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Ag(1-CB11H12, 0.33 g, 1.0 mmol) was added to a stirred solution of Ph(L1)SnCl2 (0.432 g, 1.0 mmol) in CH2Cl2 (10 mL, The suspension was stirred for 2 days at ambient temperature. After this time, the AgCl was filtered off and the solvent was evaporated in vacuo. The residue was washed with pentane to afford 1 as a white solid. Yield: 0.52 g (96, Mp: 145-148°C Anal. Caled for C17H30B11ClO2Sn (mol wt 539.50, C, 37.85; H, 5.60. Found: C, 37.81; H, 5.39. Mol wt: 540. MS: m/z 397, 100, M, CB11H12, m/z 143, 100, CB11H12, 1H NMR (CDCl 3; δ (ppm, 2.15 (s, cage CH, 3.86 (s, 6H, CH3, 5.19 (AB spin system, 4H, CH2, nJ( 1H,1H, 12.3 Hz, 7.43-7.87 complex pattern, 8H, SnPh, SnC6
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-1): v(BH) 2569.
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34547775054
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Yield: 0.42 g (40, Mp: 185-189°C Anal. Caled for C 34H62B22O6-Sn2 (mol wt 1042.11, C, 39.19; H, 6.00. Found: C, 39.21; H, 6.02. Mol wt: 1042. MS: miz 379, 100, M, 2CB11H12)]2, miz 143, 100, CB11H12, 1H NMR (CDCl3; δ (ppm, 2.24 (bs, 1H, cage CH, 3.47 (s, 6H, CH 3, 5.04 (s, 4H, CH2, 7.47-7.71 (complex pattern, 8H, SnPh, SnC6H3, 13C NMR (CDCl3; δ (ppm, 59.84 (CH3, 68.12 (cage CH, 71.12 (CH2, nJ(119Sn, 13C, 29.21 Hz, SnC 6H3, 126.49 (C(1, 144.67, 126.75, 133.06; SnPh, 135.26 (C′(1, 136.03, 131.04, 133.46. 119Sn NMR(CDCl3; δ (ppm, 315.07. 11B NMR (CDCl3; δ (ppm, 5.05 (s, 1B, B(12, 11.41 (s, 5B, B7-11
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s(SnOSn) 439.
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2 to 1 is typical for an ionization process where a Sn-X bond is cleaved.
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2 to 1 is typical for an ionization process where a Sn-X bond is cleaved.
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(b) Kašná, B.; Jambor, R.; Dostál, L.; Kolářová, L.; Císařová, I.; Holeček, J. Organometallics 2006, 25, 148.
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Kašná, B.1
Jambor, R.2
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Kolářová, L.4
Císařová, I.5
Holeček, J.6
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34547792797
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For the proposed structure of 1, see the Supporting Information.
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For the proposed structure of 1, see the Supporting Information.
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33
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0000934062
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(c) Plešek, J; Jelínek, T.; Drdáková, E.; Heřmánek, S.; Štíbr, B. Collect. Czech. Chem. Commun. 1984, 49, 1559.
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Plešek, J.1
Jelínek, T.2
Drdáková, E.3
Heřmánek, S.4
Štíbr, B.5
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34
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34547768010
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Crystallographic data for 2: C32H38O 6Sn2·2CH12B11 ·2H 2O, triclinic, P1̄ (No. 2, colorless, a, 9.5000(2) Å, b= 12.0520(3) Å, c= 13.0070(3) Å, α, 62.773(1)°, β= 76.968(1)°, γ, 76.994(1)°, V, 1277.28(5) Å3, T, 150(2) K, Z, 1, Mw, 1078.07, Dx, 1.402 Mg m-3, 5869 unique reflections, 5495 observed reflections (T > 2σ(I, R(I > 2σ(I, 0.021, wR2all data, 0.050, GOF, 1.066
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-3, 5869 unique reflections, 5495 observed reflections (T > 2σ(I)), R(I > 2σ(I)) = 0.021, wR2(all data) = 0.050, GOF = 1.066.
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