(Z)-1--1-cycloheptanols: synthesis, characterization, halodemetallation and crystal structures

Article abstract of DOI:10.1016/0022-328X(95)05170-T

The synthesis and characterization by 1H, 13C, 119Sn NMR and 119Sn Moessbauer spectroscopy of (Z)-1-<2-(triphenylstannyl)vinyl>-1-cycloheptanol, (1), and (Z)-1-<2-(tri-p-tolylstannyl)vinyl>-1-cycloheptanol, (2), are described, together with their halodemetallation by I2, Br2 and ICl1 to yield derivatives of the types (Ar = phenyl or p-tolyl, n = 1, 2; X = I, Br, Cl, respectively).The solid-state structures of four compounds have been determined by X-ray diffraction analysis.In the crystals of (1) and (2) the Sn atom has a tetrahedral geometry distorted towards trigonal bipyramid as a consequence of a close intramoleculatr contact with the hydroxyl O(1) atom of 2.742(3) Angstroem and 2.768(3) Angstroem, respectively.A trigonal bipyramidal geometry is found in (12) and (4), in which significant Sn-O(1) interactions are noted <2.437(8) Angstroem and 2.407(8) Angstroem, respectively>. Keywords: Tin; Crystal structure; NMR