2 Homometallic Alkoxides

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X-Ray Crystal Structures of Alkoxo Metal Compounds 337 In the Cr(II) complex [Na4Cr2⊲ 3-OPr i ⊳8⊲thf⊳4] the two chromiums are in axial positions and the four sodiums in the equatorial positions of an octahedron with triplebridging Pr i O ligands capping the eight faces. Each Cr atom is above the plane of its four bridging Pr i O ligands whilst each Na achieves five-coordination by virtue of the terminally bound THF ligand. 475 In the sodium chromium(II) bis-disiloxanediolate [⊲thf⊳4Na2f -O⊲SiPh2O⊳2g2Cr] the Na ions are four-coordinated and the chromiums square planar. 476 In the hydrido complex [⊲diglyme⊳Na⊲ -H⊳⊲ -OPr i ⊳4W2⊲OPr i ⊳4] (W–W, 2.431 ˚A) there is a confacial bi-octahedral W2⊲ -H⊳⊲ -OPr i ⊳2 core with the five-coordinated Na bridging two apices of this unit. 313 A cubane-like NaTc3O4 core is present in [Na⊲ 3-OMe⊳4fTc⊲CO⊳3g3] wherethe octahedral coordination of each Tc atom is completed by three terminal carbonyl ligands. 477 In the Cu(II) complex [Na2f -OCH⊲CF3⊳2g4Cu] the sodium ions are edge bridged with a near square planar CuO4 unit but five fluorines are involved in Na....F agostic interactions. 478 The octanuclear compound [Na4Cu4⊲ 3-OCEt3⊳4⊲ -OCEt3⊳4] has a structure similar to that of [Li4Cu4⊲OBu t ⊳8] (Fig. 4.59) with linear two-coordinated Cu(I). 465 The sodium tin(II) tert-butoxide [Na2⊲ 3-OBu t ⊳2⊲ -OBu t ⊳4Sn], like its lithium analogue, has the Sn2O6M2 cage comprising two seco-norcubane Sn2M2O3 units sharing a Na2O2 four-membered ring. 468 By contrast the bridging-chelating ligand ⊲Bu t O⊳3SiO gave rise to the dinuclear species [Naf , 2 -OSi⊲OBu t ⊳3g3Pb] and [Kf , 2 -OSi⊲OBu t ⊳3g3Sn] in which the alkali metal is six-coordinated and the heterometal is three-coordinated (pyramidal). 484 3.1.3 Potassium Various potassium metal alkoxides have been structurally characterized. One of the first examples reported was the homoleptic complex [K⊲ 3-OBu t ⊳2⊲ -OBu t ⊳3U2⊲OBu t ⊳4] which has the confacial bioctahedral U2O9 framework with the K ion occupying a pocket between the two uranium(IV) atoms(U–U, 3.631 ˚A). 151 In [K⊲ 3-OPr i ⊳⊲ -OPr i ⊳3Ti⊲OPr i ⊳]n both metals are five-coordinated and alternate in infinite zig-zag chains significantly different in structure from the analogous [NaTi⊲OPr i ⊳5]n. 473 A novel structure is exhibited by [⊲py⊳2K2⊲ -OCH2But⊳8M2] (MDMo, W). The bimetallic core (Mo–Mo, 2.257 ˚A; W–W, 2.335 ˚A) is encapsulated in a pseudo-O8 cube of alkoxo oxygens which are bridged to the two potassiums on opposite faces. 259 By contrast in [M2⊲ 3-OBu t ⊳2⊲ -OBu t ⊳4Zn2] (MDNa, K) the three-coordinated alkali metals are located above and below the Zn2O2 plane. 479 In potassium aluminium isopropoxide isopropanolate [⊲PriOH⊳2K⊲ -OPr i ⊳4Al]n the alternating K and Al atoms are joined by double isopropoxo bridges in a zig-zag linear chain. The two coordinated isopropanols give the potassium a distorted octahedral configuration whilst the Al is distorted tetrahedral. 480 In the Sn(II) complex [K⊲ 3-OBu t ⊳2⊲ -OBu t ⊳Sn]n both metals are in distorted five-coordinated configurations in a polymeric structure of alternating potassium and tin atoms linked by bridging alkoxo groups in a structure different from the Li and Na analogues. 468 The binuclear potassium tin(II) triphenylsiloxide exists in two forms both containing the K⊲ -OSiPh3⊳3Sn unit with three-coordinated tin. In
