Abstract
The conditions for the synthesis of two polymorph modifications of ammonium tetrafluorobismutate (III) from the heated water solution of ammonium fluoride (bifluoride) were studied with different BiF3:NH4HF2(NH4F) reagent concentrations. The crystal structure of monoclinic β–NH4BiF4 (a = 8.1014(3), b = 6.6208(2), c = 8.1045(3) Å, β = 111.003(1)°, sp.gr. P21/c) was determined for the first time. The structure of α–NH4BiF4 (a = 8.3185(6), b = 7.5902(6), c = 6.4866(5) Å, β = 93.687(1)°, sp.gr. P21/c) was refined. Both polymorph modifications have layered structures with a single nine-coordinated bismuth site. The thermal decomposition of NH4BiF4 was studied and two products of the decomposition having a cubic structure were isolated. The fluorine and ammonium mobility in obtained phases was probed with 1H, 19F NMR.
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