2 Homometallic Alkoxides

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X-Ray Crystal Structures of Alkoxo Metal Compounds 285 1,2-Mo2⊲OBu t ⊳2⊲CH2SiMe3⊳4 is ethane-like ⊲C2h symmetry). 235 Addition of dialkyl cyanamides R2NCN to Mo2⊲OR⊳6 compounds produced [Mo2⊲OR⊳6⊲ -NCNR2⊳] complexes and the crystal structure [Mo2⊲OR⊳6⊲ -OCH2Bu t ⊳⊲ -NCNMe2⊳⊲OCH2Bu t ⊳5] was determined. One Mo atom is bonded to two terminal Bu t CH2O ligands, the 2 -CN portion of the cyanamide and one bridging Bu t CH2O ligand. The second Mo is bonded to three terminal Bu t CH2O ligands, the bridging nitrogen of the cyanamide and the bridging Bu t CH2O ligand. The terminal Bu t CH2O trans to the bridging cyanamide nitrogen has a longer Mo–O bond length (1.954 ˚A) than the other terminal neopentoxide groups (av. 1.87 ˚A) whilst the alkoxo bridge is unsymmetrical (Mo–O, 1.999, 2.146 ˚A). 236 In the dimer [Mo2⊲ - 1 , 1 -O2CPh⊳2⊲OBu t ⊳4] the Mo Mo unit (d, 2.236 ˚A) is spanned by a pair of cis bridging benzoato ligands with terminal Bu t O ligands trans to each of the benzoate oxygens. 237 By contrast in the acetylacetonate [Mo2⊲OBu t ⊳4⊲acac⊳2] (Mo Mo, 2.237 ˚A) the diketonato groups are chelating in preference to bridging. 238 Addition of tert-butyl isonitrile gave the edgebridged bi-octahedral molecule [Mo2⊲ -OCH2Bu t ⊳2⊲OCH2Bu t ⊳2⊲CNBu t ⊳2⊲acac⊳2]. 239 Alkoxo-ligands in Mo2⊲OR⊳6 can be replaced by thiolato groups as in [Mo2⊲OPr i ⊳2⊲SAr⊳4] (Ar D 2,4,6-trimethylphenyl) where the M M bond distance (2.230 ˚A) is typical for this class of compound. 240 The arylselenato complex [Mo2⊲OPr i ⊳2⊲SeAr⊳4] (Mo Mo, 2.219 ˚A) is similar. 299 In the novel bromo complex [Mo2⊲ -OCH2Bu t ⊳2⊲ -Br⊳⊲OCH2Bu t ⊳4Br(py)] each Mo is in a distorted octahedral environment and the Mo–Mo distance (2.534 ˚A) implies metal–metal double bonding. 241 Reaction of Mo2⊲OBu t ⊳6 with diphenyldiazomethane gave the mononuclear five-coordinated (TBP) [Mo⊲OBu t ⊳4⊲NNCPh2⊳] where the equatorial Mo–O bond lengths (av. 1.89 ˚A) are shorter than the axial Mo–O bond (1.944 ˚A). With Mo2⊲OPr i ⊳6 in the presence of pyridine the binuclear confacial bi-octahedral complex [Mo2⊲ -OPr i ⊳3⊲NNCPh2⊳2⊲py⊳] with Mo–Mo D 2.66 ˚A indicative of a single metal–metal bond. 242 One Mo atom is coordinated to an NNCPh2 ligand, two terminal Pr i O ligands and three bridging Pr i O ligands whilst the other Mo is coordinated to one NNCPh2 ligand, one terminal Pr i O, one pyridine, and three bridging Pr i O ligands. The bridges are distinctly unsymmetrical. The binuclear phenylisocyanate insertion product [Mo2⊲OPr i ⊳4fNPhC⊲O⊳⊲OPr i ⊳g2] hastwocis bridging bidentate ligands and four terminal isopropoxo ligands with a Mo Mo (2.221 ˚A). 243 The quadruply metal–metal bonded dimers [Mo2⊲OPr i ⊳4⊲py⊳4], [Mo2⊲OCH2Bu t ⊳4 ⊲PMe3⊳4], [Mo2⊲OCH2Bu t ⊳4⊲Me2NH⊳4], and [Mo2⊲OPr i ⊳4⊲Pr i OH⊳4] are of special interest (Mo Mo; 2.195, 2.209, 2.133, 2.110 ˚A, respectively) in having no bridging ligands. 244 Generally in the [Mo2⊲OR⊳4L4] complexes the OR groups are cis to the L ligands and the two halves of the molecule are in the eclipsed conformation (Fig. 4.41). When L D Pr i OH or Me2NH there is hydrogen bonding RO....HOR(HNMe2) across the metal–metal bond which is thereby shortened. The same situation occurs in [Mo2⊲OC5H9-c⊳4⊲c-C5H9OH⊳4] although it was not possible to distinguish c-C5H9O ligands from c-C5H9OH in this structure. 245 The unsymmetrical Mo Mo (2.235 ˚A) complex [Mo2⊲OPr i ⊳4⊲CH2Ph⊳2⊲PMe3⊳] has one molybdenum bonded to benzyl groups and one PMe3 ligand. 246,247 With the bidentate phosphine ⊲Me2P⊳2CH2 (dmpm) the symmetrical dimer
