1268
S.M. Corcoran et al. / Inorganica Chimica Acta 358 (2005) 1263–1268
K) + 54. IR spectrum/cmꢀ1 (Nujol mull) 1035 m(PO),
365 st 348, 340sh m(SbCl).
[7] A.J. Barton, N.J. Hill, W. Levason, G. Reid, J. Am. Chem. Soc.
123 (2001) 11801.
[8] N.J. Hill, W. Levason, R. Patel, G. Reid, M. Webster, Dalton
Trans. (2004) 980.
4.14. [(SbCl5)2{o-C6H4(P(O)Ph2)2}]
[9] M. Zackrisson, K.I. Anden, Acta Chem. Scand. 14 (1960) 994.
[10] S. Milicev, D. Hadzi, Inorg. Chim. Acta 21 (1977) 201.
[11] L. Golic, S. Milicev, Acta Crystallogr., Sect. B 34 (1978) 3379.
[12] S. Pohl, W. Saak, R. Lotz, D. Haase, Z. Naturforsch. B 45 (1990)
1355.
[(SbCl5)2{o-C6H4(P(O)Ph2)2}] was made similarly.
The initially obtained fawn solid was recrystallised from
CH2Cl2/n-hexane to give an off-white product; 64%.
Anal. Calc. for C30H24Cl10P2Sb2: C, 33.5; H, 2.3. Found:
[13] D.J. Phillips, S.Y. Tyree Jr., J. Am. Chem. Soc. 83 (1961) 1806.
[14] S. Haupt, K. Seppelt, Z. Anorg. Allgem. Chem. 628 (2002) 729.
[15] M. Webster, Chem. Rev. 65 (1965) 87.
1
C, 32.8; H, 1.9%. H NMR (CDCl3, 300 K) 7.4–8.0(m).
31P{1H} NMR (CH2Cl2–CDCl3, 300 K) 53. IR spec-
trum/cmꢀ1 (Nujol mull) 1051 m(PO), 367, 339 (SbCl).
KM/Xꢀ1 cm2 molꢀ1 (10ꢀ3 mol dmꢀ3, CH2Cl2) 0.5.
[16] J.-E. Kessler, C.T.G. Knight, A.E. Merbach, Inorg. Chim. Acta
115 (1986) 75.
[17] J.-E. Kessler, C.T.G. Knight, A.E. Merbach, Inorg. Chim. Acta
115 (1986) 85.
[18] W. Van Der Veer, F. Jellinek, Rec. Trav. Chim. Pays-Bas. 85
(1966) 842.
4.15. [(SbCl5)2{Ph2P(S)CH2P(S)Ph2}]
[19] F. Klages, A. Gleissner, R. Ruhnau, Chem. Ber. 92 (1959)
1814.
A solution of SbCl5 (0.20 g, 0.7 mmol) in CCl4 (5
cm3) was added to a stirred solution of the ligand
(0.15 g, 0.33 mmol) in CH2Cl2 (20 cm3). After 20
min the solvent was reduced in vacuo to precipitate
a cream solid which was filtered off and dried in
vacuo; 0.20 g, 60%. Anal. Calc. for C25H22Cl10-
P2S2Sb2 Æ CCl4: C, 26.0; H, 1.8. Found: C, 25.8; H,
1.6%. 1H NMR (CDCl3, 300 K) 4.77(t) [2H] 2J(P–
H) = 18 Hz, 7.5–8.0(m) [20H]. 31P{1H} NMR
(CH2Cl2–CDCl3, 300 K) + 71. IR spectrum/cmꢀ1 (Nu-
jol mull) 545 m(PS), 345br m(SbCl).
[20] J. Bordner, G.O. Doak, T.S. Everett, J. Am. Chem. Soc. 108
(1986) 4206.
[21] Y. Matano, H. Nomura, J. Am. Chem. Soc. 123 (2001) 6443.
[22] J. Pebler, F. Weller, K. Dehnicke, Z. Anorg. Allgem. Chem. 492
(1982) 139.
[23] R.A. Zingaro, A. Merijanian, Inorg. Chem. 3 (1964) 580.
[24] N. Kuhn, H. Schumann, J. Organomet. Chem. 288 (1985) C1.
[25] N. Kuhn, H. Schumann, J. Organomet. Chem. 304 (1986) 181.
[26] C. Glidewell, J. Organomet. Chem. 116 (1976) 189.
[27] I. Lindqvist, G. Olofsson, Acta Chem. Scand. 13 (1959) 1753.
[28] C.-I. Bra¨nden, I. Lindqvist, Acta Chem. Scand. 15 (1961) 167.
[29] C.-I. Bra¨nden, I. Lindqvist, Acta Chem. Scand. 17 (1963) 353.
[30] B. Neumuller, R. Meyer, K. Dehnicke, Zeit. Kristallogr. 209
¨
(1993) 90.
4.16. [(SbCl5)2{Ph2As(O)CH2As(O)Ph2}]
[31] M. Burgard, J.-P. Brunette, M.F. Leroy, Inorg. Chem. 15 (1976)
1225.
[32] W. Levason, B. Patel, M.C. Popham, G. Reid, M. Webster,
Polyhedron 20 (2001) 2711.
[(SbCl5)2{Ph2As(O)CH2As(O)Ph2}] made similarly to
the diphosphine dioxide analogue 50%. Anal. Calc. for
C24H22As2Cl10O2Sb2 Æ CCl4: C, 24.8; H, 2.2. Found: C,
[33] P. Stilbs, G. Olofsson, Acta Chem. Scand. A 28 (1974) 647.
[34] J. Emsley, The Elements, OUP, Oxford, 1989.
[35] S.M. Godfrey, C.A. McAuliffe, R.G. Pritchard, J.M. Sheffield,
G.M. Thompson, J. Chem. Soc., Dalton Trans. (1997) 4823
(and references therein).
1
24.4; H, 2.2%. H NMR (CDCl3, 300 K) 4.95(s) [2H],
7.6–8.0(m) [20H]. IR spectrum/cmꢀ1 (Nujol mull) 849
m(AsO), 365, 340, 311 m(SbCl). KM/Xꢀ1 cm2 molꢀ1
(10ꢀ3 mol dmꢀ3, CH2Cl2) 0.1.
[36] R.L. McKenney, H.H. Sisler, Inorg. Chem. 6 (1967) 1178.
[37] B.A. Nevett, A. Perry, Spectrochim. Acta A 33 (1977) 755.
[38] T. Maeda, G. Yoshida, R. Okawara, J. Organometal. Chem. 44
(1972) 237.
References
[39] M. Shindo, Y. Matsumura, R. Okawara, J. Organomet. Chem. 11
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