Ferrous tris(trimethylsilyl) silanolates: synthesis, structure, reactivity and thermal decomposition

Kornev, A. N.; Chesnokova, T. A.; Семенов, В. В.; Zhezlova, E. V.; Zakharov, L. N.; Klapshina, Larisa G.; Домрачев, Г. А.; Rusakov, V. S.

doi:10.1016/s0022-328x(97)00213-1

Cited by 28 publications

(14 citation statements)

References 8 publications

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“…Few other examples of sodium and iron(II) heterobimetallic dimers are known. 57,60 The structures of the [Fe(L iPr ) 2 ] and [Zn(L iPr ) 2 ] reveal isomorphous four-coordinate divalent metal centers each supported by two bidentate b-ketoiminate ligands (Fig. 1, Tables 1 and 2).…”

Section: Resultsmentioning

confidence: 99%

Synthesis and Characterization of Sterically Encumbered β-Ketoiminate Complexes of Iron(ii) and Zinc(ii)

Granum

Riedel

Crawford³

et al. 2011

Dalton Trans.

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The synthesis, structure, and spectroscopic signatures of a series of four-coordinate iron(II) complexes of β-ketoiminates and their zinc(II) analogues are presented. An unusual five-coordinate iron(II) triflate with three oxygen bound protonated β-ketoimines is also synthesized and structurally characterized. Single-crystal X-ray crystallographic analysis reveals that the deprotonated bis(chelate)metal complexes are four-coordinate with various degrees of distortion depending on the degree of steric bulk and the electronics of the metal center. Each of the high-spin iron(II) centers exhibits multiple electronic transitions including ligand π to π*, metal-to-ligand charge transfer, and spin-forbidden d-d bands. The (1)H NMR spectra of the paramagnetic high-spin iron(II) centers are assigned on the basis of chemical shifts, longitudinal relaxation times (T(1)), relative integrations, and substitution of the ligands. The electrochemical studies support variations in the ligand strength. Parallel mode EPR measurements for the isopropyl substituted ligand complex of iron(II) show low-field resonances (g > 9.5) indicative of complex aggregation or crystallite formation. No suitable solvent system or glassing mixture was found to remedy this phenomenon. However, the bulkier diisopropylphenyl substituted ligand exhibits an integer spin signal consistent with an isolated iron(ii) center [S = 2; D = -7.1 ± 0.8 cm(-1); E/D = 0.1]. A tentative molecular orbital diagram is assembled.

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Section: Resultsmentioning

confidence: 99%

Synthesis and Characterization of Sterically Encumbered β-Ketoiminate Complexes of Iron(ii) and Zinc(ii)

Granum

Riedel

Crawford³

et al. 2011

Dalton Trans.

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“…A search for a tri(organosilyl)siloxy ligand attached to a metal produced six unique hits. These include Fe II and Co II complexes (Kornev et al, 1997 andChesnokova et al, 2002), lanthanide(III) complexes (Kornev et al, 1999), and Ta V complexes (Wu et al, 2002).…”

Section: Database Surveymentioning

confidence: 99%

Potassium chloridotris(hypersiloxy)aluminate dimer

Purdy

Butcher

2019

Acta Cryst E

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The tris(trimethylsilylsiloxide) ligand, also known as hypersiloxide, is an extremely bulky group. In an attempt to make the monomeric Al(OSi(SiMe3)3)3, AlCl3 was combined with 3 equiv. of potassium hypersiloxide. The crystalline product isolated (40% yield), namely di-μ3-chlorido-bis[μ2-tris(trimethylsilyl)silanolato]tetrakis[tris(trimethylsilyl)silanolato]dialuminiumdipotassium, [Al2K2Cl2(C19H27OSi4)6], is a KCl adduct of aluminium tris(hypersilyloxide) that is dimerized through a planar K2Cl2 ring, with K—Cl distances of 3.1131 (8) and 3.319 (3) Å, and ring angles of 77.41 (2) and 102.60 (2)°. This ring is on an inversion center, and there is no supramolecular coordination.

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“…Die einzige weitere strukturell untersuchte Verbindung mit einer Fe±O±Si-Einheit im Moleku È l ist das heterobimetallische Eisen(II)-Derivat (Me 3 Si) 3 SiOFe[l-OSi(SiMe 3 ) 3 ] 2 Na-(DME) (5) [16]. Hier betragen die Fe±O-Absta È nde zu den verbru È ckenden Silanolat-Liganden 184.0(2) bzw.…”

Section: Ergebnisse Und Diskussionunclassified

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Lorenz

Fischer

Edelmann

2000

Z. anorg. allg. Chem.

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Cy 7 Si 7 O 12 Fe(tmeda) (3, Cy = cyclohexyl, tmeda = N,N,N', has been prepared by reacting in situ generated Cy 7 Si 7 O 9 (OLi) 3 (2) with anhydrous FeCl 3 followed by treatment with tmeda. Pale yellow crystalline 3 represents the first example of a metallasilsesquioxane in which a late transition metal is incorporated into a silsesquioxane cage. The compound crystallizes as discrete monomers in which the coordination sphere around Fe is saturated by addition of a chelating tmeda ligand (3: monoclinic space group Cc, Z = 4, lattice dimensions at ±100°C: a = 2469.0(2), b = 1529.9(2), c = 1010.4(2) pm, b = 116.68(1)°, R = 0.052).

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Ferrous tris(trimethylsilyl) silanolates: synthesis, structure, reactivity and thermal decomposition

Cited by 28 publications

References 8 publications

Synthesis and Characterization of Sterically Encumbered β-Ketoiminate Complexes of Iron(ii) and Zinc(ii)

Synthesis and Characterization of Sterically Encumbered β-Ketoiminate Complexes of Iron(ii) and Zinc(ii)

Potassium chloridotris(hypersiloxy)aluminate dimer

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