The synthesis, characterization, and structure of (ThioH)2[OsX6] (X = Cl, Br)

被引：7
|
作者：
Rudnitskaya, Olga V. [1 ]
Kultyshkina, Ekaterina K. [1 ]
Dobrokhotova, Ekaterina V. [1 ]
Podvoyskaya, Viktoriya S. [1 ]
Dorovatovskii, Pavel V. [2 ]
Lazarenko, Vladimir A. [2 ]
Zubavichus, Yan V. [2 ]
Khrustalev, Victor N. [1 ]
机构：
[1] Peoples Friendship Univ Russia, Dept Inorgan Chem, RUDN Univ, Miklukho Maklay St 6, Moscow 117198, Russia
[2] Natl Res Ctr, Kurchatov Inst, Acad Kurchatov Sq 1, Moscow 123182, Russia
来源：
POLYHEDRON | 2017年 / 134卷
关键词：
Osmium halido compltxes; Thiourea; Protonation; IR and UV-Vis spectroscopy; Synchrotron X-ray diffraction;
D O I：
10.1016/j.poly.2017.05.057
中图分类号：
O61 [无机化学];
学科分类号：
070301 ; 081704 ;
摘要：
Novel osmium complexes (ThioH)(2)[OsCI6] (1) and (ThioH)(2)[OsBr6] (2) have been synthesized via the interaction of H-2[OSX6] (X = Cl, Br) with thiourea (Thio) in concentrated HX and characterized by chemical analysis, potentiometry, IR- and UV-Vis spectroscopy, X-ray powder and single-crystal diffraction. UV-Vis spectroscopy of 1 and 2 in solutions supports the preservation of [OsX6](2-) ions that however demonstrate considerable solvatochromism. The longer-wavelength bands experience a hypsochromic shift with respect to the crystalline state. Intense bands of Os-halogen vibrations in ATR IR spectra are red-shifted with respect to those for K-2[OsX6]. The complexes are isostructural and crystallized in the triclinic space group P (1) over bar, Z =1. Unit cell parameters are for 1: a = 7.1800(14)angstrom, b = 7.2700(15)angstrom, c = 7.7800 (16)angstrom, alpha = 78.89(3)degrees, beta = 87.83(3)degrees, gamma = 65.11(3)degrees; for 2: a= 7.3169(15)angstrom, b = 7.5504(15)angstrom, c = 8.2065 (16) angstrom, alpha = 80.00(3)degrees, beta = 88.55(3)degrees, gamma = 63.37(3)degrees. The cations (NH2)(2)CSH+ and anions [OsX6](2-) are assembled into two-tier layers by N-H ... X and S-H ... X hydrogen-bonds and S ... X non-valent contacts. (C) 2017 Elsevier Ltd. All rights reserved.
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收藏
页码：114 / 119
页数：6
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