A novel octamolybdate complex, [Fe(2,2?bipy)3]2[Mo8O26]6H2O has been synthesized via the hydrothermal technique, and it crystallizes in monoclinic, space group P21/c with two molecules in a unit cell: a = 1.21512(5), ...A novel octamolybdate complex, [Fe(2,2?bipy)3]2[Mo8O26]6H2O has been synthesized via the hydrothermal technique, and it crystallizes in monoclinic, space group P21/c with two molecules in a unit cell: a = 1.21512(5), b = 1.36840(5), c = 2.18823(9) nm, b = 90.515(1), Mr = 2340.42, Z = 2, V = 3.6384(2) nm3, Dc = 2.136 g/cm3, F(000) = 2296, l(MoKa) = 0.071073 nm, = 1.813 mm-1, R = 0.0719 and wR = 0.1093 for 4058 observed reflections with I≥2s(I). The structure is characterized by the co-existence of octahedral [Fe(2,2?bipy)3]2+ cations and b-octamolybdate [Mo8O26]4- anions. The magnetic susceptibility data show a Curie-Weiss paramagnetic behavior (q = -5.201 K) in accordance with the spin-only ground state of FeⅡ ions. IR, UV-Vis, and EPR spectra are also briefly noted in this paper.展开更多
[{Cu（phen）（DMF）2}2（β-Mo8O26）] 1 （C36H44Cu2Mo8N8O30, Mr = 1963.39, phen =- 1,10-phenanthroline） and [Cu（phen）2]2[{Cu（phen）}2Mo8O26] 2 （C72H48Cu4Mo8N12O26, Mr = 2518.90） have been synthesized from （Bu4N...[{Cu（phen）（DMF）2}2（β-Mo8O26）] 1 （C36H44Cu2Mo8N8O30, Mr = 1963.39, phen =- 1,10-phenanthroline） and [Cu（phen）2]2[{Cu（phen）}2Mo8O26] 2 （C72H48Cu4Mo8N12O26, Mr = 2518.90） have been synthesized from （Bu4N）2[Mo6O19], Cu（NO3）2·3H2O and phen using solution method and under solvothermal condition, respectively. Both compounds 1 and 2 are structurally characterized by elemental analyses, IR and single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic system, space group P21/n, with a = 16.3347（13）, b = 9.861（1）, c = 17.2827（14） A, β=99.099（4）°, V= 2748.8（3） A3, Z = 2, Dc= 2.372 g/cm^3, F（000） =1900 and μ= 2.614 mm^-1. X-ray diffraction analysis reveals that compound 1 consists of discrete {[Cu（phen）（DMF）2]2（β-Mo8O26）} clusters constructed from β-[Mo8O26]^4- subunits covalently bound to two [Cu（phen）（DMF）2]^2- coordination groups. Compound 2 crystallizes in the monoclinic system, space group C2/c, with a = 33.1401（9）, b = 16.4508（5）, c = 16.2622（4） A, β= 119.2460（10）°, V = 7735.7（4） A3, Z = 4, Dc = 2.163 g/cm^3, F（000） = 4896 and μ= 2.413mm^-1. X-ray diffraction analysis reveals that compound 2 consists of a centrosymmetric β-octamolybdate-supported complex anion [ {Cu（phen）}2Mo8O26] and two bis-phenanthroline Cu（I） cations.展开更多
A nickel-1,10-phenanthroline complex supported on an octamolybdate, [{Ni(phen)2}2(ξ-Mo8O26)], has been hydrothermally synthesized with MoO3, H2MoO4, Ni(OAc)2 · 6H2O and 1,10-phenathroline (1,10-phen) as raw mate...A nickel-1,10-phenanthroline complex supported on an octamolybdate, [{Ni(phen)2}2(ξ-Mo8O26)], has been hydrothermally synthesized with MoO3, H2MoO4, Ni(OAc)2 · 6H2O and 1,10-phenathroline (1,10-phen) as raw materials. The crystals of the compound belong to mono-clinic P21/n space group, a= 1.2952(2), b = 1.6659(10), c= 1.3956(12) nm, β=106.273(8)°, V = 2.8906(5) nm3, Z = 2. 5604 observable reflections (/>2σ(/)) were used for structure resolution and refinements to converge to final R1 = 0.0414, wR2 = 0.0815. The result of structure determination shows that the compound contains octamolybdate possessing a novel structure type (named as ξ-isomer). The feature of ξ-[Mo8O26]4- is that it is composed of Mo6O6 ring and two MoO6 octa-hedra located at cap positions on opposite faces. The Mo6O6 ring contains two octahedral and four trigonal-bipyramidal MovI atoms. Each ξ-[Mo8O26]4- unit is bonded with two [Ni(phen)2]2+ through terminal oxygen atoms of octahedral and neighbouring trigonal-bipyramidal Mo atom in the Mo6O6 ring. IR and UV-Vis spectra of the compound were measured and its electronic structure was studied by EHMO method.展开更多
