Synthesis, characterisation and reactivity of the first heptamethylindenyl-molybdenum complexes: Crystal structures of [Mo(CO)(η2≡CMe) 2(η5-C9Me7)]BF4 and [Mo(CO) 2(η3-C3H5)(η5-C9Me7)]

Michael Green; Thomas D. McGrath; Rhodri Ll Thomas; Alan P. Walker

doi:10.1016/S0022-328X(96)06751-4

Synthesis, characterisation and reactivity of the first heptamethylindenyl-molybdenum complexes: Crystal structures of [Mo(CO)(η²≡CMe) ₂(η⁵-C₉Me₇)]BF₄ and [Mo(CO) ₂(η³-C₃H₅)(η⁵-C₉Me₇)]

Michael Green, Thomas D. McGrath, Rhodri Ll Thomas, Alan P. Walker

School of Engineering & Physical Sciences

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

14 Citations (Scopus)

Abstract

The synthesis and characterisation of the first (?⁵-heptamethylindenyl)molybdenum complexes are reported. Reaction of Li[C₉Me₇] with Mo(CO)₆ in refluxing THF readily forms Li[Mo(CO)₃(?⁵-C₉Me₇)], which is shown to be a useful precursor in the formation of (carbonyl)(?⁵-heptamethylindenyl)molybdenum complexes. The compounds [MoI(CO)₃(?⁵-C₉Me₇)] 3, [Mo(Me)(CO)₃(?⁵-C₉Me₇)] 4 and [Mo(CO)₂(?³-C₃H₅)(?⁵-C₉Me₇)] 5 have been prepared from this intermediate and characterised. Treatment of 3 with AgBF₄ and MeC=CMe affords [Mo(CO)(MeC=CMe)₂(?⁵-C₉Me₇)]BF₄ 6a; for this and the indenyl analogue, a new route to carbonyl-bis(alkyne)-molybdenum derivatives is demonstrated. Reaction of 3 with T1PF₆ in MeCN forms the complex [Mo(MeCN)₂(CO)₂(?⁵-C₉Me₇)]PF₆ 7. Protonation of 5 in the presence of MeC=CMe, or reaction of 7 with the same acetylene, also yields 6 with appropriate counter anions. Single crystal X-ray diffraction studies of compounds 5 and 6a are reported.

Original language	English
Pages (from-to)	61-70
Number of pages	10
Journal	Journal of Organometallic Chemistry
Volume	532
Issue number	1-2
DOIs	https://doi.org/10.1016/S0022-328X(96)06751-4
Publication status	Published - 1 Apr 1997

Keywords

Alkyne
Carbonyl
Crystal structure
Heptamethylindenyl
Indenyl
Molybdenum
Permethylindenyl

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10.1016/S0022-328X(96)06751-4

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@article{99ecb5f4eb3b4a5582b19017f9e888bc,

title = "Synthesis, characterisation and reactivity of the first heptamethylindenyl-molybdenum complexes: Crystal structures of [Mo(CO)(η2≡CMe) 2(η5-C9Me7)]BF4 and [Mo(CO) 2(η3-C3H5)(η5-C9Me7)]",

abstract = "The synthesis and characterisation of the first (?5-heptamethylindenyl)molybdenum complexes are reported. Reaction of Li[C9Me7] with Mo(CO)6 in refluxing THF readily forms Li[Mo(CO)3(?5-C9Me7)], which is shown to be a useful precursor in the formation of (carbonyl)(?5-heptamethylindenyl)molybdenum complexes. The compounds [MoI(CO)3(?5-C9Me7)] 3, [Mo(Me)(CO)3(?5-C9Me7)] 4 and [Mo(CO)2(?3-C3H5)(?5-C9Me7)] 5 have been prepared from this intermediate and characterised. Treatment of 3 with AgBF4 and MeC=CMe affords [Mo(CO)(MeC=CMe)2(?5-C9Me7)]BF4 6a; for this and the indenyl analogue, a new route to carbonyl-bis(alkyne)-molybdenum derivatives is demonstrated. Reaction of 3 with T1PF6 in MeCN forms the complex [Mo(MeCN)2(CO)2(?5-C9Me7)]PF6 7. Protonation of 5 in the presence of MeC=CMe, or reaction of 7 with the same acetylene, also yields 6 with appropriate counter anions. Single crystal X-ray diffraction studies of compounds 5 and 6a are reported.",

keywords = "Alkyne, Carbonyl, Crystal structure, Heptamethylindenyl, Indenyl, Molybdenum, Permethylindenyl",

author = "Michael Green and McGrath, {Thomas D.} and Thomas, {Rhodri Ll} and Walker, {Alan P.}",

year = "1997",

month = apr,

day = "1",

doi = "10.1016/S0022-328X(96)06751-4",

language = "English",

volume = "532",

pages = "61--70",

journal = "Journal of Organometallic Chemistry",

issn = "0022-328X",

publisher = "Elsevier",

number = "1-2",

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Synthesis, characterisation and reactivity of the first heptamethylindenyl-molybdenum complexes : Crystal structures of [Mo(CO)(η²≡CMe) ₂(η⁵-C₉Me₇)]BF₄ and [Mo(CO) ₂(η³-C₃H₅)(η⁵-C₉Me₇)]. / Green, Michael; McGrath, Thomas D.; Thomas, Rhodri Ll et al.

