Unusual Hexacoordination in a Triorganotin Fluoride Supported by Intermolecular Hydrogen Bonds. Crystal and Molecular Structures of l-Aza-5-stanna-5-halogenotricyclo[3.3.3.0* [1][2][3][4][5]undecanes N(CH2CH2CH2)3SnF H20 and N(CH2CH2CH2)3SnX

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The reactions of the functional Grignard reagent Me2 NCH2CH2C(Me2)MgCl (4) with tin tetrachloride, dimethyltin dichloride, and tin (II) chloride are described. From the reactions the compounds bis(3‐dimethylamino‐1,1‐dimethylpropyl) tin dichloride, [Me2NCH2CH2C(Me2)]2SnCl2 (5), dimethyl(3‐dimethylamino‐1,1‐dimethylpropyl) chlorostannane, Me2ClSnC(Me2)CH2CH2NMe2 (6), 1,1,2,2‐tetramethyl‐1,2‐bis(3‐dimethylamino‐1,1‐dimethylpropyl) distannane,[Me2SnC(Me2)CH2CH2NMe2]2 (7), 3‐dimethylamino‐(1,1‐dimethyl)propyl tin (II) chloride, Me2NCH2CH2C(Me2)SnCl (8), hexakis(3‐dimethylamino‐1,1‐dimethylpropyl) cyclotristannane, {[Me2NCH2CH2C(Me2)]2Sn}3(9a), and the tin cluster [Me2NCH2CH2C(Me2)SnCl]3 · SnCl2 (10) have been isolated and characterized by means of multinuclear NMR and Mössbauer spectroscopy, and X‐ray diffraction. 10 crystallizes in the trigonal space group P31 with the unit cell dimensions a 11.938, c 21.873 Å, V 2699.6 Å3 Z = 3. The structure was refined to a final R value of 0.064. 10 represents a tetranuclear cluster the skeleton of which is composed out of 4 Sn and a bridging Cl. Formally, the central tin atom is a SnCl+ cation stabilized by three stannylene units in a Ψ‐trigonal bipyramidal environment. The tin‐tin bond lengths are 288.2, 287.3 and 315.6 pm. The intramolecular SnN interactions amount to 242.8, 247.4 and 221.0 pm.