Abstract
Abstract An X-ray analysis of the 1-methylstannatrane hexahydrate [MeSn(OCH2CH2)3N]3 . 6H2O (4) revealed a trimeric formulation. It crystallizes in the monoclinic space group C2/c (Z = 4) with a = 9.206 (3) Å, b = 13.774 (5) Å, c = 26.581 (4) Å, and β = 93.33 (2)°. The structure refined to R = 0.074 and R w = 0.086. The trimeric unit is disordered about a twofold axis, which passes through the central Sn atom. The geometry around this central atom closely approximates a pentagonal bipyramid. The two crystallographically equivalent end tin atoms have distorted-octahedral geometries. Strong association of the three monomeric methylstannatrane units formally leading to the trimer is suggested by the short Sn‒O bond lengths involved. These have values of 2.11 (1) and 2.21 (1) Å, as compared to corresponding values within the monomers of 2.17 (1) and 2.23 (1) Å, respectively. The solid-state structure agrees with solution NMR data suggesting its retention in solution. The trimeric unit is indicated in solution as is the presence of three nonequivalent tin centers. The structure of 4 is compared with other seven-coordinated tin compounds. The six water molecules of 4 appear hydrogen bonded to each other, forming hexagonal rings that contain inversion centers. Additional hydrogen bonding binds the rings to adjacent molecules of 4.
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