The highly sterically hindered compound B,B'-bis( 1,3-dicyclohexyl-1,3,2-diazaborolidin-2-yl) (1 ) was prepared by transamination of B,( NMe,),. It is unreactive towards air or moisture. Crystals of (1) are monoclinic, a = 16.829(3), b = 12.021 (2), c = 14.744(3) A, p = 95.06(2)", Z = 4, and space group C2/c. The structure was solved by direct methods and refined by full-matrix leastsquares calculations to R = 0.097 for 1 247 reflections with I > 3 a ( I ) . The molecule has crystallographic two-fold symmetry and the two halves of the molecule are linked through boron atoms, with B-6 1.721 (1 2) A. Other ring distances are: mean 6-N 1.393(7), mean C-N 1.454(6), and mean C-C 1.494(9) A. The five-membered ring BN, C, planes form a dihedral angle of 80.7".Both cyclohexyl rings are in chair conformations. A comparison of the photoelectron spectrum of compound (1 ) with that of B,( NMe,), suggests that both compounds are in a staggered conformation in the gas phase; a reassignment of the B,( NMe,), spectrum is proposed.Compounds of the type X2B-BX, (X = halide, OR, or NR,) are well known.' The halides (X = F or C1) are structurally interesting because they appear to adopt planar (D2J configurations in the solid state and either planar (X = F) or non-planar ( D 2 d ) configurations (X = C1) in the liquid or gas phase. Dialkylamino derivatives, B,(NMe,),,' and B,Bbis( 1,3-dimethyl-1,3,2-diazaborolidin-2-yl) (I; R = Me)3 are