under different condition have been investigated. The different degree of hydrolysis reaction leads to two different adducts being produced, namely, [（Hdiam Quin）＋（H2btc）-]（1）, and [（diam Quin）4（Imi Quin）·4H2O]（2）. Both compounds were characterized by X-ray crystallography. Crystal data for 1： monoclinic, space group Pn with a = 9.868（2）, b = 5.3172（11）, c = 15.387（3）A, β = 91.10（3）°, C17H14N4O6, Mr = 370.32, V = 807.2（3）A3, Z = 2, Dc = 1.524 g/cm3, μ（Mo Kα） = 0.118 mm-1, F（000） = 384, the final R = 0.0385 and w R = 0.0869 for 2294 observed reflections（I 〉 2σ（I））. Crystal data for 2： triclinic, space group P1 with a = 9.825（2）, b = 14.144（3）, c = 16.054（3） A, α = 101.06（3）, β = 102.55（3）, γ = 92.46（3）°, C（44）H40N（20）O4, Mr = 912.96, V = 2128.8（7） A3, Z = 2, Dc = 1.424 g/cm3, μ（Mo Kα） = 0.099 mm-1, F（000） = 952, the final R = 0.0554 and w R = 0.1662 for 6563 observed reflections（I 〉 2σ（I））. X-ray diffraction analysis reveals that compound 1 is a salt. Imidazoquinoxaline was wholly hydrolyzed into 2,3-diaminoquinoxaline and protonated as a cation with H2btc-acting as an anion. However, in compound 2, the imidazoquinoxaline is only partly hydrolyzed, and the resulting 2,3-diaminoquinoxaline forms adduct with the intacted imidazoquinoxaline. Both are further aggregated into 3D frameworks by strong hydrogen bonding even π-π interactions.展开更多
A novel cadmium coordination polymer [Cdls（OH）4（SO4）4（L1）6（L2）12]n （HL1 = 1,2,3-1H-triazole, HL2 = 5-methyl-lH-tetrazole） has been synthesized and characterized by elemental analysis and single-crystal X-ray...A novel cadmium coordination polymer [Cdls（OH）4（SO4）4（L1）6（L2）12]n （HL1 = 1,2,3-1H-triazole, HL2 = 5-methyl-lH-tetrazole） has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The compound crystallizes in cubicI-43d space group with a = 21.5247（4）, V = 9972.7（3） A3, Z = 4, Dc = 2.360 g/cm3, Mr = 3543.68, μ（MoKα） = 3.298 mm^-1, F（000） = 6696, the final R = 0.0340 and wR = 0.0992 for 1909 observed reflections （I 〉 2σ（I））. The compound contains two crystallographicatly independent Cd coordination centers linked up through one L1 and two L2 bridges. The structure displays an inorganic-organic hybrid cadmium coordination polymer.展开更多
The crystals of the title compounds (H3O)(C3H5N2)[Mn(OH)6Mo6O18]?3.5H2O 1 and (H3O)3[Co(OH)6Mo6O18]?7H2O 2 have been prepared and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes ...The crystals of the title compounds (H3O)(C3H5N2)[Mn(OH)6Mo6O18]?3.5H2O 1 and (H3O)3[Co(OH)6Mo6O18]?7H2O 2 have been prepared and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group C2/c with a = 21.5018(9), b = 10.9331(5), c = 11.8667(5) ?, β = 95.3570(10)o, V = 2777.5(2) ?3, Z = 4, Dc = 2.802 g/cm3, Mr = 1171.80, μ(MoKα) = 3.173 mm-1, F(000) = 223, the final R = 0.0458 and wR = 0.1041 for 2093 observed reflections (I > 2σ(I)); Compound 2 crystallizes in monoclinic, space group P21/c with a = 11.4042(12), b = 10.9481(11), c = 11.6722(12) ?, β = 99.948(2)o, V = 1435.4(3) ?3, Z = 2, Dc = 2.794 g/cm3, Mr = 1207.80, μ(MoKα) = 3.223 mm-1, F(000) = 1160, the final R = 0.0544 and wR = 0.1066 for 1906 observed reflections (I > 2σ(I)). Both compounds 1 and 2 adopt the Anderson structure, in which the anion is of centrosymmetry and formed by six octahedral edge-sharing MoO6units surrounding the central MO6 (M = Mn or Co) octahedron.展开更多
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-cry...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.展开更多
文摘A binuclear vanadium complex NH4[(VⅣO)2( Ⅲ(H2O)9] wa s synthesized by reaction of NH3VO3, nitrilotriacetic acid and EuCl3 in one aque ous solution. The crystal X-ray analysis shows that the complex contains one bin uclear vanadium anion [(VⅣO)2( -and one [EuⅢ(H2O)9]3+ cation. T he molecules are built up to a three-dimensional supramolecular structure throug h hydrogen bonding. CCDC: 238716.
