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

doi:10.1039/DT9770001755

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

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

22 Citations (Scopus)

Abstract

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-K_αX-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 Mo^I metal atom in an approximate octahedral geometry. The tetrafluoroboratecounter ion is essentially tetrehedral.

Original language	English
Pages (from-to)	1755-1761
Number of pages	7
Journal	Journal of the Chemical Society, Dalton Transactions
Issue number	18
DOIs	https://doi.org/10.1039/DT9770001755
Publication status	Published - 1977

ASJC Scopus subject areas

General Chemistry

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Green, M., Kirsch, H. P., Stone, F. G. A., & Welch, A. J. (1977). 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. Journal of the Chemical Society, Dalton Transactions, (18), 1755-1761. https://doi.org/10.1039/DT9770001755

Green, Michael ; Kirsch, Howard P. ; Stone, F. Gordon A. et al. / 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. In: Journal of the Chemical Society, Dalton Transactions. 1977 ; No. 18. pp. 1755-1761.

@article{04592d77089d4716bd76472179d26f44,

title = "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",

abstract = "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){\AA}, 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){\AA}. The cation features a formally MoI metal atom in an approximate octahedral geometry. The tetrafluoroboratecounter ion is essentially tetrehedral. ",

author = "Michael Green and Kirsch, \{Howard P.\} and Stone, \{F. Gordon A.\} and Welch, \{Alan J.\}",

year = "1977",

doi = "10.1039/DT9770001755",

language = "English",

pages = "1755--1761",

journal = "Journal of the Chemical Society, Dalton Transactions",

issn = "1472-7773",

number = "18",

}

Green, M, Kirsch, HP, Stone, FGA & Welch, AJ 1977, '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', Journal of the Chemical Society, Dalton Transactions, no. 18, pp. 1755-1761. https://doi.org/10.1039/DT9770001755

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. / Green, Michael; Kirsch, Howard P.; Stone, F. Gordon A. et al.
In: Journal of the Chemical Society, Dalton Transactions, No. 18, 1977, p. 1755-1761.

Research output: Contribution to journal › Article › peer-review

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 - https://www.scopus.com/pages/publications/51149202307

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 -

Green M, Kirsch HP, Stone FGA, Welch AJ. 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. Journal of the Chemical Society, Dalton Transactions. 1977;(18):1755-1761. doi: 10.1039/DT9770001755