超声辅助形成{Fe6Ln / Y4}轮状团簇和凝聚的{Fe4Ln / Y2}团聚体,European Journal of Inorganic Chemistry

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超声辅助形成{Fe6Ln / Y4}轮状团簇和凝聚的{Fe4Ln / Y2}团聚体
European Journal of Inorganic Chemistry ( IF 2.2 ) Pub Date : 2019-04-16 , DOI: 10.1002/ejic.201900175
Olga Botezat _{1,

2} , Jan van Leusen ₂ , Paul Kögerler ₂ , Svetlana G. Baca ₁

Affiliation

发现由异丁酸酯和氨基醇酸酯连接基组成的两个电荷中性杂金属Fe-4f配位化合物家族仅在超声辐照下形成。在单锅条件下，三核前体[Fe ₃ O（O ₂ CCHMe ₂）₆（H ₂ O）₃ ]（NO ₃）· 2（MeCN）· 2（H ₂ O）与Ln（NO ₃）反应₃· x H ₂ O或Y（NO ₃）₃· 6H ₂ O，正丁基二乙醇胺（bdeaH ₂）和甲醇中的NaN ₃生成十核簇[Fe ₆ M ₄（O ₂ CCHMe ₂）₈（N ₃）₂（bdea）₁₀ ] · n（溶剂）（M ^III = Y（1a·3MeOH），Gd （2a·2.5MeOH），Dy（3a·3.5MeOH·0.5H ₂ O），Tb（4a·2MeOH），Ho（5a·2MeOH）以及随后的六核化合物[Fe ₄ M ₂（OH）₂（O ₂ CCHMe ₂）₆（N ₃）₂（bdea）₄ ] · 2（溶剂）（M ^III = Y（1b·2MeOH），Gd（2b·2MeOH），Dy（3b·2MeOH，3c·2EtOH），Tb（4b· 2MeOH），Er（6b·2MeOH），Tm（7b·2MeOH））。{Fe ₆ M _4}团簇具有轮状结构，金属离子通过羧酸盐和多元醇胺桥相互连接，形成一个鞍状环。六核{Fe ₄ M _2}簇包含两个{Fe ₂ M}三角形，通过两个桥接µ ₃连接-OH ^-基团，其形成金属的稠芯附加地通过去质子化的三足bdeaH联₂配体和桥接羧酸盐。磁性测量显示，化合物1 – 7中主要存在强反铁磁相互作用，并且{Fe ₆ Dy _4}（3a·3.5MeOH·0.5H ₂ O），{Fe ₆ Tb _4}（4a·2MeOH）的信号异相，和{Fe ₄ Dy _2}（3b·2MeOH）。

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Ultrasound‐Assisted Formation of {Fe6Ln/Y4} Wheel‐Shaped Clusters and Condensed {Fe4Ln/Y2} Aggregates

Two families of charge‐neutral heterometallic Fe‐4f coordination compounds comprising isobutyrate and amino alcoholate linkers were found to form exclusively upon ultrasonication irradiation. Under one‐pot conditions, the trinuclear precursor [Fe₃O(O₂CCHMe₂)₆(H₂O)₃](NO₃)·2(MeCN)·2(H₂O) reacts with Ln(NO₃)₃·xH₂O or Y(NO₃)₃·6H₂O, N‐butyldiethanolamine (bdeaH₂) and NaN₃ in methanol to yield the decanuclear clusters [Fe₆M₄(O₂CCHMe₂)₈(N₃)₂(bdea)₁₀]·n(solvent) (M^III = Y (1a·3MeOH), Gd (2a·2.5MeOH), Dy (3a·3.5MeOH·0.5H₂O), Tb (4a·2MeOH), Ho (5a·2MeOH), as well as subsequently the hexanuclear compounds [Fe₄M₂(OH)₂(O₂CCHMe₂)₆(N₃)₂(bdea)₄]·2(solvent) (M^III = Y (1b·2MeOH), Gd (2b·2MeOH), Dy (3b·2MeOH, 3c·2EtOH), Tb (4b·2MeOH), Er (6b·2MeOH), Tm (7b·2MeOH)). The {Fe₆M_4} clusters feature a wheel‐shaped architecture with the metal ions, interlinked by carboxylate and polyalcoholamine bridges, forming a saddle‐like ring. The hexanuclear {Fe₄M_2} clusters comprise two {Fe₂M} triangles, connected via two bridging µ₃‐OH^– groups, which form a condensed core of metals additionally linked by deprotonated tripodal bdeaH₂ ligands and bridging carboxylates. Magnetic measurements revealed predominant strong antiferromagnetic interactions within compounds 1–7 and out‐of‐phase signals for {Fe₆Dy_4} (3a·3.5MeOH·0.5H₂O), {Fe₆Tb_4} (4a·2MeOH), and {Fe₄Dy_2} (3b·2MeOH).

更新日期：2019-04-16

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