2 Homometallic Alkoxides

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574 Alkoxo and Aryloxo Derivatives of Metals dimeric with chloro bridges. 398 Although the tribromide [Ta(OC6HPh4-2,3,5,6)2Br3] is also square pyramidal, the iodide [Nb(OC6HPh4-2,3,5,6)2I3] is trigonal bipyramidal with axial OAr. There is an extensive series of six-coordinate adducts with O, 399 N, 400 and P 398 donor ligands. These d 0 -adducts are distorted from strict octahedral and this distortion has been analysed. 398 A more pronounced distortion is present in the dihydrides [Ta(OAr)2Cl(H)2(PMePh2)] and [Ta(OAr)3(H)2(PMe2Ph)] (see below). 401 Treatment of the dimeric [TaCl3(THF)2]2( -N2) with six equivalents of [LiOC6H3Pr i 2 - 2,6] was found to lead to the compound [(THF)(ArO)3Ta(NN)Ta(OAr)3(THF)]. 402 The structure contains a hydrazido(4-) ligand with an N–N distance of 1.32 (1) ˚A. The alkylation of chloro, aryloxides of niobium and tantalum with Grignard or lithium reagents leads to a wide range of mixed alkyl, aryloxides. Alkylation of the metal–chloride bonds occurs first, but subsequent displacement of aryloxide groups can occur with excess alkylating agent. 403 With very bulky aryloxide ligands, alkylation can lead to alkylidene derivatives via an ˛-hydrogen abstraction process. It is also possible to photochemically generate corresponding alkylidene species. Mechanistic studies show that irradiation into alkyl-to-metal charge transfer bands leads to transient alkyl radicals that abstract the adjacent ˛-hydrogen. 203 A series of tris-aryloxide neopentylidene compounds [Ta(DCHCMe3)(OAr)3(THF)] (OAr D OC6H3Pr i 2 -2,6, OC6H3Me2-2,6) have been obtained by treating [Ta(DCHCMe3)Cl3(THF)2] with LiOAr. 404 They react with a variety of olefins to produce isolable tantalacyclobutane derivatives, e.g. styrene produces [Ta⊲OC6H3Pr i 2 - 2,6⊳3fCH⊲Ph⊳CH⊲Bu t ⊳CH2g] whose structure shows the Bu t substituent at the ˇ-position. An equilibrium between the tantalacyclobutane and alkylidene/THF adduct was observed accounting for both formation of new alkylidenes (e.g. [Ta(DCHSiMe3)(OAr)3(THF)] from CH2DCHSiMe3) and tantalacyclobutane isomerization. Addition of ethylene generates the simplest tantalacyclobutane [Ta(OC6H3Pr i 2 -2,6)3(CH2CH2CH2)] which forms a pyridine adduct without fragmenting. The compound [Ta⊲OC6H3Pr i 2 - 2,6⊳3fCHBu t CH⊲C5H8CH⊳g] (structurally characterized) formed from norbornene acts as a living polymerization catalyst for the formation of polynorbornene. 404 Kinetic studies show that the rate determining step is ring opening of the metallacycle. Treatment of the compound [(Me3SiCH2)2Ta( -CSiMe3)2Ta(CH2SiMe3)2] with bulky phenols leads to a series of substitution products in which the central 1,3dimetallacyclobutadiene core remains intact. 136 The relative rates of substitution of the first alkyl group by a series of phenols have been obtained by competition reactions. In the case of 2,6-diarylphenols the relative rate of substitution decreases as the bulk of the meta-substituent increases. 405 This is argued to be a consequence of a decrease in the conformational flexibility of the ortho-phenyl rings hence leading to a bulkier ligand. Mixed hydrido, aryloxides of niobium and tantalum are important reagents. The addition of bulky phenols to [Cp Ł Ta(PMe3)(H)2( 2 -CH2PMe2)] has been shown to lead to [Cp Ł Ta(H)2(OAr)2] derivatives. 153 Treatment of [Ta(OAr)(R)(Cl)( 6 -C6Me6)] precursors with [LiBEt3H] leads to [Ta(OAr)(R)(H)( 6 -C6Me6)] species. 406 The hydrogenolysis of mixed alkyl, aryloxides of tantalum in the presence of phosphine donor ligands can produce the corresponding hydrides (Scheme 6.8). 401 It is also possible to generate hydride compounds by addition of [Bu3SnH] to chloro, aryloxides of tantalum (Scheme 6.8). In the case of niobium this reaction does not lead to stable hydrides but to the d 1 -species all-trans-[Nb(OAr)2Cl2(PR3)2]. 407 The corresponding
