Attempts to prepare the tricyclohexylphosphine or triphenylstibine ana
logues of the recently reported (triphenylphosphine)CuX(2)(-) anions w
ere unsuccessful and instead resulted in the formation of a variety of
polyhalocuprate anions. The structure of one of these, [CH3P(C6H5)(3)
]2Cu2I4, has been determined; monoclinic, P2(1)/c; a = 16.715(3), b =
10.787(2), c = 23.196(3) Angstrom, beta = 98.59(1)degrees, Z = 4; R =
6.3%, R(W) =3.1%. The Cu-63 NQR spectra of twelve such polyhalocuprate
anions were observed and the results compared with those of previousl
y reported polyhalocuprates.