2 Homometallic Alkoxides

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610 Table 6.34 (Continued) Bond length ( ˚A) Bond angle ( Ž ) Compound Aryloxide M–O M–O–Ar Reference [⊲H⊳2Ru6⊲CO⊳16⊲ 2-O- 2 -C6H3OMe-4)] raft cluster, metallated C bridges two metals, phenoxy ring -binds to another [⊲Ph3PAu⊳(H)Ru 6⊲CO⊳16⊲ 2-O- 2 -C6H3OMe-4⊳] raft cluster, metallated C bridges two metals, phenoxy ring -binds to another [Ru3⊲CO⊳8⊲ 2- 2-OAr⊳2] aryloxides both chelate through Cl and bridge one edge of triangular cluster 2-O- 2 -C6H3OMe-4 2.132 (5), 2.159 (5) xvi 2-O- 2 -C6H3OMe-4 2.14 (2), 2.15 (2) xvi 2-OC6H4Cl-2 2.110 (4), 2.163 (4) 2.093 (4), 2.161 (4) [Ru4⊲ 3-OAr⊳2⊲ 2-Cl⊳2⊲CO⊳10] 3-OC6H5 2.144 (1)–2.218 (1) xviii [Ru4⊲ 3-OAr⊳2⊲ 2-OAr⊳⊲ 2-Cl⊳⊲CO⊳10] 2-OC6H4OMe-2 2.029 (7)–2.230 (6) xix two molecules 3-OC6H4OMe-2 2.121 (7)–2.218 (7) xvi M.P. Cifuentes, T.P. Jeynes, M.G. Humphrey, B.W. Skelton, and A.H. White, J. Chem. Soc., Dalton Trans., 925 (1994). xvii D.J. Darensbourg, B. Fontal, S.S. Chojnacki, K.K. Klausmeyer, and J.H. Reibenspies, Inorg. Chem., 33, 3526 (1994). xviii S. Bhaduri, N. Sapre, K. Sharma, P.G. Jones, and G. Carpenter, J. Chem. Soc., Dalton Trans., 1305 (1990). xix T.P. Jeynes, M.P. Cifuentes, M.G. Humphrey, G.A. Koutsantonis, and C.L. Raston, J. Organomet. Chem., 476, 133 (1994). xvii
Table 6.35 Simple aryloxides of osmium Metal Aryloxides 611 Bond length ( ˚A) Bond angle ( Ž ) Compound Aryloxide M–O M–O–Ar Ref. [Os(OAr)(H)(CO)⊲PPri 3⊳2] chelated aryloxide, H trans to bound Cl, trans P OC6Cl5 2.124 (3) 123 i [Os(porphyrin)⊲OAr⊳2] OC6H51.938 (2) 128 ii i M.A. Tena, O. Nurnberg, and H. Werner, Chem. Ber., 126, 1597 (1993). ii Ming-Chu Cheng, Chih-Chieh Wang, and Yu Wang, Inorg. Chem., 31, 5220 (1992). tantalum species [Ta(OAr)2Cl2(L)2] (LD various P and N donor ligands) are produced by sodium amalgam reduction of the trichlorides. 400 Two general structural motifs are found for the isolated hydrides of tantalum. The seven-coordinate compounds adopt pentagonal bipyramidal geometry with trans, axial aryloxide ligands. Spectroscopic studies show that the molecules are stereochemically rigid. 401 There is no evidence that the colourless trihydride compounds exist as 2 -H2 species. With very bulky aryloxides or with three aryloxide ligands, six-coordinate hydrides are produced. There is a dramatic bending of the two hydride ligands towards the donor phosphine ligand. This can be accounted for by an increase in -bonding between the Cl or OAr ligand trans to P upon bending the hydride ligands. 398 It can be seen that during the hydrogenolysis of alkyls containing 2,6-diphenylphenoxide ligands, the intramolecular hydrogenation of the ortho-phenyl rings takes place. 31 These hydride species of tantalum and in particular niobium will carry out the catalytic hydrogenation of simple arenes as well as aryl-phosphines. 408,409 Polynuclear aromatic hydrocarbons are hydrogenated faster than simple benzenes. 410 The catalysts exhibit a high degree of regioselectivity and have been shown to carry out the all-cis hydrogenation of many arenes. 411 The most active catalysts for arene hydrogenation are the solutions generated by hydrogenolysis of either the isolated alkyls [Nb(OAr)2R3] or the mixture [Nb(OAr)2Cl3/3n-BuLi]. This reactivity has also been developed into a process for the bulk synthesis of cyclohexylphosphines from their aryl counterparts. 408 Studies have shown the reaction proceeds in a predominantly all-cis fashion with no intermediate cyclohexadienyl or cyclohexenylphosphines being detected by 31 PNMR spectroscopy. The two-electron reduction of mixed chloro, aryloxides can lead to cyclometallated derivatives via CH bond activation by low valent intermediates (Section 5.1). However, reduction in the presence of unsaturated organic substrates can lead to interesting compounds. The presence of the -donating aryloxide ligands results in highly reducing d 2 -metal fragments that can strongly bind and activate the organic substrate. 