PHOTOCHEMICAL-REACTION OF W(CO)(6) WITH SNCL4 .2. SYNTHESIS AND X-RAYSTRUCTURE OF TETRACHLOROBIS(TRIPHENYLPHOSPHINE OXIDE)TUNGSTEN(IV), [WCL4(OPPH(3))(2)]
T. Szymanskabuzar et T. Glowiak, PHOTOCHEMICAL-REACTION OF W(CO)(6) WITH SNCL4 .2. SYNTHESIS AND X-RAYSTRUCTURE OF TETRACHLOROBIS(TRIPHENYLPHOSPHINE OXIDE)TUNGSTEN(IV), [WCL4(OPPH(3))(2)], Journal of organometallic chemistry, 490(1-2), 1995, pp. 203-207
The crystal structure of [WCl4(OPPh(3))(2)] (1), formed in the photoch
emical reaction of W(CO)(6) with SnCl4 in the presence of triphenylpho
sphine, has been determined by the single-crystal X-ray diffraction me
thod. The compound crystallizes in the monoclinic space group C2/c, wi
th a = 14.027(3), b = 13.163(3), c = 19.621(4) Angstrom beta = 96.36(3
)degrees, Z = 4. The structure solved by heavy-atom methods has been r
efined to R = 0.0466, for 3489 observed reflections. The [WCl4(OPPh(3)
)(2)] molecule possesses a crystallographically imposed C-2 axis passi
ng through the tungsten atom. Despite steric demands, a mutually cis a
rrangement of triphenylphosphine oxide oxygens is found for [WCl4(OPPh
(3))(2)], while there is a slight lengthening of the W-Cl bonds trans
to the oxygen atoms.