摘要:
Reaction of [TcOCl4]- with hydralazine.HCl in methanol at room temperature yields the Tc(V)-hydrazido(3-) complex [Tc(C8H5N4)Cl2(PPh3)2].0.75C8H7 (1). In contrast, the reaction in refluxing methylene chloride produces the Tc(V)-nitrido complex [TcNCl2(PPh3)2].0.25CH2Cl2 (2). Crystal data. 1: triclinic P1BAR, a = 11.592(3), b = 12.105(3), c = 17.884(4) angstrom, alpha = 107.76(2)degrees, beta = 99.03(2)degrees, gamma = 106.11(2)degrees, V = 2232.7(9) angstrom 3, Z = 2, D(calc) = 1.40 g/m3; structure solution and refinement based on 2623 reflections (F greater-than-or-equal-to 6-sigma-(F(o)); Mo K-alpha, lambda = 0.71073 angstrom) converged at R = 0.058. 2: monoclinic C2/c, a = 24.081(9), b = 9.539(4), c = 15.650(6) angstrom, beta = 116.18(1)degrees, V = 3226.8(11) angstrom 3, Z = 4, D(calc) = 1.37 g/cm3; 3118 reflections; R = 0.052.