TY - JOUR
T1 - 2-Hetero-1λ5,3λ5-diphosphabenzenes as Ligands in Molybdenum Complexes
AU - Gamper, Siegfried F.
AU - Schmidbaur, Hubert
PY - 1992/8/1
Y1 - 1992/8/1
N2 - Treatment of (2,5-norbornadiene)molybdenum tetracarbonyl with 5-methyl-1,1,3,3-tetraphenyl-1λ5- phospha-3-phosphonia-2-boratabenzene (1) results in the formation of a complex 1·Mo(CO)4 (4). Likewise, the reaction of (cycloheptatriene)molybdenum tricarbonyl with 5-methyl-1,1,3,3-tetraphenyl-1λ5,3λ5-diphosphabenzene (2) gives a complex 2·Mo(CO)3 (5). Complexes 4 and 5, obtained in high yields, have been characterized on the basis of their IR and 1H, 13C{1H}, and 31P{1H} NMR spectra, as well as by mass spectrometry and elemental analysis. Ocher-yellow crystals of composition 4-THF were grown from tetrahydrofuran/hexane and studied by X-ray crystallography: space group C2/m, a = 23.343 (4) Å, b = 14.016 (1) Å, c = 13.352 (2) Å, β =122.90 (1)°, V = 3667.83 Å3, Z = 8/2. Bright yellow crystals of composition 5·0.5THF were obtained by crystallization from THF: space group Pbca, a = 16.687 (2) Å, b = 17.375 (2) Å, c = 22.929 (3) Å, V = 6647.96 Å3, Z= 8. Compounds 4 and 5 feature zero-valent molybdenum centers in a pseudooctahedral coordination sphere with the heterocycles 1 and 2 bound as four-electron donors via their methallylic functions and the semiylidic function PCHP as an additional two-electron donor in 5.
AB - Treatment of (2,5-norbornadiene)molybdenum tetracarbonyl with 5-methyl-1,1,3,3-tetraphenyl-1λ5- phospha-3-phosphonia-2-boratabenzene (1) results in the formation of a complex 1·Mo(CO)4 (4). Likewise, the reaction of (cycloheptatriene)molybdenum tricarbonyl with 5-methyl-1,1,3,3-tetraphenyl-1λ5,3λ5-diphosphabenzene (2) gives a complex 2·Mo(CO)3 (5). Complexes 4 and 5, obtained in high yields, have been characterized on the basis of their IR and 1H, 13C{1H}, and 31P{1H} NMR spectra, as well as by mass spectrometry and elemental analysis. Ocher-yellow crystals of composition 4-THF were grown from tetrahydrofuran/hexane and studied by X-ray crystallography: space group C2/m, a = 23.343 (4) Å, b = 14.016 (1) Å, c = 13.352 (2) Å, β =122.90 (1)°, V = 3667.83 Å3, Z = 8/2. Bright yellow crystals of composition 5·0.5THF were obtained by crystallization from THF: space group Pbca, a = 16.687 (2) Å, b = 17.375 (2) Å, c = 22.929 (3) Å, V = 6647.96 Å3, Z= 8. Compounds 4 and 5 feature zero-valent molybdenum centers in a pseudooctahedral coordination sphere with the heterocycles 1 and 2 bound as four-electron donors via their methallylic functions and the semiylidic function PCHP as an additional two-electron donor in 5.
UR - http://www.scopus.com/inward/record.url?scp=0043075745&partnerID=8YFLogxK
U2 - 10.1021/om00044a028
DO - 10.1021/om00044a028
M3 - Article
AN - SCOPUS:0043075745
SN - 0276-7333
VL - 11
SP - 2863
EP - 2867
JO - Organometallics
JF - Organometallics
IS - 8
ER -