2 Homometallic Alkoxides

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265 [Nd2⊲ -Cl⊳2⊲OCBu t 3⊳4⊲thf⊳2] [Nd⊲OCBu 5 2.090–2.114 (3) – – 130 t 3⊳3⊲CH3CN⊳2] [Nd4⊲ -ONp⊳8⊲ONp⊳4] Np D CH2Bu 5 5 2.149–2.171 (5) av. 2.162 2.138 (8) – 2.320–2.381 (12) 167.5–171.8 av. 170.3 163.9 (t) 131 118 t [Nd2⊲ -OCHBu av. 2.341 126.6 (b, av.) t t 2⊳2⊲OCHBu2⊳4⊲CH3CN⊳] 4 and 5 2.132–2.151 (4) av. 2.143 2.359–2.394 (4) av. 2.374 166.4 (t, av.) 127.0 (b, av.) 132 [Nd6⊲ 6-Cl⊳⊲ 3-OPr i ⊳2⊲ -OPr i ⊳9⊲OPr i ⊳6] [Nd2⊲ -Cl⊳2⊲OCBu 6 av. 2.05 (2) 2.36 (4) ( ,av.) 2.45 (5) ( 3, av.) – 129 t 3⊳4⊲thf⊳2] 5 2.108–2.114 av. 2.105 – 163.8–174.4 av. 168 130 [Nd2⊲ -OCHPr i i 2⊳2⊲OCHPr2⊳4⊲thf⊳2] 5 2.146, 2.160 (4) 2.368, 2.394 (4) 159.6, 170.2 (t) 117.9, 130.6 (b) 133 [Nd2⊲ -OCHPr i i 2⊳2⊲OCHPr2⊳4⊲C5H5N⊳2] 5 2.133, 2.158 (4) 2.380, 2.383 (4) 173.6, 176.1 (t) 120.8, 130.8 (b) 133 [Nd2⊲ -OCHPr i 2⊳⊲OCHPri2 ⊳4⊲ -dme⊳]1 dme D MeOC2H4OMe [Li(thf) 4] 5 2.144–2.145 (6) 2.359–2.391 (5) 169.3, 174.3 (t) 117.7, 133.0 (b) 133 C [Nd⊲OSiMe3⊳fN⊲SiMe3⊳2g3] [⊲C5Me5⊳2Sm⊲ -O2C16H10⊳Sm⊲C5Me5⊳2] 4 3 2.173 (11) – 177.1 134 1 [⊲thf⊳⊲C5Me5⊳2Sm⊲ -O2C16H10⊳Sm⊲C5Me5⊳2⊲thf⊳] 4 2.08 (2) – 173.2 135 1 [C5Me5⊳2Sm⊲OC4H8C5Me5⊳⊲thf⊳] 4 2.099 (9) – 166.3 135 1 [⊲thf⊳⊲C5Me5⊳2Sm⊲ - OSiMe2OSiMe2O⊳Sm⊲C5Me5⊳2⊳⊲thf⊳] 4 2.08 (1) – 165.2 136 1 [SmfOC⊲Bu 2.157 (5) – 173.6 137 t⊳⊲2-CH2NC5H3Me-6⊳2g3] [Dy⊲OCHBu 5 2.116 (2) (t) 2.142, 2.172 (3) (c) – 168.6 (t) 137.8, 147.8 (c) 138 t 2⊳3⊲CH3CN⊳2] [Yb2⊲ -OCBu 5 2.057, 2.064, 2.063 (5) – 177.0, 177.2, 177.7 132 t 3⊳2fN⊲SiMe3⊳2g2] [Yb⊲OCBu 3 – 2.294–2.320 (6) av. 2.307 129.6–136.2 av. 133.0 140 t 3⊳2⊲thf⊳2] [f⊲Me3Si⊳3Cg2Yb2⊲ -OEt⊳2⊲Et2O⊳2] [YbfOC⊲Bu 4 4 2.07, 2.09 (2) – – 2.267, 2.276 (10) 155, 175 120.9, 121.0 140 141 t⊳⊲2-CH2NC5H3Me-6⊳g2fN⊲SiMe3⊳2g] [Yb2⊲ -OSiMe2Bu 5 – 2.057, 2.072 (3) 142.3, 143.0 (c) 138 t⊳2⊲OSiMe2But⊳2⊲dme⊳2] [Lu2⊲ -OCMe2CH2OMe⊳3⊲OCMe2CH2OMe⊳3] 5 6 and 7 2.163 (11) 2.053, 2.058 (3) (t) 2.123 (c) 2.269, 2.311 (8) 2.196–2.373 (3) av. 2.260 172.9 (t) 119.1, 141.5 (b) 166.4, 174.8 (t) 126.6 (c) 129.7 (b, av.) 142 143 b D bridging, c D chelating, t D terminal. 1 Coordination doubtful.