基金the National Natural Science Foundation of China (20425313)the Natural Science Foundation of Fujian Province (2005HZ01-1, 2006L2005, 2006F3135, 2006J0183)
文摘The reactions of Co（C1O4）2·6H2O and Co（NO3）2.6H2O with the di-Schiff base ligand N,N＇-bis-（1-benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine （LA） in ethanol have been investigated. The reactions of LA with excess amount of cobalt salts yield the six-coordinate complexes [CoL2]（ClO4）E·H2O 1 and [CoL2]（NO3）E·H2O 2 as isolatable products （L= N-（1- benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine）, where L is a tri-dentate mono-Schiff base ligand, resulting from the hydrolysis of the precursor di-Schiff base LA. Both complexes were characterized by X-ray crystallography. Crystal data for complex 1： monoclinic, space group P21/c, a = 11.9214（10）, b = 23.5828（17）, c = 14.0387（12）A, β = 135.219（4）°, C22H30Cl2CoN8O9, Mr = 680.37, V = 2780.1（4） A^3 ,Z = 4, Dc = 1.625 g/cm^3,μ（MoKa） = 0.876 mm^-1, F（000） = 1404, the final R = 0.0725 and wR = 0.1530 for 5726 observed reflections （I 〉 2σ（I））. Crystal data for complex 2： monoclinic, space group P21/c, a = 18.2162（16）, b = 10.0610（6）, c = 18.593（2）A, β = 130.099（3）°, C22H30CoN10O7, Mr = 605.49, V = 2606.5（4） A3 Z = 4, Dc = 1.543 g/cm^3,μ（MoKa） = 0.722 mm^-1, F（000） = 1260, the final R = 0.0619 and wR = 0.1429 for 5194 observed reflections （I 〉 2σ（I））. X-ray diffraction analysis reveals that each cobalt atom in the two complexes is chelated by six nitrogen atoms from two tridentate iigands L, exhibiting a slightly distorted octahedral coordination sphere. In both complexes, the strong hydrogen-bonding interactions between the lattice waters and N-H groups of the ligands result in 1D chains which are further connected by ClO4^- （or NO3^-） groups to form a 3D framework. In complex 2, the strong π-π interactions increase the stability of the structure.
基金supported by the Natural Science Foundation of Fujian Province (2007HZ0001-1, 2009HZ0004-1, 2009HZ0006-1 and 2006L2005)
文摘The reactions of SbCl3 and HgCl2 with 2-（3-pyridyl）benzimidazole （PyBIm） in solution acidified with HCl have been investigated. The PyBIm ligands are protonated into 2-（3-pyridinio）benzimidazolium （H2PyBIm） cations and the corresponding metal ions are bonded with chloride atoms into coordination anions, forming two new coordination compounds, namely, （H2PyBIm）（SbCl5） 1 and （H2PyBIm）2（Hg2Cl8） 2. Both compounds were characterized by X-ray crystallography. Crystal data for 1： triclinic, space group P1^- with a = 5.7030（7）, b = 9.0625（11）, c = 16.5929（18） A, α = 91.808（7）°, β = 93.234（6）, γ = 99.216（7）°, C12H11N3SbCl5, Mr = 496.24, V = 844.44（17） A^3, Z = 2, Dc = 1.952 g/cm^3, μ（MoKα） = 2.419 mm^-1, F（000） = 480, the final R = 0.0496 and wR = 0.1382 for 3433 observed reflections （I 〉 2σ（I））. Crystal data for 2： monoclinic, space group P21/c with a = 7.8061（5）, b = 15.8127（9）, c = 12.2435（9） , β = 91.955（4）o, C24H22N6Hg2Cl8, Mr = 1079.26, V = 1510.40（17） 3, Z = 2, Dc = 2.373 g/cm3, μ（MoKα） = 10.889 mm-1, F（000） = 1008, the final R = 0.0293 and wR = 0.0562 for 2854 observed reflections （I 〉 2σ（I））. X-ray diffraction analysis reveals that the antimony（III） is five-coordinated, exhibiting a slightly distorted square-pyramidal coordination geometry; while in 2, a dimeric [Hg2Cl8]^4-anion consists of two trigonal bipyramids sharing two common edges. The organic cations and coordination anions are connected into a one-dimensional belt and a two-dimensional sheet through N-H···Cl hydrogen bonding interactions in compounds 1 and 2, respectively; both are further aggregated into 3D frameworks by strong π-π contacts.