575 Table 6.26 Tantalum aryloxides Bond length ( ˚A) Bond angle ( Ž ) Compound Aryloxide M–O M–O–Ar Reference [Ta2⊲ 2-OAr⊳2⊲OAr⊳8] 6-coord. Ta [Ta(OAr) 2Cl3] square pyramidal Ta, axial ArO [Ta(OAr) 3Cl2] square pyramidal Ta, axial ArO [Ta(OAr) 3Cl2] square pyramidal Ta, axial ArO [Ta(OAr) 3Cl2] square pyramidal Ta, axial ArO [Ta(OAr) 2Br3] square pyramidal Ta, axial ArO [Ta(OAr) 3Br2] square pyramidal Ta, axial ArO Homoleptic aryloxides and adducts OC6H4Me-4 1.836 (10) 1.898 (10) 2-OC6H4Me-4 1.925 (9) 1.924 (9) 2.084 (8) Mixed aryloxy halides, amides, hydrides, etc. OC6H3But 2-2,6 1.872 (5) 1.836 (4) OC6H3But 2-2,6 1.90 (2) 1.90 (2) 1.83 (2) OC6HPh2-2,6-Me2-3,5 1.803 (3) 1.862 (3) OC6HPh2-2,6-But 2-3,5 1.810 (2) 1.883 (2) OC6HPh4-2,3,5,6 1.865 (3) 1.825 (3) OC6H3Pr i 2 -2,6 1.839 (6) 1.840 (7) 1.861 (7) i L.N. Lewis and M.F. Garbauskas, Inorg. Chem., 24, 363 (1985). ii L.R. Chamberlain, I.P. Rothwell, and J.C. Huffman, Inorg. Chem, 23, 2575 (1984). iii G.R. Clark, A.J. Nielson, and C.E.F. Rickard, Polyhedron, 6, 1765 (1987). iv J.S. Vilardo, M.A. Lockwood, L.G. Hanson, J.R. Clark, B.C. Parkin, P.E. Fanwick, and I.P. Rothwell, J. Chem. Soc., Dalton Trans., 3353 (1997). v E.S. Freeman, P.E. Fanwick, and I.P. Rothwell, results to be published. (continued overleaf ) 156 166 148 144 112 157 172 148 153 162 168 151 178 141 153 162 152 161 171 i ii iii iv iv v v
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Alkoxo and Aryloxo Derivatives of M
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1 Introduction In 1978 the book ent
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1 INTRODUCTION 2 Homometallic Alkox
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Homometallic Alkoxides 5 to complet
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Table 2.1 (Continued) Homometallic
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Homometallic Alkoxides 15 reactivit
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Homometallic Alkoxides 17 By contra
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Homometallic Alkoxides 19 2.3 React
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Homometallic Alkoxides 21 has been
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Homometallic Alkoxides 23 obtain on
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y Evans and co-workers: 160,161 Hom
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Homometallic Alkoxides 27 The heter
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Homometallic Alkoxides 29 not conve
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Homometallic Alkoxides 31 In view o
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2.7.2 Steric Factors Homometallic A
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Homometallic Alkoxides 35 (b) When
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Homometallic Alkoxides 37 2.8 Trans
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Homometallic Alkoxides 39 with orga
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2.9.1.1 Alkoxides of Be, Mg, Ca, Sr
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MfN⊲SiMe3⊳2g2thfx C2HOR, Cpy !C
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Homometallic Alkoxides 45 2.10 Misc
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Zr⊲CH2Bu t ⊳4 C 4RfOH benzene !
