New Fe(III) and Os(VI) silsesquioxanes

Patricia A. Shapley; W. Stuart Bigham; Michael T. Hay

doi:10.1016/S0020-1693(02)01346-4

New Fe(III) and Os(VI) silsesquioxanes

Patricia A. Shapley, W. Stuart Bigham, Michael T. Hay

Penn State Beaver

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Abstract

The high-spin iron(III) silsesquioxane complexes [N(ⁿBu)₄][(cyclo-C₅H₉) ₇Si₇O₁₂FeCl] and [N(ⁿBu)₄][(cyclo-C₅H₉) ₇Si₇O₁₂Fe(OSiMe₃)] result from the reaction of (cyclo-C₅H₉)₇Si₇O₉ (OH)₃ with either [N(ⁿBu)₄][FeCl₄] or [N(ⁿBu)₄][Fe(OSiMe₃)₄]. Substitution of the terminal chloride or (trimethyl)silanolate ligands with tert-butoxide produces [N(ⁿBu)₄][(cyclo-C₅H₉) ₇Si₇O₁₂Fe(OCMe₃)]. Similar substitution reactions with the methyl ester of N-acetylcysteine produce [N(ⁿBu)₄][(cyclo-C₅H₉) ₇Si₇O₁₂Fe(SCH₂CH(NHCOCH ₃)CO₂Me)]. A dimeric complex, [(cyclo-C₅H₉)₇Si₇O ₁₂Fe(NEt₃)]₂, forms in the reaction of (cyclo-C₅H₉)₇Si₇O₉ (OH)₃ with NEt₃ and FeCl₃. The reaction between (cyclo-C₅H₉)₇Si₇O₉ (OH)₂(OSiMe₃) and [Ph₄P][Os(N)Cl ₄] forms [PPh₄][(cyclo-C₅H₉)₇Si ₇O₁₁(OSiMe₃)Os(N)Cl₂], a square- pyramidal Os(VI) complex with a bidentate siloxy ligand.

Original language	English (US)
Pages (from-to)	255-260
Number of pages	6
Journal	Inorganica Chimica Acta
Volume	345
DOIs	https://doi.org/10.1016/S0020-1693(02)01346-4
State	Published - Mar 10 2003

All Science Journal Classification (ASJC) codes

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/S0020-1693(02)01346-4

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@article{62d748ae05134277af4885ac4681b855,

title = "New Fe(III) and Os(VI) silsesquioxanes",

abstract = "The high-spin iron(III) silsesquioxane complexes [N(nBu)4][(cyclo-C5H9) 7Si7O12FeCl] and [N(nBu)4][(cyclo-C5H9) 7Si7O12Fe(OSiMe3)] result from the reaction of (cyclo-C5H9)7Si7O9 (OH)3 with either [N(nBu)4][FeCl4] or [N(nBu)4][Fe(OSiMe3)4]. Substitution of the terminal chloride or (trimethyl)silanolate ligands with tert-butoxide produces [N(nBu)4][(cyclo-C5H9) 7Si7O12Fe(OCMe3)]. Similar substitution reactions with the methyl ester of N-acetylcysteine produce [N(nBu)4][(cyclo-C5H9) 7Si7O12Fe(SCH2CH(NHCOCH 3)CO2Me)]. A dimeric complex, [(cyclo-C5H9)7Si7O 12Fe(NEt3)]2, forms in the reaction of (cyclo-C5H9)7Si7O9 (OH)3 with NEt3 and FeCl3. The reaction between (cyclo-C5H9)7Si7O9 (OH)2(OSiMe3) and [Ph4P][Os(N)Cl 4] forms [PPh4][(cyclo-C5H9)7Si 7O11(OSiMe3)Os(N)Cl2], a square- pyramidal Os(VI) complex with a bidentate siloxy ligand.",

author = "Shapley, {Patricia A.} and Bigham, {W. Stuart} and Hay, {Michael T.}",

note = "Funding Information: We gratefully acknowledge the financial support of the Donors of The Petroleum Research Fund, administered by the American Chemical Society (ACS-PRF 36240-AC) and the United States EPA (EPA R 829553). NMR spectra were obtained in the Varian Oxford Instrument Center for Excellence in NMR Laboratory. Funding for this instrumentation was provided in part from the W.M. Keck Foundation, the National Institutes of Health (PHS 1 S10 RR10444-01), and the National Science Foundation (NSF CHE 96-10502). Purchase of the Siemens Platform/CCD diffractometer by the School of Chemical Sciences was supported by National Science Foundation grant CHE 9503145.",

year = "2003",

month = mar,

day = "10",

doi = "10.1016/S0020-1693(02)01346-4",

language = "English (US)",

volume = "345",

pages = "255--260",

journal = "Inorganica Chimica Acta",

issn = "0020-1693",

publisher = "Elsevier B.V.",

}

TY - JOUR

T1 - New Fe(III) and Os(VI) silsesquioxanes

AU - Shapley, Patricia A.