286 Alkoxo and Aryloxo Derivatives of Metals Figure 4.41 Structure of [Mo2⊲OPr i ⊳4⊲Pr i OH⊳4] ( D O;ž D Mo; H atoms omitted). [Mo2⊲OPr i ⊳4⊲CH2Ph⊳2(dmpm)] was formed with the dmpm ligand bridging across the Mo Mo bond (2.253 ˚A). 247 Interestingly in the dimer [Mo2⊲OPr i ⊳4⊲dmpe⊳2] the dmpe ligands chelate a single Mo atom giving an unsymmetrical Mo(IV)-Mo(0) complex with a Mo Mo triple bond (2.236 ˚A). 248 From the reaction of 2-butyne with [Mo2⊲OCH2Bu t ⊳6⊲NCNEt2⊳] the novel complexes [Mo2⊲ -OCH2Bu t ⊳⊲ -C4Me4⊲OCH2Bu t ⊳5⊲NCNEt2⊳] and [Mo2( -OCH2Bu t ) f -C4Me3CH2(NEt2)NHg(OCH2Bu t )5] were obtained. 249 Addition of quinones to Mo2⊲OPr i ⊳6 gave rise to edge-shared isopropoxo-bridged bi-octahedral complexes [Mo2⊲ -OPr i ⊳2⊲OPr i ⊳4⊲O2C6Cl4⊳2] and[Mo2⊲ -OPr i ⊳2⊲OPr i ⊳2⊲O2C14H8⊳3] inwhich the diolate ligands are chelating. 250 The adduct of 1,4-diisopropyl-1,4-diazabutadiene with Mo2⊲OPr i ⊳6 is the unsymmetrical binuclear complex [Mo2( - OPr i )2(OPr i )4(Pr i NCHCHNPr i )] in which one Mo is bonded to three terminal Pr i O ligands and two isopropoxo bridges whilst the other is chelated by the nitrogen-donor ligand, one terminal Pr i O ligand and the two isopropoxo bridges. The Mo coordination is distorted TBP in each case. 251 In the dimer [Mo2⊲ -NMe2⊳2⊲NMe2⊳2⊲OC6H10- 4Me⊳4] which also has five-coordinated Mo (TBP) the c-4-MeC6H10O ligands are all terminal. 252 Treatment of Mo2⊲NMe2⊳6 with perfluoro-tert-butanol gave the Mo Mo (2.216 ˚A) bonded centrosymmetric dimer [Mo2fOC⊲CF3⊳3g4⊲NMe2⊳2] having an anti, staggered rotational conformation and a planar C2NMo MoNC2 unit. 253 A similar conformation was exhibited by [Mo2⊲OCPh3⊳2⊲NMe2⊳4]. 300 With the hexafluoro-tert-butoxo ligand (hftb) the familiar non-bridged dinuclear molecule [Mo2⊲hftb⊳6] was obtained. 255 In the arylimido-bridged complex [Mo2⊲ - NAr⊳2⊲OBu t ⊳2] (Ar D 2,6-diisopropylphenyl), terminal tert-butoxo ligands give a distorted tetrahedral structure for this Mo(IV) compound (Mo–Mo, 2.654 ˚A). 256 In the metal–metal triply bonded (Mo Mo, 2.254 ˚A) dimer [Mo2⊲OBu t ⊳4⊲NHPh⊳2⊲NH2Ph⊳2] the eclipsed geometry is due to hydrogen bonding across the metal–metal bond. 257
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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 235 and 236: 234 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
Page 265 and 266: 264 Table 4.7 Alkoxides of lanthani
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 301 and 302: 300 Table 4.11 Alkoxides of chromiu
Page 303 and 304: 302 Table 4.11 (Continued) Metal M-
Page 317 and 318: 316 Table 4.11 (Continued) Metal M-
Page 323 and 324: 322 Table 4.12 Alkoxides of mangane
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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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Page 681 and 682:
Page 683 and 684:
Page 685 and 686:
Page 687 and 688:
688 Index alkoxometallate(IV) ligan
Page 689 and 690:
690 Index cerium oxo-isopropoxide 3
Page 691 and 692:
692 Index gas-phase photoelectron s
Page 693 and 694:
694 Index lead tert-butoxide 386 Le
Page 695 and 696:
696 Index metal-hydrogen bonds clea
Page 697 and 698:
698 Index oxo-alkoxides 384, 385, 3
Page 699 and 700:
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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