In: Journal of Organometallic Chemistry, Vol. 532, No. 1-2, 01.04.1997, p. 61-70.

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

TY - JOUR

T1 - Synthesis, characterisation and reactivity of the first heptamethylindenyl-molybdenum complexes

T2 - Crystal structures of [Mo(CO)(η2≡CMe) 2(η5-C9Me7)]BF4 and [Mo(CO) 2(η3-C3H5)(η5-C9Me7)]

AU - Green, Michael

AU - McGrath, Thomas D.

AU - Thomas, Rhodri Ll

AU - Walker, Alan P.

PY - 1997/4/1

Y1 - 1997/4/1

N2 - The synthesis and characterisation of the first (?5-heptamethylindenyl)molybdenum complexes are reported. Reaction of Li[C9Me7] with Mo(CO)6 in refluxing THF readily forms Li[Mo(CO)3(?5-C9Me7)], which is shown to be a useful precursor in the formation of (carbonyl)(?5-heptamethylindenyl)molybdenum complexes. The compounds [MoI(CO)3(?5-C9Me7)] 3, [Mo(Me)(CO)3(?5-C9Me7)] 4 and [Mo(CO)2(?3-C3H5)(?5-C9Me7)] 5 have been prepared from this intermediate and characterised. Treatment of 3 with AgBF4 and MeC=CMe affords [Mo(CO)(MeC=CMe)2(?5-C9Me7)]BF4 6a; for this and the indenyl analogue, a new route to carbonyl-bis(alkyne)-molybdenum derivatives is demonstrated. Reaction of 3 with T1PF6 in MeCN forms the complex [Mo(MeCN)2(CO)2(?5-C9Me7)]PF6 7. Protonation of 5 in the presence of MeC=CMe, or reaction of 7 with the same acetylene, also yields 6 with appropriate counter anions. Single crystal X-ray diffraction studies of compounds 5 and 6a are reported.

AB - The synthesis and characterisation of the first (?5-heptamethylindenyl)molybdenum complexes are reported. Reaction of Li[C9Me7] with Mo(CO)6 in refluxing THF readily forms Li[Mo(CO)3(?5-C9Me7)], which is shown to be a useful precursor in the formation of (carbonyl)(?5-heptamethylindenyl)molybdenum complexes. The compounds [MoI(CO)3(?5-C9Me7)] 3, [Mo(Me)(CO)3(?5-C9Me7)] 4 and [Mo(CO)2(?3-C3H5)(?5-C9Me7)] 5 have been prepared from this intermediate and characterised. Treatment of 3 with AgBF4 and MeC=CMe affords [Mo(CO)(MeC=CMe)2(?5-C9Me7)]BF4 6a; for this and the indenyl analogue, a new route to carbonyl-bis(alkyne)-molybdenum derivatives is demonstrated. Reaction of 3 with T1PF6 in MeCN forms the complex [Mo(MeCN)2(CO)2(?5-C9Me7)]PF6 7. Protonation of 5 in the presence of MeC=CMe, or reaction of 7 with the same acetylene, also yields 6 with appropriate counter anions. Single crystal X-ray diffraction studies of compounds 5 and 6a are reported.

KW - Alkyne

KW - Carbonyl

KW - Crystal structure

KW - Heptamethylindenyl

KW - Indenyl

KW - Molybdenum

KW - Permethylindenyl

UR - http://www.scopus.com/inward/record.url?scp=0031116081&partnerID=8YFLogxK

U2 - 10.1016/S0022-328X(96)06751-4

DO - 10.1016/S0022-328X(96)06751-4

M3 - Article

SN - 0022-328X

VL - 532

SP - 61

EP - 70

JO - Journal of Organometallic Chemistry

JF - Journal of Organometallic Chemistry

IS - 1-2

ER -

Synthesis, characterisation and reactivity of the first heptamethylindenyl-molybdenum complexes: Crystal structures of [Mo(CO)(η²≡CMe) ₂(η⁵-C₉Me₇)]BF₄ and [Mo(CO) ₂(η³-C₃H₅)(η⁵-C₉Me₇)]

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Keywords

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