The structure of μ‐carbonato‐bis(tetraphenylantimony), , has been determined from 2394 independent X‐ray intensities measured on a four‐circle diffractometer. The material is triclinic, space group P1, with a = 10.108, b = 14.018, c = 15.702 Å, α = 73.92, β = 79.84, β = 74.39°, Z = 2. The structure was solved by the heavy‐atom method and refined by least‐squares calculations to R = 0.049. The structure consists of well separated molecules. One antimony atom, Sb(1), is in a slightly distorted trigonal bipyramidal environment with a carbonato oxygen apical. The mean C(axial)‐Sb(1)‐C(equatorial) angle is 95.2° and corresponds to a displacement of Sb(1) 0.19 Å out of the plane of the three equatorial carbon atoms towards the apical phenyl group. The other antimony, Sb(2), has distorted octahedral coordination. The two antimony polyhedra are linked by a planar carbonato group whose C‐O distances do not differ significantly from their mean value 1.292 (13) Å. The Sb‐O distances are Sb(1)‐O(1), 2.257 (7), Sb(2)‐O(2) 2.325 (7), Sb(2)‐O(3) 2.185 (7). At Sb(1), the mean Sb‐C (equatorial) bond length is 2.120 (11) and the Sb‐C(apical) distance is 2.153 (11) Å. The mean value of the Sb(2)‐C bonds is 2.152 (11) Å.
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