基金supported by the 973 key program of the MOST(2010CB933501,2012CB821705)the Chinese Academy of Sciences(KJCX2-YW-319,KJCX2-EW-H01)+1 种基金the National Natural Science Foundation of Chinathe Natural Science Foundation of Fujian Province(2007HZ0001-1,2009HZ0004-1,2009HZ0005-1,2009HZ0006-1,2006L2005)
文摘The title complex, [Cd（MeHbibzim）（1,4-bdc）]n （1, MelToibzim = 1-methyl-2,2＇- bibenzimidazole, 1,4-bdc = terephthalate）, was synthesized with hydrothermal reactions. The compound crystallizes in monoclinic, space group C2/c with a = 9.822（4）, b = 18.510（7）, c = 22.372（9） A, β = 98.359（6）°, C23H16CdN4O4, Mr = 524.81, V= 4024（3） A3, Z = 8, Dc. = 1.733 g/cm3, μ（MoKa） = 1.126 mm-1, F（000） = 2096, the final R = 0.0597 and wR = 0.1374 for 3906 observed reflections （1 〉 2σ（I））. X-ray diffraction analysis reveals that the Cd atom is coordinated by two nitrogen atoms from the chelating MeHbibzim and three carboxyl oxygen atoms from three terephthalate ligands, thus forming a distorted square pyramidal coordination sphere, [CdN2O3]. Every two Cd atoms are linked together via two carboxyl groups into a dinuclear unit with Cd...Cd separation of 3.806（4） A. The dinuclear building units are linked by terephthalate ligands into two-dimensional layers, which are further aggregated into a 3D framework via hydrogen bonding interactions.
基金supported by the National Natural Science Foundation of China(21373221,21221001,91122027,51172232,21403236)
文摘The title complex, [Co2（bibzim）（H2bibzim）4]·Co2（H2bibzim）2（Hbibzim）（HL）]2- 2H2O （1） （HEbibzim = 2,2＇-bibenzimidazole, H5L = N,N-bis（phosphonomethyl）aminoacetic acid （HO2CCH2N（CH2PO3H2）2））, was synthesized with hydrothermal reactions. The compound crystallizes in triclinic, space group P1 with a = 13.71020（10）, b = 14.9165（5）, c = 20.9924（5） A, a = 86.344（9）, β = 71.214（8）, γ = 73.757（7）°, C162HI24Co6N46O18P4, Mr = 3478.52, V = 3900.55（16） A3, Z = 2, Dc = 1.482 g/cm3,μ（MoKa） = 0.747 mm^-1, F（000） = 1784, the final R = 0.0777 and wR = 0.2091 for 13598 observed reflections （I 〉 2σ（I））. X-ray diffraction analysis reveals that there are three crystallographically independent Co（II） atoms in the complex. The complex consists of binuclear coordination cation, binuclear coordination anion, as well as lattice water molecules, which further aggregate into a 3D framework via hydrogen bonding as well as π-π interactions.
