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  • 1
    Language: English
    In: Journal of the American Chemical Society, 23 March 2011, Vol.133(11), pp.3824-7
    Description: The four-coordinate iron(II) phosphoraniminato complex PhB(MesIm)(3)Fe-N═PPh(3) undergoes an S = 0 to S = 2 spin transition with T(C) = 81 K, as determined by variable-temperature magnetic measurements and Mössbauer spectroscopy. Variable-temperature single-crystal X-ray diffraction revealed that the S = 0 to S = 2 transition is associated with an increase in the Fe-C and Fe-N bond distances and a decrease in the N-P bond distance. These structural changes have been interpreted in terms of electronic structure theory.
    Keywords: Chemistry;
    ISSN: 00027863
    E-ISSN: 1520-5126
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  • 2
    Language: English
    In: Science (New York, N.Y.), 25 February 2011, Vol.331(6020), pp.1049-52
    Description: Despite being implicated as important intermediates, iron(V) compounds have proven very challenging to isolate and characterize. Here, we report the preparation of the iron(V) nitrido complex, [PhB((t)BuIm)(3)Fe(V)≡N]BAr(F24) (PhB((t)BuIm)(3)(-) = phenyltris(3-tert-butylimidazol-2-ylidene)borato, BAr(F24) = B(3,5-(CF(3))(2)C(6)H(3))(4)(-)), by one electron oxidation of the iron(IV) nitrido precursor. Single-crystal x-ray diffraction of the iron(V) complex reveals a four-coordinate metal ion with a terminal nitrido ligand. Mößbauer and electron paramagnetic resonance spectroscopic characterization, supported by electronic structure calculations, provide evidence for a d(3) iron(V) metal center in a low spin (S = 1/2) electron configuration. Low-temperature reaction of the iron(V) nitrido complex with water under reducing conditions leads to high yields of ammonia with concomitant formation of an iron(II) species.
    Keywords: Ferric Compounds -- Chemistry ; Iron -- Chemistry
    ISSN: 00368075
    E-ISSN: 1095-9203
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  • 3
    Language: English
    In: Journal of the American Chemical Society, 28 November 2012, Vol.134(47), pp.19350-3
    Description: Addition of 2,2,6,6-tetramethylpiperidine-N-oxyl (TEMPO) to MCl(3) (M = Fe, Al) results in the formation of MCl(3)(η(1)-TEMPO) [M = Fe (1), Al (2)]. Both 1 and 2 oxidize alcohols to generate ketones or aldehydes along with the reduced complexes MCl(3)(η(1)-TEMPOH) [M = Fe (3), Al (4)]. Complexes 1-4 were fully characterized, including analysis by X-ray crystallography. Additionally, control experiments indicated that neither MCl(3) (M = Al, Fe) nor TEMPO are capable of effecting the oxidation of alcohols independently.
    Keywords: Aluminum Compounds -- Chemistry ; Chlorides -- Chemistry ; Cyclic N-Oxides -- Chemistry ; Ferric Compounds -- Chemistry ; Lewis Acids -- Chemistry
    ISSN: 00027863
    E-ISSN: 1520-5126
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  • 4
    Language: English
    In: Inorganic chemistry, 03 October 2011, Vol.50(19), pp.9508-17
    Description: The mechanism of nitrogen atom transfer from four-coordinate tris(carbene)borate iron(IV) nitrido complexes to phosphines and phosphites has been investigated. In the absence of limiting steric effects, the rate of nitrogen atom transfer to phosphines increases with decreasing phosphine σ-basicity. This trend has been quantified by a Hammett study with para-substituted triarylphosphines, and is contrary to the expectations of an electrophilic nitrido ligand. On the basis of electronic structure calculations, a dual-nature transition state for nitrogen atom transfer is proposed, in which a key interaction involves the transfer of electron density from the nitrido highest occupied molecular orbital (HOMO) to the phosphine lowest unoccupied molecular orbital (LUMO). Compared to analogous atom transfer reactions from a 5d metal, these results show how the electronic plasticity of a 3d metal results in rapid atom transfer from pseudotetrahedral late metal complexes.
    Keywords: Electron Transport -- Analysis ; Iron Compounds -- Chemical Properties ; Iron Compounds -- Atomic Properties ; Molecular Orbitals -- Research ; Nitrogen Compounds -- Chemical Properties ; Nitrogen Compounds -- Atomic Properties ; Transition State (Chemistry) -- Research;
    ISSN: 00201669
    E-ISSN: 1520-510X
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  • 5
    Language: English
    In: Journal of the American Chemical Society, 2014, Vol.136
    Description: The three-fold symmetric, four-coordinate iron(II) phosphoraminimato complexes PhB(MesIm)3Fe− N=PRR′R″ (PRR′R″ = PMePh2, PMe2 Ph, PMe3, and PnPr3) undergo a thermally induced S = 0 to S = 2 spincrossover in fluid solution. Smaller phosphoraminimato ligands stabilize the low-spin state,...
