Reactivity of cyclooligophosphanes: Synthesis and structural characterisation of cyclo-1,4-(BH3)2(P4Ph 4CH2) and cyclo-1,2-(BH3)2(P 5Ph5)

Robert Wolf; Markus Finger; Carolin Limburg; Anthony C. Willis; S. Bruce Wild; Evamarie Hey-Hawkins

doi:10.1039/b511833f

Reactivity of cyclooligophosphanes: Synthesis and structural characterisation of cyclo-1,4-(BH₃)₂(P₄Ph ₄CH₂) and cyclo-1,2-(BH₃)₂(P ₅Ph₅)

Robert Wolf, Markus Finger, Carolin Limburg, Anthony C. Willis, S. Bruce Wild, Evamarie Hey-Hawkins^*

^*Corresponding author for this work

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

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Abstract

The borane complexes cyclo-1,4-(BH₃)₂(P ₄Ph₄CH₂) (3) and cyclo-1,2-(BH ₃)₂(P₅Ph₅) (4) were prepared by reaction of cyclo-(P₄Ph₄CH₂) and cyclo-(P ₅Ph₅) with BH₃(SMe₂). Only the 2: 1 complexes 3 and 4 were isolated, even when an excess of the borane source was used. In solution, 3 exists as a mixture of the two diastereomers (R _P*,S_P*,S_P*,R _P*)-(±)-3 and (R_P*,R _P*,R_P*,R_P*)-(±)-3. However, in the solid state the (R_P*,S_P*, S_P*,R_P*)-(±) diastereomer is the major stereoisomer. Similarly, while only one isomer of 4 is observed in its X-ray structure, NMR spectroscopic investigations reveal that it forms a complex mixture of isomers in solution. 3 may be deprotonated with ^tBuLi to give the lithium salt cyclo-1,4-(BH₃)₂(P ₄Ph₄CHLi) (3·Li), though this could not be isolated in pure form.

Original language	English
Pages (from-to)	831-837
Number of pages	7
Journal	Dalton Transactions
Issue number	6
DOIs	https://doi.org/10.1039/b511833f
Publication status	Published - 2006

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title = "Reactivity of cyclooligophosphanes: Synthesis and structural characterisation of cyclo-1,4-(BH3)2(P4Ph 4CH2) and cyclo-1,2-(BH3)2(P 5Ph5)",

abstract = "The borane complexes cyclo-1,4-(BH3)2(P 4Ph4CH2) (3) and cyclo-1,2-(BH 3)2(P5Ph5) (4) were prepared by reaction of cyclo-(P4Ph4CH2) and cyclo-(P 5Ph5) with BH3(SMe2). Only the 2: 1 complexes 3 and 4 were isolated, even when an excess of the borane source was used. In solution, 3 exists as a mixture of the two diastereomers (R P*,SP*,SP*,R P*)-(±)-3 and (RP*,R P*,RP*,RP*)-(±)-3. However, in the solid state the (RP*,SP*, SP*,RP*)-(±) diastereomer is the major stereoisomer. Similarly, while only one isomer of 4 is observed in its X-ray structure, NMR spectroscopic investigations reveal that it forms a complex mixture of isomers in solution. 3 may be deprotonated with tBuLi to give the lithium salt cyclo-1,4-(BH3)2(P 4Ph4CHLi) (3·Li), though this could not be isolated in pure form.",

author = "Robert Wolf and Markus Finger and Carolin Limburg and Willis, {Anthony C.} and Wild, {S. Bruce} and Evamarie Hey-Hawkins",

year = "2006",

doi = "10.1039/b511833f",

language = "English",

pages = "831--837",

journal = "Dalton Transactions",

issn = "1477-9226",

publisher = "Royal Society of Chemistry",

number = "6",

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TY - JOUR

T1 - Reactivity of cyclooligophosphanes

T2 - Synthesis and structural characterisation of cyclo-1,4-(BH3)2(P4Ph 4CH2) and cyclo-1,2-(BH3)2(P 5Ph5)

AU - Wolf, Robert

AU - Finger, Markus

AU - Limburg, Carolin

AU - Willis, Anthony C.

AU - Wild, S. Bruce

AU - Hey-Hawkins, Evamarie

PY - 2006

Y1 - 2006

N2 - The borane complexes cyclo-1,4-(BH3)2(P 4Ph4CH2) (3) and cyclo-1,2-(BH 3)2(P5Ph5) (4) were prepared by reaction of cyclo-(P4Ph4CH2) and cyclo-(P 5Ph5) with BH3(SMe2). Only the 2: 1 complexes 3 and 4 were isolated, even when an excess of the borane source was used. In solution, 3 exists as a mixture of the two diastereomers (R P*,SP*,SP*,R P*)-(±)-3 and (RP*,R P*,RP*,RP*)-(±)-3. However, in the solid state the (RP*,SP*, SP*,RP*)-(±) diastereomer is the major stereoisomer. Similarly, while only one isomer of 4 is observed in its X-ray structure, NMR spectroscopic investigations reveal that it forms a complex mixture of isomers in solution. 3 may be deprotonated with tBuLi to give the lithium salt cyclo-1,4-(BH3)2(P 4Ph4CHLi) (3·Li), though this could not be isolated in pure form.

AB - The borane complexes cyclo-1,4-(BH3)2(P 4Ph4CH2) (3) and cyclo-1,2-(BH 3)2(P5Ph5) (4) were prepared by reaction of cyclo-(P4Ph4CH2) and cyclo-(P 5Ph5) with BH3(SMe2). Only the 2: 1 complexes 3 and 4 were isolated, even when an excess of the borane source was used. In solution, 3 exists as a mixture of the two diastereomers (R P*,SP*,SP*,R P*)-(±)-3 and (RP*,R P*,RP*,RP*)-(±)-3. However, in the solid state the (RP*,SP*, SP*,RP*)-(±) diastereomer is the major stereoisomer. Similarly, while only one isomer of 4 is observed in its X-ray structure, NMR spectroscopic investigations reveal that it forms a complex mixture of isomers in solution. 3 may be deprotonated with tBuLi to give the lithium salt cyclo-1,4-(BH3)2(P 4Ph4CHLi) (3·Li), though this could not be isolated in pure form.

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U2 - 10.1039/b511833f

DO - 10.1039/b511833f

M3 - Article

SN - 1477-9226

SP - 831

EP - 837

JO - Dalton Transactions

JF - Dalton Transactions

IS - 6

ER -

Reactivity of cyclooligophosphanes: Synthesis and structural characterisation of cyclo-1,4-(BH₃)₂(P₄Ph ₄CH₂) and cyclo-1,2-(BH₃)₂(P ₅Ph₅)

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