Dichloridobis{2-[(dimethylamino)methyl]phenyl}bis{2-[(dimethylazaniumyl)methyl]phenyl}di-μ-hydroxido-di-μ3-oxido-tetraphenyltetratin(IV) dichloride deuterochloroform decasolvate

The ladder-like structure of the tetranuclear title compound, [Sn4(C6H5)4Cl2O2(OH)2(C9H13N)2(C9H12N)2]Cl2·10CDCl3, consists of two five- and two six-coordinated SnIV atoms bridged by oxide or hydroxide groups. The chelating ligands reveal rather strong Sn—N bonds [2.517 (4) Å], but the protonated dimethylamino groups in the periphery of the complex show no interaction with the metal atoms. The complex cation is located on an inversion centre. The chloride anion is linked to the complex molecule by strong intramolecular O—H⋯Cl and N—H⋯Cl hydrogen bonds. Five independent deuterochloroform accompany the complex, two of them are disordered [occupancy ratios 0.63 (2):0.27 (2) and 0.60 (2):0.40 (2)].


Experimental
Crystal data [Sn 4 (C 6 H 5 ) 4 Cl 2 O 2 (OH) 2 (C 9 H 13 N) 2 - (C 9 Table 1 Hydrogen-bond geometry (Å , ). two central L CN PhSnO units and two peripherical L CN PhSn(OH)Cl units (L CN = 2-(Me 2 NCH 2 )C 6 H 4 -). Similar tetranuclear aggregates were found earlier, for example for octabenzyl- (Mohamed et al., 2004), octaisopropyl-(Puff et al., 1983, octa(trimethylsilylmethyl)- (Puff et al., 1983), octaphenyl-(Vollano et al., 1984, octa(2-chlorobenzyl)- (Zhang et al., 2009) , octa(4-chlorobenzyl)- (Lo & Ng, 2009) octaphenyl (Kresinski et al, 1994Cox & Tiekink, 1994;Tiekink, 1991) and tetra(trimethylsilylmethyl)-tetra-t-butyl- (Beckmann et al., 2001) derivative, respectively. The major difference between I and the rest of compounds is that all these compounds have all the tin atoms five coordinated. In I, the chelating dimethylaminomethyl arms of outer units are protonated by HCl. The chlorine anion is being out of the primary tin coordination sphere but is strongly connected by hydrogen bridges to both OH and NH groups (3.079 (4) Å, 3.106 (5) Å; Fig. 2). These hydrogen bonds are typical for C,N-chelated organotin compounds, as for example for L CN (n-Bu) 2 SnCl.HCl (Švec et al., 2010) or [L CN (n-Bu)SnOC(O)CF 3 ] 2 (µ-OH) 2 (Švec et al., 2011), but the presence of both types of hydrogen bonds in the same molecule were not observed before. The inner tin atoms coordination polyhedra are of very deformed trigonal bipyramids with both carbon atoms of the ligand and phenyl substituent and the bridging oxygen atom in equatorial positions, despite of that the value of the sum of interatomic angles in equatorial girdle is rather low (323.7°). The axial positions of these tin atoms are filled with the bridging OH group and the second bridging oxygen atom, where Sn1-O2 distances are a bit longer than in cases of the equatorial ones. The equatorial angle is shorter than ideally 180° being only 150.66 (13)°.
The outer tin atoms have the C,C-transoidal coordination geometry of strongly deformed octahedron with mutually cis-coordinated O and OH groups, and chlorine and strongly interacting amino nitrogen (Sn-N 2.517 (4) Å) atoms, respectively.

Experimental
The title compound (I, Scheme 1) has been obtained from the reaction mixture of ethylacetoacetate, cyclohexanol and

Special details
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.
Refinement. Refinement of F 2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F 2 , conventional R-factors R are based on F, with F set to zero for negative F 2 . The threshold expression of F 2 > 2sigma(F 2 ) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F 2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.  (7) 0.0332 (7) 0.0328 (7