Platinum bis(phosphine) complexes of 1,8-naphthosultam

Louise M. Diamond; Fergus R. Knight; Rebecca A. M. Randall; Amy L. Fuller; Alexandra M. Z. Slawin; J. Derek Woollins

doi:10.1016/j.ica.2014.08.048

Platinum bis(phosphine) complexes of 1,8-naphthosultam

Louise M. Diamond, Fergus R. Knight, Rebecca A. M. Randall, Amy L. Fuller, Alexandra M. Z. Slawin, J. Derek Woollins^*

^*Corresponding author for this work

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

Abstract

A series of bis(phosphine) platinum complexes 1-4 and 6-8 that bear the 1,8-naphthosultam ligand (L) have been synthesised. The nitrogen atom in L was deprotonated with sodium tert-butoxide to form the sodium salt. Metathetical reaction of the sodium salt (1 eq.) with the appropriate cis-dichlorobis(phosphine) platinum (1 eq.) in THF resulted in the formation of platinum complexes [Pt(PR₃)₂(L)Cl] (R₃ = Ph₃; 1, Ph₂Me; 2, PhMe₂; 3, Me₃; 4), whilst reaction with [Pt(COD)Cl₂] afforded [Pt(COD)(L)Cl] (5). The corresponding reaction employing two equivalents of L, two equivalents of NaOtBu and one equivalent of [Pt(PR₃)₂Cl₂]/[Pt(COD)Cl₂] yielded complexes [Pt(PR₃)₂(L)₂] (R₃ = Ph₂Me; 6, PhMe₂; 7, Me₃; 8) and [Pt(COD)(L)₂] (9). L, 1, 5 and 9 have been fully characterised, principally by multinuclear magnetic resonance and IR spectroscopy and mass spectrometry, the remaining members of the series were analysed by ³¹P NMR only. Unsymmetrical complexes 1-4 provide examples of AX spin systems, with appropriate satellites attributed to ³¹P NMR-¹⁹⁵Pt coupling. X-ray structures determined for 1,8-naphthosultam L, and complexes 1, 5 and 9 and where appropriate the platinum metal geometry, N-S distance and ligand distortions were compared.

Original language	English
Pages (from-to)	313-319
Number of pages	7
Journal	Inorganica Chimica Acta
Volume	423
Issue number	Part A
Early online date	6 Sept 2014
DOIs	https://doi.org/10.1016/j.ica.2014.08.048
Publication status	Published - 1 Nov 2014

Keywords

Platinum
Naphthalene
Sulfam
Complex
X-ray structure
Ray-diffraction data
X-ray
Metal tetrathiolenes
Arenethiolatocopper(I) complexes
Crystal-structures
Ligands
Coordination
Cod
Tetrathionaphthalene

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Inorg Chim Acta_revised
Copyright © 2014 Elsevier B.V. All rights reserved. NOTICE: this is the author’s version of a work that was accepted for publication in Inorganica Chimica Acta. Changes resulting from the publishing process, such as peer review, editing, corrections, structural formatting, and other quality control mechanisms may not be reflected in this document. Changes may have been made to this work since it was submitted for publication. A definitive version was subsequently published in Inorganica Chimica Acta, 423 (Part A), 2014, doi:10.1016/j.ica.2014.08.048
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@article{9e80c446d42149f1a932963a0543eb7f,

title = "Platinum bis(phosphine) complexes of 1,8-naphthosultam",

abstract = "A series of bis(phosphine) platinum complexes 1-4 and 6-8 that bear the 1,8-naphthosultam ligand (L) have been synthesised. The nitrogen atom in L was deprotonated with sodium tert-butoxide to form the sodium salt. Metathetical reaction of the sodium salt (1 eq.) with the appropriate cis-dichlorobis(phosphine) platinum (1 eq.) in THF resulted in the formation of platinum complexes [Pt(PR3)2(L)Cl] (R3 = Ph3; 1, Ph2Me; 2, PhMe2; 3, Me3; 4), whilst reaction with [Pt(COD)Cl2] afforded [Pt(COD)(L)Cl] (5). The corresponding reaction employing two equivalents of L, two equivalents of NaOtBu and one equivalent of [Pt(PR3)2Cl2]/[Pt(COD)Cl2] yielded complexes [Pt(PR3)2(L)2] (R3 = Ph2Me; 6, PhMe2; 7, Me3; 8) and [Pt(COD)(L)2] (9). L, 1, 5 and 9 have been fully characterised, principally by multinuclear magnetic resonance and IR spectroscopy and mass spectrometry, the remaining members of the series were analysed by 31P NMR only. Unsymmetrical complexes 1-4 provide examples of AX spin systems, with appropriate satellites attributed to 31P NMR-195Pt coupling. X-ray structures determined for 1,8-naphthosultam L, and complexes 1, 5 and 9 and where appropriate the platinum metal geometry, N-S distance and ligand distortions were compared.",

keywords = "Platinum, Naphthalene, Sulfam, Complex, X-ray structure, Ray-diffraction data, X-ray, Metal tetrathiolenes, Arenethiolatocopper(I) complexes, Crystal-structures, Ligands, Coordination, Cod, Tetrathionaphthalene",

