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• W2023843363 abstract "Addition of Li[N(SiMe3)2] to the halogenobis(alkyne) complexes [MoBr(η2-MeC2R)2(η-C5H5)](R = Me or Ph) resulted in a dehydrohalogenation reaction and formation of the σ,η2(3e)-prop-2-ynyl/η2(4e)-alkyne-substituted complexes [Mo{σ,η2(3e)-CH2C2R}{η2(4e)-MeC2R}(η-C5H5)](R = Ph 7 or Me). The structure when R = Ph has been confirmed by a single-crystal X-ray diffraction study. The η2(4e)-bonded alkyne and σ,η2(3e)-prop-2-ynyl ligands lie in planes essentially parallel to that of the η-C5H5 ligand, with a C(1)–C(2)–C(3) angle and Mo–C(1), Mo–C(2) and Mo–C(3) bond lengths for the prop-2-ynyl fragment of 146.1(6)°, 2.278(6), 2.164(5) and 2.105(5)A respectively. The nature of the M–σ,η2-C3H3 bonding in complex 7 and in the related species [Mo{σ,η2(3e)CH2C2H}(CO)2(η6-C6Me6)][BF4] and [ZrMe{σ,η2(3e)-CH2C2Ph}(η-C5H5)2] has been examined using a comparative standard extended-Huckel molecular orbital (EHMO) study. Reprotonation of the new complexes with CF3CO2H affords [Mo(O2CCF3)(η2-MeC2R)2(η-C5H5)](R = Ph or Me), and it is suggested in agreement with an EHMO charge-distribution calculation that protonation occurs initially on an alkyne contact carbon followed by transfer of the hydrogen via the metal to the prop-2-ynyl ligand. An attempt to extend the deprotonation reaction to the X-ray crystallographically identified η2-alkene/η2(4e)-alkyne-substituted complex [Mo{η2(4e) MeC2Ph}(dpps)(η-C5H5)][BF4](dpps =o-diphenylphosphinostyrene) resulted in an unexpected reaction. Treatment with Li[N(SiMe3)2]afforded the η5-pentadienyl complex [Mo{η2,η3(5e)-CH2CHC(Ph)CHCHC6H4PPh2-o}(η-C5H5)], which was structurally characterised by single-crystal X-ray crystallography. The pentadienyl ligand is wrapped around the molybdenum atom resulting in a dihedral angle of 122° for C(27)–C(26)–C(25)–C(24). The bond length C(25)–C(26) of 1.484(11)A indicates there is little interaction between the η3 and η2π systems. Reaction of this complex with HBF4·Et2O resulted in the formation of a cationic trans(twisted)η4-1,3-diene substituted complex stabilised by an Mo(µ-H) C interaction. A single-crystal X-ray diffraction study confirmed these features. The trans-1,3-diene carbons adopt a twisted, non-planar arrangement with a dihedral angle of 123°. The agostic interaction is not displaced by carbon monoxide." @default.
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• W2023843363 title "Deprotonation of η²(4e)-bonded alkynes as a pathway to σ,η²(3e)-prop-2-ynyl, η⁵-pentadienyl and η⁴-trans-1,3-diene substituted molybdenum complexes" @default.
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