Banerjee Sangeeta Ray, Wei Lihui, Levadala Murali K, Lazarova Neva, Golub Vladimir O, O'Connor Charles J, Stephenson Karin A, Valliant John F, Babich John W, Zubieta Jon
Department of Chemistry, Syracuse University, Syracuse, NY 13244, USA.
Inorg Chem. 2002 Nov 4;41(22):5795-802. doi: 10.1021/ic020391d.
The reactions of the Re(V) starting material [ReO(PPh(3))(2)Cl(3)] with ligands of the type XN(Y)Z [X = Y = 2-pyridylmethyl, Z = -CH(2)CO(2)Et (L(1)Et), -CH(2)CH(2)CO(2)Et (L(2)Et), -CH(2)CH(2)CH(2)CH(2)CH(NHCO(2)Bu(t))CO(2)H (L(3)H); X = 2-pyridylmethyl, Y = 2-(1-methylimidazolyl)methyl, Z = -CH(2)CO(2)Et (L(4)Et)] yielded the Re(III) trichloride complexes of the type [ReCl(3)(L(n)R)]. The complexes are mononuclear, paramagnetic species with a facial geometry of the chloride ligands. The nitrogen donors of the tridentate L(n)()R ligands complete the distorted octahedral coordination spheres of the complexes. Crystal data: [ReCl(3)(L(1)Et)] (1), monoclinic, C2/m, a = 16.088(3) A, b = 9.980(2) A, c = 12.829(2) A, beta = 91.384(3) degrees, Z = 4, D(calc) = 1.967 g/cm(-)(3); [ReCl(3)(L(4)Et)] (4), monoclinic, C2/c, a = 22.880(1) A, b = 7.4926(4) A, c = 22.560(1) A, beta = 94.186(1) degrees, Z = 8, D(calc) = 2.001 g/cm(-3).
Re(V)起始原料[ReO(PPh(3))(2)Cl(3)]与XN(Y)Z类型的配体[X = Y = 2 - 吡啶甲基，Z = -CH(2)CO(2)Et (L(1)Et)，-CH(2)CH(2)CO(2)Et (L(2)Et)，-CH(2)CH(2)CH(2)CH(2)CH(NHCO(2)Bu(t))CO(2)H (L(3)H)；X = 2 - 吡啶甲基，Y = 2 - (1 - 甲基咪唑基)甲基，Z = -CH(2)CO(2)Et (L(4)Et)]反应，生成了[ReCl(3)(L(n)R)]类型的Re(III)三氯化物配合物。这些配合物是单核、顺磁性物种，其氯配体具有面式几何构型。三齿L(n)()R配体的氮供体完善了配合物扭曲的八面体配位球。晶体数据：[ReCl(3)(L(1)Et)] (1)，单斜晶系，C2/m，a = 16.088(3) Å，b = 9.980(2) Å，c = 12.829(2) Å，β = 91.384(3)°，Z = 4，D(calc) = 1.967 g/cm(-)(3)；[ReCl(3)(L(4)Et)] (4)，单斜晶系，C2/c，a = 22.880(1) Å，b = 7.4926(4) Å，c = 22.560(1) Å，β = 94.186(1)°，Z = 8，D(calc) = 2.001 g/cm(-3)。