author = "Diamond, \{Louise M.\} and Knight, \{Fergus R.\} and Randall, \{Rebecca A. M.\} and Fuller, \{Amy L.\} and Slawin, \{Alexandra M. Z.\} and Woollins, \{J. Derek\}",

note = "The work in this project was supported by the Engineering and Physical Sciences Research Council (EPSRC). ",

year = "2014",

month = nov,

day = "1",

doi = "10.1016/j.ica.2014.08.048",

language = "English",

volume = "423",

pages = "313--319",

journal = "Inorganica Chimica Acta",

issn = "0020-1693",

publisher = "Elsevier",

number = "Part A",

}

TY - JOUR

T1 - Platinum bis(phosphine) complexes of 1,8-naphthosultam

AU - Diamond, Louise M.

AU - Knight, Fergus R.

AU - Randall, Rebecca A. M.

AU - Fuller, Amy L.

AU - Slawin, Alexandra M. Z.

AU - Woollins, J. Derek

N1 - The work in this project was supported by the Engineering and Physical Sciences Research Council (EPSRC).

PY - 2014/11/1

Y1 - 2014/11/1

N2 - A series of bis(phosphine) platinum complexes 1-4 and 6-8 that bear the 1,8-naphthosultam ligand (L) have been synthesised. The nitrogen atom in L was deprotonated with sodium tert-butoxide to form the sodium salt. Metathetical reaction of the sodium salt (1 eq.) with the appropriate cis-dichlorobis(phosphine) platinum (1 eq.) in THF resulted in the formation of platinum complexes [Pt(PR3)2(L)Cl] (R3 = Ph3; 1, Ph2Me; 2, PhMe2; 3, Me3; 4), whilst reaction with [Pt(COD)Cl2] afforded [Pt(COD)(L)Cl] (5). The corresponding reaction employing two equivalents of L, two equivalents of NaOtBu and one equivalent of [Pt(PR3)2Cl2]/[Pt(COD)Cl2] yielded complexes [Pt(PR3)2(L)2] (R3 = Ph2Me; 6, PhMe2; 7, Me3; 8) and [Pt(COD)(L)2] (9). L, 1, 5 and 9 have been fully characterised, principally by multinuclear magnetic resonance and IR spectroscopy and mass spectrometry, the remaining members of the series were analysed by 31P NMR only. Unsymmetrical complexes 1-4 provide examples of AX spin systems, with appropriate satellites attributed to 31P NMR-195Pt coupling. X-ray structures determined for 1,8-naphthosultam L, and complexes 1, 5 and 9 and where appropriate the platinum metal geometry, N-S distance and ligand distortions were compared.

AB - A series of bis(phosphine) platinum complexes 1-4 and 6-8 that bear the 1,8-naphthosultam ligand (L) have been synthesised. The nitrogen atom in L was deprotonated with sodium tert-butoxide to form the sodium salt. Metathetical reaction of the sodium salt (1 eq.) with the appropriate cis-dichlorobis(phosphine) platinum (1 eq.) in THF resulted in the formation of platinum complexes [Pt(PR3)2(L)Cl] (R3 = Ph3; 1, Ph2Me; 2, PhMe2; 3, Me3; 4), whilst reaction with [Pt(COD)Cl2] afforded [Pt(COD)(L)Cl] (5). The corresponding reaction employing two equivalents of L, two equivalents of NaOtBu and one equivalent of [Pt(PR3)2Cl2]/[Pt(COD)Cl2] yielded complexes [Pt(PR3)2(L)2] (R3 = Ph2Me; 6, PhMe2; 7, Me3; 8) and [Pt(COD)(L)2] (9). L, 1, 5 and 9 have been fully characterised, principally by multinuclear magnetic resonance and IR spectroscopy and mass spectrometry, the remaining members of the series were analysed by 31P NMR only. Unsymmetrical complexes 1-4 provide examples of AX spin systems, with appropriate satellites attributed to 31P NMR-195Pt coupling. X-ray structures determined for 1,8-naphthosultam L, and complexes 1, 5 and 9 and where appropriate the platinum metal geometry, N-S distance and ligand distortions were compared.

KW - Platinum

KW - Naphthalene

KW - Sulfam

KW - Complex

KW - X-ray structure

KW - Ray-diffraction data

KW - X-ray

KW - Metal tetrathiolenes

KW - Arenethiolatocopper(I) complexes

KW - Crystal-structures

KW - Ligands

KW - Coordination

KW - Cod

KW - Tetrathionaphthalene

UR - http://www.sciencedirect.com/science/article/pii/S0020169314005489#appd002

UR - https://www.scopus.com/pages/publications/84907571876

U2 - 10.1016/j.ica.2014.08.048

DO - 10.1016/j.ica.2014.08.048

M3 - Article

SN - 0020-1693

VL - 423

SP - 313

EP - 319

JO - Inorganica Chimica Acta

JF - Inorganica Chimica Acta

IS - Part A

ER -

Platinum bis(phosphine) complexes of 1,8-naphthosultam

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Keywords

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