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A slow leak synthetic route to organically templated gallium sulfates

机译:缓慢泄漏合成有机模板化硫酸镓的途径

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摘要

Single crystals of the first four organically templated gallium sulfates were prepared under mild hydrothermal conditions: [C_2H _(10)N_2][H_3O][Ga(SO_4)_3], [C_2H_(10)N_2][Ga(OH)(SO_4) _2]?H_2O, [C_6H_(18)N _2][Ga(H_2O)_2(SO_4)_2] _2, and [C_4H_(14)N_2][Ga(H _2O)_2(SO_4)_2]_2. These compounds contain either [Ga(SO_4)_3]_n~(3n-), [Ga(OH)(SO_4)_2]_n~(2n-), or [Ga(H_2O)_2(SO_4)_2]_n~(n-) chains or [Ga(H_2O)_2(SO_4) _2]_n~(n-) layers, respectively, and protonated organic amine dications. Reactions were conducted in 15 mL polypropylene bottles at 100 °C. A slow leak solvent evaporation technique allowed for the use of sparingly soluble oxide starting materials, gently increased reactant concentrations, and facilitated the growth of high quality single crystals over 1.5 d. Differences in composition and structure between [C_2H _(10)N_2][H_3O][Ga(SO_4)_3], [C_2H_(10)N_2][Ga(OH)(SO_4) _2]?H_2O, [C_4H_(14)N _2][Ga(H_2O)_2(SO_4)_2] _2, and [C_6H_(18)N_2][Ga(H _2O)_2(SO_4)_2]_2 reflect the initial reagent concentrations and amine structures.
机译:在温和的水热条件下制备了前四种有机模板化硫酸镓的单晶:[C_2H _(10)N_2] [H_3O] [Ga(SO_4)_3],[C_2H_(10)N_2] [Ga(OH)(SO_4) )_2]?H_2O,[C_6H_(18)N _2] [Ga(H_2O)_2(SO_4)_2] _2和[C_4H_(14)N_2] [Ga(H _2O)_2(SO_4)_2] _2)。这些化合物包含[Ga(SO_4)_3] _n〜(3n-),[Ga(OH)(SO_4)_2] _n〜(2n-)或[Ga(H_2O)_2(SO_4)_2] _n〜( n-)链或[Ga(H_2O)_2(SO_4)_2] _n〜(n-)层,以及质子化的有机胺指示剂。反应在100°C的15 mL聚丙烯瓶中进行。缓慢泄漏的溶剂蒸发技术允许使用微溶的氧化物原料,缓慢增加反应物的浓度,并在1.5 d内促进高质量单晶的生长。 [C_2H _(10)N_2] [H_3O] [Ga(SO_4)_3],[C_2H_(10)N_2] [Ga(OH)(SO_4)_2]?H_2O,[C_4H_(14)之间的组成和结构差异N _2] [Ga(H_2O)_2(SO_4)_2] _2和[C_6H_(18)N_2] [Ga(H _2O)_2(SO_4)_2] _2反映了初始试剂浓度和胺结构。

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