69680-95-1Relevant academic research and scientific papers
Irida-, rhoda-, nickela-, and cuprapentaboranes derived from the arachno-[B4H9]- ion. Crystal structure of [Ir(η4-B4H9)(CO){P(CH3) 2C6H5}2], an analogue of arachno-B5H11 and [Ir(η4-C4H ...
Boocock, Simon K.,Toft, Mark A.,Inkrott, Kenneth E.,Hsu, Leh-Yeh,Huffman, John C.,Folting, Kirsten,Shore, Sheldon G.
, p. 3084 - 3091 (2008/10/08)
Full title: Irida-, rhoda-, nickela-, and cuprapentaboranes derived from the arachno-[B4H9]- ion. Crystal structure of [Ir(η4-B4H9)(CO){P(CH3) 2C6H5}2], an analogue of arachno-B5H11 and [Ir(η4-C4H6)(CO){P(CH3) 2C6H5}2]+. The reaction of K[B4H9] with trans-[IrCl(CO){P(CH3)2C6H5} 2], [RhCl{P(C6H5)3}3], [NiBr2{(C6H5)2P(CH2) 2P(C6H5)2}] (in the presence of an additional 1 equiv of KH), and [CuBr{P(C6H5)3}2·1/2C 6H6] yields respectively [Ir(η4-B4H9)-(CO){P(CH3) 2C6H5}2] (I), [Rh(η4-B4H8)H{P(C6H 5)3}2] (II), [Ni(η3-B4H8){(C6H 5)2P(CH2)2P(C6H 5)2}] (III), and [Cu-(η3-B4H9){P(C6H 5)3}2] (IV). Boron-11 and 1H{11B} NMR spectroscopies were used to characterize these metallapentaboranes. Complex I crystallized from pentane at -20°C as colorless needles; the crystal structure of [Ir(η4-B4H9)(CO){P(CH3) 2C6H5}2] was determined. Crystal parameters: space group P21/c, a = 9.324 (2) A?, b = 23.162 (10) A?, c = 12.286 (3) A?, β = 55.95 (1)°, V = 2198.5 A?3, Z = 4, mol wt = 548.84, ρc = 1.658 g cm-3, μc = 61.989 cm-1 for Mo Kα. The structure analysis is based upon 3159 independent reflections with F > 2.33σ(F) collected on a Picker four-circle diffractometer, the range being 5° ≤ 2θ ≤ 50° at -162 ± 4°C. Final R(F) = 0.054 and Rw(F) = 0.050. In the crystalline state complex I has Ci symmetry. The molecule consists of an open five-atom cluster in which the [Ir(CO){P(CH3)2C6H5}2] fragment occupies an apical vertex site and is bound to the four boron atoms of the [η4-B4H9] ligand. Complex I is an analogue of arachno-B5H11 and the [Ir(η4-C4H6)(CO){P(CH3) 2C6H5}2]+ cation.
