EMAIL THIS PAGE TO A FRIEND

Acta crystallographica. Section B, Structural science

Crystal structure and thermal vibrations of cholesteryl acetate from neutron diffraction at 123 and 20 K.


PMID 2025409

Abstract

Cholesteryl acetate (C29H48O2) at 20 K is monoclinic, space group P2(1) with a = 16,521 (4), b = 9,220 (2), c = 17,620 (5) A, beta = 107.18 (2) degrees and Z = 4 (two molecules in the asymmetric unit). The crystal structure, earlier determined by X-ray diffraction at 123 K, has been redetermined at 123 and 20 K by neutron diffraction (7447 reflections at 123 K, 7281 at 20 K; sin theta/lambda less than 0.69 A-1) and refined by full-matrix least squares with 1423 variables to give R(F2) = 0.10 at 123 K, 0.06 at 20 K. Results at 20 K are more accurate not only because nuclear thermal vibrations have reduced amplitudes but also because a larger crystal was used for data collection. At 20 K, the average of 44 methylene C-H bond lengths is 1,102 (8) A (sigma from the observed distribution) and 1.103 (6) A for 16 methine groups. The 22 methylene H-C-H angles [106.2 (9) degrees] all fall within a narrow range. Analysis of nuclear anisotropic thermal parameters shows that intramolecular vibrations of the H nuclei are highly significant with similar mean-square amplitudes at 123 and 20 K. Torsional vibrations around the C-CH3 bonds of the C18 and C19 methyl groups have r.m.s. amplitudes of about 7 degrees. For methylene groups, mean-square amplitudes are a minimum for C-H bond stretching (0.006 A2) and a maximum for CH2 in-plane vibrations (0.024 A2). Values of Beq for the H-atom intramolecular vibrations are 0.8, 1.2 and 1.6 A2 for methine, methylene and methyl H atoms respectively. These results can be used to estimate Beq for H atoms in crystal structure determinations carried out by X-ray diffraction. The anisotropic intramolecular vibrations of the H nuclei contribute to the effective shape of the H atoms which, from the observed anisotropy in the distribution of intermolecular H...H distances, appears to be flattened along the direction of the C-H bond.

Related Materials

Product #

Image

Description

Molecular Formula

Add to Cart

151114
Cholesteryl acetate, 97%
C29H48O2