(Z)-1-[2-(TRIARYLSTANNYL)VINYL]-1-CYCLOHEPTANOLS - SYNTHESIS, CHARACTERIZATION, HALODEMETALLATION AND CRYSTAL-STRUCTURES

The synthesis and characterization by H-1, C-13, Sn-119 Mossbauer spec troscopy of (Z)-1-[2-(triphenylstannyl)vinyl]-1-cycloheptanol, CH2(CH2 )(5)C(OH)CH=CHSnPh(3) (1), and )-1-[2-(tri-p-tolylstannyl)vinyl]-1-cyc loheptanol, CH2(CH2)(5)C(OH)CH=CHSn(p-tol)(3) (2), are described, toge ther with their halodemetallation by I-2, Br-2 and ICI1 to yield deriv atives of the types CH2(CH2)(5)C(OH)CH=CHSnAr(3-n)X(n) (Ar = phenyl or p-tolyl, n = 1, 2; X = I, Br, CI, respectively). The solid-state stru ctures of four compounds been determined by X-ray diffraction analysis . In the crystals of CH2(CH2)(5)C(OH)CH=CHSnPh(3) (1) and CH2(CH2)(5)C (OH)CH=CHSn(p-tol)(3) (2) the Sn atom has a tetrahedral geometry disto rted towards trigonal bipyramid as a consequence of a close intramolec ular contact with the hydroxyl O(1) atom of 2.742(3) Angstrom and 2.76 8(3) Angstrom respectively. A trigonal bipyramidal geometry is found i n CH2(CH2)(5)C(OH)CH=CHSn(p-tol)Br-2 (12) and CH2(CH2)(5)C(OH)CH=CHSn( p-tol)(2)Cl (4), in which significant Sn-O(1) interactions are noted [ 2.437(8) Angstrom and 2.407(8) Angstrom, respectively].