基金This work was supported by the Introduction of Overseas Elitists Program (No.IB990168) the Chinese Academy of Sciences
文摘A novel octamolybdate complex, [Fe(2,2?bipy)3]2[Mo8O26]6H2O has been synthesized via the hydrothermal technique, and it crystallizes in monoclinic, space group P21/c with two molecules in a unit cell: a = 1.21512(5), b = 1.36840(5), c = 2.18823(9) nm, b = 90.515(1), Mr = 2340.42, Z = 2, V = 3.6384(2) nm3, Dc = 2.136 g/cm3, F(000) = 2296, l(MoKa) = 0.071073 nm, = 1.813 mm-1, R = 0.0719 and wR = 0.1093 for 4058 observed reflections with I≥2s(I). The structure is characterized by the co-existence of octahedral [Fe(2,2?bipy)3]2+ cations and b-octamolybdate [Mo8O26]4- anions. The magnetic susceptibility data show a Curie-Weiss paramagnetic behavior (q = -5.201 K) in accordance with the spin-only ground state of FeⅡ ions. IR, UV-Vis, and EPR spectra are also briefly noted in this paper.
基金This work was supported by the 973 Program of the MOST (001CB108906), the National Natural Science Foundation of China (90206040, 20425313, 20333070, 20521101, and 20303021), the Natural Science Foundation of Fujian Province (2005HZ01-1), and the Chinese Academy of Sciences
文摘[{Cu（phen）（DMF）2}2（β-Mo8O26）] 1 （C36H44Cu2Mo8N8O30, Mr = 1963.39, phen =- 1,10-phenanthroline） and [Cu（phen）2]2[{Cu（phen）}2Mo8O26] 2 （C72H48Cu4Mo8N12O26, Mr = 2518.90） have been synthesized from （Bu4N）2[Mo6O19], Cu（NO3）2·3H2O and phen using solution method and under solvothermal condition, respectively. Both compounds 1 and 2 are structurally characterized by elemental analyses, IR and single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic system, space group P21/n, with a = 16.3347（13）, b = 9.861（1）, c = 17.2827（14） A, β=99.099（4）°, V= 2748.8（3） A3, Z = 2, Dc= 2.372 g/cm^3, F（000） =1900 and μ= 2.614 mm^-1. X-ray diffraction analysis reveals that compound 1 consists of discrete {[Cu（phen）（DMF）2]2（β-Mo8O26）} clusters constructed from β-[Mo8O26]^4- subunits covalently bound to two [Cu（phen）（DMF）2]^2- coordination groups. Compound 2 crystallizes in the monoclinic system, space group C2/c, with a = 33.1401（9）, b = 16.4508（5）, c = 16.2622（4） A, β= 119.2460（10）°, V = 7735.7（4） A3, Z = 4, Dc = 2.163 g/cm^3, F（000） = 4896 and μ= 2.413mm^-1. X-ray diffraction analysis reveals that compound 2 consists of a centrosymmetric β-octamolybdate-supported complex anion [ {Cu（phen）}2Mo8O26] and two bis-phenanthroline Cu（I） cations.
文摘A nickel-1,10-phenanthroline complex supported on an octamolybdate, [{Ni(phen)2}2(ξ-Mo8O26)], has been hydrothermally synthesized with MoO3, H2MoO4, Ni(OAc)2 · 6H2O and 1,10-phenathroline (1,10-phen) as raw materials. The crystals of the compound belong to mono-clinic P21/n space group, a= 1.2952(2), b = 1.6659(10), c= 1.3956(12) nm, β=106.273(8)°, V = 2.8906(5) nm3, Z = 2. 5604 observable reflections (/>2σ(/)) were used for structure resolution and refinements to converge to final R1 = 0.0414, wR2 = 0.0815. The result of structure determination shows that the compound contains octamolybdate possessing a novel structure type (named as ξ-isomer). The feature of ξ-[Mo8O26]4- is that it is composed of Mo6O6 ring and two MoO6 octa-hedra located at cap positions on opposite faces. The Mo6O6 ring contains two octahedral and four trigonal-bipyramidal MovI atoms. Each ξ-[Mo8O26]4- unit is bonded with two [Ni(phen)2]2+ through terminal oxygen atoms of octahedral and neighbouring trigonal-bipyramidal Mo atom in the Mo6O6 ring. IR and UV-Vis spectra of the compound were measured and its electronic structure was studied by EHMO method.
