MACROBICYCLIC D-METAL TRIS-DIOXIMATES OBTAINED BY CROSS-LINKING WITH P-BLOCK ELEMENTS .10. THE 1ST CRYSTAL AND MOLECULAR-STRUCTURE OF CLATHROCHELATE TRIS-DIOXIMATES WITH NONSYMMETRICAL DIOXIMES - MER ISOMERS OF AN IRON(II) COMPLEX WITH A MACROBICYCLIC PHENYLBORON PHENYLGLYOXIMATE LIGAND

Single crystals of the FePhm3(BC6H5)2.BF3 complex contain two mer isomers with different orientations of phenyl substituents in dioxime fragments have been obtained by the template cross-linking of three phenylglyoximate (H-2Phm) molecules with two phenylboric acid molecules in the presence of boron trifluoride. They crystallize in space group P1BAR, a = 13.962 (5), b = 13.519 (2), c = 12.343 (6) angstrom, alpha = 63.63(7), beta = 100.78(4), gamma = 79.88(7)degrees, V = 1959.9 angstrom3, Z = 2. The structure has been determined by X-ray methods. The trigonal prismatic coordination polyhedron formed by six nitrogen atoms of the macrobicyclic ligand has a distortion angle of 21.8-degrees. The Fe-N bond length (1.91 angstrom) and the bite angle (39.2-degrees) are typical for clathrochelate tris-dioximates of iron(II). A comparison between the value of quadrupole splitting in Mossbauer (Fe-57) spectra obtained experimentally and its calculated value has been made.