TY - JOUR
T1 - The cluster cation [os4(CO)12H4(OH)]+
T2 - Preparation and crystal structure
AU - Johnson, Brian F.G.
AU - Lewis, Jack
AU - Raithby, Paul R.
AU - Zuccaro, Camillo
PY - 1980
Y1 - 1980
N2 - The cluster cation [Os4(CO)12H4(OH)]+ has been prepared in high yields by the reaction of [Os4(CO)12H4] with NOX (X = NO3, PF6, BF4, or Cl) in MeCN or CH2Cl2. The cation is also isolated as the [Os(CO)3(NO3)3]- salt from the reaction with N2O4 in toluene. The salt [Os4(CO)12H4(OH)][Os(CO)3(NO 3)3] crystallises in the triclinic space group P1, with cell dimensions a = 9.701 (5), b = 11.504(6), c = 14.352(6) Å, α = 83.03(2), β = 84.79(2), γ = 85.38(2)°, and Z = 2. The structure has been solved by a combination of direct methods and Fourier-difference techniques and refined by blocked-cascade least squares to R = 0.037 for 5 538 observed reflections. The four osmium atoms in the cation define a 'butterfly' configuration with two triangles sharing a common edge but which are not coplanar. The space above the butterfly is occupied by the OH group. The hydrido-ligands are not located directly but the carbonyl arrangement suggests that they bridge each of the four wing-tip-hinge Os-Os 'bonds'.
AB - The cluster cation [Os4(CO)12H4(OH)]+ has been prepared in high yields by the reaction of [Os4(CO)12H4] with NOX (X = NO3, PF6, BF4, or Cl) in MeCN or CH2Cl2. The cation is also isolated as the [Os(CO)3(NO3)3]- salt from the reaction with N2O4 in toluene. The salt [Os4(CO)12H4(OH)][Os(CO)3(NO 3)3] crystallises in the triclinic space group P1, with cell dimensions a = 9.701 (5), b = 11.504(6), c = 14.352(6) Å, α = 83.03(2), β = 84.79(2), γ = 85.38(2)°, and Z = 2. The structure has been solved by a combination of direct methods and Fourier-difference techniques and refined by blocked-cascade least squares to R = 0.037 for 5 538 observed reflections. The four osmium atoms in the cation define a 'butterfly' configuration with two triangles sharing a common edge but which are not coplanar. The space above the butterfly is occupied by the OH group. The hydrido-ligands are not located directly but the carbonyl arrangement suggests that they bridge each of the four wing-tip-hinge Os-Os 'bonds'.
UR - https://www.scopus.com/pages/publications/37049105722
U2 - 10.1039/DT9800000716
DO - 10.1039/DT9800000716
M3 - Article
AN - SCOPUS:37049105722
SN - 1472-7773
SP - 716
EP - 720
JO - Journal of the Chemical Society, Dalton Transactions
JF - Journal of the Chemical Society, Dalton Transactions
IS - 5
ER -