Solvothermal reaction of aromatic terphenyl-2,5,2＇,5＇-tetracarboxylic acid （Hnqptc） ligand and the transitional metal cation of Mn11 in the presence of 3-（2-pyridyl）pyrazole （pp） affords one new coordination p...Solvothermal reaction of aromatic terphenyl-2,5,2＇,5＇-tetracarboxylic acid （Hnqptc） ligand and the transitional metal cation of Mn11 in the presence of 3-（2-pyridyl）pyrazole （pp） affords one new coordination polymer, [Mn（qptc）0.5（pp）2]n·n（H2O） （1）. The structure has been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR, TGA, and magnetism. The carboxyl groups of qptc4 exhibit a μ1-η1：η0 coordination mode, and the qptc4- acts as a H-shaped ligand linking the Mn11 centers together to form a 2D polymeric [Mn（qptc）0.5]n layer. The crystal of 1 crystallizes in orthorhombic, space group Pbca with a = 9.3119（12）, b = 20.848（3）, c = 26.134（3） A, V= 5073.4（11） A3, Z= 8, C27HIgMnN6O5,Mr=562.42, Dc = 1.473 g/cm3, F（000） = 2304 and μ（MoKa） = 0.571 mm-1. The final R = 0.0468 and wR = 0.1196 for 4429 observed reflections with I 〉 2σ（I） and R = 0.0797 and wR = 0.1383 for all data.展开更多
One new polyoxometalate compound connected via cobalt/potassium cations,namely H5K{[Co（H2O）5]2（H2Mo3.24W8.76O42）}·19H2O 1,was prepared and characterized by ele- mental analysis and IR spectroscopy. Single-cry...One new polyoxometalate compound connected via cobalt/potassium cations,namely H5K{[Co（H2O）5]2（H2Mo3.24W8.76O42）}·19H2O 1,was prepared and characterized by ele- mental analysis and IR spectroscopy. Single-crystal X-ray diffraction analysis result reveals that anions of {[Co（H2O）5]2（H2Mo3.24W8.76O42）}6- in compound 1 are linked by potassium cations to form one- dimensional chain,based on which a three-dimensional network is further constructed with the help of hydrogen bonds. Crystal data： H67Co2KMo3.24O72W8.76,Mr = 3297.87,monoclinic,C2/c,a = 19.0126（10）,b = 16.6025（5）,c = 19.1908（10）A,β = 106.713（1）°,V = 5801.8（5） A^3,Z = 4,Dc = 3.755 g/cm^3,F（000） = 5961,μ = 18.730 mm^-1,R = 0.0569 and wR = 0.1437 （I 〉 2σ（I））.展开更多
The new copper(II) complex Cu(C13H9N3O2Br)2H2O (N-(2-hydroxy-5-bromo- benzoyl)-N-(picolinylidene)hydrazine is abbreviated as HL ) was obtained from the refluxing solution of Cu(CH3COO)2H2O and HL in the ethanol-N, N-d...The new copper(II) complex Cu(C13H9N3O2Br)2H2O (N-(2-hydroxy-5-bromo- benzoyl)-N-(picolinylidene)hydrazine is abbreviated as HL ) was obtained from the refluxing solution of Cu(CH3COO)2H2O and HL in the ethanol-N, N-dimethylformamide mix solvent. Crystal data: triclinic, space group P , a = 10.8620(3), b = 11.7453 (3), c = 12.4417(2) ? ?= 62.255(0), ?= 79.097(2), ?= 86.764(2)? V = 1378.52(6) ?, Z = 2, Mr = 719.835, Dc = 1.734 g/cm3, F(000) = 714, (MoK) = 3.739 mm-1, T = 293(2) K, final R = 0.0594 and wR = 0.1416 for 2943 observed reflections with I > 2.0(I). The structure of Cu(C13H9N3O2Br)2H2O has been determined by X-ray analysis and revealed that two L-1 ligands coordinate to the copper(Ⅱ) ion through two oxygen and two nitrogen atoms from the hydrazine groups and two pyridine nitrogen atoms to form an elongated and distorted square-bipyramidal environment for Cu(Ⅱ). The complex is also characterized by 1H NMR spectroscopies展开更多
One novel copper（II）-organic compound,namely Cu[Cu2（PP）2]（CBPC）2]·2（H2O）（1,H2CBPC = 1-[（2＇-carboxybiphenyl-4-yl）methyl]-2-propylimidazole-4-carboxylic acid,HPP = 3-（2-pyridyl）pyrazole）,was designed...One novel copper（II）-organic compound,namely Cu[Cu2（PP）2]（CBPC）2]·2（H2O）（1,H2CBPC = 1-[（2＇-carboxybiphenyl-4-yl）methyl]-2-propylimidazole-4-carboxylic acid,HPP = 3-（2-pyridyl）pyrazole）,was designed and synthesized under hydrothermal conditions.X-ray diffraction analysis reveals that two Cu（II）ions in the quasi-planar dimmer of [Cu2（PP）2] are linked by the carboxylate oxygen atoms on the phenyl ring and the imidazole ring,respectively,yielding one snake-shaped structure.Magnetic measurements reveal that compound 1 shows the strongly antiferromagnetic property.Crystal data of 1：C58H52Cu3N10O10,Mr = 1239.72,monoclinic,P21/c,a = 14.900（7）,b = 15.029（7）,c = 12.308（6）,β = 102.519（9）o,V = 2691（2）3,Z = 2,Dc = 1.530 g/cm3,F（000）= 1274,μ = 1.246 mm-1,R = 0.0416,wR = 0.0780（I 2σ（I））and S = 0.999.展开更多