338 Alkoxo and Aryloxo Derivatives of Metals one form (monoclinic) the potassium is further coordinated by two chelating DME ⊲CH3OC2H4OMe⊳ ligands and in the other (triclinic) the K ion is bonded to one bidentate and one monodentate DME. 481 With Sn(IV) a helical polymer chain is formed of alternating four-coordinated K and five-coordinated (TBP) Sn linked by double alkoxo bridges [K⊲ -OBu t ⊳4Sn⊲OBu t ⊳]n. 482 With the tervalent non-transition metals Sb and Bi the chain polymers [K⊲ -OBu t ⊳4M 0 ]n (M 0 D Sb, Bi) and formed; the KO4 units have square planar configurations and the M 0 O4 units display 9-trigonal bipyramidal structures. 483 In [⊲ , 2 -dioxane⊳K2⊲ 3-OBu t ⊳2⊲ -OBu t ⊳3Sb] the K2SbO5 unit involves a trigonal pyramid of oxygens with the metal ions inserted in the three equatorial edges giving four-coordinated Sb(II) atoms. The dioxane ligands bridge across the K2SbO5 units to generate a polymer and give the potassium atoms five-coordination. 483 3.2 Magnesium, Strontium, or Barium Bimetallic <strong>Alkoxides</strong> 3.2.1 Magnesium Several magnesium heterometal alkoxides have been reported. The complex [⊲ 2 -dioxane⊳2Mg⊲ -OMe⊳4Al2Me4]n (Table 4.18, pp. 348–352) is an infinite polymer in which the trinuclear MgAl 2 O4 units are crosslinked by bridging dioxane ligands giving the Mg atom an octahedral configuration and the Al atoms a pseudo-tetrahedral coordination. 485 In the hexanuclear complex [Mg 2 ⊲ 3-OEt⊳4⊲ -OEt⊳4⊲ -Cl⊳4Ti4⊲OEt⊳8] all of the metals are in distorted octahedral configurations with the two halves of the molecule held together by an edge-sharing Mg 2 ⊲ -Cl⊳2 bridge. 486 A large family of trinuclear molecules [M 0 ⊲ -OBu t ⊳3M⊲ -OBu t ⊳3M 0 ](MD Mg, Ca, Sr, Ba; M 0 D Ge, Sn, Pb) has been reported. The central metal, as in [Ge⊲OBu t ⊳3Mg⊲OBu t ⊳3Ge], is octahedral and the outer metals are three-coordinated (pyramidal). 487 An interesting variation on this theme is the linear tetranuclear bimetallic homoleptic complexes [Bu t O⊳M 0 ⊲ -OBu t ⊳2M⊲ -OBu t ⊳2M⊲ -OBu t ⊳2M 0 ⊲OBu t ⊳], (M D Mg, M 0 D Sn; M D Cr, M 0 D Sn; M D Mn, M 0 D Sn; M D Co, M 0 D Ge, Sn; M D Ni, M 0 D Ge, Sn) in which M is in a distorted tetrahedral configuration and M 0 is three-coordinated (pyramidal). 523 Also of special interest are the pentanuclear trimetallic mixed ligand alkoxo complexes [Mf⊲ -OBu t ⊳3M 0 M 00 ⊲CO⊳x g2] (MD Sr, M 0 D Sn, M 00 D Fe, x D 4; M D Ba, M 0 D Sn, M 00 D Cr, x D 5) in which the central metal M is octahedrally coordinated whilst M 0 and M 00 are joined by a metal–metal bond. 524 The homoleptic hexanuclear magnesium antimony(III) complex [Mg 2 ⊲ 3-OEt⊳2⊲ - OEt⊳8Sb4⊲OEt⊳6] has a core of two edge-sharing MgO 6 octahedra with edge-bridging (EtO)Sb⊲ -OEt⊳2 units chelating each Mg and tridentate EtOSb⊲ 3-OEt⊳⊲ -OEt⊳2 units bridging the two Mg atoms. 488 The “bent” ⊲Al �MgAl D 141.6 Ž ⊳ trinuclear complex [⊲Pr i OH⊳2Mg⊲ -OPr i ⊳4Al2⊲OPr i ⊳4] hascis-octahedral Mg and tetrahedral Al. 489 One of the terminal Pr i O groups on each Al is hydrogen bonded to a Pr i OH which is coordinated to the magnesium. 3.2.2 Strontium Strontium, cadmium, and hafnium are present in the remarkable trimetallic octanuclear complex [Sr2Cd2Hf4⊲OPr i ⊳24] (Fig. 4.61). 200 This centrosymmetric molecule has
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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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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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Page 287 and 288: 286 Alkoxo and Aryloxo Derivatives
Page 301 and 302: 300 Table 4.11 Alkoxides of chromiu
Page 303 and 304: 302 Table 4.11 (Continued) Metal M-
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Page 323 and 324: 322 Table 4.12 Alkoxides of mangane
Page 333 and 334: 332 Table 4.16 Alkoxides of zinc, c
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Page 341 and 342: 340 Table 4.17 (Continued) Coordina
Page 349 and 350: 348 Table 4.18 Bimetallic alkoxides
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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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