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2.10.5 By Insertion of Oxygen into
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Homometallic Alkoxides 51 First hom
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O M R M OR M OR RO M (M = Tl; R = M
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Homometallic Alkoxides 55 3. Nuclea
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Homometallic Alkoxides 57 explain t
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Decomposition (%) 100 80 60 40 20 0
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Table 2.6 Volatilities of tetravale
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Homometallic Alkoxides 63 deduced t
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Table 2.10 Vapour pressure of Ti, Z
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Homometallic Alkoxides 67 Table 2.1
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3.2.10 Alkoxides of Later 3d Metals
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Homometallic Alkoxides 71 Table 2.1
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Homometallic Alkoxides 73 affected
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Homometallic Alkoxides 75 the range
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Homometallic Alkoxides 77 several c
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Homometallic Alkoxides 81 In toluen
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Bu t O Bu t O Bu t O Th O O Bu O t
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Homometallic Alkoxides 85 1H NMR st
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Homometallic Alkoxides 87 septet wa
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Homometallic Alkoxides 89 experimen
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Table 2.21 1 H NMR spectra of Al4(O
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Homometallic Alkoxides 93 3.5 Elect
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Homometallic Alkoxides 95 ligand fi
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Homometallic Alkoxides 97 susceptib
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10 −1 /xM 12 10 −200 −100 0 [
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Homometallic Alkoxides 101 alkoxide
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Homometallic Alkoxides 103 fragment
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Homometallic Alkoxides 105 The mass
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Homometallic Alkoxides 107 [Al⊲OP
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Homometallic Alkoxides 109 Under ca
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4.3.2 Phenol-Alcohol Exchange React
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4.4 Reactions with Alkanolamines Ho
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Homometallic Alkoxides 115 R D Pr i
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Homometallic Alkoxides 117 La(OPr i
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Homometallic Alkoxides 119 with the
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Homometallic Alkoxides 121 about 1.
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Homometallic Alkoxides 123 concentr
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Homometallic Alkoxides 125 and othe
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Homometallic Alkoxides 127 Interest
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OH Monofunctional bidentate HC N R
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Homometallic Alkoxides 131 metal al
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Homometallic Alkoxides 133 which yi
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shown in Eq. (2.286): O Mo2(OEt)6 H
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Homometallic Alkoxides 137 Phenyl i
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Homometallic Alkoxides 139 The 1990
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Eqs (2.312)-(2.315): where R D l-ad
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Homometallic Alkoxides 143 On the b
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Homometallic Alkoxides 145 The form
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Homometallic Alkoxides 147 On furth
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4.16 Interactions Between Two Diffe
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4Mo2(OPr i )6 + 18CO (excess) Homom
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isolobality of CR 0 and W⊲OR⊳3
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W2(OR)8 (R = CH2Bu t ) + CO + H2C C
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Homometallic Alkoxides 157 43. J.S.
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Homometallic Alkoxides 159 122. P.N
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Homometallic Alkoxides 161 201. A.
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Homometallic Alkoxides 163 281. R.C
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Homometallic Alkoxides 165 358. L.A
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Homometallic Alkoxides 167 430. M.R
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Homometallic Alkoxides 169 521. I.
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Homometallic Alkoxides 171 N.I. Koz
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Homometallic Alkoxides 177 876. J.