AU - Bigham, W. Stuart

AU - Hay, Michael T.

N1 - Funding Information: We gratefully acknowledge the financial support of the Donors of The Petroleum Research Fund, administered by the American Chemical Society (ACS-PRF 36240-AC) and the United States EPA (EPA R 829553). NMR spectra were obtained in the Varian Oxford Instrument Center for Excellence in NMR Laboratory. Funding for this instrumentation was provided in part from the W.M. Keck Foundation, the National Institutes of Health (PHS 1 S10 RR10444-01), and the National Science Foundation (NSF CHE 96-10502). Purchase of the Siemens Platform/CCD diffractometer by the School of Chemical Sciences was supported by National Science Foundation grant CHE 9503145.

PY - 2003/3/10

Y1 - 2003/3/10

N2 - The high-spin iron(III) silsesquioxane complexes [N(nBu)4][(cyclo-C5H9) 7Si7O12FeCl] and [N(nBu)4][(cyclo-C5H9) 7Si7O12Fe(OSiMe3)] result from the reaction of (cyclo-C5H9)7Si7O9 (OH)3 with either [N(nBu)4][FeCl4] or [N(nBu)4][Fe(OSiMe3)4]. Substitution of the terminal chloride or (trimethyl)silanolate ligands with tert-butoxide produces [N(nBu)4][(cyclo-C5H9) 7Si7O12Fe(OCMe3)]. Similar substitution reactions with the methyl ester of N-acetylcysteine produce [N(nBu)4][(cyclo-C5H9) 7Si7O12Fe(SCH2CH(NHCOCH 3)CO2Me)]. A dimeric complex, [(cyclo-C5H9)7Si7O 12Fe(NEt3)]2, forms in the reaction of (cyclo-C5H9)7Si7O9 (OH)3 with NEt3 and FeCl3. The reaction between (cyclo-C5H9)7Si7O9 (OH)2(OSiMe3) and [Ph4P][Os(N)Cl 4] forms [PPh4][(cyclo-C5H9)7Si 7O11(OSiMe3)Os(N)Cl2], a square- pyramidal Os(VI) complex with a bidentate siloxy ligand.

AB - The high-spin iron(III) silsesquioxane complexes [N(nBu)4][(cyclo-C5H9) 7Si7O12FeCl] and [N(nBu)4][(cyclo-C5H9) 7Si7O12Fe(OSiMe3)] result from the reaction of (cyclo-C5H9)7Si7O9 (OH)3 with either [N(nBu)4][FeCl4] or [N(nBu)4][Fe(OSiMe3)4]. Substitution of the terminal chloride or (trimethyl)silanolate ligands with tert-butoxide produces [N(nBu)4][(cyclo-C5H9) 7Si7O12Fe(OCMe3)]. Similar substitution reactions with the methyl ester of N-acetylcysteine produce [N(nBu)4][(cyclo-C5H9) 7Si7O12Fe(SCH2CH(NHCOCH 3)CO2Me)]. A dimeric complex, [(cyclo-C5H9)7Si7O 12Fe(NEt3)]2, forms in the reaction of (cyclo-C5H9)7Si7O9 (OH)3 with NEt3 and FeCl3. The reaction between (cyclo-C5H9)7Si7O9 (OH)2(OSiMe3) and [Ph4P][Os(N)Cl 4] forms [PPh4][(cyclo-C5H9)7Si 7O11(OSiMe3)Os(N)Cl2], a square- pyramidal Os(VI) complex with a bidentate siloxy ligand.

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U2 - 10.1016/S0020-1693(02)01346-4

DO - 10.1016/S0020-1693(02)01346-4

M3 - Article

AN - SCOPUS:0037430495

SN - 0020-1693

VL - 345

SP - 255

EP - 260

JO - Inorganica Chimica Acta

JF - Inorganica Chimica Acta

ER -

New Fe(III) and Os(VI) silsesquioxanes

Abstract

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