THE SYNTHESES, SE-77 CP-MAS SOLID-STATE NMR-SPECTRA AND CRYSTAL-STRUCTURES OF ADDUCTS OF THE SELENIUM CORONAND, 1,5,9,13-TETRASELENACYCLOHEXADECANE, WITH COPPER(I) TRIFLUOROMETHANESULFONATE AND MERCURY(II) CYANIDE

The preparation, characterization, X-ray crystal structures and Se-77 CP-MAS solid state NMR spectra of adducts of 1,5,9,13-tetraselenacyclohexadecane with copper(I)trifluoromethanesulfonate and mercury(II)cyanide are reported. Crystal data: [(Cu(Se(CH2)3)4)][SO3CF3] (1); orthorhombic; space group B22(1)2; a = 8.947 (2); b = 15.184(2); c = 15.918(2) angstrom; V = 2162.2 angstrom 3; Z = 4; FW = 696.77; rho-c = 2.140 g cm-3; lambda = 0.71069 angstrom; R(F) = 0.044 for 622 data (I greater-than-or-equal-to 2.5-sigma(I)). (Hg(CN)2)((Se(CH2)3)4) (2); monoclinic; space group P2(1)/c; a = 5.822(1); b = 12.457(2); c = 14.074(2) angstrom; beta = 99.07(1)-degrees; V = 1008.1 angstrom 3; Z = 2; FW = 736.79; rho-c = 2.427 g cm-3; lambda = 0.71069 angstrom; R(F) = 0.038 for 1153 data (I greater-than-or-equal-to 2.5-sigma(I)). 1 displays orientational disorder of the SO3CF3- anion and correlated disorder of the complex cation. The refinement was stabilized using soft restraints. The cation is a three-dimensional polymeric complex with pseudo-tetrahedral coordination about copper to four distinct ligands. 2 consists of linear Hg(CN)2 molecules which interact weakly with four selenium atoms from different ligands to give a tetragonally distorted octahedral arrangement.