TY - JOUR
T1 - CycloheptatrienylmolybdenumComplexes. Part 2. Synthesis of Cationic AcetylacetoneDerivatives [Mo(acac)L(η7-C7H7)]+(L=H2O,Et3P, Me2PhP, MePh2P, (MeO)3P, Me2PhAsor py); Molecular and Crystal Structure of [Mo(acac)(H2O)(η7-C7H7)]BF4
AU - Green, Michael
AU - Kirsch, Howard P.
AU - Stone, F. Gordon A.
AU - Welch, Alan J.
PY - 1977
Y1 - 1977
N2 - The cations [Mo(CO)3(η7-C7H7)]+ and [Mo(η6-C6H5Me)(η7-C7H7)]+ react with an excess of acetylacetone in dry tetrahydrofuran to form the seventeen-electron aqua-complex [Mo(acac)(H2O)(η7-C7H7)]+, from which the water molecule may be displaced affording the species [Mo(acac)L(η7-C7H7)]+(L = PEt3, PMe2Ph, PMePh2, P(OMe)3, AsMe2Ph, or py). 1,2-Bis(diphenylphosphino)ethane (dppe) reacts with the aqua-complex to give a dimolybdenum dication [Mo2(acac)2(dppe)(η7-C7H7)2]2+. Crystals of the title compound are monoclinic, space group P21/n, with a= 8.664(9), b= 18.997(4), c= 9.625(13)Å, β= 112.39(8)°. The structure has been refined to R 0.059 (R′ 0.071) for 3 226 independent observed reflections to 2θ 65°(Mo-KαX-radiation) collected at ca. 215 K. All hydrogen atoms present have been located and positionally and thermally refined.The crystal structure is built up of two pairs of [Mo(acac)(H2O)(η7-C7H7)]+ cations and [BF4]– anions surrounding a symmetry centre and linked via two independent H ⋯ F contacts of 1.84(9) and 2.07(12)Å. The cation features a formally MoI metal atom in an approximate octahedral geometry. The tetrafluoroboratecounter ion is essentially tetrehedral.
AB - The cations [Mo(CO)3(η7-C7H7)]+ and [Mo(η6-C6H5Me)(η7-C7H7)]+ react with an excess of acetylacetone in dry tetrahydrofuran to form the seventeen-electron aqua-complex [Mo(acac)(H2O)(η7-C7H7)]+, from which the water molecule may be displaced affording the species [Mo(acac)L(η7-C7H7)]+(L = PEt3, PMe2Ph, PMePh2, P(OMe)3, AsMe2Ph, or py). 1,2-Bis(diphenylphosphino)ethane (dppe) reacts with the aqua-complex to give a dimolybdenum dication [Mo2(acac)2(dppe)(η7-C7H7)2]2+. Crystals of the title compound are monoclinic, space group P21/n, with a= 8.664(9), b= 18.997(4), c= 9.625(13)Å, β= 112.39(8)°. The structure has been refined to R 0.059 (R′ 0.071) for 3 226 independent observed reflections to 2θ 65°(Mo-KαX-radiation) collected at ca. 215 K. All hydrogen atoms present have been located and positionally and thermally refined.The crystal structure is built up of two pairs of [Mo(acac)(H2O)(η7-C7H7)]+ cations and [BF4]– anions surrounding a symmetry centre and linked via two independent H ⋯ F contacts of 1.84(9) and 2.07(12)Å. The cation features a formally MoI metal atom in an approximate octahedral geometry. The tetrafluoroboratecounter ion is essentially tetrehedral.
UR - http://www.scopus.com/inward/record.url?scp=51149202307&partnerID=8YFLogxK
U2 - 10.1039/DT9770001755
DO - 10.1039/DT9770001755
M3 - Article
AN - SCOPUS:51149202307
SN - 1472-7773
SP - 1755
EP - 1761
JO - Journal of the Chemical Society, Dalton Transactions
JF - Journal of the Chemical Society, Dalton Transactions
IS - 18
ER -