Peculiarities of the Reactions of Tris(2-methoxy-5-bromphenyl)stibine with Silver Nitrate
Abstract
By the reaction of tris(2-methoxy-5-bromophenyl)stibine with silver nitrate in a solution of dioxane and acetonitrile, a complex of nitrato-O,O'-(acetonitrile)[tris(2-methoxy-5-bromophenyl)stibine]silver in the form of solvate with dioxane (2-MeO-5-BrC6H3)3SbAg(NO3)(MeCN)×(C4H8O2) (1) was synthesized. The structure of 1 was determined by X-ray diffraction analysis and IR spectroscopy. The IR spectrum of complex 1 contains bands, characteristic for tris[(2-methoxy)(5-bromo) phenyl]stibine, C≡N and NO3 groups.
X-ray diffraction analysis of the complex was performed on a Bruker D8 Quest automatic four-circle diffractometer (МоКα radiation, λ = 0.71073 Å, graphite monochromator) at 293 K. Crystal Data: triclinic, space group P-1, a = 9.35(2), b = 17.04(3), c = 22.01(4) Å,
a = 104.22(5)°, β = 94.33(10)°, g = 99.30(8)°, V = 3329(12) Å3, Z = 2, rcalc 1.9529g/cm3,
2q 5.78-47.14°, 44984 reflections measured, 9679 unique reflections, the number of refinement variables 765, Rint = 0.2108, GOOF 1.107, R factors for F2 > 2σ(F2) R1 = 0.0584, wR2 = 0.1500,
R factors for all reflections R1 = 0.0818, wR2 = 0.1750, largest diff. peak and hole, 1.11/-1.74 e/Å3.
In crystal 1, there are two types of crystallographically independent molecules (A, B) and two types of crystallographically independent dioxane solvate molecules. In the distorted tetrahedral surroundings of silver atoms, there are acetonitrile molecules coordinated by cyano group nitrogen atom, a triarylstibine molecule, and O,O'-coordinated nitrate group. The distances Ag-N and Ag-Sb are 2.260(13), 2.291(12) Å and 2.625(5), 2.618(5) Å, respectively. Ag-O distances vary (2.428(11) and 2.493(10) Å; 2.426(9) and 2.534(10) Å).