    Keywords: Chemical Sciences ; Material Chemistry ; Steric and Electronic ; Four-Coordinate Iron(II) Complexes ; Chemistry
    ISSN: 0002-7863
    E-ISSN: 1520-5126
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  • 6
    Language: English
    In: European Journal of Inorganic Chemistry, 06 August 2013, Vol.2013(22‐23), pp.3817-3820
    Description: Addition of TEMPO (TEMPO = 2,2,6,6‐tetramethylpiperidine‐‐oxyl) to a toluene slurry of AlBr results in rapid formation of AlBr(η‐TEMPO) (), which can be isolated in 65 % yield. In contrast, addition of TEMPO to a hexanes solution of BBr results in formation of [TEMPO][BBr] () and (TEMPO)BBr (), the products of TEMPO disproportionation. Complexes – have been fully characterized, including analysis by X‐ray crystallography. The divergent reactivity is likely dictated by the Lewis acidity of the group 13 halide, and in the case of the stronger Lewis acid BBr, coordination of TEMPO to the boron center generates an adduct that is capable of oxidizing free TEMPO. The outcome of the reaction between TEMPO and MBr (M = B, Al) was found to depend on the Lewis acidity of the group 13 element. Addition of TEMPO to AlBr results in formation of the 1:1 adduct, AlBr(η‐TEMPO). In contrast, addition of TEMPO to BBr results in TEMPO disproportionation and formation of [TEMPO][BBr] and (TEMPO)BBr.
    Keywords: Radicals ; Halides ; Lewis Acids ; Redox Chemistry ; Main Group Elements
    ISSN: 1434-1948
    E-ISSN: 1099-0682
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  • 7
    Language: English
    In: Angewandte Chemie (International ed. in English), 11 July 2011, Vol.50(29), pp.6630-3
    ISSN: 14337851
    E-ISSN: 1521-3773
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  • 8
    In: Dalton Transactions, Dalton Transactions, 2012, Vol.41(26), pp.7859-7861
    Description: Arylation of tris(2-benzylnitrile)amine with PhLi, followed by aqueous work-up, results in the formation of a tripodal tris(ketimine) scaffold, N(ArCNHPh) 3 . N(ArCNHPh) 3 readily coordinates a number of Cu I salts, generating complexes that exhibit trigonal pyramidal geometries in the solid-state.
    ISSN: 1477-9226
    E-ISSN: 1477-9234
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  • 9
    Language: English
    In: Inorganic chemistry, 18 August 2014, Vol.53(16), pp.8425-30
    Description: The iron(IV) nitrido complex PhB(MesIm)3Fe≡N reacts with 1,3-cyclohexadiene to yield the iron(II) pyrrolide complex PhB(MesIm)3Fe(η(5)-C4H4N) in high yield. The mechanism of product formation is proposed to involve sequential [4 + 1] cycloaddition and retro Diels-Alder reactions. Surprisingly, reaction with 1,4-cyclohexadiene yields the same iron-containing product, albeit in substantially lower yield. The proposed reaction mechanism, supported by electronic structure calculations, involves hydrogen-atom abstraction from 1,4-cyclohexadiene to provide the cyclohexadienyl radical. This radical is an intermediate in substrate isomerization to 1,3-cyclohexadiene, leading to formation of the pyrrolide product.
    Keywords: Cyclohexenes -- Chemistry ; Hydrogen -- Chemistry ; Iron Compounds -- Chemical Synthesis ; Nitrogen Compounds -- Chemistry
    ISSN: 00201669
    E-ISSN: 1520-510X
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  • 10
    Language: English
    In: Angewandte Chemie International Edition, 01 September 2015, Vol.54(36), pp.10600-10603
    Description: Thermolysis of the iron(IV) nitride complex [PhB(BuIm)FeN] with styrene leads to formation of the high‐spin iron(II) aziridino complex [PhB(BuIm)Fe‐N(CHCHPh)]. Similar aziridination occurs with both electron‐rich and electron‐poor styrenes, while bulky styrenes hinder the reaction. The aziridino complex [PhB(BuIm)Fe‐N(CHCHPh)] acts as a nitride synthon, reacting with electron‐poor styrenes to generate their corresponding aziridino complexes, that is, aziridine cross‐metathesis. Reaction of [PhB(BuIm)Fe‐N(CHCHPh)] with MeSiCl releases the N‐functionalized aziridine MeSiN(CHCHPh) while simultaneously generating [PhB(BuIm)FeCl]. This closes a synthetic cycle for styrene azirdination by a nitride complex. While the less hindered iron(IV) nitride complex [PhB(MesIm)FeN] reacts with styrenes below room temperature, only bulky styrenes lead to tractable aziridino products. : Iron(IV) nitride complexes react with a range of styrenes to form the corresponding high‐spin iron(II) aziridino complexes. The reversibility of the aziridination reaction allows for aziridine cross‐metathesis reactions. A synthetic cycle for the formation of N‐silylated aziridines has been established.
    Keywords: Alkenes ; Iron ; Nitrides
    ISSN: 1433-7851
    E-ISSN: 1521-3773
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