One novel cobalt coordination polymer, {[Co（HTCB）（4,4＇btb）]＇HzO}n （1, H3TCB = 1,3,5-tris（4-carboxyphenyl）benzene, 4,4＇-btb = 4,4＇-bis（1,2,4-triazol-3-yl）biphenyl）, has been synthesized and characterized ...One novel cobalt coordination polymer, {[Co（HTCB）（4,4＇btb）]＇HzO}n （1, H3TCB = 1,3,5-tris（4-carboxyphenyl）benzene, 4,4＇-btb = 4,4＇-bis（1,2,4-triazol-3-yl）biphenyl）, has been synthesized and characterized by elemental analysis, IR, powder X-ray diffraction （PXRD）, and thermogravimetric （TG） analyses. X-ray diffraction analysis reveals that complex 1 is a 2D 2-fold interpenetrated {44,62}-sql [Co（HTCB）（4,4＇-btb）] sheet based on the 1D [Co（HTCB）]n chains and 1D [Co（4,4＇-btb）]n chains. The crystal of 1 crystallizes in triclinic, space group P1 with a = 9.529（12）, b = 13.914（16）, c = 14.906（17） A, V= 1903（4） A3, Z = 2, C45H34N6CoO71 Mr= 829.71, Dc = 1.448 g/cm3, F（000） = 858 andμ（MoKa） = 0.514 mm-1. The final R = 0.0655 and wR = 0.1136 for 6603 observed reflections with 1 〉 2a（/） and R = 0.1136 and wR = 0.1747 for all data.展开更多
Two new coordination polymers,[Zn（bdc）（1,3-bimb）]n（1） and {[Mn2（ox）2（1,3,5tib）4/3]·4H2O}n（2）（H2ox = oxalic acid,H2bdc = terephthalic acid,1,3-bimb = 1,3-bis（imidazol-1ylmethyl）benzene,1,3,5-tib = 1...Two new coordination polymers,[Zn（bdc）（1,3-bimb）]n（1） and {[Mn2（ox）2（1,3,5tib）4/3]·4H2O}n（2）（H2ox = oxalic acid,H2bdc = terephthalic acid,1,3-bimb = 1,3-bis（imidazol-1ylmethyl）benzene,1,3,5-tib = 1,3,5-tri（imidazol-1-yl）benzene）,were synthesized and characterized by elemental analysis,IR,powder X-ray diffraction（PXRD）,and thermogravimetric（TG） analyses.X-ray diffracation analysis reveals that two kinds of zigzag chains [Zn（bdc）]n and [Zn（1,3-bimb）]n in compound 1 are interweaved to form a 3D 4-fold interpenetrated 66-dia framework.In compound 2,Mn（1） and Mn（2） are linked via 1,3,5-tib ligands to form two different nets of [Mn6（1,3,5-tib）6 ]n along the ab plane with inner-or outer-shape N–Mn–N angles,which are connected by 1D infinite [Mn2（ox）2 ]n chains via Mn–O bonds to result in a（3,3,3,4,4）-connected（4·8·10）3（4·82）3（4·83·102）6（82·104·3）3（83）4 topology.Moreover,the photoluminescence of 1 has been investigated.The crystal of 1 crystallizes in orthorhombic,space group Pna2 with a = 13.2267（6）,b = 9.1717（4）,c = 17.4492（8）,V = 2116.79（16）3,Z = 4,C22 H18N4O4 Zn,Mr = 467.77,Dc = 1.468 g/cm3,F（000） = 960 and μ（MoKα） = 1.197 mm-1.The final R = 0.0280 and wR = 0.0618 for 3695 observed reflections with I 2（I） and R = 0.0389 and wR = 0.0653 for all data.The crystal of 2 crystallizes in rhombohedral,space group R-3 with a = 22.080（8）,c = 31.19（2）,V = 13167（11） 3,Z = 18,C24 H25 Mn2 N8 O13,Mr = 743.40,Dc = 1.688 g/cm3,F（000） = 6822 and μ（MoKα） = 0.945 mm-1.The final R = 0.0429 and wR = 0.1035 for 5160 observed reflections with I 2（I） and R = 0.0824 and wR = 0.1244 for all data.展开更多
One novel 1-D copper（Ⅱ）-organic compound,namely {[Cu2（PP）2（CBPC）]2·7H2O}n（1,H2CBPC=1-[（2＇-carboxybiphenyl-4-yl）methyl]-2-propylimidazole-4-carboxylic acid,HPP=3-（2-pyridyl）pyrazole）,was synthesized ...One novel 1-D copper（Ⅱ）-organic compound,namely {[Cu2（PP）2（CBPC）]2·7H2O}n（1,H2CBPC=1-[（2＇-carboxybiphenyl-4-yl）methyl]-2-propylimidazole-4-carboxylic acid,HPP=3-（2-pyridyl）pyrazole）,was synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that the two Cu（Ⅱ） ions in the distorted dimer [Cu2（PP）2] of 1 are linked by the carboxylate oxygen atoms on the phenyl and imidazole rings,respectively,forming one interesting snake-like chain.Single-crystal X-ray analyses reveal that it crystallizes in monoclinic,space group C2/c with a=30.656（8）,b=12.715（3）,c=22.405（5）,β=122.758（3）°,V=7344（3）3,Z=4,Mr=1681.65,Dc=1.521 g/cm3,F（000）=3464,μ=1.221 mm-1,the final R=0.0453 and wR=0.1023 for 4617 observed reflections with Ⅰ 〉2σ（Ⅰ）.展开更多
