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-BrC 6 H 3 ) 3 SbAg(NO 3 )(MeCN)×(C 4 H 8 O 2 ) ( 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 NO 3 groups. X-ray diffraction analysis of the complex was performed on a Bruker D8 Quest automatic four-circle diffractometer (Мо К α 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) Å 3 , Z = 2, r calc 1.9529g/cm 3 , 2q 5.78-47.14°, 44984 reflections measured, 9679 unique reflections, the number of refinement variables 765, R int = 0.2108, GOOF 1.107, R factors for F 2 > 2σ( F 2 ) R 1 = 0.0584, wR 2 = 0.1500, R factors for all reflections R 1 = 0.0818, wR 2 = 0.1750, largest diff. peak and hole, 1.11/-1.74 e /Å 3 . 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).

Highlights

  • Взаимодействием трис(2-метокси-5-бромфенил)стибина с нитратом серебра в растворе диоксана и ацетонитрила получен комплекс нитрато-О,О’-(ацетонитрил)[трис(2метокси-5-бромфенил)стибин]серебро в форме сольвата с диоксаном

  • В комплексах с тремя фрагментами Ph3Sb в координационной сфере серебра четвертое место занимает галоген (Cl, Br, I), псевдогалоген (SCN, NCS, CN) [9], остаток оксима [10], другой лиганд большого объема [11, 12] или бидентатный лиганд, повышающий координационное число серебра до пяти [13]

  • 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-5bromophenyl)stibine]silver in the form of solvate with dioxane (2-MeO-5BrC6H3)3SbAg(NO3)(MeCN) (C4H8O2) (1) was synthesized

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Summary

Introduction

Взаимодействием трис(2-метокси-5-бромфенил)стибина с нитратом серебра в растворе диоксана и ацетонитрила получен комплекс нитрато-О,О’-(ацетонитрил)[трис(2метокси-5-бромфенил)стибин]серебро в форме сольвата с диоксаном В ИК-спектре комплекса 1 присутствуют полосы, характерные для трис(2-метокси-5-бромфенил)стибина, C≡N- и NO3-групп. Кристаллографические характеристики: триклинная сингония, пространственная группа P-1, a = 9,35(2), b = 17,04(3), c = 22,01(4) Å, = 104,22(5), β = 94,33(10), = 99,30(8) град., V = 3329(12) Å3, Z = 2, выч 1,9529 г/см3, 2 5,78 47,14 град., всего отражений 44984, независимых отражений 9679, число уточняемых параметров 765, Rint = 0,2108, GOOF 1,107, R-факторы по F2 > 2σ(F2) R1 = 0,0584, wR2 = 0,1500, R-факторы по всем отражениям R1 = 0,0818, wR2 = 0,1750, остаточная электронная плотность (max/min), 1,11/ 1,74 e/Å3.

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