Abstract One of the diastereomeres of 2,3,4,6,7,8-hexamethyl-2,3,4,6,7,8-hexaphosphabicyclo-[3,3,0]octane (PMe)6C2H2 crystallizes in the space group P21/n with four molecules per unit cell. Two independent molecules are nearly identical in shape but differ by inter-molecular packing. The five-membered rings have a skew chair conformation with all exocyclic methyl groups in axial positions leading to a staggered all-trans conformation of the bicyclic system. The mean bond lengths are P-P = 220.9 pm, P-C = 185.9 pm and C-C = 151.9 pm.
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