REACTION OF TIN METAL-POWDER WITH TRIORGANOPHOSPHORUS DIHALIDES - ISOLATION AND SPECTROSCOPIC CHARACTERIZATION OF [PR(3)X][SNX(3)] AND CIS-SN(PR(3))(2)X(4) AND TRANS-SN(PR(3))(2)X(4) (X=BR OR I R(3)=PH(3), PH(2)ME OR PHME(2))
N. Bricklebank et al., REACTION OF TIN METAL-POWDER WITH TRIORGANOPHOSPHORUS DIHALIDES - ISOLATION AND SPECTROSCOPIC CHARACTERIZATION OF [PR(3)X][SNX(3)] AND CIS-SN(PR(3))(2)X(4) AND TRANS-SN(PR(3))(2)X(4) (X=BR OR I R(3)=PH(3), PH(2)ME OR PHME(2)), Journal of the Chemical Society. Dalton transactions, (10), 1995, pp. 1593-1596
The novel reaction of some R(3)PX(2) compounds (X = Br or I; R(3) = Ph
(3), Ph(2)Me or PhMe(2)) with unactivated coarse-grain tin metal powde
r has been investigated. Initially a tin(ll) species results which is
then further oxidised leading to the formation of both cis- and trans-
Sn(PR(3))(2)X(4). The products formed have been characterised by eleme
ntal analysis. NMR, Raman and Mossbauer spectroscopy and compared to a
nalogous complexes. The synthesis and isolation of the iodo complexes
Sn(PR(3))(2)I-4 by this new synthetic route is straightforward and con
trasts with difficulties using conventional techniques, viz. the react
ion of SnI4 with PR(3). The relative proportions of cis- and trans-SnX
(4)(PR(3))(2) isomers formed from the reaction have been determined fr
om Mossbauer spectroscopic studies and the reason for their formation
is discussed.