The title compound, [Ni（C8N3H7）3]4[Mo8O26]2·6H2O 1, has been synthesized from the reaction of 2-（1H-pyrazol-3-yl）-pyridine （L） with （NH4）2MoO4·2H2O and NiCl2·6H2O. Elemental analysis, IR, UV spe...The title compound, [Ni（C8N3H7）3]4[Mo8O26]2·6H2O 1, has been synthesized from the reaction of 2-（1H-pyrazol-3-yl）-pyridine （L） with （NH4）2MoO4·2H2O and NiCl2·6H2O. Elemental analysis, IR, UV spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure of the compound. Crystal data： C96H96Mo16N36Ni4O58, Mr = 4451.97, monoclinic system, space group P21/n, a = 20.846（5）, b = 14.825（5）, c = 23.122（5） A ,β= 91.594（5）°, V = 7143（3）A^3, Z = 2, F（000） = 4344, Dc = 2.070 g/cm^3,μ = 1.968 mm^-1, R = 0.0452 and wR = 0.1056 for 17102 independent reflections （Rint = 0.0442） and 11074 observed reflections （I 〉 2σ（I））. Structural analysis indicates that two kinds of octamolybdates （[α-Mo8026]^4- and [β-Mo8026]^4-） co-exist in the compound. This is the first example of a supramolecular structure containing L complex as well as both α- and β-octamolybdate clusters.展开更多
The reaction of picolinic acid (Hpic) and (n-Bu_4N)_4[Mo_8O_(26)] in thepresence of CH_3CN gave a supramolecular compound (n-Bu_4N)_2[Mo_2O_6(pic)_2] (1), and its structurewas characterized by elemental analysis, IR s...The reaction of picolinic acid (Hpic) and (n-Bu_4N)_4[Mo_8O_(26)] in thepresence of CH_3CN gave a supramolecular compound (n-Bu_4N)_2[Mo_2O_6(pic)_2] (1), and its structurewas characterized by elemental analysis, IR spectra and single crystal X-ray diffraction analysis.The single crystal X-ray diffraction study shows that the crystal is in monoclinic crystal system,P2_1/c space group with cell parameters a = 0.9941(2), b = 1.3719(2), c = 1.8824(2) nm, β = 100.840(10)°, M_r = 508.50, V = 2.5214(9) nm^3, F(000) = 1072. Compound 1 is a dimer through two μ_2-Obridging to two MoO_3(pic)^- unit, then connected one-dimensional anion-chain by unclassicalhydrogen bonding, and the anion-chain across the channels formed via (n-Bu_4N)^+ cations. By meansof unclassical hydrogen bonding, the anion-chain and cation-channels assemble into three-dimensionalsupramolecular networks.展开更多
基金supported by the National Natural Science Foundation of China (No. 20671016)Education Committee of Jilin Province "11th Five-year Plan" Natural Science Foundation (No. 2006124)
文摘The title compound, [Ni（C8N3H7）3]4[Mo8O26]2·6H2O 1, has been synthesized from the reaction of 2-（1H-pyrazol-3-yl）-pyridine （L） with （NH4）2MoO4·2H2O and NiCl2·6H2O. Elemental analysis, IR, UV spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure of the compound. Crystal data： C96H96Mo16N36Ni4O58, Mr = 4451.97, monoclinic system, space group P21/n, a = 20.846（5）, b = 14.825（5）, c = 23.122（5） A ,β= 91.594（5）°, V = 7143（3）A^3, Z = 2, F（000） = 4344, Dc = 2.070 g/cm^3,μ = 1.968 mm^-1, R = 0.0452 and wR = 0.1056 for 17102 independent reflections （Rint = 0.0442） and 11074 observed reflections （I 〉 2σ（I））. Structural analysis indicates that two kinds of octamolybdates （[α-Mo8026]^4- and [β-Mo8026]^4-） co-exist in the compound. This is the first example of a supramolecular structure containing L complex as well as both α- and β-octamolybdate clusters.
文摘The reaction of picolinic acid (Hpic) and (n-Bu_4N)_4[Mo_8O_(26)] in thepresence of CH_3CN gave a supramolecular compound (n-Bu_4N)_2[Mo_2O_6(pic)_2] (1), and its structurewas characterized by elemental analysis, IR spectra and single crystal X-ray diffraction analysis.The single crystal X-ray diffraction study shows that the crystal is in monoclinic crystal system,P2_1/c space group with cell parameters a = 0.9941(2), b = 1.3719(2), c = 1.8824(2) nm, β = 100.840(10)°, M_r = 508.50, V = 2.5214(9) nm^3, F(000) = 1072. Compound 1 is a dimer through two μ_2-Obridging to two MoO_3(pic)^- unit, then connected one-dimensional anion-chain by unclassicalhydrogen bonding, and the anion-chain across the channels formed via (n-Bu_4N)^+ cations. By meansof unclassical hydrogen bonding, the anion-chain and cation-channels assemble into three-dimensionalsupramolecular networks.