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Homometallic Alkoxides 179 966. H.
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Homometallic Alkoxides 181 1054. M.
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184 Alkoxo and Aryloxo Derivatives
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236 Table 4.1 (Continued) M-O Bond
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244 Table 4.3 Alkoxides of aluminiu
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248 Table 4.4 Alkoxides of germaniu
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256 Table 4.6 Alkoxides of scandium
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264 Table 4.7 Alkoxides of lanthani
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276 Table 4.9 Alkoxides of titanium
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278 Table 4.9 (Continued) Bond leng
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300 Table 4.11 Alkoxides of chromiu
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302 Table 4.11 (Continued) Metal M-
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316 Table 4.11 (Continued) Metal M-
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322 Table 4.12 Alkoxides of mangane
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332 Table 4.16 Alkoxides of zinc, c
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340 Table 4.17 (Continued) Coordina
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348 Table 4.18 Bimetallic alkoxides
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354 Table 4.19 Heterometallic alkox
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394 Table 5.2 Chemical shifts from
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400 Table 5.3 Scandium, yttrium, la
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402 Table 5.3 (continued) Metal Oxo
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406 Table 5.4 Titanium and zirconiu
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420 Table 5.6 Chromium sub-group me
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1 INTRODUCTION 6 Metal Aryloxides T
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Metal Aryloxides 447 or both of the
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R1 OH O R2 R3NH2 −H2O Scheme 6.3
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Cl S N N OH O Cl Me 3C NH HN OH HO
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N OH N OH Me 3C Me3C HO HO N N OH H
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Metal Aryloxides 455 2Ln C 3Hg⊲C6
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Metal Aryloxides 457 Mixed halo, ar
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product metal aryloxide 1e,1f (Eqs
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Metal Aryloxides 461 Eqs 6.39 and 6
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O Mg Mg OAr O Metal Aryloxides 463
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3.7 From Metal Hydrides Metal Arylo
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Metal Aryloxides 467 Two other impo
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Metal Aryloxides 469 Table 6.1 Meta
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Table 6.3 W-OAr distances for vario
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Metal Aryloxides 473 At first it is
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Zr−O distance (Å) V−O distance
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Metal Aryloxides 477 as expected ar
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Metal Aryloxides 479 whereas R D Me
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where OAr = O But But H3C H3C O Ta
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PPh 2 Ph P Pt OAr PPh2 where OAr =
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6 SURVEY OF METAL ARYLOXIDES 6.1 Sp
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487 Na2[V(O) 2(OAr) 2]2.4H2O.DMF 6-
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489 [Tc(O)(OAr)(di-OAr)] 8-quin 2.0
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491 [Ni3⊲OAr⊳6][ClO4].EtOH 8-qu
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493 [Pt(OAr⊳2](tcnq) sq. planar P
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495 [Al(OAr) 3].MeOH 8-quin 1.850 (
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497 [Sb(OAr) 2⊲S2COEt⊳] pentago
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499 [Tc(O)(OAr)(N-salicylideneDD-gl
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Metal Aryloxides 501 A contribution
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503 Table 6.8 Metal bi-phenolates B
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505 Table 6.9 Metal binaphtholates
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507 [TiCl2(di-OAr)]2 two tetrahedra
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Metal Aryloxides 509 co-workers hav
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511 [Li⊲ 2-OAr⊳]3 planar Li3O3
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513 Table 6.11 Sodium aryloxides Bo
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Table 6.12 Potassium aryloxides Met
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Table 6.15 Magnesium aryloxides Met
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519 Table 6.18 Barium aryloxides Bo
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521 Table 6.19 Group 3 metal and la
