Sodium molybdate was reduced to produce ring-like compounds in the presence of carboxylic acids. Compound 1: Na8(H2O)28(H3O)+{Na(DMSO)2[MoVI10MoV8O52(OH)4(CH3C- OO)2]}11H2O (C8H103O102Na9S2Mo18, Mr = 3829.85), where ...Sodium molybdate was reduced to produce ring-like compounds in the presence of carboxylic acids. Compound 1: Na8(H2O)28(H3O)+{Na(DMSO)2[MoVI10MoV8O52(OH)4(CH3C- OO)2]}11H2O (C8H103O102Na9S2Mo18, Mr = 3829.85), where the {Mo18} ring is built up by two acetic acids connecting two {Mo9} building blocks and the 1-D chain of 1 is formed through the coordinated sodium cations. Crystal data: triclinic, space group P, a = 11.3228(2), b = 15.4170(2), c = 16.7209(3) ? a = 113.006(1), b = 108.455(1), g = 92.430(1), V = 2501.98(7) 3, Z = 1, Dc = 2.542 g/cm3, F(000) = 1854, (MoKa) = 2.381 mm-1, T = 293(2) K, final R = 0.0532 and wR = 0.1203 for 7291 observed reflections with I > 2(I) from 8775 independent reflections. Compound 2: Na8(H2O)22(H3O)+{Na(DMSO)2[MoVI10MoV8O52(OH)4(C2H5COO)2]}10H2O (C10H93O94Na9- S2Mo18, Mr = 3715.79). Crystal data: monoclinic, space group C2/m, a = 18.044(1), b = 25.944(2), c = 10.4087(6) ? b = 106.613(2), V = 4669.3(5) 3, Z = 2, Dc = 2.643 g/cm3, F(000) = 3584, (MoKa) = 2.542 mm-1, T = 293(2) K, final R = 0.0536 and wR = 0.1621 for 4617 observed reflections with I > 2(I) from 5398 independent reflections. Similar to 1, the {Mo18} ring is built up by two {Mo9} building blocks that are connected up by two propanoic acids and these {Mo18} rings are further linked into a two-dimensional layer through the coordinated sodium cations.展开更多
A hydrothermal reaction of copper acetate with ammonium molybdate, 4,4-bpy (4,4-bipyridine) and 1,10-phen (1,10-phenanthroline) led to the formation of brown crystals of [Cu2(1,10-phen)2(4,4-bpy)]2 [Mo8O26]4H2O 1. Si...A hydrothermal reaction of copper acetate with ammonium molybdate, 4,4-bpy (4,4-bipyridine) and 1,10-phen (1,10-phenanthroline) led to the formation of brown crystals of [Cu2(1,10-phen)2(4,4-bpy)]2 [Mo8O26]4H2O 1. Single-crystal X-ray analysis has revealed that 1 (C68H56N12O30Cu4Mo8) crystallizes in the triclinic system, space group P with a = 11.270(3), b = 13.113(6), c = 13.906(3) ? = 103.33(4), b = 98.54(2), g = 101.29(2)? V = 1920.1(1) ?3, Mr = 2542.93, Z = 1, Dc = 2.199 g/cm3, m = 2.435 mm-1, F(000) = 1240, the final R = 0.0445, wR = 0.1082 and S = 1.021 for 5052 observed reflections with I >2s(I). It consists of copper (Ⅰ) tetramer units and -[Mo8O26]4- anions, which are further attached into a three-dimensional framework through hydrogen bonding and - stacking interactions.展开更多
基金the National Natural Science Foundation of China (20073048),NSF of Fujian province (2002F015) and the Chinese Academy of Sciences
文摘Sodium molybdate was reduced to produce ring-like compounds in the presence of carboxylic acids. Compound 1: Na8(H2O)28(H3O)+{Na(DMSO)2[MoVI10MoV8O52(OH)4(CH3C- OO)2]}11H2O (C8H103O102Na9S2Mo18, Mr = 3829.85), where the {Mo18} ring is built up by two acetic acids connecting two {Mo9} building blocks and the 1-D chain of 1 is formed through the coordinated sodium cations. Crystal data: triclinic, space group P, a = 11.3228(2), b = 15.4170(2), c = 16.7209(3) ? a = 113.006(1), b = 108.455(1), g = 92.430(1), V = 2501.98(7) 3, Z = 1, Dc = 2.542 g/cm3, F(000) = 1854, (MoKa) = 2.381 mm-1, T = 293(2) K, final R = 0.0532 and wR = 0.1203 for 7291 observed reflections with I > 2(I) from 8775 independent reflections. Compound 2: Na8(H2O)22(H3O)+{Na(DMSO)2[MoVI10MoV8O52(OH)4(C2H5COO)2]}10H2O (C10H93O94Na9- S2Mo18, Mr = 3715.79). Crystal data: monoclinic, space group C2/m, a = 18.044(1), b = 25.944(2), c = 10.4087(6) ? b = 106.613(2), V = 4669.3(5) 3, Z = 2, Dc = 2.643 g/cm3, F(000) = 3584, (MoKa) = 2.542 mm-1, T = 293(2) K, final R = 0.0536 and wR = 0.1621 for 4617 observed reflections with I > 2(I) from 5398 independent reflections. Similar to 1, the {Mo18} ring is built up by two {Mo9} building blocks that are connected up by two propanoic acids and these {Mo18} rings are further linked into a two-dimensional layer through the coordinated sodium cations.
基金This work was supported by the National Natural Science Foundation of China (20073048) NSF of Fujian and the Chinese Academy of Sciences
文摘A hydrothermal reaction of copper acetate with ammonium molybdate, 4,4-bpy (4,4-bipyridine) and 1,10-phen (1,10-phenanthroline) led to the formation of brown crystals of [Cu2(1,10-phen)2(4,4-bpy)]2 [Mo8O26]4H2O 1. Single-crystal X-ray analysis has revealed that 1 (C68H56N12O30Cu4Mo8) crystallizes in the triclinic system, space group P with a = 11.270(3), b = 13.113(6), c = 13.906(3) ? = 103.33(4), b = 98.54(2), g = 101.29(2)? V = 1920.1(1) ?3, Mr = 2542.93, Z = 1, Dc = 2.199 g/cm3, m = 2.435 mm-1, F(000) = 1240, the final R = 0.0445, wR = 0.1082 and S = 1.021 for 5052 observed reflections with I >2s(I). It consists of copper (Ⅰ) tetramer units and -[Mo8O26]4- anions, which are further attached into a three-dimensional framework through hydrogen bonding and - stacking interactions.
