Abstract. (rIs-CsHs)2Mo204, Cl0H1004Mo2, M r = 386.1, orthorhombic, a = 18.500 (3), b = 8.993 (2), c = 6.731 (1) A, U = 1119.8 A 3. Systematic extinctions: Okl, k + l = 2n + I; hk0, h = 2n + 1. Space group Pnma or Pn2~a; Pnma from structure analysis. D c = 2.29 g cm -3 for Z = 4, Mo Krt radiation, 2 = 0.71069 A, /t = 22 cm-k The structure contains discrete molecules of crystallographic point group symmetry C s, the mirror plane passing through the two cis terminal oxo ligands, the two Mo atoms and the centroid of each r/5-cyclopentadienyl ring. The two bridging O atoms complete the distorted octahedral coordination of each Mo atom.Introduetlon. Small brown hexagonal plates of (r/5-CsHs)zMo204 were kindly supplied by Dr M. L. H. Green and Mr M. Bunker. They were sensitive to air and moisture and were sealed under dry nitrogen in glass capillary tubes. It was not possible to measure their density. After survey precession photography, the selected crystal was set up on a Nonius CAD-4F PDPS-controlled x geometry diffractometer; cell dimensions and the orientation matrix were obtained by a least-squares fit to the setting angles of 25 reflexions.The intensities of reflexions with sin 0/2 < 0.70 A-1 were measured by an o3/20 scan, a variable scan rate and an o3-scan angle of (1.00 + 0.35 tan 0) °. Mo Kct radiation was used with a graphite monochromator. Reflexions with I < 3a(I), where a(I) is the standard deviation based on simple counting statistics, were not included in subsequent calculations. Corrections were made for Lorentz and polarization effects, but not for absorption. A set of 1512 independent structure amplitudes was obtained.The structure was solved by Patterson and Fourier techniques, with full-matrix least-squares refinement. All non-H atoms had anisotropic temperature factors. Difference syntheses permitted the location of the H atoms in their expected positions. They were positioned geometrically (C-H = 1.0 A; Uis o = 0.05 A 2) and included in the structure factor calculations, their location being readjusted after each cycle. In the final stages an overall isotropic extinction parameter (109.5) was introduced (Larson, 1967). Each reflexion was assigned a weight w -l = 1 + (0. l lFol -1.5) 2, chosen to minimize the variation of w(IFol --IFcl) 2 with F o.