Polymeric thallium(I) O,O'-diisopropyl dithiophosphate [Tl{S2P(O-iso-C3H7)2}] n : Synthesis, structure, and 13C and 31P CP/MAS NMR spectra

被引：8
|
作者：
Ivanov, A. V. [1 ]
Konfederatov, V. A. [1 ]
Gerasimenko, A. V. [2 ]
Larsson, A. -C. [3 ]
机构：
[1] Russian Acad Sci, Inst Geol & Nat Management, Far E Div, Blagoveshchensk 675000, Russia
[2] Russian Acad Sci, Inst Chem, Far E Div, Vladivostok 690022, Russia
[3] Lulea Univ Technol, S-97187 Lulea, Sweden
来源：
RUSSIAN JOURNAL OF COORDINATION CHEMISTRY | 2009年 / 35卷 / 11期
基金：
俄罗斯基础研究基金会;
关键词：
X-RAY-DIFFRACTION; CHEMICAL-SHIFT ANISOTROPY; CRYSTAL-STRUCTURE; O; O'-DIALKYLDITHIOPHOSPHATE ZINC(II); MOLECULAR-STRUCTURE; LEAD(II) COMPLEXES; STATE; POLYCRYSTALLINE; DIETHYLDITHIOCARBAMATE; ORGANIZATION;
D O I：
10.1134/S1070328409110116
中图分类号：
O61 [无机化学];
学科分类号：
070301 ; 081704 ;
摘要：
The crystalline polymeric thallium(I) O,O'-diisopropyl dithiophosphate [Tl{S2P(O-iso-C3H7)(2)}] (n) (I) was obtained and examined by solid-state C-13 and P-31 CP/MAS NMR spectroscopy. Diagrams of the chi(2) statistic were constructed from the complete P-31 MAS NMR spectra and used to calculate the P-31 chemical shift anisotropy (delta(aniso) = (delta (zz) - delta(iso))) and the asymmetry parameter (eta = (delta (yy) - delta (xx) )/(delta (zz) - delta(iso))). The P-31 chemical shift tensor has a nearly axial symmetry (eta = 0.22, delta (zz) < delta (yy) a parts per thousand delta (xx) ). The MAS NMR spectral patterns correspond to the negative sign of delta(aniso) (delta (zz) < delta (yy) < delta (xx) ), which indicates bridging or chelating-bridging coordination of the dithiophosphate ligands (Dtph). X-ray diffraction analysis revealed a polymeric structure of compound I. The polymer chain consists of alternating mononuclear [Tl{S2P(O-iso-C3H7)(2)}] molecules with opposite spatial orientations. The Dtph ligands are coordinated in a mixed, chelating-mu(3)-bridging fashion. The shape of the P-31 NMR signal was interpreted in terms of the P-31-Tl-203,Tl-205 coupling pattern proposed from crystallographic data.
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收藏
页码：857 / 863
页数：7
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