Acta Crystallographica Section E
Structure Reports Online
Yong-Xin Li, Ru-Fen Zhang and Chun-Lin Ma*
Department of Chemistry, Liaocheng University, Liaocheng 252059, People’s Republic of China
The title complex, [Sn(C6H5)(C9H18NS2)2Cl], contains two bidentate dithiocarbamate groups, resultingin a distorted SnS4CCl octahedral geometry for the Sn atom.
Received 3 October 2005 Accepted 18 October 2005 Online 22 October 2005
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Key indicators Single-crystal X-ray study T = 273 K ˚ Mean (C–C) = 0.020 A R factor = 0.075 wR factor = 0.254 Data-to-parameter ratio = 19.0 For details of how these key indicators were automatically derivedfrom the article, see http://journals.iucr.org/e.
In recent years, dithiocarbamate complexes have been extensively studied (Burgmayer & Templeton, 1985). Such groups usually bond to the metal in a bidentate fashion (Mak et al., 1985); typical examples range from transition metal complexes such as Co(S2CNMe2)NO, where the Co atom is at the centre of a square pyramid (Alderman et al., 1962), andCu4[S2CNEt2]4 (Hesse, 1963), containing a Cu4 tetrahedron, to main group compounds such as C4H9Sn(S2CNEt2)2, where the geometry around the tin atom is pentagonal bipyramidal (Morris & Schlemper, 1979). We report here the structure of the title complex, (I), (Fig. 1).
# 2005 International Union of Crystallography Printed in Great Britain – all rights reserved
The hexacoordinate Sn atom in (I)is situated at the centre of a distorted octahedral arrangement of four S atoms from the two chelating dithiocarbamate groups, a chloride ion and a benzene C atom. As with other dithiocarbamate complexes, the MS2C ring is almost planar (Khan et al., 1987). Selected geometrical values are listed in Table 1. The chelating ligands result in acute S—Sn—S angles (Table 1) which are consistent withthose in related complexes (Bell et al., 1989). The two dithiocarbamate ligands in (I) show different behaviour in their bonding to Sn. The C1 ligand shows distinctly different Sn—S bond lengths [Sn1—S1 = ˚ 2.514 (3), Sn1—S2 = 2.627 (3) A]. The longer Sn—S bond is associated with the shorter adjacent C—S bond [C1—S1 = ˚ 1.745 (11), C1—S2 = 1.712 (11) A]. This corresponds to the asymmetrical bondingmode described by Bell et al. (1989). The difference in Sn—S bond lengths for the other (C10) ligand is much less pronounced. The C—N bond lengths in both ligands indicate substantial double-bond character, which would reﬂect a signiﬁcant
doi:10.1107/S1600536805033635 Li et al.
Acta Cryst. (2005). E61, m2365–m2366
RefinementReﬁnement on F 2 R[F 2 > 2(F 2)] = 0.075 wR(F 2) = 0.254 S = 1.03 5498 reﬂections 289 parameters H-atom parameters constrained w = 1/[ 2(Fo2) + (0.1431P)2 + 1.7378P] where P = (Fo2 + 2Fc2)/3 (Á/)max < 0.001 ˚ Ámax = 1.30 e AÀ3 ˚ Ámin = À0.93 e AÀ3
˚ Selected geometric parameters (A, ).
Sn1—C19 Sn1—Cl1 Sn1—S1 Sn1—S4 Sn1—S3 Sn1—S2 2.157 2.456 2.514 2.566 2.569 2.627 (12) (3) (3) (3) (3)(3) C1—S1 C1—S2 C10—S3 C10—S4 C1—N1 C10—N2 S1—Sn1—S2 1.745 1.707 1.715 1.737 1.312 1.308 (11) (11) (12) (12) (13) (14)
The structure of (I), showing 30% probability displacement ellipsoids (H atoms omitted for clarIty).
contribution to the structure made by the canonical form discussed by Casas et al. (1989).
The synthesiswas carried out under a nitrogen atmosphere. Potassium N,N-dibutyldithiocarbamate (0.243 g, 1 mmol) was suspended in 20 ml benzene and phenyltin trichloride (0.150 g, 0.5 mmol) was added to the mixture. After 12 h at room temperature the solution was ﬁltered and the solvent was gradually removed by evaporation under vacuum until a solid product was obtained. The solid was then recrystallized...
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