Dihydroxyoligosilanes as novel ligands in coordination chemistry - First synthesis of 2,5-dioxa-3,4-disilatitanacyclopentanes

Douglas Hoffmann; Helmut Reinke; Clemens Krempner

doi:10.1016/S0022-328X(02)01776-X

Dihydroxyoligosilanes as novel ligands in coordination chemistry - First synthesis of 2,5-dioxa-3,4-disilatitanacyclopentanes

Douglas Hoffmann, Helmut Reinke, Clemens Krempner

Chemistry and Biochemistry

Research output: Contribution to journal › Article › peer-review

21 Scopus citations

Abstract

The reaction of two equivalents of (Me₃Si)₂RSi-K x 3THF (1 R = SiMe₃, 2 R = Ph) with Cl₂MeSi-SiMeCl₂, followed by hydrolysis in the presence of NH₄(NH₂COO) leads to the formation of the dihydroxyoligosilanes MeR(HO)Si-Si(OH)RMe [4 R = Si(SiMe₃)₃, 6 R = Si(SiMe₃)₂Ph] as diastereomeric mixtures. Addition of two equivalents of n-BuLi to the diastereomerically pure ligands (meso)-4/6 and (rac )-4/6, respectively, and subsequent treatment with Cp₂TiCl₂ yields the (Z) and (E) arranged five-membered rings (MeRSi-O)₂TiCp₂ [7 R = Si(SiMe₃)₃, 8 R = Si(SiMe₃)₂Ph], respectively. The crystal structures of the ligand (rac)-6 as well as of the titanacycles (E)-8 and (Z)-7 are reported.

Original language	English
Pages (from-to)	1-8
Number of pages	8
Journal	Journal of Organometallic Chemistry
Volume	662
Issue number	1-2
DOIs	https://doi.org/10.1016/S0022-328X(02)01776-X
State	Published - Nov 15 2002

Keywords

Dihydroxydisilanes
Hexasilanes
Silicon
Titanacycles
Titanium

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10.1016/S0022-328X(02)01776-X

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title = "Dihydroxyoligosilanes as novel ligands in coordination chemistry - First synthesis of 2,5-dioxa-3,4-disilatitanacyclopentanes",

abstract = "The reaction of two equivalents of (Me3Si)2RSi-K x 3THF (1 R = SiMe3, 2 R = Ph) with Cl2MeSi-SiMeCl2, followed by hydrolysis in the presence of NH4(NH2COO) leads to the formation of the dihydroxyoligosilanes MeR(HO)Si-Si(OH)RMe [4 R = Si(SiMe3)3, 6 R = Si(SiMe3)2Ph] as diastereomeric mixtures. Addition of two equivalents of n-BuLi to the diastereomerically pure ligands (meso)-4/6 and (rac )-4/6, respectively, and subsequent treatment with Cp2TiCl2 yields the (Z) and (E) arranged five-membered rings (MeRSi-O)2TiCp2 [7 R = Si(SiMe3)3, 8 R = Si(SiMe3)2Ph], respectively. The crystal structures of the ligand (rac)-6 as well as of the titanacycles (E)-8 and (Z)-7 are reported.",

keywords = "Dihydroxydisilanes, Hexasilanes, Silicon, Titanacycles, Titanium",

author = "Douglas Hoffmann and Helmut Reinke and Clemens Krempner",

note = "Funding Information: We thank Prof. Dr. H. Oehme for his generous support and R. Kempe for carrying out the X-ray data collection for ( Z )- 7 and ( E )- 8 . We gratefully acknowledge the support of our research by the Deutsche Forschungsgemeinschaft and the Fonds der Chemischen Industrie. ",

year = "2002",

month = nov,

day = "15",

doi = "10.1016/S0022-328X(02)01776-X",

language = "English",

volume = "662",

pages = "1--8",

journal = "Journal of Organometallic Chemistry",

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number = "1-2",

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T1 - Dihydroxyoligosilanes as novel ligands in coordination chemistry - First synthesis of 2,5-dioxa-3,4-disilatitanacyclopentanes

AU - Hoffmann, Douglas

AU - Reinke, Helmut

AU - Krempner, Clemens

N1 - Funding Information: We thank Prof. Dr. H. Oehme for his generous support and R. Kempe for carrying out the X-ray data collection for ( Z )- 7 and ( E )- 8 . We gratefully acknowledge the support of our research by the Deutsche Forschungsgemeinschaft and the Fonds der Chemischen Industrie.

PY - 2002/11/15

Y1 - 2002/11/15

N2 - The reaction of two equivalents of (Me3Si)2RSi-K x 3THF (1 R = SiMe3, 2 R = Ph) with Cl2MeSi-SiMeCl2, followed by hydrolysis in the presence of NH4(NH2COO) leads to the formation of the dihydroxyoligosilanes MeR(HO)Si-Si(OH)RMe [4 R = Si(SiMe3)3, 6 R = Si(SiMe3)2Ph] as diastereomeric mixtures. Addition of two equivalents of n-BuLi to the diastereomerically pure ligands (meso)-4/6 and (rac )-4/6, respectively, and subsequent treatment with Cp2TiCl2 yields the (Z) and (E) arranged five-membered rings (MeRSi-O)2TiCp2 [7 R = Si(SiMe3)3, 8 R = Si(SiMe3)2Ph], respectively. The crystal structures of the ligand (rac)-6 as well as of the titanacycles (E)-8 and (Z)-7 are reported.

AB - The reaction of two equivalents of (Me3Si)2RSi-K x 3THF (1 R = SiMe3, 2 R = Ph) with Cl2MeSi-SiMeCl2, followed by hydrolysis in the presence of NH4(NH2COO) leads to the formation of the dihydroxyoligosilanes MeR(HO)Si-Si(OH)RMe [4 R = Si(SiMe3)3, 6 R = Si(SiMe3)2Ph] as diastereomeric mixtures. Addition of two equivalents of n-BuLi to the diastereomerically pure ligands (meso)-4/6 and (rac )-4/6, respectively, and subsequent treatment with Cp2TiCl2 yields the (Z) and (E) arranged five-membered rings (MeRSi-O)2TiCp2 [7 R = Si(SiMe3)3, 8 R = Si(SiMe3)2Ph], respectively. The crystal structures of the ligand (rac)-6 as well as of the titanacycles (E)-8 and (Z)-7 are reported.

KW - Dihydroxydisilanes

KW - Hexasilanes

KW - Silicon

KW - Titanacycles

KW - Titanium

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U2 - 10.1016/S0022-328X(02)01776-X

DO - 10.1016/S0022-328X(02)01776-X

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AN - SCOPUS:0037111765

SN - 0022-328X

VL - 662

SP - 1

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JO - Journal of Organometallic Chemistry

JF - Journal of Organometallic Chemistry

IS - 1-2

ER -

Dihydroxyoligosilanes as novel ligands in coordination chemistry - First synthesis of 2,5-dioxa-3,4-disilatitanacyclopentanes

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