Page 523 and 524: 523 [Me4N]La2Na2⊲ 4-OAr⊳⊲ 3-O
Page 525 and 526: 525 [Nd⊲OC6H3Ph- 6-C6H5⊳⊲OC6H
Page 527 and 528: 527 [⊲THF⊳Li⊲ 2-OAr⊳2Sm⊲C
Page 529 and 530: 529 [Eu⊲ 2-OAr⊳4⊲OAr⊳2⊲ 3
Page 531 and 532: 531 [Yb(OAr) 3⊲THF⊳2].THF squar
Page 533 and 534: Metal Aryloxides 533 carbon atoms a
Page 535 and 536: 535 [Cp Ł Th(OAr)⊲CH2SiMe3⊳2]
Page 537 and 538: Metal Aryloxides 537 amido compound
Page 539 and 540: 539 Table 6.21 Titanium aryloxides
Page 541 and 542: 541 [Ti2⊲ 2-OAr⊳2(OAr) 2Cl4]2 e
Page 543 and 544: 543 [Ti(OAr) 2⊲NMe2⊳2] tetrahed
Page 545 and 546: 545 [Ti(OAr) 3Bu t ] tetrahedral Ti
Page 547 and 548: 547 [⊲ArO⊳2Ti⊲ 2-ButNDCC4Et4C
Page 549 and 550: 549 [Cp⊲C5H3Me-Pri-1,2)Ti(OAr)Cl]
Page 551 and 552: 551 [CpTi(OAr) 2⊲HPPh⊳] OC6H3Pr
Page 553 and 554: 553 [Ti⊲di-OAr⊳Cl2].THF 6-coord
Page 555 and 556: 555 Table 6.22 Zirconium aryloxides
Page 557 and 558: 557 [Zr(Ind-OAr) 2] 1-indenylphenox
Page 559 and 560: 559 [Cp2Zr(OAr)] 18-electron Zr, tw
Page 561 and 562: Metal Aryloxides 561 The thermal st
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Page 565 and 566: 565 1.839 (2) 138 1.854 (2) 140 [(t
Page 567 and 568: 567 [V(OAr) 3-N-Li(THF) 3] tetrahed
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Page 571 and 572: 571 cis,mer-[Nb(OAr) 2Cl3(THF)] dis
Page 573: 573 [Nb⊲OC6H3Ph- 4-C6H7⊳⊲OAr
Page 577 and 578: 577 [(THF)(ArO) 3Ta⊲DNND⊳Ta(OAr
Page 579 and 580: 579 [Ta(OAr) 2Cl2⊲CH2C6H5⊳] tbp
Page 581 and 582: 581 [Ta(OAr) 2Cl⊲ 6-C6Me6⊳] OC6
Page 583 and 584: 583 [Ta(OAr)⊲OC6H3Pri- 2-CMeDCH2
Page 585 and 586: 585 [f(TMEDA)Na⊲ 2-OAr⊳2g2Cr] 4
Page 587 and 588: 587 Table 6.28 Molybdenum aryloxide
Page 589 and 590: 589 [Mo2⊲OAr⊳5⊲NMe2⊳⊲HNMe
Page 591 and 592: 591 [Mo(Hdi-OAr) 2] 6-coord. Mo, on
Page 593 and 594: 593 [W2⊲OAr⊳6⊲HNMe2⊳2] OC6F
Page 595 and 596: 595 [W(OAr) 2⊲DNBu t ⊳2] OC6H3P
Page 597 and 598: 597 [W(OC6H3Ph- 1-C6H4⊳2⊲PMePh2
Page 599 and 600: 599 [W⊲OC6HPh3- 1-C6H4-c-C5H8C- O
Page 601 and 602: 601 [⊲OC⊳3Mn⊲C4H4N⊳Mn⊲CO3
Page 603 and 604: 603 Table 6.32 Simple aryloxides of
Page 605 and 606: 605 Table 6.33 Simple aryloxides of
Page 607 and 608: 607 [NEt4]3fFe6⊲ 4-S⊳4⊲OAr⊳
Page 609 and 610: 609 [Ru(OAr) 2(CO)(py-CMeO-4)] cis-
Page 611 and 612: Table 6.35 Simple aryloxides of osm
Page 613 and 614: Metal Aryloxides 613 states, e.g. [
Page 615 and 616: Bu t O Bu t (6-I) Bu t Bu t O Metal
Page 617 and 618: 6.2.10 Group 9 Metal Aryloxides Met
Page 619 and 620: Table 6.38 Simple aryloxides of iri
Page 621 and 622: Metal Aryloxides 621 Table 6.39 (Co
Page 623 and 624: 623 [Pd(OAr)⊲C6H3fCH2NMe2g2-2,6)]
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Metal Aryloxides 625 Table 6.41 Sim
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627 Table 6.42 Simple aryloxides of
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629 [(RNC) 2Cu⊲ 2-OAr⊳2Cu(CNR)
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Metal Aryloxides 631 The two-coordi
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Table 6.45 (Continued) Metal Arylox
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Table 6.47 Simple aryloxides of mer
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637 Table 6.48 Aluminium aryloxides
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639 [⊲ArO⊳2Al⊲ -OAr⊳2Mg(THF
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641 [Al(OAr) 2⊲i-Bu⊳] trigonal
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643 [Al(OAr)Cl(Me)⊲NH2But⊳] OC6
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645 Table 6.49 Gallium aryloxides B
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647 Table 6.50 Indium aryloxides Bo
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Metal Aryloxides 649 Table 6.53 Tin
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651 Table 6.56 Bismuth aryloxides B
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REFERENCES Metal Aryloxides 653 1.
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Metal Aryloxides 655 56. Y. Nakayam
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Metal Aryloxides 657 123. T.W. Coff
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Metal Aryloxides 659 202. A. Bell,
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Metal Aryloxides 661 268. K. Ishiha
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Metal Aryloxides 663 341. B.S. Kali
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Metal Aryloxides 665 405. P.N. Rile
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Metal Aryloxides 667 483. Y. Hayash
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Metal Aryloxides 669 561. A.P. Shre
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688 Index alkoxometallate(IV) ligan
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690 Index cerium oxo-isopropoxide 3
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692 Index gas-phase photoelectron s
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694 Index lead tert-butoxide 386 Le
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696 Index metal-hydrogen bonds clea
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698 Index oxo-alkoxides 384, 385, 3
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700 Index sodium hydroxide 142 sodi
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702 Index titanium dichloride dieth
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704 Index X X-ray Absorption Near E
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2 Homometallic Alkoxides

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