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Synthesis, properties and structures of NbOF3 complexes and comparisons with NbOCl3 analogues

Synthesis, properties and structures of NbOF3 complexes and comparisons with NbOCl3 analogues
Synthesis, properties and structures of NbOF3 complexes and comparisons with NbOCl3 analogues
The first series of complexes of niobium(V) oxide trifluoride, [NbOF3(OPR3)2] (R = Me or Ph), [NbOF3(dppmO2)] (dppmO2 = Ph2P(O)CH2P(O)Ph2), [NbOF3(dmso)2], [NbOF3(tmeda)] (tmeda = Me2N(CH2)2NMe2) and [NbOF3(diimine)] (diimine = 2,2?-bipy, 1,10-phen) have been prepared, either by reaction of the corresponding complexes of NbF5 and hexamethyldisiloxane (HMDSO) in CH2Cl2–MeCN solution, or directly from NbF5, ligand and HMDSO. They were characterised by IR, 1H, 31P{1H} and 19F{1H} NMR spectroscopy, and X-ray crystal structures are reported for [NbOF3(OPR3)2] (R = Me or Ph) and [NbOF3(dppmO2)]. Complexes of NbOCl3, [NbOCl3(OPPh3)2], [NbOCl3(dppmO2)], [NbOCl3(dppeO2)] (dppeO2 = Ph2P(O)(CH2)2P(O)Ph2), [NbOCl3(tmeda)] and [NbOCl3(diimine)] were made from NbCl5 and HMDSO in MeCN (which forms [NbOCl3(MeCN)2] in situ), followed by addition of the neutral ligand. Their properties are compared with the oxide fluoride analogues. X-ray structures are reported for [NbOCl3(dppmO2)], [NbOCl3(dppeO2)], [NbOCl3(tmeda)] and [NbOCl3(2,2?-bipy)]. The synthesis and spectroscopic characterisation of [MF5L] (M = Nb or Ta; L = OPR3, OAsPh3) and [MF4(diimine)2][MF6] are also described, and the key properties of the four series of complexes compared.
0300-9246
3649-3659
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Trayer, Jonathan
d4e3ba19-d5c3-470a-8f3c-8ae337dff071
Zhang, Wenjian
1f80ac5e-d4c2-4720-b19e-be700cd411e7
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Trayer, Jonathan
d4e3ba19-d5c3-470a-8f3c-8ae337dff071
Zhang, Wenjian
1f80ac5e-d4c2-4720-b19e-be700cd411e7

Levason, William, Reid, Gillian, Trayer, Jonathan and Zhang, Wenjian (2014) Synthesis, properties and structures of NbOF3 complexes and comparisons with NbOCl3 analogues. Dalton Transactions, 43 (9), 3649-3659. (doi:10.1039/c3dt53322k).

Record type: Article

Abstract

The first series of complexes of niobium(V) oxide trifluoride, [NbOF3(OPR3)2] (R = Me or Ph), [NbOF3(dppmO2)] (dppmO2 = Ph2P(O)CH2P(O)Ph2), [NbOF3(dmso)2], [NbOF3(tmeda)] (tmeda = Me2N(CH2)2NMe2) and [NbOF3(diimine)] (diimine = 2,2?-bipy, 1,10-phen) have been prepared, either by reaction of the corresponding complexes of NbF5 and hexamethyldisiloxane (HMDSO) in CH2Cl2–MeCN solution, or directly from NbF5, ligand and HMDSO. They were characterised by IR, 1H, 31P{1H} and 19F{1H} NMR spectroscopy, and X-ray crystal structures are reported for [NbOF3(OPR3)2] (R = Me or Ph) and [NbOF3(dppmO2)]. Complexes of NbOCl3, [NbOCl3(OPPh3)2], [NbOCl3(dppmO2)], [NbOCl3(dppeO2)] (dppeO2 = Ph2P(O)(CH2)2P(O)Ph2), [NbOCl3(tmeda)] and [NbOCl3(diimine)] were made from NbCl5 and HMDSO in MeCN (which forms [NbOCl3(MeCN)2] in situ), followed by addition of the neutral ligand. Their properties are compared with the oxide fluoride analogues. X-ray structures are reported for [NbOCl3(dppmO2)], [NbOCl3(dppeO2)], [NbOCl3(tmeda)] and [NbOCl3(2,2?-bipy)]. The synthesis and spectroscopic characterisation of [MF5L] (M = Nb or Ta; L = OPR3, OAsPh3) and [MF4(diimine)2][MF6] are also described, and the key properties of the four series of complexes compared.

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e-pub ahead of print date: 3 January 2014
Published date: 7 March 2014
Organisations: Chemistry

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Local EPrints ID: 368638
URI: http://eprints.soton.ac.uk/id/eprint/368638
ISSN: 0300-9246
PURE UUID: 176b4b15-66b7-4e0a-bbda-3f93ca60dadf
ORCID for William Levason: ORCID iD orcid.org/0000-0003-3540-0971
ORCID for Gillian Reid: ORCID iD orcid.org/0000-0001-5349-3468

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Date deposited: 05 Sep 2014 11:01
Last modified: 18 Feb 2021 16:34

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Contributors

Author: William Levason ORCID iD
Author: Gillian Reid ORCID iD
Author: Jonathan Trayer
Author: Wenjian Zhang

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