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Thomas, J.M.7
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2
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33746840970
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(a) Hungria, A. B.; Raja, R.; Adams, R. D.; Captain, B.; Thomas, J. M.; Midgley, P. A.; Golovko, V.; Johnson, B. F. G. Angew. Chem., Int. Ed. 2006, 45, 4782-4785.
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4
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51549104243
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Pt(COD)2 (100.00 mg, 0.243 mmol) was dissolved in 20 mL of hexane. Ph3SnH (171.2 mg, 0.488 mmol) was added and allowed to stir at rt for 1 h. The product was purified by chromatography (silica gel column) to yield a light-yellow band (108.0 mg, 44% yield) of Pt(COD)(SnPh 3)2 (1, Spectral data for 1: 1H NMR (CDCl 3, rt, δ= 7.06-7.33 (m, 30 H, Ph, 5.57 (s, 4H, CH, 2JPt-H, 47 Hz, 2.21 (broad, 8H, CH2, 119Sn(1H) NMR (CD2Cl2, rt, δ, 84.3 (s, 2 Sn 1Z195119Sn, 12 737 Hz, 2J119Sn_117Sn, 711 Hz, Crystal data for 1: PtSn2C44H42, Mr, 1003.25, monoclinic, space group P21/n, a, 9.9731(2) Å, b, 16.5529(3) Å, c, 22.9675(5) Å, β= 95.500(1)°, V, 3
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2) was 0.0313 for 7013 reflections I > 2σ(I).
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5
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37049136225
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To a solution of 30 mg of Ru3(CO)10(NCCH 3)2 in CH2Cl2 was added 50 mg of HSnPh3 (0.142 mmol, The solution was stirred for 30 min at rt. The product was separated by TLC on silica gel to yield 16.1 mg (13, of colorless Ru(CO)4(SnPh3)2 (2, Spectral data for 2: IR vCO (cm-1 in CH2Cl2, 2031(vs, Mass spectrometry for Ru(CO)4(SnPh3J 2: EI/MS m/z; 914, M, 830, M, 3CO.
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2) was 0.0338 for 8240 reflections I > 2σ(I). For alternative syntheses for 2, see Cotton, J. D.; Knox, S. A. R.; Stone, F. G. A. Chem. Commun. 1967, 965-966.
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