Organotin derivatives of alpha-[X(III)W9O33](9-) (X = AS, Sb) heteropolytungstates. Solution- and solid-state characterization of [{(C6H5Sn)(2)O}(2)H(alpha-AsW9O33)(2)](9-) and [(C6H5Sn)(3)Na-3(alpha-SbW9O33)(2)](6-)

The tris(phenyltin)-substituted tungstoantimonate(III) Cs-6[(PhSn)(3)Na-3(a lpha-SbW9O33)(2)]. 20H(2)O (1) and the tetrakis(phenyltin)-substituted tung stoarsenate(III) Nas[{(PhSn)(2)O}(2)H(alpha-AsW9O33)(2)]. 20H(2)O (2) have been prepared by reaction of phenyltin trichloride with Na-9[alpha-SbW9O33] . 19.5H(2)O and Na-9[alpha-AsW9O33]. 19.5H(2)O, respectively, in aqueous so lution. The products were characterized by elemental analysis, X-ray crysta llography, multinuclear NMR, and infrared spectroscopy. Crystals of 1 are m onoclinic, space group P2(1)/n, with a 13.7952(1) Angstrom, b = 22.3133(2) Angstrom, c = 34.4493(2) Angstrom, beta = 90.933(1)degrees, and Z = 4. Anio n 1 has nominal D-3h symmetry and contains three PhSn3+ groups and three so dium ions sandwiched between [alpha-SbW9O33](9-) units. Crystals of 2 are t riclinic, space group P (1) over bar, with a = 15.272(6) Angstrom, b = 15.3 03(6) Angstrom, c = 16.760(7) Angstrom, alpha = 93.59(3)degrees, beta = 106 .187(19)degrees, gamma = 112.23(3)degrees, and Z = 1. Anion 2 has nominal C -2h symmetry and contains four PhSn3+ groups sandwiched between two [alpha- AsWs(9)O(33)](9-) units.