The reaction of pentaphenylantimony with triphenylantimony dinitrate in toluene gives tetraphenylantimony nitrate in 99% yield. The X-ray diffraction data show that the antimony atom in the molecule of tetraphenyl antimony nitrate has a distorted trigonal-bipyramidal coordination with axial location of the oxygen atom of the nitrate group. The Sb-O, Sb-ax, and Sb-C-eq bond lengths in two independent molecules of tetraphenylantimony nitrate are 2.498(3), 2.548(2); 2.134(3), 2.138(3); and 2.101(3)-2.112 Angstrom.
作者:V. V. Sharutin、O. K. Sharutina、N. V. Nasonova、A. P. Pakusina、A. N. Zakharova、D. V. Krivolapov、A. T. Gubaidullin、I. A. Litvinov
DOI:10.1023/a:1013268827590
日期:——
The reaction of mu-oxobis(nitratotriphenylantimony) with pentaphenylantimony in toluene in the presence of moisture and carbon dioxide gives the toluene solvate of tris(tetraphenylstiboxy)amine hydronitrate [(Ph4SbO)(3)N].NO3-.H3O+.2C(7)H(8). According to X-ray diffraction data, the three Ph(4)ShO groups are bound with the central nitrogen atom by simple bonds [the N-O interatomic distances are 1.31(1)Angstrom]. The NO2 fragment is planar (the sum of the bond angles at N-1 is 359.7degrees). The antimony atom has a slightly distorted trigonal-bipyramidal coordination.
Adducts of tetraphenylstibium nitrate with nitric acid and of tetraphenylstibium acetate with acetic acid: Syntheses and structures
作者:V. V. Sharutin、V. S. Senchurin、O. K. Sharutina、L. P. Panova
DOI:10.1134/s0036023608070206
日期:2008.7
The reactions of tetraphenylstibium nitrate with nitric acid and of tetraphenylstibium acetate with acetic acid yield adducts Ph4SbONO2 center dot HNO3 (I) and Ph4SbOC(O)CH3 center dot CHH3COOH (II). According to X-ray diffraction data, the antimony atom in [Ph4Sb](+)[O2N-O center dot center dot center dot H center dot center dot center dot O-NO2](-) has a tetrahedral coordination. The CSbC bond angles and Sb-C bond lengths vary within 108.04(6)degrees-109.75(4)angstrom and 2.096(1)-2.098(1) angstrom, respectively. The anion includes the intermolecular hydrogen bond O(1)-H(1)center dot center dot center dot O(1)'' the O(1)-H(1), H(1)center dot center dot center dot O(1)'', and O(1)center dot center dot center dot O(1)'' distances are 0.91(4), 1.56(4), and 2.460(2) angstrom, respectively; and the OHO angle is 169(5)angstrom. The nitrate groups are usually planar. Complex II also contains the intermolecular hydrogen bond with the following parameters: O(3)-H(3), 0.92 angstrom; H(3)center dot center dot center dot O(2), 1.68 angstrom; and O(3)center dot center dot center dot O(2) 2.594 angstrom; the O(2)H(3)O(3) angle is 172.1 angstrom. This H-bond noticeable changes the coordination polyhedron of the antimony atom compared to that in tetraphenylstibium acetate.