2321 rather large (see Fig. 3). For this reason an attempt was made to refine the structure in the noncentrosymmetric space group P6 a. Isotropic least-squares refinement converged with positional and isotropic thermal parameters equivalent within error to those obtained in the similar refinement in the centrosymmetric space group, except for atoms H(1A), H(1B), and H(2) on the ethyl sulfate group. However, attempts to continue refinement with anisotropic thermal parameters were unsuccessful, in that the temperature factors for the S atom and atom H(1A) became non-positive definite. It is our feeling that the true space group is P63/m, and that the large ellipsoids for the ethyl sulfate hydrogens are due to extreme thermal motion. It is possible that the H atoms are disordered, in which case a lowering of the local symmetry of the Y site is not completely ruled out. However, since the Y(OH2)39 + moiety still conformed, within error, to C3h site symmetry when refinement was attempted in the P63 space group, it is likely that the possible perturbation of the crystal-field levels of Yb 3+ (which partially substitutes Y in the crystals used in a spin refrigerator) would be extremely small. ) distance is 1.363 (8) A and the Rh-Rh length is 2.651 (1) A. The CO group is symmetrically bridging, and an approximate mirror plane passes through this group and the four C and two F atoms of the alkyne. The CO group is 0-43 A closer to one alkyne C than the other. The two (CsHs)Rh units are in an eclipsed orientation.
References
ABRAGAM, A. (1963