STRUCTURES OF TRANS-[TCCL4(P(CH3)3)2] AND [P(C7H7)3(C(CH3)2CH2COCH3)]2[TCCL6]

Tetrachlorobis(trimethylphosphine)technetium, trans-[TcCl4(C3H9P)2] (1 ), M(r) 392.88, monoclinic, P2(1)/c, a = 6.639 (2), b = 8.443 (3), c = 13.559 (4) angstrom, 8 = 100.73 (2)-degrees, V = 746.7 (4) angstrom3, z = 2, D(x) = 1.738 Mg m-3, lambda(Mo Kalpha) = 0.71069 angstrom, mu = 1.82 mm-1, F(000) = 390, T = 295 and R = 0.036 for 932 observed refl ections. The Tc atom is located on an inversion centre. The Tc-P dista nces are 2.524 (2) angstrom while the Tc-Cl bonds are 2.320 (1) and 2. 330(2) angstrom. methyl-3-oxobutyl)tris(4-methylphenyl)phosphonium] he xachlorotechnetate, [P(C7H7)3(C6H110)][TCC16] (II), M(r) = 1118.68, mo noclinic, P2(1)/c, a = 15.120 (4), b = 11.038 (3), c = 21.146 (6) angs trom, beta = 128.59 (2)-degrees, V = 2759 (i) angstrom3, z = 2, D(x) = 1.344 Mg m-3, lambda(Mo Kalpha) = 0.71069 angstrom, mu = 0.64 mm-1, F (000) = 11 58, T = 295 K and R = 0.041 for 3019 observed reflections. The Tc atom of the [TcCl6]2- anion is located on an inversion center. The Tc-Cl bonds vary from 2.352 (2) to 2.359 (1) angstrom. The [(C7H7) 3PC(CH3)2CH2COCH3]+ cation was formed from the reaction Of P(P-tolYl)3 with acetone as solvent.