基金supported by the National Natural Science Foundation of China(No.21171075)Start-up Fund for Advanced Professional of Jiangsu University(No.08JDG031)
文摘The reactions of imidazoquinoxaline and 1,3,5-H3 btc acid under different condition have been investigated. The different degree of hydrolysis reaction leads to two different adducts being produced, namely, [（Hdiam Quin）＋（H2btc）-]（1）, and [（diam Quin）4（Imi Quin）·4H2O]（2）. Both compounds were characterized by X-ray crystallography. Crystal data for 1： monoclinic, space group Pn with a = 9.868（2）, b = 5.3172（11）, c = 15.387（3）A, β = 91.10（3）°, C17H14N4O6, Mr = 370.32, V = 807.2（3）A3, Z = 2, Dc = 1.524 g/cm3, μ（Mo Kα） = 0.118 mm-1, F（000） = 384, the final R = 0.0385 and w R = 0.0869 for 2294 observed reflections（I 〉 2σ（I））. Crystal data for 2： triclinic, space group P1 with a = 9.825（2）, b = 14.144（3）, c = 16.054（3） A, α = 101.06（3）, β = 102.55（3）, γ = 92.46（3）°, C（44）H40N（20）O4, Mr = 912.96, V = 2128.8（7） A3, Z = 2, Dc = 1.424 g/cm3, μ（Mo Kα） = 0.099 mm-1, F（000） = 952, the final R = 0.0554 and w R = 0.1662 for 6563 observed reflections（I 〉 2σ（I））. X-ray diffraction analysis reveals that compound 1 is a salt. Imidazoquinoxaline was wholly hydrolyzed into 2,3-diaminoquinoxaline and protonated as a cation with H2btc-acting as an anion. However, in compound 2, the imidazoquinoxaline is only partly hydrolyzed, and the resulting 2,3-diaminoquinoxaline forms adduct with the intacted imidazoquinoxaline. Both are further aggregated into 3D frameworks by strong hydrogen bonding even π-π interactions.
基金supported by the Anhui Provincial Education Department(No.KJ2007A014)and Key Laboratory of Powder and Energy Materials of Hefei University
文摘A novel cadmium coordination polymer [Cdls（OH）4（SO4）4（L1）6（L2）12]n （HL1 = 1,2,3-1H-triazole, HL2 = 5-methyl-lH-tetrazole） has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The compound crystallizes in cubicI-43d space group with a = 21.5247（4）, V = 9972.7（3） A3, Z = 4, Dc = 2.360 g/cm3, Mr = 3543.68, μ（MoKα） = 3.298 mm^-1, F（000） = 6696, the final R = 0.0340 and wR = 0.0992 for 1909 observed reflections （I 〉 2σ（I））. The compound contains two crystallographicatly independent Cd coordination centers linked up through one L1 and two L2 bridges. The structure displays an inorganic-organic hybrid cadmium coordination polymer.
基金This work was supported by the National Natural Science Foundation of China (90206040 20333070and 20303021) and Natural Science Foundation of Fujian Province (20002F015 and 2002J006)
文摘The crystals of the title compounds (H3O)(C3H5N2)[Mn(OH)6Mo6O18]?3.5H2O 1 and (H3O)3[Co(OH)6Mo6O18]?7H2O 2 have been prepared and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group C2/c with a = 21.5018(9), b = 10.9331(5), c = 11.8667(5) ?, β = 95.3570(10)o, V = 2777.5(2) ?3, Z = 4, Dc = 2.802 g/cm3, Mr = 1171.80, μ(MoKα) = 3.173 mm-1, F(000) = 223, the final R = 0.0458 and wR = 0.1041 for 2093 observed reflections (I > 2σ(I)); Compound 2 crystallizes in monoclinic, space group P21/c with a = 11.4042(12), b = 10.9481(11), c = 11.6722(12) ?, β = 99.948(2)o, V = 1435.4(3) ?3, Z = 2, Dc = 2.794 g/cm3, Mr = 1207.80, μ(MoKα) = 3.223 mm-1, F(000) = 1160, the final R = 0.0544 and wR = 0.1066 for 1906 observed reflections (I > 2σ(I)). Both compounds 1 and 2 adopt the Anderson structure, in which the anion is of centrosymmetry and formed by six octahedral edge-sharing MoO6units surrounding the central MO6 (M = Mn or Co) octahedron.
基金supported by Industry High Technology Foundation of Jiangsu (BG2007025)Doctoral Fund from National Ministry of Education (20093227110009),China
文摘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.
