Organophosphonate- and dimethylarsinate-functionalized hexamolybdates(v) and their solution and gas phase properties†

IF 6.4 1区化学 Q1 CHEMISTRY, INORGANIC & NUCLEAR Inorganic Chemistry Frontiers Pub Date : 2025-02-18 DOI:10.1039/D4QI03215B

Vinaya Siby, Arun Pal, Bassem S. Bassil, Saurav Bhattacharya, Anusree Sundar, Juliane Oberstein, Damin Kim, Rizul Gupta, Alisher Kuanysh, Jana Hölscher, Dorothea Schmidt, Nikolai Kuhnert and Ulrich Kortz

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Abstract

Here we report a comprehensive study on the synthesis and characterization of dimethylarsinate-functionalized phosphomolybdates(V), [RPMo^V₆O₁₅(OH)₃{AsO₂(CH₃)₂}₃]²⁻ (R = H, HO, CH₃, HO₂CCH₂, HO₂CC₂H₄, C₆H₅, 4-FC₆H₄, 4-F₃COC₆H₄) and the monoanionic mixed-valent heptamolybdate [HOMo^VIMo^V₆O₁₅(OH)₃{AsO₂(CH₃)₂}₃]⁻. These nine novel polyanions feature a reduced, cyclic hexanuclear {Mo^V₆O₂₄} core, decorated peripherally by three dimethylarsinate ligands and centrally by six different organophosphonate groups including fluorinated ones, as well as phosphate and phosphite. The polyanions were synthesized under simple one-pot aqueous solution conditions and characterized (i) in the solid state by single-crystal and powder XRD, TGA, elemental analysis, (ii) in solution by multinuclear (¹H, ³¹P, ¹⁹F, ¹³C) NMR, and (iii) in the gas phase by ESI mass spectrometry.

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有机膦酸盐和二甲基膦酸盐功能化的六聚酸盐(V)及其溶液和气相性质

本文报道了二甲基膦酸盐功能化磷酸钼酸盐(V), [RPMoV6O15(OH)3{AsO2(CH3)2}3]2- （R = H， HO, CH3, HO2CCH2, HO2CC2H4, C6H5, 4-FC6H4, 4-F3COC6H4）和单阴离子混合价七胺酸盐[HOMoVIMoV6O15(OH)3{AsO2(CH3)2}3]-的合成和表征。这9个新型多阴离子具有还原的环六核{MoV6O24}核，外围由3个二甲基膦酸盐配体装饰，中心由6个不同的有机膦酸基团（包括氟化基团）以及磷酸盐和亚磷酸盐装饰。在简单的一罐水溶液条件下合成了聚阴离子，并在固态下通过单晶和粉末XRD， TGA，元素分析进行了表征，（ii）在溶液中通过多核（1H, 31P, 19F, 13C） NMR进行了表征，（iii）在气相中通过ESI质谱进行了表征。

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