TY - JOUR
T1 - Use of the 2,4,6-Tris(trifluoromethyl)phenyl Ligand in Organogallium Chemistry
AU - Schluter, Rodney D.
AU - Isom, Harold S.
AU - Cowley, Alan H.
AU - Atwood, David A.
AU - Jones, Richard A.
AU - Olbrich, Falk
AU - Corbelin, Siegfried
AU - Lagow, Richard J.
PY - 1994/10/1
Y1 - 1994/10/1
N2 - The compounds [RFGa(μ-Cl)Cl]2 (1), [(RF)2Ga(μ-Cl)]2 (3), and (RF)3Ga (4) (RF = 2,4,6- (CF3)3C6H2) have been prepared by treatment of the aryllithium reagent [RFLi·Et2O]2 with gallium trichloride. The hydroxy derivative [RFGa(μ-OH)Cl]2 (2) was obtained as a hydrolysis product of 1. All compounds have been characterzed by elemental analysis and multinuclear NMR and mass spectroscopy. X-ray crystallographic studies reveal that compound 1 adopts a chloride-bridged dimeric structure in which the gallium atoms are tetrahedrally coordinated and that 4 is monomeric and features a trigonal-planar geometry at gallium. X-ray analysis reveals a hydroxy-bridged dimeric structure for 2. Single-crystal data are as follows: [RF- Ga(μ-Cl)Cl]2 (1), orthorhombic, Pbca, with a = 9.569(2) Å, b = 16.787(1) Å,c = 16.608(3) Å, V = 2667.9(7) Å3, Z = 4, and R = 0.0543 (Rw = 0.0602); [RFGa(μ-OH)Cl]2 (2), triclinic, P21/n, with a = 8.063(1) Å,b = 18.335(3) Å, c = 24.234(3) Å, β = 90.21(1)°, V = 3582.6(8) Å3, Z = 4, and R = 0.0521 (Rw = 0.114); (RF)3Ga (4), triclinic, P1, with a = 8.808(2) Å,b = 12.764(2) Å,c = 14.184(2) Å, α = 97.69(1)°, β = 95.19(1)°, γ = 106.46(1)°, V = 1501.5(4) Å3, Z = 2, and R = 0.0434 (Rw = 0.0507). In general, it was found that the air stability and volatility of the new compounds increased with the degree of RF substitution. Compounds 2 and 4 are stable to moist air.
AB - The compounds [RFGa(μ-Cl)Cl]2 (1), [(RF)2Ga(μ-Cl)]2 (3), and (RF)3Ga (4) (RF = 2,4,6- (CF3)3C6H2) have been prepared by treatment of the aryllithium reagent [RFLi·Et2O]2 with gallium trichloride. The hydroxy derivative [RFGa(μ-OH)Cl]2 (2) was obtained as a hydrolysis product of 1. All compounds have been characterzed by elemental analysis and multinuclear NMR and mass spectroscopy. X-ray crystallographic studies reveal that compound 1 adopts a chloride-bridged dimeric structure in which the gallium atoms are tetrahedrally coordinated and that 4 is monomeric and features a trigonal-planar geometry at gallium. X-ray analysis reveals a hydroxy-bridged dimeric structure for 2. Single-crystal data are as follows: [RF- Ga(μ-Cl)Cl]2 (1), orthorhombic, Pbca, with a = 9.569(2) Å, b = 16.787(1) Å,c = 16.608(3) Å, V = 2667.9(7) Å3, Z = 4, and R = 0.0543 (Rw = 0.0602); [RFGa(μ-OH)Cl]2 (2), triclinic, P21/n, with a = 8.063(1) Å,b = 18.335(3) Å, c = 24.234(3) Å, β = 90.21(1)°, V = 3582.6(8) Å3, Z = 4, and R = 0.0521 (Rw = 0.114); (RF)3Ga (4), triclinic, P1, with a = 8.808(2) Å,b = 12.764(2) Å,c = 14.184(2) Å, α = 97.69(1)°, β = 95.19(1)°, γ = 106.46(1)°, V = 1501.5(4) Å3, Z = 2, and R = 0.0434 (Rw = 0.0507). In general, it was found that the air stability and volatility of the new compounds increased with the degree of RF substitution. Compounds 2 and 4 are stable to moist air.
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U2 - 10.1021/om00022a048
DO - 10.1021/om00022a048
M3 - Article
AN - SCOPUS:0001381301
SN - 0276-7333
VL - 13
SP - 4058
EP - 4063
JO - Organometallics
JF - Organometallics
IS - 10
ER -