Synthesis and characterization of chromium-isothiocyanate-4-methylpyridine complexes

被引：1
|
作者：
Young, Jennifer L. [1 ]
Harris, Jerry D. [1 ]
Benjamin, Joshua A. [1 ]
Fitch, Jannah E. [1 ]
Nogales, Daniel F. [1 ]
Walker, Joanna R. [1 ]
Frost, Brian J. [2 ]
Thurber, Aaron [3 ]
Punnoose, Alex [3 ]
机构：
[1] NW Nazarene Univ, Dept Chem, Nampa, ID 83686 USA
[2] Univ Nevada, Dept Chem, Reno, NV 89557 USA
[3] Boise State Univ, Dept Phys, Boise, ID 83725 USA
来源：
INORGANICA CHIMICA ACTA | 2011年 / 377卷 / 01期
基金：
美国国家科学基金会;
关键词：
Chromium; Isothiocyanate; Methylpyridine; Crystal structure; Thermal analysis; CHARGE-TRANSFER SALTS; THERMAL-DECOMPOSITION; CR-III; THERMOGRAVIMETRIC DATA; KINETIC-ANALYSIS; METAL POWDERS; TM-TTF; FE-III; ANIONS; TETRAMETHYLTETRATHIAFULVALENE;
D O I：
10.1016/j.ica.2011.07.023
中图分类号：
O61 [无机化学];
学科分类号：
070301 ; 081704 ;
摘要：
The synthesis and single crystal X-ray structure of trans-[HNC6H7][Cr(NCS)(4)(NC6H7)(2)] (1) and mer[Cr(NCS)(3)(NC6H7)(3)] (2) are reported. Compound 1 was synthesized by refluxing chromium powder and thiourea in 4-methylpyridine. The isothiocyanate ligand is believed to be generated from the isomerization of thiourea to ammonium thiocyanate during synthesis. Compound 2 was prepared from CrCl3 and KSCN in 4-methylpyridine. The reaction conditions for both compounds yielded a mixture of [Cr(NCS)(x)(NC6H7)(6) (x)](3) (x) isomers (x = 0-6), which were analyzed by HPLC. The thermal properties of trans-[HNC6H7][Cr(NCS)(4)(NC6H7)(2)] were analyzed by thermogravimetric analysis/differential scanning calorimetry-mass spectroscopy (TGA/DSC-MS), and the compound was found to oxidize to CrO2 in three major weight loss steps when heated to 1000 degrees C in dry air. (C) 2011 Elsevier B. V. All rights reserved.
引用
收藏
页码：14 / 19
页数：6
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