2 Homometallic Alkoxides

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325 Table 4.14 <strong>Alkoxides</strong> of nickel, palladium, and platinum M–O Bond lengths ( ˚A) Metal Bond angles ( Ž ) Compound coordination Terminal Bridging � MOC Reference [Ni4⊲ -OMe⊳4⊲MeOH⊳4⊲OC6H4CHO⊳4] 6 2.099 (9) (MeOH) 2.019, 2.043, 117.2, 120.7, 400 2.054 (8) 120.8 (b) [Ni2fOC⊲CF3⊳2CH2CMeDN⊲CH2⊳6NDCMeCH2C⊲CF3⊳2Og2] 4 1.841, 1.843 (2) – – 401 [NifO2C2⊲CF3⊳4g2] 2 4 1.852 (3) – 111.8 402 [Ni4⊲ -OMe⊳4⊲MeOH⊳4⊲OC6H2Cl3⊳4] 6 2.06–2.09 (MeOH) 2.02–2.08 118–123 403 av. 2.08 av. 2.04 [NifOC⊲CF3⊳2CH2C(Me)DNC2H4C6H4Ng2] 6 2.086 (4) – 126.6 404 [NifOC⊲CF3⊳2CH2PPh2g2] 4 1.837–1.844 (7) av. 1.839 – 121.1–123.9 405 [NifO2C⊲CF3⊳2gL] L D cyclo-NDC(Me)CH2C(Me) 2NH⊲C3H6⊳NH⊲C3H6⊳ [NifOC⊲CF3⊳2CH2C(O)DCHC⊲CF3⊳2OHg⊲Me2NC2H4NMe2⊳] [Ni4⊲ -OMe⊳4⊲MeOH⊳4fPhCO(CH)COPhg4] 5 4 6 2.037, 2.039 (4) 1.825, 1.897 – – – 2.015–2.072 (9) av. 2.045 91.1, 91.4 119.4, 123.1 – 406 407 408 [PdfOC⊲CF3⊳2CH2PPh2gCl⊲PMe2Ph⊳] 4 2.046 (2) – 122.7 409 [PdfOC⊲CF3⊳2C6H4SMegCl⊲PMePh2⊳] 4 2.053 (3) – 125.0 410 [Pt⊲OMe⊳2⊲Ph2PC2H4PPh2⊳] 4 2.037, 2.041 (7) – 117.0, 121.0 411 [Pt(OMe)Me⊲Ph2PC2H4PPh2⊳] 4 1.990 (10) – 119 411 [PtfOC⊲CF3⊳2CH2SMeg⊲PPh3⊳2]⊲BF4⊳ 4 2.041 (5) – 121.2 412 [PtfOC⊲CF3⊳2CH2SMeg⊲PMePh2⊳]⊲BF4⊳ 4 2.058 (6) – 117.3 412 [PtfOC⊲CF3⊳2CH2PPh2g2] 4 2.030–2.034 (6) – – 413 [PtfO2C⊲CF3⊳2g⊲PPh3⊳2] 4 2.040, 2.056 (5) – 91.8, 92.2 414 [Pt⊲OCH2CH2PPh2⊳2] 4 2.039 (5) – 114.8 416 [PtfOCH⊲CF3⊳2gMe⊲PMe3⊳2] 4 2.07 (1) – 125.3 417 [PtfOCH⊲CF3⊳2gfHOCH⊲CF3⊳2gMe⊲PMe3⊳2] 4 2.07 (3) – 123 418 [Pt(D-mannitolate)(DPPP)] 4 2.033, 2.042 (9) – – 419 b D bridging.
