Et_4N)_3 [V(mp)_3Na(mp)_3V] was obtained from the reaction of (NH_4)_3VS_4, FeCl_2, Na_2mp(H_2mp=o-mercaptophenol,o-HSC_6H_4OH) and Et_4NCl in CH_3CN. C_(60)H_(84)N_3NaO_6S_6V_2, M_r=1260. 61, monoclinic, space group ...Et_4N)_3 [V(mp)_3Na(mp)_3V] was obtained from the reaction of (NH_4)_3VS_4, FeCl_2, Na_2mp(H_2mp=o-mercaptophenol,o-HSC_6H_4OH) and Et_4NCl in CH_3CN. C_(60)H_(84)N_3NaO_6S_6V_2, M_r=1260. 61, monoclinic, space group C2/c with a=24. 825(8) . b=14.716(5) , c=18. 419(10)A,β=94. 57(3)°, V=6707. 54 A ̄3;Z=4, Dc=1. 248 g/cm ̄3. μ= 5. 002 cm ̄(-1). F(000)=2664. The structure was solved by direct methods and refined to final R(Rω)=0.059(0.059) for 3183 observed reflections with I≥2.5σ(I). The centrosymmetric anion of the title compound contains two [V(mp)_3] ̄(2-) fragments linked by a sodium ion, the crystallographic center of symmetry , through the μ2-O bridges. The Ⅴ(Ⅳ) atom is in a coordination environment intermediate between a trigonal prism and an ideal octahedron.展开更多
文摘Et_4N)_3 [V(mp)_3Na(mp)_3V] was obtained from the reaction of (NH_4)_3VS_4, FeCl_2, Na_2mp(H_2mp=o-mercaptophenol,o-HSC_6H_4OH) and Et_4NCl in CH_3CN. C_(60)H_(84)N_3NaO_6S_6V_2, M_r=1260. 61, monoclinic, space group C2/c with a=24. 825(8) . b=14.716(5) , c=18. 419(10)A,β=94. 57(3)°, V=6707. 54 A ̄3;Z=4, Dc=1. 248 g/cm ̄3. μ= 5. 002 cm ̄(-1). F(000)=2664. The structure was solved by direct methods and refined to final R(Rω)=0.059(0.059) for 3183 observed reflections with I≥2.5σ(I). The centrosymmetric anion of the title compound contains two [V(mp)_3] ̄(2-) fragments linked by a sodium ion, the crystallographic center of symmetry , through the μ2-O bridges. The Ⅴ(Ⅳ) atom is in a coordination environment intermediate between a trigonal prism and an ideal octahedron.