One novel entangled cobalt compound, {[Co3（nbta）2（4,4＇-bpy）2（H2O）2]（H2O）2}n （1, H3nbta = 5-nitro-1,2,3-benzenetricarboxylic acid, 4,4＇-bpy = 4,4＇-bipyridyl）, was prepared and characterized by X-my diffrac...One novel entangled cobalt compound, {[Co3（nbta）2（4,4＇-bpy）2（H2O）2]（H2O）2}n （1, H3nbta = 5-nitro-1,2,3-benzenetricarboxylic acid, 4,4＇-bpy = 4,4＇-bipyridyl）, was prepared and characterized by X-my diffraction, magnetism, elemental analysis, XPS, TGA and IR spectroscopy. The crystal of 1 crystallizes in monoclinic, space group Pc with a = 13.0717（16）, b = 11.4167（14）, c = 15.9342（19） A, β = 90.5190（10）°, V= 2377.9（5） A3, Z= 2, C48H36Co3N8O20, Mr = 1221.64, Dc = 1.706 g/cm3, F（000） = 1242 and μ（MoKa） = 1.128 mm^-1. The final R = 0.0497 and wR = 0.1461 for 4185 observed reflections with I 〉 20（0 and R = 0.0721 and wR = 0.1619 for all data. X-ray diffraction analyses revealed that Co（l） is linked by the nbta3- ligands to form the ladder shape along the c axis, which is further extended into two-dimensional networks via the joint of Co（2） along the a axis. Moreover, these two dimensional motifs are interconnected by the 4,4＇-bpy bridges to form a complicated 3-D polymeric framework. Magnetic measurements revealed that compound 1 shows strong antiferromagnetic property.展开更多
Hydrothermal reactions of two imidazole derivatives （1,3,5-tib = 1,3,5-tris（1H- imidazol- 1 -yl）benzene, 1,4-bimb = 1,4-bis（1 H-imidazol- 1 -ylmethyl）benzene） and the ZnⅡ cations in the presence of oxalic acid ...Hydrothermal reactions of two imidazole derivatives （1,3,5-tib = 1,3,5-tris（1H- imidazol- 1 -yl）benzene, 1,4-bimb = 1,4-bis（1 H-imidazol- 1 -ylmethyl）benzene） and the ZnⅡ cations in the presence of oxalic acid （H2ox） afford two coordination polymers, namely, {[Zn（ox）（1,3,5- tib）]·2（H20）}n （1） and [Znl.5（OX）1.5（1,4-bimb）l.5]n （2）. Their structures have been determined by single-crystal X-ray diffraction analyses, elemental analyses, IR spectra, and powder X-ray diffraction （PXRD） analyses. Both complexes 1 and 2 are based on the 1D zigzag [Zn（ox）]n chains, and their final structures are controlled by the two different imidazole linkers, which expanded the structure along different directions, finally giving a 3D dia net for 1 and a 2D sql layer for 2. Moreover, the luminescent properties of 1 and 2 have been investigated.展开更多
A new polyoxomolybdate compound [Ag 3 （HL） 4 ]（PMo 12 O 40）] 1 （HL=3-（2-pyridyl）pyrazole） has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analys...A new polyoxomolybdate compound [Ag 3 （HL） 4 ]（PMo 12 O 40）] 1 （HL=3-（2-pyridyl）pyrazole） has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in triclinic,space group P1 with a=10.375（3）,b=12.076（3）,c=13.196（4）,α=84.170（4）,β=71.961（3）,γ=86.326（4）°,V=1563.1（7）3,C 32 H 28 Ag 3 Mo 12 N 12 O 40 P,M r=2726.52,D c=2.897 g/cm 3,μ（MoKα）=3.366 mm 1,F（000）=1284,Z=1,the final R=0.0587 and wR=0.1312 for 4139 observed reflections （I 2σ（Ⅰ））.X-ray diffraction analyses reveal that the PMo 12 O 40 3clusters in compound 1 are linked by four Ag 3 （HL） 4 3＋ units via the terminal oxygen atoms to form a two-dimensional architecture.The symmetrical unit of Ag 3 （HL） 4 3＋ exhibits two distinct Ag（Ⅰ） environments：a two-coordinate {AgN 2 } site and a five-coordinate {AgN 3 O 2 } site which links to two molybdate clusters.展开更多
A new polyoxomolybdate compound,namely {[MnII（L）（4,4？-Hbipy）（H2O）2]2 [Mo5O15（PO4）2]}.2H2O 1（L = 3-（2-pyridyl）pyrazole,4,4＇-Hbipy = protonated 4,4＇-bipyridine）,was designed and synthesized under hydrothe...A new polyoxomolybdate compound,namely {[MnII（L）（4,4？-Hbipy）（H2O）2]2 [Mo5O15（PO4）2]}.2H2O 1（L = 3-（2-pyridyl）pyrazole,4,4＇-Hbipy = protonated 4,4＇-bipyridine）,was designed and synthesized under hydrothermal conditions.Single-crystal X-ray diffraction analysis result reveals that the [Mo5O15（PO4）2]6-cluster in compound 1 links to two MnII cations via the oxygen of PO43-,which is further coordinated by one 3-（2-pyridyl）pyrazole,one 4,4＇-Hbipyridine,and two water molecules.展开更多
A new polyoxomolybdate compound [Zn（HL）2（Mo8O26）（4,4＇-Bipy）]·（4,4＇-Bipy） （HL = 3-（2-pyridyl）pyrazole, 4,4＇-Bipy = 4,4＇-bipyridine） 1 has been hydrothermally synthesized and structurally characteri...A new polyoxomolybdate compound [Zn（HL）2（Mo8O26）（4,4＇-Bipy）]·（4,4＇-Bipy） （HL = 3-（2-pyridyl）pyrazole, 4,4＇-Bipy = 4,4＇-bipyridine） 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, TG and IR spectroscopy. The compound crystallizes in monoclinic, space group C2/c with a = 18.060（4）, b = 13.870（3）, c = 19.360（4） A, β = 93.50（3）°, V = 4840.5（17） 3, C36H30Mo8N10O26Zn, Mr = 1851.59, Dc = 2.541 g/cm^3, μ（MoKα） = 2.589 mm·1, F（000） = 3560, Z = 4, the final R = 0.0328 and wR = 0.0870 for 4005 observed reflections （I 〉 2σ（I））. X-ray diffraction analyses reveal that compound 1 is constructed from Mo8O264-units linked by Zn（HL）22＋ and 4,4＇-Bipy. Mo8O264-is connected by Zn（HL）2^2＋ via terminal oxygen atoms along the [010] axis forming chains, which are further linked by 4,4＇-Bipy along the [001] axis forming a two-dimensional network structure.展开更多
