Synthesis and Crystal Structure of the Dimethylformamide Solvate of Bis(4,7,13,16,21,24-Hexaoxa-1, 10-Diazoniabicyclo[8.8.8]Hexacosane) Tetrakis(Dihydrogenphosphate) Pentakis(Trihydrogenphosphate)

摘要

A new crystalline adduct, dimethylformamide solvate of bis(4,7,13,16,21,24-hexaoxa-l,10-diazoniabicyclo[8.8.8]hexacosane) tetrakis(dihydrogenphosphate) pentakis(trihydrogenphosphate), 2[H_2(Crypt-222)]~(2+) centre dot 4(H_2PO_4~-) centre dot 5(H_3PO_4) centre dot C_3H_7NO (I), was prepared and studied by X-ray diffraction. The structure of I (space group P2_1/c, alpha = 23.502 A, b = 12.780 A, c s= 27.092 A, (3 = 112.05 deg, Z = 4) was solved by the direct method and refined by full-matrix least-squares calculations in the anisotropic approximation to R = 0.072 for all 11176 independent reflections (CAD4 automated diffractometer, lambda CuK_(alpha) radiation). In structure I, all ions and molecules, except for the DMF molecule, are markedly disordered. Two independent 2.2.2-cryptand dications have different conformations. In the crystal of I, all the H_2PO_4~- anions and the H_3PO_ 4 and DMF molecules are combined by strong O-H…O hydrogen bonds to form infinite thick layers.