5-氨基-3H-1,3,4-噻二唑-2-硫酮的某些有机锡（IV）衍生物的合成、光谱及热学研究
Synthesis, spectral and thermal studies of some organotin(IV) derivatives of 5-amino-3H-1,3,4-thiadiazole-2-thione.
作者信息
Nath Mala, Song Xueqing, Eng George
机构信息
Department of Chemistry, Indian Institute of Technology-Roorkee, Roorkee 247667, India.
出版信息
Spectrochim Acta A Mol Biomol Spectrosc. 2006 May 1;64(1):148-55. doi: 10.1016/j.saa.2005.07.009. Epub 2005 Aug 10.
Some tri- and diorganotin(IV) compounds of the general formula, RnSnL4-n (where n=2, R=Me, n-Bu and Ph; n=3, R=Me, n-Bu, n-Pr and Ph; HL=5-amino-3H-1,3,4-thiadiazole-2-thione) have been synthesized by the reaction of RnSnCl4-n (where n=2 or 3, R=Me, n-Bu, n-Pr and Ph) and the sodium salt of the ligand. Oct2SnL2 was obtained by the reaction of Oct2SnO with HL in a 1:2 molar ratio under azeotropic removal of water. The bonding and coordination behavior in these derivatives are discussed on the basis of IR, Far-IR, multinuclear (1H, 13C and 119Sn) NMR and 119Sn Mössbauer spectroscopic studies. These investigations suggest that in all the compounds the ligand acts as monoanionic bidentate coordinating through ring N(3) and exocyclic S. Thermal studies of five compounds, viz., Ph3SnL, Me2SnL2, n-Bu2SnL2, Oct2SnL2 and Ph2SnL2 have been carried out in the temperature range 25-1000 degrees C using TG, DTG and DTA techniques under an atmosphere of dry nitrogen.
通过通式为RnSnL4-n（其中n = 2，R = 甲基、正丁基和苯基；n = 3，R = 甲基、正丁基、正丙基和苯基；HL = 5-氨基-3H-1,3,4-噻二唑-2-硫酮）的一些三有机锡（IV）和二有机锡（IV）化合物，是由RnSnCl4-n（其中n = 2或3，R = 甲基、正丁基、正丙基和苯基）与配体的钠盐反应合成的。辛基二锡（II）二配体化合物（Oct2SnL2）是通过辛基二锡（II）氧化物（Oct2SnO）与HL以1:2的摩尔比在共沸脱水条件下反应得到的。基于红外光谱（IR）、远红外光谱（Far-IR）、多核（1H、13C和119Sn）核磁共振（NMR）以及119Sn穆斯堡尔光谱研究，对这些衍生物中的键合和配位行为进行了讨论。这些研究表明，在所有化合物中，配体通过环上的N(3)和环外的S作为单阴离子双齿配体进行配位。使用热重分析（TG）、微商热重分析（DTG）和差示热分析（DTA）技术，在干燥氮气气氛下，对五种化合物，即苯基三锡（IV）配体化合物（Ph3SnL）、二甲基二锡（IV）二配体化合物（Me2SnL2）、二正丁基二锡（IV）二配体化合物（n-Bu2SnL2）、辛基二锡（II）二配体化合物（Oct2SnL2）和二苯基二锡（IV）二配体化合物（Ph2SnL2），在25至1000摄氏度的温度范围内进行了热研究。
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