Solvothermal reaction of aromatic 2,6-bis（4＇-carboxyphenyl）-4-phenylpyridine （H2bpp） ligand and nickel cation in the presence of 1,10-phenanthroline （phen） affords one new coordination polymer （CPs）, [Ni（bp...Solvothermal reaction of aromatic 2,6-bis（4＇-carboxyphenyl）-4-phenylpyridine （H2bpp） ligand and nickel cation in the presence of 1,10-phenanthroline （phen） affords one new coordination polymer （CPs）, [Ni（bpp）（phen）（H20]n （1）. The structure has been determined by single-crystal X-ray diffraction analysis and further characterized by elemental analyses, IR, PXRD and luminescence. Ions of Nin in 1 are linked via bpp2 to form chains, which are further connected through non-covalent interactions （including O-H...O and n...zr interactions） to form a 3D packing diagram. The crystal ofl crystallizes in triclinic, space group PI with a = 10.998（10）, b = 12.019（10）, c = 12.485（11） A, a = 75.774（14）, β = 85.828（16）, y = 66.542（13）°, V= 1467（2）/k^3, Z = 2, C38H26N2O5Ni, Mr= 649.32, Dc = 1.470 g/cm^3, F（000） = 672 andμ（MoKa） = 0.721 mm-1. The final R = 0.0692 and wR = 0.1048 for 5116 observed reflections with/〉 20（/） andR = 0.0874 and wR = 0.1364 for all data.展开更多
Two new polyoxomolybdate compounds,namely（CuIIL2）2[CuⅡ（HL）2]2[Mo8O26（HL）2].（H2O）4（1） and [CuⅡ（HL）2]2[β-Mo8O26]（HL）2（2）（HL=imidazole）,were designed and synthesized under hydrothermal conditions.X-r...Two new polyoxomolybdate compounds,namely（CuIIL2）2[CuⅡ（HL）2]2[Mo8O26（HL）2].（H2O）4（1） and [CuⅡ（HL）2]2[β-Mo8O26]（HL）2（2）（HL=imidazole）,were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one Mo8O26（HL）24-cluster,two CuL2,two Cu（HL）22＋,and four disassociated water molecules;and compound 2 is constructed by one β-Mo8O264-cluster,two Cu（HL）22＋,and two uncoordinated imidazole molecules.展开更多
Hydrothermal reactions of three aromatic polycarboxylic acids and the transitional metal cations in the presence of phen and 1,4-bib afford three new coordination polymers： [Cd2（bpp）1.5（Hbpp）（phen）2]n （1）, [...Hydrothermal reactions of three aromatic polycarboxylic acids and the transitional metal cations in the presence of phen and 1,4-bib afford three new coordination polymers： [Cd2（bpp）1.5（Hbpp）（phen）2]n （1）, [Mn3（Htptc）2（phen）2（H2O）2]n （2）, and {[Cu（btc）0.5（1,4- bib）]·2H2O}n（3） （H2bpp = 2,6-bis（4＇-carboxyphenyl）-4-phenylpyridine, H4tptc = terphenyl-2,5,2＇,5＇-tetracar- boxylic acid, H4btc =biphenyl-2,2＇,4,4＇-tetracarboxylic acid, phen =1,10-phenanthroline, and 1,4-bib = 1,4-bis（1H-imidazol-1-yl）benzene）. Their structures have been determined by single- crystal X-ray diffraction analyses, elemental analyses, IR spectra, and powder X-ray diffraction （PXRD） analyses. In compound 1, the CdII cations are linked by bpp2- to form one ladder structure, based on which a 3D network is constructed with the help of non-covalent interactions. The topology of 2 is a 3D （3,4,5）-connected framework with the Point Schl？fli symbol of （42.6）2（43.62.8）（45.64.8）2. Compound 3 shows an unprecedented 3D （4,4）-connected framework with the Point Schl？fli symbol of （64.82）2（65.8）. Moreover, the luminescent property of 1 has been investigated.展开更多
A new polyoxomolybdate compound [Mn II （L） 2 （Mo 8 O 26） 0.5 ] 2n （1,L=3-（2-pyridyl）pyrazole） has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental an...A new polyoxomolybdate compound [Mn II （L） 2 （Mo 8 O 26） 0.5 ] 2n （1,L=3-（2-pyridyl）pyrazole） has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in the triclinic system,space group P1 with a=10.063（4）,b=11.554（5）,c=11.554（5）,α=88.89,β=74.839（4）,γ=74.839（4）o,V=1249.8（9） 3,C 16 H 14 MnMo 4 N 6 O 13,M r=937.03,D c=2.490 g/cm 3,μ（MoKα）=2.521 mm 1,F（000）=898,Z=2,the final R=0.0390 and wR=0.0970 for 4000 observed reflections （I 2σ（Ⅰ））.Single-crystal X-ray diffraction analysis results reveal that compound 1 owns a chain structure based on β-[Mo 8 O 26 ] 4anions,which are linked by Mn II （L） 2 units via the terminal oxygen atoms.展开更多