266 Alkoxo and Aryloxo Derivatives of Metals was formed using the dimethyl-tert-butyl siloxo ligand with DME as supporting ligand in [Yb2⊲ -OCMe2Bu t ⊳2⊲OCMe2Bu t ⊳2(dme) 2]. 142 2.7.8 Lutetium Lutetium(III) forms a novel unsymmetrical dinuclear molecule [Lu2( - OCMe2CH2OMe)3(OCMe2CH2OMe)3] in which one Lu is seven-coordinated and the other six-coordinated (Fig. 4.33). 143 The six-coordinated Lu is bonded to three bridging ligands (one of which is chelating) and two terminals whilst the seven-coordinated metal is bonded to three bridging (two of which are chelating) and one chelating ligand. 2.8 <strong>Alkoxides</strong> of the Actinides 2.8.1 Thorium Although thorium(IV) alkoxides have been known for many years it was only in 1992 that the X-ray crystal structure of a homoleptic thorium compound was reported. Using the bulky di-isopropylcarbinolate ligand the dimeric compound [Th2⊲ - OCHPr i 2 ⊳2⊲OCHPr i 2 ⊳6] was obtained in which each Th is in a distorted TBP coordination. 144 The monomeric tert-butoxide [Th⊲OBu t ⊳4⊲C5H5N⊳2] has a distorted octahedral configuration with pyridine ligands occupying cis positions. 145 With the less sterically demanding Et2CHO ligand an edge-shared bi-octahedral complex [Th2⊲ - OCHEt2⊳2⊲OCHEt2⊳6⊲C5H5N⊳2] was obtained. Each thorium is coordinated to one pyridine ligand located cis to the bridging alkoxo groups in a centrosymmetric molecule. 146 With the isopropoxo ligand the remarkable tetranuclear complex [Th4⊲ -OPr i ⊳6⊲OPr i ⊳10⊲C5H5N⊳2] was obtained (Fig. 4.34). 146 The thorium ions are all octahedrally coordinated forming a zigzag chain through cis pairs of bridging isopropoxides. The two inner thoriums each have cis pairs of terminal isopropoxo groups whilst the end thoriums each have a pyridine ligand acting as chain blocker. The series of edge-sharing bi-octohedral dimers give rise to a centrosymmetrical molecule. The edge-sharing bi-octahedral structure was also found in the dimer [Th2⊲ -OPr i ⊳2⊲OPr i ⊳2I4⊲Pr i OH⊳2] where the bridging isopropoxo group is unsymmetrical with a short Th–O (2.327 ˚A) trans to an iodide and the longer Th–O Figure 4.33 Structure of [Lu2⊲ - OCMe2CH2OMe⊳3⊲OCMe2CH2OMe⊳3] (H atoms omitted).
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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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Page 215 and 216: 214 Alkoxo and Aryloxo Derivatives
Page 237 and 238: 236 Table 4.1 (Continued) M-O Bond
Page 245 and 246: 244 Table 4.3 Alkoxides of aluminiu
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Page 257 and 258: 256 Table 4.6 Alkoxides of scandium
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Page 277 and 278: 276 Table 4.9 Alkoxides of titanium
Page 279 and 280: 278 Table 4.9 (Continued) Bond leng
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Page 303 and 304: 302 Table 4.11 (Continued) Metal M-
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316 Table 4.11 (Continued) Metal M-
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318 Table 4.11 (Continued) M-O Bond
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322 Table 4.12 Alkoxides of mangane
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328 Table 4.15 (Continued) M-O Bond
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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
Page 701 and 702:
702 Index titanium dichloride dieth
Page 703:
704 Index X X-ray Absorption Near E
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2 Homometallic Alkoxides

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