Synthesis of 4-Hydroxy-2,6-di(pyrazol-1-yl) pyridine, and the Spin State Behaviour of Its Iron(II) Complex Salts

被引:9
作者
Cook, Laurence J. Kershaw [1 ]
Halcrow, Malcolm A. [1 ]
机构
[1] Univ Leeds, Sch Chem, Woodhouse Lane, Leeds LS2 9JT, W Yorkshire, England
基金
英国工程与自然科学研究理事会;
关键词
iron; N-donor ligand; spin-crossover; crystal structure; magnetic measurements; calorimetry;
D O I
10.3390/magnetochemistry1010003
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Treatment of 4-hydroxy-2,6-dibromopyridine with four equivalent of deprotonated pyrazole in hot diglyme affords 4-hydroxy-2,6-di(pyrazol-1-yl) pyridine (L) in low yield. The three complex salts [FeL2] X-2 (X-=BF4-, 1; X- = ClO4-, 2; X- = PF6-, 3) have been prepared, and crystallographically characterised as their methanol solvates. The solvate structures contain complexes that are fully high-spin (1 and 3), or in a mixed high: low spin state population at 150 K (2). Bulk samples of 1 and 2 obtained from methanol/diethyl ether contain a second, minor crystal phase that exhibits an abrupt spin-transition near 200 K. Recrystallisation of 1 and 2 from nitromethane/diethyl ether affords powder samples that are highly enriched in this spin-transition phase.
引用
收藏
页码:3 / 16
页数:14
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