基金supported from the Opening Foundation of Shandong Provincial Key Laboratory of Fluorine Chemistry and Chemical Materials,the National Natural Science Foundation of China(20873150)the Natural Science Foundation of Shandong Province(ZR2010BQ023)the Outstanding Middle-aged Scientists Foundation of Shandong Province(2008BS04031)
文摘Solvothermal reaction of aromatic terphenyl-2,5,2＇,5＇-tetracarboxylic acid （Hnqptc） ligand and the transitional metal cation of Mn11 in the presence of 3-（2-pyridyl）pyrazole （pp） affords one new coordination polymer, [Mn（qptc）0.5（pp）2]n·n（H2O） （1）. The structure has been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR, TGA, and magnetism. The carboxyl groups of qptc4 exhibit a μ1-η1：η0 coordination mode, and the qptc4- acts as a H-shaped ligand linking the Mn11 centers together to form a 2D polymeric [Mn（qptc）0.5]n layer. The crystal of 1 crystallizes in orthorhombic, space group Pbca with a = 9.3119（12）, b = 20.848（3）, c = 26.134（3） A, V= 5073.4（11） A3, Z= 8, C27HIgMnN6O5,Mr=562.42, Dc = 1.473 g/cm3, F（000） = 2304 and μ（MoKa） = 0.571 mm-1. The final R = 0.0468 and wR = 0.1196 for 4429 observed reflections with I 〉 2σ（I） and R = 0.0797 and wR = 0.1383 for all data.
基金supported by the National Ministry of Science and Technology of China (No. 2001CB6105-07)
文摘One new polyoxometalate compound connected via cobalt/potassium cations,namely H5K{[Co（H2O）5]2（H2Mo3.24W8.76O42）}·19H2O 1,was prepared and characterized by ele- mental analysis and IR spectroscopy. Single-crystal X-ray diffraction analysis result reveals that anions of {[Co（H2O）5]2（H2Mo3.24W8.76O42）}6- in compound 1 are linked by potassium cations to form one- dimensional chain,based on which a three-dimensional network is further constructed with the help of hydrogen bonds. Crystal data： H67Co2KMo3.24O72W8.76,Mr = 3297.87,monoclinic,C2/c,a = 19.0126（10）,b = 16.6025（5）,c = 19.1908（10）A,β = 106.713（1）°,V = 5801.8（5） A^3,Z = 4,Dc = 3.755 g/cm^3,F（000） = 5961,μ = 18.730 mm^-1,R = 0.0569 and wR = 0.1437 （I 〉 2σ（I））.
基金Acknowledgments: The authors thank the Chinese Academy of Sciences the National Science Foundation of China (20073048)the NSF of Fujian for financial support
文摘The new copper(II) complex Cu(C13H9N3O2Br)2H2O (N-(2-hydroxy-5-bromo- benzoyl)-N-(picolinylidene)hydrazine is abbreviated as HL ) was obtained from the refluxing solution of Cu(CH3COO)2H2O and HL in the ethanol-N, N-dimethylformamide mix solvent. Crystal data: triclinic, space group P , a = 10.8620(3), b = 11.7453 (3), c = 12.4417(2) ? ?= 62.255(0), ?= 79.097(2), ?= 86.764(2)? V = 1378.52(6) ?, Z = 2, Mr = 719.835, Dc = 1.734 g/cm3, F(000) = 714, (MoK) = 3.739 mm-1, T = 293(2) K, final R = 0.0594 and wR = 0.1416 for 2943 observed reflections with I > 2.0(I). The structure of Cu(C13H9N3O2Br)2H2O has been determined by X-ray analysis and revealed that two L-1 ligands coordinate to the copper(Ⅱ) ion through two oxygen and two nitrogen atoms from the hydrazine groups and two pyridine nitrogen atoms to form an elongated and distorted square-bipyramidal environment for Cu(Ⅱ). The complex is also characterized by 1H NMR spectroscopies
基金supported by Financial support from the Natural Science Foundation of Shandong (BR2010BQ023) and Qilu Normal University
文摘One novel copper（II）-organic compound,namely Cu[Cu2（PP）2]（CBPC）2]·2（H2O）（1,H2CBPC = 1-[（2＇-carboxybiphenyl-4-yl）methyl]-2-propylimidazole-4-carboxylic acid,HPP = 3-（2-pyridyl）pyrazole）,was designed and synthesized under hydrothermal conditions.X-ray diffraction analysis reveals that two Cu（II）ions in the quasi-planar dimmer of [Cu2（PP）2] are linked by the carboxylate oxygen atoms on the phenyl ring and the imidazole ring,respectively,yielding one snake-shaped structure.Magnetic measurements reveal that compound 1 shows the strongly antiferromagnetic property.Crystal data of 1：C58H52Cu3N10O10,Mr = 1239.72,monoclinic,P21/c,a = 14.900（7）,b = 15.029（7）,c = 12.308（6）,β = 102.519（9）o,V = 2691（2）3,Z = 2,Dc = 1.530 g/cm3,F（000）= 1274,μ = 1.246 mm-1,R = 0.0416,wR = 0.0780（I 2σ（I））and S = 0.999.
