کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
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1312522 | 975457 | 2011 | 6 صفحه PDF | دانلود رایگان |
![عکس صفحه اول مقاله: Synthesis and characterization of chromium-isothiocyanate-4-methylpyridine complexes Synthesis and characterization of chromium-isothiocyanate-4-methylpyridine complexes](/preview/png/1312522.png)
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 °C in dry air.
The synthesis and characterization of [Cr(NCS)x(NC6H7)6–x]3–x (x = 1–6) compounds from Cr powder and thiourea is presented.Figure optionsDownload as PowerPoint slideHighlights
► Cr powder and thiourea in refluxing 4-methylpyridine yield multiple products.
► Reactions products were analyzed by HPLC.
► [Cr(NCS)4(NC6H7)2]− and [Cr(NCS)3(NC6H7)3] were characterized by crystallography.
► [HNC6H7][Cr(NCS)4(NC6H7)2] was characterized by TGA/DSC–MS.
► [HNC6H7][Cr(NCS)4(NC6H7)2] decomposes to CrO4 when heated in air to 1000 °C.
Journal: Inorganica Chimica Acta - Volume 377, Issue 1, 1 November 2011, Pages 14–19