The crystal structure of anhydrous alpha,alpha-trehalose at -150 degrees.

The crystal structure of alpha,alpha-trehalose (alpha-D-glucopyranosyl alpha-D-glucopyranoside), C12H22O11, is monoclinic, P2(1), Z = 2, with unit cell dimensions at -150 degrees [20 degrees] of a = 12.971(5) [13.003(5)], b = 8.229(4) [8.252(4)], c = 6.789(3) [6.799(3)] A, beta = 98.12(4) [98.33(4)]. The crystal structure was solved by using MULTAN, and refined to R = 0.059, Rw = 0.048 for 1564 intensities, measured with MoK alpha radiation. The molecular structure is very similar to that observed in the dihydrate crystals. It has approximate C2 symmetry. Both glucopyranosyl groups are in the 4C1 conformation. The linkage torsion angles, O-5-C-1-O-1-C-1, are +60.8 degrees and +60.1 degrees. The primary alcohol groups are oriented gauche/gauche and gauche/trans, as in the dihydrate structure. A comparison of the cross-polarization, magic-angle-spinning (c.p.-m.a.s.), 13C-n.m.r. spectra for powders of the crystalline anhydrous and dihydrate forms shows differences in resonances assigned to C-1 and C-4 that would not be anticipated from the results of the crystal-structure analyses.