A Slow Leak Synthetic Route to Organically Templated Gallium Sulfates

作者：Kaufman Elizabeth A; Zeller Matthias; Norquist Alexander J^*

来源：Crystal Growth & Design, 2010, 10(10): 4656-4661.

DOI：10.1021/cg1009412

Single crystals of the first four organically templated gallium sulfates were prepared under mild hydrothermal conditions: [C(2)H(10)N(2)][H(3)O][Ga(SO(4))(3)], [C(2)H(10)N(2)][Ga(OH)(SO(4))(2)]center dot H(2)O, [C(6)H(18)N(2)][Ga(H(2)O)(2)(SO(4))(2)](2), and [C(4)H(14)N(2)][Ga(H(2)O)(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(2)O)(2)(SO(4))(2)](n)(n-) chains for [Ga(H(2)O)(2)(SO(4))(2)](n)(n-) layers, respectively, and protonated organic amine dications. Reactions were conducted in 15 ml. polypropylene bottles at 100 degrees 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(2)H(10)N(2)][H(3)O][Ga(SO(4))(3)], [C(2)H(10)N(2)][Ga(OH)(SO(4))(2)]center dot H(2)O, [C(4)H(14)N(2)][Ga(H(2)O)(2)(SO(4))(2)](2), and [C(6)H(18)N(2)][Ga(H(2)O)(2)(SO(4))(2)](2) reflect the initial reagent concentrations and amine structures.

• 出版日期2010-10