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

Michael Green, Howard P. Kirsch, F. Gordon A. Stone, Alan J. Welch

Research output: Contribution to journalArticle

Abstract

The cations [Mo(CO)37-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.

Original languageEnglish
Pages (from-to)1755-1761
Number of pages7
JournalJournal of the Chemical Society, Dalton Transactions
Issue number18
DOIs
Publication statusPublished - 1977

ASJC Scopus subject areas

  • Chemistry(all)

Fingerprint Dive into the research topics of 'CycloheptatrienylmolybdenumComplexes.  Part 2.  Synthesis of Cationic AcetylacetoneDerivatives [Mo(acac)L(η<sup>7</sup>-C<sub>7</sub>H<sub>7</sub>)]<sup>+</sup>(L=H<sub>2</sub>O,Et<sub>3</sub>P, Me<sub>2</sub>PhP, MePh<sub>2</sub>P, (MeO)<sub>3</sub>P, Me<sub>2</sub>PhAsor py); Molecular and Crystal Structure of [Mo(acac)(H<sub>2</sub>O)(η<sup>7</sup>-C<sub>7</sub>H<sub>7</sub>)]BF<sub>4</sub>'. Together they form a unique fingerprint.

  • Cite this