基金supported by the National Natural Science Foundation of China(20873150)the Natural Science Foundation of Shandong Province(ZR2010BQ023)
文摘One novel cobalt coordination polymer, {[Co（HTCB）（4,4＇btb）]＇HzO}n （1, H3TCB = 1,3,5-tris（4-carboxyphenyl）benzene, 4,4＇-btb = 4,4＇-bis（1,2,4-triazol-3-yl）biphenyl）, has been synthesized and characterized by elemental analysis, IR, powder X-ray diffraction （PXRD）, and thermogravimetric （TG） analyses. X-ray diffraction analysis reveals that complex 1 is a 2D 2-fold interpenetrated {44,62}-sql [Co（HTCB）（4,4＇-btb）] sheet based on the 1D [Co（HTCB）]n chains and 1D [Co（4,4＇-btb）]n chains. The crystal of 1 crystallizes in triclinic, space group P1 with a = 9.529（12）, b = 13.914（16）, c = 14.906（17） A, V= 1903（4） A3, Z = 2, C45H34N6CoO71 Mr= 829.71, Dc = 1.448 g/cm3, F（000） = 858 andμ（MoKa） = 0.514 mm-1. The final R = 0.0655 and wR = 0.1136 for 6603 observed reflections with 1 〉 2a（/） and R = 0.1136 and wR = 0.1747 for all data.
基金Supported by the National Natural Science Foundation of China(20873150)Natural Science Foundation of Shandong Province(ZR2010BQ023)
文摘Two new coordination polymers,[Zn（bdc）（1,3-bimb）]n（1） and {[Mn2（ox）2（1,3,5tib）4/3]·4H2O}n（2）（H2ox = oxalic acid,H2bdc = terephthalic acid,1,3-bimb = 1,3-bis（imidazol-1ylmethyl）benzene,1,3,5-tib = 1,3,5-tri（imidazol-1-yl）benzene）,were synthesized and characterized by elemental analysis,IR,powder X-ray diffraction（PXRD）,and thermogravimetric（TG） analyses.X-ray diffracation analysis reveals that two kinds of zigzag chains [Zn（bdc）]n and [Zn（1,3-bimb）]n in compound 1 are interweaved to form a 3D 4-fold interpenetrated 66-dia framework.In compound 2,Mn（1） and Mn（2） are linked via 1,3,5-tib ligands to form two different nets of [Mn6（1,3,5-tib）6 ]n along the ab plane with inner-or outer-shape N–Mn–N angles,which are connected by 1D infinite [Mn2（ox）2 ]n chains via Mn–O bonds to result in a（3,3,3,4,4）-connected（4·8·10）3（4·82）3（4·83·102）6（82·104·3）3（83）4 topology.Moreover,the photoluminescence of 1 has been investigated.The crystal of 1 crystallizes in orthorhombic,space group Pna2 with a = 13.2267（6）,b = 9.1717（4）,c = 17.4492（8）,V = 2116.79（16）3,Z = 4,C22 H18N4O4 Zn,Mr = 467.77,Dc = 1.468 g/cm3,F（000） = 960 and μ（MoKα） = 1.197 mm-1.The final R = 0.0280 and wR = 0.0618 for 3695 observed reflections with I 2（I） and R = 0.0389 and wR = 0.0653 for all data.The crystal of 2 crystallizes in rhombohedral,space group R-3 with a = 22.080（8）,c = 31.19（2）,V = 13167（11） 3,Z = 18,C24 H25 Mn2 N8 O13,Mr = 743.40,Dc = 1.688 g/cm3,F（000） = 6822 and μ（MoKα） = 0.945 mm-1.The final R = 0.0429 and wR = 0.1035 for 5160 observed reflections with I 2（I） and R = 0.0824 and wR = 0.1244 for all data.
基金supported by the Chinese Academy of Sciences (KJCX2-YW-M05,KJCX2-YW-319)the Natural Science Foundation of Fujian Province (2007HZ0001-1,2009HZ0004-1)
文摘One novel 1-D copper（Ⅱ）-organic compound,namely {[Cu2（PP）2（CBPC）]2·7H2O}n（1,H2CBPC=1-[（2＇-carboxybiphenyl-4-yl）methyl]-2-propylimidazole-4-carboxylic acid,HPP=3-（2-pyridyl）pyrazole）,was synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that the two Cu（Ⅱ） ions in the distorted dimer [Cu2（PP）2] of 1 are linked by the carboxylate oxygen atoms on the phenyl and imidazole rings,respectively,forming one interesting snake-like chain.Single-crystal X-ray analyses reveal that it crystallizes in monoclinic,space group C2/c with a=30.656（8）,b=12.715（3）,c=22.405（5）,β=122.758（3）°,V=7344（3）3,Z=4,Mr=1681.65,Dc=1.521 g/cm3,F（000）=3464,μ=1.221 mm-1,the final R=0.0453 and wR=0.1023 for 4617 observed reflections with Ⅰ 〉2σ（Ⅰ）.
