Synthesis and X-ray structure of [(H_3O)(C_(14)H_(20)O_5)_2][Me_2NH_2]_2 [PMo_(12)O_(40)]·2C_(14)H_(20)O_5 (C_(14)H_(20)O_5 = benzo-15-crown-5; Me_2NH = dimethylamine)

摘要

[(H_3O)(C_(14)H_(20)O_5)_2][Me_2NH_2]_2 [PMo_(12)O_(40)]·2C_(14)H_(20)O_5 1 was synthesized from benzo-15-crown-5 and H_3PMo_(12)O_(40)·24H_2O in N,N'-dimethylformamide for the first time. 1 crystallizes in the monoclinic space group C2/c with a = 18.583(4), b = 25.510(5), c = 19.904(4) A, β = 94.66(3)°, D_c = 2.124 mg/m~3 for Z = 4. Refinement based on 7358 observed reflections led to a R1(wR2) = 0.0378(0.0761). The complex cation, [(H_3O)(C_(14)H_(20)O_5)_2]~+, exhibits a sandwich structure by hydrogen-bonding in the mean distance of 2.955 A. The anion, PMo_(12)O_(40)~(3-), is a α-Keggin structure.