Synthesis and crystal structure of (2.2.2-cryptand)potassium N-benzoyldiisopropylphosphoramidate monohydrate

Abstract

A new complex, (2.2.2-cryptand)potassium N-benzoyldiisopropylphosphoramidate monohydrate [K(Crypt-222)]+ · (iso-PrO)2P(O)N−C(O)Ph · H2O (I), was synthesized. Its crystal structure was studied by X-ray diffraction analysis: space group P\( \bar 1 \), a = 11.804 A, b = 12.043 A, c = 15.607 A, α = 87.29°, β = 84.59°, γ = 61.32°, Z = 2. The triclinic structure of I was solved by direct methods and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.052 for all 5410 independent reflections (CAD-4 automated diffractometer, λMoKα). In structure I, the host-guest [K(Crypt-222)]+ complex cation has approximate D3 symmetry. Its K+ cation is coordinated by all the eight (6O + 6N) heteroatoms of the cryptand ligand. The coordination polyhedron of K+ (CN = 8) is a dicapped trigonal prism slightly distorted toward an antiprism. In the phosphoramidate anion (with the deprotonated nitrogen atom), eight non-hydrogen atoms of two terminal iso-PrO substituents are disordered each over two positions: main and low-occupancy positions. The water molecule in complex I is disordered, and its H atoms form hydrogen bonds.