412–416 Reduction in the presence of alkynes can lead to mono-alkyne complexes, tantalacyclocyclopentadiene rings or 6 -arene derivatives, hence mapping out the overall cyclotrimerization process. 417 The alkyne complex [Ta(OC6H3Pr i 2 -2,6)3( 2 - PhC CPh)] 418 has tantalacyclopropene character and reacts with ketones to produce 2-oxa-tantalacyclopent-4-ene rings. With aldehydes, coupling is followed by a hydride transfer to a second aldehyde to produce an alkoxide species, e.g. [Ta(OC6H3Pr i 2 - 2,6)3(OCH2Ph)(CPhDCPhCPhDO)] from benzaldehyde. 419 Addition of nitriles to the alkyne complex produces adducts which thermolyse to produce metallacyclic
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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
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523 [Me4N]La2Na2⊲ 4-OAr⊳⊲ 3-O
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525 [Nd⊲OC6H3Ph- 6-C6H5⊳⊲OC6H
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527 [⊲THF⊳Li⊲ 2-OAr⊳2Sm⊲C
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529 [Eu⊲ 2-OAr⊳4⊲OAr⊳2⊲ 3
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531 [Yb(OAr) 3⊲THF⊳2].THF squar
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Metal Aryloxides 533 carbon atoms a
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535 [Cp Ł Th(OAr)⊲CH2SiMe3⊳2]
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Metal Aryloxides 537 amido compound
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539 Table 6.21 Titanium aryloxides
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541 [Ti2⊲ 2-OAr⊳2(OAr) 2Cl4]2 e
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543 [Ti(OAr) 2⊲NMe2⊳2] tetrahed
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545 [Ti(OAr) 3Bu t ] tetrahedral Ti
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547 [⊲ArO⊳2Ti⊲ 2-ButNDCC4Et4C
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549 [Cp⊲C5H3Me-Pri-1,2)Ti(OAr)Cl]
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551 [CpTi(OAr) 2⊲HPPh⊳] OC6H3Pr
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553 [Ti⊲di-OAr⊳Cl2].THF 6-coord
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555 Table 6.22 Zirconium aryloxides
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557 [Zr(Ind-OAr) 2] 1-indenylphenox
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Page 561 and 562: Metal Aryloxides 561 The thermal st
Page 563 and 564: Metal Aryloxides 563 can only arise
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
Page 569 and 570: 569 [V(O)(di-OAr)] 6-coord. V, both
Page 571 and 572: 571 cis,mer-[Nb(OAr) 2Cl3(THF)] dis
Page 573 and 574: 573 [Nb⊲OC6H3Ph- 4-C6H7⊳⊲OAr
Page 575 and 576: 575 Table 6.26 Tantalum aryloxides
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
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Page 591 and 592: 591 [Mo(Hdi-OAr) 2] 6-coord. Mo, on
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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 607 and 608: 607 [NEt4]3fFe6⊲ 4-S⊳4⊲OAr⊳
Page 609: 609 [Ru(OAr) 2(CO)(py-CMeO-4)] cis-
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)]
Page 625 and 626: Metal Aryloxides 625 Table 6.41 Sim
Page 629 and 630: 629 [(RNC) 2Cu⊲ 2-OAr⊳2Cu(CNR)
Page 631 and 632: Metal Aryloxides 631 The two-coordi
Page 633 and 634: Table 6.45 (Continued) Metal Arylox
Page 635 and 636: Table 6.47 Simple aryloxides of mer
Page 637 and 638: 637 Table 6.48 Aluminium aryloxides
Page 639 and 640: 639 [⊲ArO⊳2Al⊲ -OAr⊳2Mg(THF
Page 641 and 642: 641 [Al(OAr) 2⊲i-Bu⊳] trigonal
Page 643 and 644: 643 [Al(OAr)Cl(Me)⊲NH2But⊳] OC6
Page 645 and 646: 645 Table 6.49 Gallium aryloxides B
Page 647 and 648: 647 Table 6.50 Indium aryloxides Bo
Page 649 and 650: Metal Aryloxides 649 Table 6.53 Tin
Page 651 and 652: 651 Table 6.56 Bismuth aryloxides B
Page 653 and 654: REFERENCES Metal Aryloxides 653 1.
Page 655 and 656: Metal Aryloxides 655 56. Y. Nakayam
Page 657 and 658: Metal Aryloxides 657 123. T.W. Coff
Page 659 and 660: 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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