基金supported by the National Natural Science Foundation of China (20873163)the Natural Science Foundation of Shandong Province (BR2010BQ023)+1 种基金Shandong Provincial Education Department (J09LB55)Qilu Normal University
文摘One novel entangled cobalt compound, {[Co3（nbta）2（4,4＇-bpy）2（H2O）2]（H2O）2}n （1, H3nbta = 5-nitro-1,2,3-benzenetricarboxylic acid, 4,4＇-bpy = 4,4＇-bipyridyl）, was prepared and characterized by X-my diffraction, magnetism, elemental analysis, XPS, TGA and IR spectroscopy. The crystal of 1 crystallizes in monoclinic, space group Pc with a = 13.0717（16）, b = 11.4167（14）, c = 15.9342（19） A, β = 90.5190（10）°, V= 2377.9（5） A3, Z= 2, C48H36Co3N8O20, Mr = 1221.64, Dc = 1.706 g/cm3, F（000） = 1242 and μ（MoKa） = 1.128 mm^-1. The final R = 0.0497 and wR = 0.1461 for 4185 observed reflections with I 〉 20（0 and R = 0.0721 and wR = 0.1619 for all data. X-ray diffraction analyses revealed that Co（l） is linked by the nbta3- ligands to form the ladder shape along the c axis, which is further extended into two-dimensional networks via the joint of Co（2） along the a axis. Moreover, these two dimensional motifs are interconnected by the 4,4＇-bpy bridges to form a complicated 3-D polymeric framework. Magnetic measurements revealed that compound 1 shows strong antiferromagnetic property.
基金supported by the National Natural Science Foundation of China(20873150)the Natural Science Foundation of Shandong Province(ZR2010BL012,ZR2010BQ023)
文摘Hydrothermal reactions of two imidazole derivatives （1,3,5-tib = 1,3,5-tris（1H- imidazol- 1 -yl）benzene, 1,4-bimb = 1,4-bis（1 H-imidazol- 1 -ylmethyl）benzene） and the ZnⅡ cations in the presence of oxalic acid （H2ox） afford two coordination polymers, namely, {[Zn（ox）（1,3,5- tib）]·2（H20）}n （1） and [Znl.5（OX）1.5（1,4-bimb）l.5]n （2）. Their structures have been determined by single-crystal X-ray diffraction analyses, elemental analyses, IR spectra, and powder X-ray diffraction （PXRD） analyses. Both complexes 1 and 2 are based on the 1D zigzag [Zn（ox）]n chains, and their final structures are controlled by the two different imidazole linkers, which expanded the structure along different directions, finally giving a 3D dia net for 1 and a 2D sql layer for 2. Moreover, the luminescent properties of 1 and 2 have been investigated.
基金supported by the Science and Technology Research Projects of the Education Department of Jilin Province (No. 2009. 272)
文摘A new polyoxomolybdate compound [Ag 3 （HL） 4 ]（PMo 12 O 40）] 1 （HL=3-（2-pyridyl）pyrazole） has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in triclinic,space group P1 with a=10.375（3）,b=12.076（3）,c=13.196（4）,α=84.170（4）,β=71.961（3）,γ=86.326（4）°,V=1563.1（7）3,C 32 H 28 Ag 3 Mo 12 N 12 O 40 P,M r=2726.52,D c=2.897 g/cm 3,μ（MoKα）=3.366 mm 1,F（000）=1284,Z=1,the final R=0.0587 and wR=0.1312 for 4139 observed reflections （I 2σ（Ⅰ））.X-ray diffraction analyses reveal that the PMo 12 O 40 3clusters in compound 1 are linked by four Ag 3 （HL） 4 3＋ units via the terminal oxygen atoms to form a two-dimensional architecture.The symmetrical unit of Ag 3 （HL） 4 3＋ exhibits two distinct Ag（Ⅰ） environments：a two-coordinate {AgN 2 } site and a five-coordinate {AgN 3 O 2 } site which links to two molybdate clusters.
基金supported by the Science and Technology Research Projects of the Education Department of Jilin Province (No.2009.272)
文摘A new polyoxomolybdate compound,namely {[MnII（L）（4,4？-Hbipy）（H2O）2]2 [Mo5O15（PO4）2]}.2H2O 1（L = 3-（2-pyridyl）pyrazole,4,4＇-Hbipy = protonated 4,4＇-bipyridine）,was designed and synthesized under hydrothermal conditions.Single-crystal X-ray diffraction analysis result reveals that the [Mo5O15（PO4）2]6-cluster in compound 1 links to two MnII cations via the oxygen of PO43-,which is further coordinated by one 3-（2-pyridyl）pyrazole,one 4,4＇-Hbipyridine,and two water molecules.
