Alkylpyridinium lodobismuthates(III),Journal of Chemical Crystallography

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Alkylpyridinium lodobismuthates(III)
Journal of Chemical Crystallography ( IF 0.4 ) Pub Date : 2021-08-25 , DOI: 10.1007/s10870-021-00901-5
Robert D. Pike ₁ , Neal E. Marshall ₁ , Abigail L. Martucci ₁

Affiliation

The reaction of N-alkyl pyridinium iodide salts (RPy⁺I⁻, R = Me, Et, ⁿPr, ⁿBu) with BiI₃ produced various alkyl pyridinium iodobismuthate(III) compounds, (RPy)_y−3x[Bi_xI_y]. A wide nuclearity range was observed in the iodobismuthate(III) clusters when crystallized from acetone/acetonitrile: For R = Me, the dominant phase, {(MePy)[BiI₄]}_n, is a chain of edge-sharing BiI₆ octahedra. Another phase, (MePy)₃[Bi₂I₉]‧MeCN, has a face-sharing dimer of BiI₆ octahedra. Five phases are reported for R = Et: (EtPy)₃[Bi₂I₉]·${\raise0.5ex\hbox{$\scriptstyle 2$} \kern-0.1em/\kern-0.15em \lower0.25ex\hbox{$\scriptstyle 3$}}$ MeCN, (EtPy)₃[Bi₃I₁₂], (EtPy)₃[Bi₃I₁₂]·MeCN (a new V-shaped trimeric anion structural type), (EtPy)₄[Bi₄I₁₆], and (EtPy)₄[Bi₆I₂₂]·2MeCN. Two R = ⁿPr phases were found: (PrPy)₃[Bi₂I₉] and (PrPy)₄[Bi₄I₁₆]·MeCN. Two phases were also found for R = ⁿBu: (BuPy)₃[Bi₂I₉] and (BuPy)₄[Bi₄I₁₆]. Bulk synthesized products shown diffraction matches to {(MePy)[BiI₄]}_n, (EtPy)₃[Bi₃I₁₂], (PrPy)₄[Bi₄I₁₆], and (BuPy)₄[Bi₄I₁₆], respectively. Thermal analysis of all four bulk compounds showed near complete mass loss above 300 °C.

Graphic Abstract

The structures, phases, and thermal behavior of N-alkyl pyridinium iodobismuthate(III) compounds (RPy)_y−3x[Bi_xI_y] (R = Me, Et, ⁿPr, ⁿBu) are presented and discussed.

中文翻译：

烷基吡啶鎓碘化铋(III)

N-烷基吡啶鎓碘化物盐 (RPy ⁺ I ⁻ , R = Me, Et, ⁿ Pr, ⁿ Bu) 与 BiI _{3 的反应}产生了各种烷基吡啶鎓碘化铋 (III) 化合物，(RPy) _y−3x [Bi _x I _ÿ ]。当从丙酮/乙腈结晶时，在碘铋 (III) 簇中观察到广泛的核度范围：对于 R = Me，主相 {(MePy)[BiI ₄ ]} _n是一条共享边缘的 BiI ₆八面体链. 另一相，(MePy) ₃ [Bi ₂ I ₉ ]‧MeCN，具有BiI ₆的共享面二聚体八面体。报告了 R = Et 的五个阶段：(EtPy) ₃ [Bi ₂ I ₉ ]· ${\raise0.5ex\hbox{$\scriptstyle 2$} \kern-0.1em/\kern-0.15em \lower0。 25ex\hbox{$\scriptstyle 3$}}$ MeCN, (EtPy) ₃ [Bi ₃ I ₁₂ ], (EtPy) ₃ [Bi ₃ I ₁₂ ]·MeCN（一种新的V型三聚阴离子结构类型）， (EtPy) ₄ [Bi ₄ I ₁₆ ]和(EtPy) ₄ [Bi ₆ I ₂₂ ]·2MeCN。发现两个 R = ⁿ Pr 相：(PrPy) ₃ [Bi ₂ I₉ ]和(PrPy) ₄ [Bi ₄ I ₁₆ ]·MeCN。对于 R = ⁿ Bu ，还发现了两个相：(BuPy) ₃ [Bi ₂ I ₉ ] 和 (BuPy) ₄ [Bi ₄ I ₁₆ ]。显示与 {(MePy)[BiI ₄ ]} _n、(EtPy) ₃ [Bi ₃ I ₁₂ ]、(PrPy) ₄ [Bi ₄ I ₁₆ ] 和 (BuPy) ₄ [Bi ₄ I ₁₆衍射匹配的批量合成产品]，分别。所有四种本体化合物的热分析表明，在 300 °C 以上时质量几乎完全损失。