Diorganotin(IV) Complexes of a Cyclic Thiosemicarbazone Ligand
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725.1 (15) [SnPh(C15H10N3S)2]ϩ, 803 (10) [SnPh2(C15H10N3S)2
ϩ
´
´
´
1]ϩ. Selected spectroscopic data: IR (KBr): ν˜ ϭ 1597 w, 1578 w
(CϭN); 1486 s (thioamide I); 806 w (thioamide IV); 729 m (Ph)
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B. Wrackmeyer in: M. Gielen, R. Willem, B. Wrackmeyer
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cmϪ1 13C NMR (300 MHz, CDCl3, 25 °C): δ ϭ 128.2, 128.4,
.
128.8, 129.2, 129.3, 129.7, 129.8, 130.6, 134.8, 134.9, 135.5, 141.1
(Ph); 153.1, 156.6 (CϭN); 173.3 (CϭS); J(119SnϪ13C) ϭ 56.1 Hz.
2
119Sn NMR (300 MHz, CDCl3, 25 °C):
δ ϭ Ϫ206.8 ppm;
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B. Wrackmeyer, Annu. Rep. NMR Spectrosc. 1999, 38,
(300 MHz, [D6]DMSO, 25 °C): δ ϭ Ϫ220.9 ppm.
203Ϫ264.
´
P. Souza, M. A. Mendiola, A. Arquero, V. Fernandez, E. Guti-
Complex 4: Yield 79%, m.p. 224 °C. C32H26N6SSn (677.40): calcd.
C 56.74, H 3.84, N 12.41, S 9.45; found C 56.45, H 4.04, N 12.30,
S 9.50. MS (FABϩ): m/z (%) ϭ 413.9 (25) [SnMe2(C15H10N3S)]ϩ,
662.8 (5) [SnMe(C15H10N3S)2]ϩ, 678.9 (5) [SnMe2(C15H10N3S)2 ϩ
1]ϩ. Selected spectroscopic data: IR (KBr): ν˜ ϭ 1597 w, 1578 w
(CϭN); 1485 s (thioamide I); 820 w (thioamide IV); 557 w (νasy
SnϪC); 511 w (νsym SnϪC) cmϪ1. 1H NMR (300 MHz, CDCl3, 25
°C): δ ϭ 1.29 [s, 6 H, CH3, 2J(119SnϪ1H) ϭ 75.0 Hz], 7.30Ϫ7.55
(m, 20 H, Ph) ppm. 13C NMR (300 MHz, CDCl3, 25 °C): δ ϭ 6.2
[CH3, 1J(119SnϪ13C) ϭ 557.0]; 128.4, 128.6, 129.2, 129.3, 129.8,
130.9, 135.0, 135.1 (Ph); 153.0, 157.2 (CϭN); 174.2 (CϭS) ppm.
119Sn NMR (300 MHz, CDCl3, 25 °C): δ ϭ Ϫ84.3 ppm. 119Sn
NMR (300 MHz, [D6]DMSO, 25 °C): δ ϭ Ϫ108.7 ppm. 119Sn CP/
MAS NMR: δ ϭ Ϫ251 ppm.
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Acknowledgments
We thank the DGICYT for financial support (Project BQU2001-
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Received February 14, 2003
Eur. J. Inorg. Chem. 2003, 2711Ϫ2717
2003 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
2717