基金supported by the Science and Technology Research Projects of the Education Department of Jilin Province (No. 2009. 272)
文摘A new polyoxomolybdate compound [Zn（HL）2（Mo8O26）（4,4＇-Bipy）]·（4,4＇-Bipy） （HL = 3-（2-pyridyl）pyrazole, 4,4＇-Bipy = 4,4＇-bipyridine） 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, TG and IR spectroscopy. The compound crystallizes in monoclinic, space group C2/c with a = 18.060（4）, b = 13.870（3）, c = 19.360（4） A, β = 93.50（3）°, V = 4840.5（17） 3, C36H30Mo8N10O26Zn, Mr = 1851.59, Dc = 2.541 g/cm^3, μ（MoKα） = 2.589 mm·1, F（000） = 3560, Z = 4, the final R = 0.0328 and wR = 0.0870 for 4005 observed reflections （I 〉 2σ（I））. X-ray diffraction analyses reveal that compound 1 is constructed from Mo8O264-units linked by Zn（HL）22＋ and 4,4＇-Bipy. Mo8O264-is connected by Zn（HL）2^2＋ via terminal oxygen atoms along the [010] axis forming chains, which are further linked by 4,4＇-Bipy along the [001] axis forming a two-dimensional network structure.
基金supported by the National Natural Science Foundation of China (No.21101097)Natural Science Foundation of Shandong Province (ZR2010BQ023)+1 种基金the State Key Laboratory of Solid Lubrication (No.0701)the Project of Education Department of Shandong Province (No.J10LB53)
文摘Solvothermal reaction of aromatic 2,6-bis（4＇-carboxyphenyl）-4-phenylpyridine （H2bpp） ligand and nickel cation in the presence of 1,10-phenanthroline （phen） affords one new coordination polymer （CPs）, [Ni（bpp）（phen）（H20]n （1）. The structure has been determined by single-crystal X-ray diffraction analysis and further characterized by elemental analyses, IR, PXRD and luminescence. Ions of Nin in 1 are linked via bpp2 to form chains, which are further connected through non-covalent interactions （including O-H...O and n...zr interactions） to form a 3D packing diagram. The crystal ofl crystallizes in triclinic, space group PI with a = 10.998（10）, b = 12.019（10）, c = 12.485（11） A, a = 75.774（14）, β = 85.828（16）, y = 66.542（13）°, V= 1467（2）/k^3, Z = 2, C38H26N2O5Ni, Mr= 649.32, Dc = 1.470 g/cm^3, F（000） = 672 andμ（MoKa） = 0.721 mm-1. The final R = 0.0692 and wR = 0.1048 for 5116 observed reflections with/〉 20（/） andR = 0.0874 and wR = 0.1364 for all data.
基金supported by Financial support from the Natural Science Foundation of Shandong Province (BR2010BQ023)Shandong Provincial Education Department,and Qilu Normal University
文摘Two new polyoxomolybdate compounds,namely（CuIIL2）2[CuⅡ（HL）2]2[Mo8O26（HL）2].（H2O）4（1） and [CuⅡ（HL）2]2[β-Mo8O26]（HL）2（2）（HL=imidazole）,were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one Mo8O26（HL）24-cluster,two CuL2,two Cu（HL）22＋,and four disassociated water molecules;and compound 2 is constructed by one β-Mo8O264-cluster,two Cu（HL）22＋,and two uncoordinated imidazole molecules.
基金supported by the National Natural Science Foundation of China(20873150)the Natural Science Foundation of Shandong Province(ZR2010BL012,ZR2010BQ023)
文摘Hydrothermal reactions of three aromatic polycarboxylic acids and the transitional metal cations in the presence of phen and 1,4-bib afford three new coordination polymers： [Cd2（bpp）1.5（Hbpp）（phen）2]n （1）, [Mn3（Htptc）2（phen）2（H2O）2]n （2）, and {[Cu（btc）0.5（1,4- bib）]·2H2O}n（3） （H2bpp = 2,6-bis（4＇-carboxyphenyl）-4-phenylpyridine, H4tptc = terphenyl-2,5,2＇,5＇-tetracar- boxylic acid, H4btc =biphenyl-2,2＇,4,4＇-tetracarboxylic acid, phen =1,10-phenanthroline, and 1,4-bib = 1,4-bis（1H-imidazol-1-yl）benzene）. Their structures have been determined by single- crystal X-ray diffraction analyses, elemental analyses, IR spectra, and powder X-ray diffraction （PXRD） analyses. In compound 1, the CdII cations are linked by bpp2- to form one ladder structure, based on which a 3D network is constructed with the help of non-covalent interactions. The topology of 2 is a 3D （3,4,5）-connected framework with the Point Schl？fli symbol of （42.6）2（43.62.8）（45.64.8）2. Compound 3 shows an unprecedented 3D （4,4）-connected framework with the Point Schl？fli symbol of （64.82）2（65.8）. Moreover, the luminescent property of 1 has been investigated.
基金supported by the Science and Technology Research Projects of the Education Department of Jilin Province (No. 2009. 272)
文摘A new polyoxomolybdate compound [Mn II （L） 2 （Mo 8 O 26） 0.5 ] 2n （1,L=3-（2-pyridyl）pyrazole） has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in the triclinic system,space group P1 with a=10.063（4）,b=11.554（5）,c=11.554（5）,α=88.89,β=74.839（4）,γ=74.839（4）o,V=1249.8（9） 3,C 16 H 14 MnMo 4 N 6 O 13,M r=937.03,D c=2.490 g/cm 3,μ（MoKα）=2.521 mm 1,F（000）=898,Z=2,the final R=0.0390 and wR=0.0970 for 4000 observed reflections （I 2σ（Ⅰ））.Single-crystal X-ray diffraction analysis results reveal that compound 1 owns a chain structure based on β-[Mo 8 O 26 ] 4anions,which are linked by Mn II （L） 2 units via the terminal oxygen atoms.
