2 Homometallic Alkoxides

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Heterometallic <strong>Alkoxides</strong> 207 with similar covalent characteristics, as confirmed by Nyholm et al. 185 in 1970. This suggestion of ⊲Pr i OH⊳2K⊲ -OPr i ⊳2Al⊲OPr i ⊳2 adduct formation received confirmation in 1993 from the X-ray structural elucidation of this low-melting polymeric unit by Gilje et al. 38 In fact, these workers have shown that the unsolvated KAl⊲OPr i ⊳4 is a white solid (m.p. 380 Ž C) insoluble in noncoordinating solvents, whereas the adduct KAl⊲OPr i ⊳4.2Pr i OH (m.p. 31 Ž C) is soluble in aromatic solvents. The most intense peak in the mass spectrum of this material corresponds to [K2Al2⊲OPr i ⊳7⊲HOPr i ⊳] C and a major fragment contains three K and two Al atoms, which might correspond to a product of the composition K3Al2⊲OPr i ⊳9, isolated 35 in a 3:2 molar reaction of KOPr i and Al⊲OPr i ⊳3. Compared to KAl⊲OPr i ⊳4, which dissolves in isopropanol to give a homogeneous solution, NaOPr i yields only a thick suspension of white powder in isopropanol. The coordination sphere of K in [⊲Pr i O⊳2Al⊲ -OPr i ⊳2K.2Pr i OH] was found to be similar to that of magnesium 37 in [f⊲Pr i O⊳2Al⊲ -OPr i ⊳2g2Mg.2Pr i OH]2. This latter product along with a series of volatile soluble products with the formula, MfM 0 ⊲OR⊳4g2 (M D Mg, Ca, Sr, Ba; M 0 D Al, Ga; R D Et, Pr i ) were isolated (Eq. 3.25) by the dissolution of metal M in alcohol in the presence of 2 moles of M 0 ⊲OR⊳3. This comparatively facile dissolution of bivalent metal in alcohol has been ascribed 16 to the coordination of alcohol to the M⊲OR⊳3, rendering the proton more labile and reactive. The mass and NMR spectra of MgfAl⊲OBu s ⊳4g2 liquid, and the X-ray structure 206 of Mg⊲ -OPh⊳2Al⊲OPh⊳2, confirm a similar coordination model. Table 3.1 lists some representative tetra-alkoxoaluminate derivatives. Compared to the polymeric insoluble and nonvolatile nature of homo-alkoxides of bivalent metals [M⊲OR⊳2]n in general (where M D ⊲i⊳ Mg, Ca, Sr, Ba (Eq. 3.25), (ii) Be, Zn, Cd, Hg(II), Sn(II) (Eq. 3.35), and (iii) Mn(II), Fe(II), Co(II), Ni(II), Cu(II) (Eq. 3.40)), their tetraalkoxoaluminate derivatives MfAl⊲OR⊳4g2 are volatile and soluble in organic solvents, in which they exhibit monomeric (and in a few cases slightly associated) behaviour. Synthesized by the reactions (Eqs 3.35 and 3.40) of their anhydrous chlorides with 2 moles of KAl⊲OPr i ⊳4, their framework MfAl⊲OPr i ⊳4g2 (M D Mg, Zn, Cd, Hg) appears to be so stable that even in 1:1 molar reaction of MCl2 with KAl⊲OPr i ⊳4, only half the amount of MfAl⊲OPr i ⊳4g2 is obtained leaving the remaining MCl2 unreacted. However, a product ClBefAl⊲OPr i ⊳4g could be obtained in such a 1:1 molar reaction; this was converted by reaction with KOPr i into volatile monomeric ⊲Pr i O⊳BefAl⊲OPr i ⊳4g which could be distilled at ¾157 Ž C/0.3 mm pressure. However, this monomeric product tended to dimerize on standing for a few days as shown by its molecular weight and 1 H NMR spectrum. This change could be ascribed to the tendency of beryllium to attain the four-coordination state by assuming a structure of the type: [⊲Pr i O⊳2Al⊲ -OPr i ⊳2Be⊲ -OPr i ⊳2Be⊲ -OPr i ⊳2Al⊲OPr i ⊳2]. 207 This observation immediately led to the synthesis of the first heterotrimetallic alkoxides 7 [⊲Pr i O⊳2Al⊲ -OPr i ⊳2Be⊲ -OPr i ⊳2Zr⊲OPr i ⊳3] and[⊲Pr i O⊳2Al⊲ -OPr i ⊳2Be⊲ - OPr i ⊳2Nb⊲OPr i ⊳4] by the reactions of ⊲Pr i O⊳2Al⊲ -OPr i ⊳2Be⊲OPr i ⊳ with Zr⊲OPr i ⊳4 and Nb⊲OPr i ⊳5, respectively. The structural features of derivatives (iii) of later 3d transition metals, MfAl⊲OPr i ⊳4g2 97,101–104 were elucidated by their UV-Vis spectra and paramagnetic characteristics, techniques commonly employed in the conventional coordination derivatives dealing with such 3d 5 –3d 9 systems and explaining the observations with the help of ligand field theory. For example, the selective exchange ability of branched
208 Alkoxo and Aryloxo Derivatives of Metals Table 3.1 Preparation and characterization of some representative tetraalkoxometallate derivatives Synthetic Characterization Compound route1 techniques References KAl(OPri )4.2PriOH A-1 IR, NMR, MS, 1, 35, 38, 52, X-ray 53, 76, 204 MgfAl(OPri )4g2.2PriOH MgfAl(OBu B NMR, X-ray 35, 36, 37 s )4g2 MfAl(OPr F NMR, MS 206 i )4g2 M D Mg, Ca, Sr, Ba B IR, NMR, volatility, solubility, MW, alcoholysis 35, 36, 85 Mg2Al3(OPri )13 B IR, NMR, X-ray 90 BaAl3(OPri )11, Ba2Al3(OPri )13 MfAl(OPr B IR, NMR, MW, alcoholysis 91 i )4g2, ClMfAl(OPri )4g M D Be, Zn, Cd, Hg(II) C IR, NMR, MW, solubility, volatility, alcoholysis 94 fAl(OPri )4BeOPrig2 C NMR, MW 207 [MfAl(OPr alcoholysis i )4g2] M D Mn(II), Fe(II), Co(II), Ni(II), Cu(II) MfAl(OBu C 42, 97, 100–104 t )4g2 M D Mn, Fe, Co, Ni, Cu, Zn [MfAl(OPr ⎫ C ⎪⎬ UV-Vis, paramagnetism, solubility, volatility, alcoholysis ⎪⎭ ⎧ ⎪⎨ 101, 109, 110, 108 ⎪⎩ i )4g3] M D Cr(III), Fe(III), In(III) LnfAl(OPr C 105, 106, 69, 77 i )4g3 ⎫ A-2, C NMR, MS, ⎪⎬ X-ray of 80 40 [ErfAl(OPr ⎪⎭ i ⎧ ⎪⎨ [(Pr )4g3], volatility, solubility ⎪⎩ iO)2ZrfAl(OPri )4g2] [(Pr A-2, C 209–211 iO)2HffAl(OPri )4g2] [(Pr A-2 X-ray 77 iO)3MfAl(OPri )4g2] M D Nb, Ta A-2 NMR, volatility, MW 75 [fPrf( -OPri )2Al(OPri )2g2(PriOH)( -Cl)g2] C X-ray 39 [I2SnfAl(OPri )4g2] C X-ray 236 [ThfAl(OPri )4g4] C NMR, volatility, MW 52, 74 1 See Section 2 for details of routes listed. alkoxides of Co and Ni with primary alcohols has been explained 97 on the basis of ligand field effects. Alkoxoaluminates of these transition metals are again volatile and monomeric, whereas their simple alkoxides are polymerized insoluble entities. These alkoxoaluminates of later 3d metals undergo facile exchange reactions with other alcohols or ˇ-diketones. The properties of a few of these bimetallic alkoxide products are illustrated in Table 3.2.
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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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Page 173 and 174: Homometallic Alkoxides 171 N.I. Koz
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Page 183 and 184: Homometallic Alkoxides 181 1054. M.
Page 185 and 186: 184 Alkoxo and Aryloxo Derivatives
Page 207: 206 Alkoxo and Aryloxo Derivatives
Page 237 and 238: 236 Table 4.1 (Continued) M-O Bond
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258 Alkoxo and Aryloxo Derivatives
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264 Table 4.7 Alkoxides of lanthani
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270 Table 4.8 (Continued) M-O Bond
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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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559 [Cp2Zr(OAr)] 18-electron Zr, tw
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Metal Aryloxides 561 The thermal st
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Metal Aryloxides 563 can only arise
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565 1.839 (2) 138 1.854 (2) 140 [(t
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567 [V(OAr) 3-N-Li(THF) 3] tetrahed
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569 [V(O)(di-OAr)] 6-coord. V, both
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571 cis,mer-[Nb(OAr) 2Cl3(THF)] dis
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573 [Nb⊲OC6H3Ph- 4-C6H7⊳⊲OAr
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575 Table 6.26 Tantalum aryloxides
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577 [(THF)(ArO) 3Ta⊲DNND⊳Ta(OAr
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579 [Ta(OAr) 2Cl2⊲CH2C6H5⊳] tbp
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581 [Ta(OAr) 2Cl⊲ 6-C6Me6⊳] OC6
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583 [Ta(OAr)⊲OC6H3Pri- 2-CMeDCH2
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585 [f(TMEDA)Na⊲ 2-OAr⊳2g2Cr] 4
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587 Table 6.28 Molybdenum aryloxide
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589 [Mo2⊲OAr⊳5⊲NMe2⊳⊲HNMe
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591 [Mo(Hdi-OAr) 2] 6-coord. Mo, on
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593 [W2⊲OAr⊳6⊲HNMe2⊳2] OC6F
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595 [W(OAr) 2⊲DNBu t ⊳2] OC6H3P
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597 [W(OC6H3Ph- 1-C6H4⊳2⊲PMePh2
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599 [W⊲OC6HPh3- 1-C6H4-c-C5H8C- O
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601 [⊲OC⊳3Mn⊲C4H4N⊳Mn⊲CO3
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603 Table 6.32 Simple aryloxides of
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607 [NEt4]3fFe6⊲ 4-S⊳4⊲OAr⊳
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609 [Ru(OAr) 2(CO)(py-CMeO-4)] cis-
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Table 6.35 Simple aryloxides of osm
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Metal Aryloxides 613 states, e.g. [
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Bu t O Bu t (6-I) Bu t Bu t O Metal
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6.2.10 Group 9 Metal Aryloxides Met
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Table 6.38 Simple aryloxides of iri
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Metal Aryloxides 621 Table 6.39 (Co
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623 [Pd(OAr)⊲C6H3fCH2NMe2g2-2,6)]
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Metal Aryloxides 625 Table 6.41 Sim
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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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