A comparative study of the crystal structures of 2-(4-(2-(4-(3-chlorophenyl)pipera -zinyl)ethyl) benzyl)isoindoline-1,3-dione by synchrotron radiation X-ray powder diffraction and single-crystal X-ray diffraction

Abstract

The crystal structures of the title compound, C27H26ClN3O2, were established by single-crystal X-ray diffraction and synchrotron radiation X-ray powder diffraction. The simulated annealing approach and rigid-body Rietveld refinement were applied to the structure solution from powder data. Direct methods and full-matrix least-squares techniques were used to solve and refine the crystal structure from single-crystal data. The title compound crystallized in space group P 1¯$\bar{1}$ with lattice parameters a=17.396(7) Å, b= 10.010(4) Å, c=6.833(3) Å, α=77.345(12) °, β= 93.534(6) °, γ=97.210(9) °, unit-cell volume V= 1151.0(2) Å3, Z=2 from powder data, and in space group P 1¯$\bar{1}$with lattice parameters α=82.485(2) °, β= 86.5110(10) °, γ=77.518(2) °, a=6.8159(6) Å, b= 10.0003(9) Å, c=17.4140(15) Å, unit-cell volume V =1148.3(2) Å3, Z=2 from single-crystal data. No detectable impurities were observed.

Keywords

• crystal structure
• synchrotron radiation x-ray powder diffraction
• rietveld refinement
• single-crystal x-ray diffraction