137541-64-1Relevant articles and documents
Reduction of biscarborane: Molecular structures of [(15-crown-5)3Na2](C2B10H 11)2 and [P(C6H5)3CH3] 2[μ-9,10-CH-(μ-9′,10′-CH-nido-7′-CB 10H11)-nido-7-CB10H11]
Getman, Thomas D.,Knobler, Carolyn B.,Hawthorne, M. Frederick
, p. 101 - 105 (2008/10/08)
The synthesis, characterization, and elucidation of the structures of [(15-crown-5)3Na2](C2B10H 11)2 ([(15-crown-5)3Na2](1)) and [P(C6H5)3CH3] 2[μ-9,10,-CH-(μ-9′,10′-CH-nido-7′-CB 10H11)-nido-7-CB10H11] ([P(C6H5)3CH3]2(2)) are described. A comparison is made between the solid-state structures of the anion, 1, in [(15-crown-5)3Na2](1) and [P(C6H5)3CH3]2(1). The structure of the cation [(15-crown-5)3Na2]2+, described in detail, represents the first structural characterization of a 3:2 15-crown-5:Na club sandwich complex. [(15-crown-5)3Na2](C2B10H 11)2 crystallized in th triclinic space group P1 with a = 12.411 (1), b = 14.676 (2), and c = 14.988 (2) A?, α = 101.371 (3), β = 96.222 (3), and γ = 91.549 (4)°, V = 2657 A?3, and Z = 2. Data were collected at 128 K on a modified Picker FACS-1 diffractometer using Mo Kα radiation, to a maximum 2θ = 56°, giving 12832 unique reflections. The structure was solved by direct methods. The final discrepancy indices were R = 0.057 and Rw = 0.062 for 5012 independent reflections with I > 3σ(I). The protonation of the species formed by the reduction of biscarborane by 4 equiv or an excess of sodium naphthalide resulted in the formation of Na2(2). [P(C6H5)3CH3]2(2) crystallized in the monoclinic space group P21/n with a = 11.429 (3), b = 15.075 (4), and c = 16.520 (4) A?, β = 119.648 (8)°, V = 2474 A?3, and Z = 2. Data were collected on a Huber diffractomer (constructed at UCLA) using Mo Kα radiation, to a maximum 2θ = 50°, giving 4368 unique reflections. The structure was solved by direct methods (MULTAN80). The final discrepancy indices were R = 0.070 and Rw = 0.101 for 3264 independent reflections with I > 3σ(I).
