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
The novel vanadophosphate （DETAH）（DETAH3）3 [V18O42（PO4）]·（PO4）·2H2O has been synthesized under hydrothermal conditions and its structure was determined by single-crystal X-ray diffraction. The compou...The novel vanadophosphate （DETAH）（DETAH3）3 [V18O42（PO4）]·（PO4）·2H2O has been synthesized under hydrothermal conditions and its structure was determined by single-crystal X-ray diffraction. The compound crystallizes in monoclinic, space group C2/c with a = 23.857（3）, b = 12.9619（18）, c = 20.204（3） A, β = 105.692（2）°, V= 6015.0（14） A3, Z = 4, Dc= 2.473 g/cm^3, M,.= 2239.68, F（000） = 4432, R = 0.0725, wR = 0.1524 and GOOF= 1.095. The metaloxo cluster contains a novel six-capped pesudo-Keggin structure unit which encloses a disorder PO4^3- vip.展开更多
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.
基金This work was supported by the Science and Technology Development Foundation of Fuzhou University (No.2004-xq-05)the Scientific Research Foundation of Fujian Provincial Education Department (No. JB04010)
文摘The novel vanadophosphate （DETAH）（DETAH3）3 [V18O42（PO4）]·（PO4）·2H2O has been synthesized under hydrothermal conditions and its structure was determined by single-crystal X-ray diffraction. The compound crystallizes in monoclinic, space group C2/c with a = 23.857（3）, b = 12.9619（18）, c = 20.204（3） A, β = 105.692（2）°, V= 6015.0（14） A3, Z = 4, Dc= 2.473 g/cm^3, M,.= 2239.68, F（000） = 4432, R = 0.0725, wR = 0.1524 and GOOF= 1.095. The metaloxo cluster contains a novel six-capped pesudo-Keggin structure unit which encloses a disorder PO4^3- vip.