326 Alkoxo and Aryloxo Derivatives of Metals Ni(II) atom is chelated by a salicylaldehydato ligand and with one coordinated methanol achieves an octahedral configuration (Table 4.14, p. 325). 400 The tetradentate iminoalkoxo ligand formed from the template reaction of ⊲CF3⊳2C⊲OH⊳CH2COMe with the diamine NH2⊲CH2⊳6NH2 gave a dimeric Ni(II) complex [Ni2f - OC⊲CF3⊳2CH2CMeDN⊲CH2⊳6NDCMeCH2C⊲CF3⊳2⊳2Og2] in which the two square planar (trans-O2N2) nickel units are linked by N⊲CH2⊳6N moieties. 401 A mononuclear square planar complex was also found in the anion of K2[NifO2C2⊲CF3⊳4g2]. 4H2O in which the perfluoropinacolato ligands are chelating. 402 Another tetranuclear complex with the cubane-like Ni4⊲ -OMe⊳4 core was established in [Ni4⊲ -OMe⊳4⊲MeOH⊳⊲OC6H2Cl3-2,4,6⊳], where the 2,4,6-trichlorophenoxo group acts as an O, Cl chelating ligand to complete the octahedral coordination of the nickel. 403 Template condensation of MeC⊲O⊳CH2C⊲CF3⊳2OH with NC5H4CH2CH2NH2 gave rise to the octahedral complex [NifOC⊲CF3⊳2CH2C⊲Me⊳DNCH2CH2C6H4Ng2]. The tridentate chelating ligands occupy facial configurations. 404 The phosphino functionalized fluorinated alkoxo ligand PPh2CH2C⊲CF3⊳2O gave the mononuclear trans-square planar chelated Ni(II) complex [NifOC⊲CF3⊳2CH2PPh2g2]. 405 A five-coordinated complex was formed using the chelating fluorinated diol ⊲CF3⊳2CO 2 2 and the tridentate triaza-macrocyle 2,2,4-trimethyl-1,5,9-triaza- cyclododec-1-ene ligand L in [NifO2C⊲CF3⊳2⊳gL]. A distorted square pyramidal configuration was found and the four-membered NiOCO chelate ring led to acute Ni � OC bond angles (91 Ž ). 406 The potentially tridentate fluorinated ketodiol ⊲CF3⊳2C⊲OH⊳CH2C⊲O⊳CH2C⊲CF3⊳2OH acts as a bidentate chelating ligand in the square planar complex [NifOC⊲CF3⊳2CH2C⊲O⊳DCHC⊲CF3⊳2OHg⊲tmed⊳]⊲tmed D Me2NC2H4NMe2). 407 Another tetranuclear cubane-like structure was found in [Ni4⊲ -OMe⊳4⊲MeOH⊳4⊲dbm⊳4] (dbm D PhCO(CH)COPh). 408 2.15.2 Palladium and Platinum Some square planar Pd(II) complexes involving functionalized fluorinated alkoxo ligands have also been characterized: e.g. [PdfOC⊲CF3⊳2CH2PPh2gCl⊲PMe2Ph⊳], 409 [PdfOC⊲CF3⊳2C6H4SMeg⊲PMePh2⊳Cl]. 410 Several square planar Pt(II) complexes have been structurally characterized such as the bis-phosphine-stabilized methoxo compounds [Pt⊲OMe⊳2⊲Ph2PC2H4PPh2⊳] and [Pt⊲OMe⊳Me⊲Ph2PC2H4PPh2⊳]. 411 The functionalized fluorinated alkoxo ligands are also well represented in [PtfOC⊲CF3⊳2CH2SMeg⊲PPh3⊳2] C ⊲BF4⊳ , [PtfOC⊲CF3⊳2CH2SMeg⊲PMePh2⊳2] C ⊲BF4⊳ , 412 [cis-PtfOC⊲CF3⊳2CH2PPh2g2] 413 and [PtfO2C⊲CF3⊳2g⊲PPh3⊳2]. 414 Complexes of nonfluorinated phosphino alkoxo ligands have also revealed square planar Pt(II) as in [PtfOCMe2CH2PPh2g2] 415 and [Pt⊲OCH2CH2PPh2⊳2]. 416 The stability of chelate-alkoxo complexes was deemed to be kinetic in origin. Interestingly the cis-complex [PtfOCH⊲CF3⊳2gMe⊲PMe3⊳2] 417 readily forms the hydrogen-bonded adduct [PtfOCH⊲CF3⊳2gfHOCH⊲CF3⊳2gMe⊲PMe3⊳2] 418 but the Pt–O bond length (2.07 ˚A) is the same in each molecule. In the structure of [Pt(Dmannitolate)(dppp)] (dppp D Ph2P⊲CH2⊳3PPh2) the mannitolate ligand is bonded to Pt by the oxygens on C(3) and C(4) giving a 2,5-dioxaplatinacyclopentane chelate ring. 419
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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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Page 275 and 276: 274 Alkoxo and Aryloxo Derivatives
Page 277 and 278: 276 Table 4.9 Alkoxides of titanium
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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-
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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
Page 665 and 666:
Metal Aryloxides 665 405. P.N. Rile
Page 667 and 668:
Metal Aryloxides 667 483. Y. Hayash
Page 669 and 670:
Metal Aryloxides 669 561. A.P. Shre
Page 671 and 672:
Page 673 and 674:
Page 675 and 676:
Page 677 and 678:
Page 679 and 680:
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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