Synthesis and structural studies of dicationic Pd(II) and Pt(II) complexes of 2-(alkylchalcogenomethyl)pyridines, [M{NC5H4-2-(CH2ER)}2][PF6]2

Roderick C. Jones, Michael G. Gardiner, Brian W. Skelton, Vicki Anne Tolhurst

Research output: Contribution to journalArticle

Abstract

Six novel dicationic complexes of the formula [ML2][PF6]2, were prepared from the reaction of MCl2 (M = Pd, Pt) with two equivalents of Tl[PF6] in acetonitrile (MeCN), followed by addition of two equivalents of 2-(alkylchalcogenomethyl)pyridine (N,E) ligands (L) [L = 2-(methylthiomethyl)pyridine (L1), 2-(phenylthiomethyl)pyridine (L2), 2-(methylselenomethyl)pyridine (L3)] at room temperature. Structures of the synthesised complexes [M(L1)2][PF6]2 [M = Pd (1a), Pt (1b)] and [M(L3)2][PF6]2 [M = Pd (3a), Pt (3b)] were characterised by single crystal X-ray diffraction studies, illustrating they crystallise in the triclinic crystal system in the space group P1¯. The metal centres exhibit a distorted square planar geometry, with the donor atoms of the chelated N,E ligands arranged trans with respect to each other. The orientation of the methyl moieties of the ligands with respect to each other and the square planar metal were varied, with the methyl moieties in [Pt(L3)2][PF6]2 (3b) having anti-geometry in the solid state while those of [M(L1)2][PF6]2 [M = Pd (1a), Pt (1b)] and [Pd(L3)2][PF6]2 (3a) show the methylselenoether groups to have syn-geometries with respect to themselves and the metal plane. All synthesised complexes were further characterised by elemental analysis, FT-IR spectroscopy and liquid secondary ionisation mass spectrometry (LSIMS) techniques.

Original languageEnglish
Pages (from-to)291-296
Number of pages6
JournalPolyhedron
Volume156
DOIs
Publication statusPublished - 1 Dec 2018

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Pyridines
Pyridine
pyridines
Metals
Ligands
synthesis
ligands
Geometry
geometry
metals
Acetonitrile
acetonitrile
Ionization
Mass spectrometry
Infrared spectroscopy
mass spectroscopy
Single crystals
solid state
X ray diffraction
ionization

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@article{96c48475553d4758b388c88d13268fbf,
title = "Synthesis and structural studies of dicationic Pd(II) and Pt(II) complexes of 2-(alkylchalcogenomethyl)pyridines, [M{NC5H4-2-(CH2ER)}2][PF6]2",
abstract = "Six novel dicationic complexes of the formula [ML2][PF6]2, were prepared from the reaction of MCl2 (M = Pd, Pt) with two equivalents of Tl[PF6] in acetonitrile (MeCN), followed by addition of two equivalents of 2-(alkylchalcogenomethyl)pyridine (N,E) ligands (L) [L = 2-(methylthiomethyl)pyridine (L1), 2-(phenylthiomethyl)pyridine (L2), 2-(methylselenomethyl)pyridine (L3)] at room temperature. Structures of the synthesised complexes [M(L1)2][PF6]2 [M = Pd (1a), Pt (1b)] and [M(L3)2][PF6]2 [M = Pd (3a), Pt (3b)] were characterised by single crystal X-ray diffraction studies, illustrating they crystallise in the triclinic crystal system in the space group P1¯. The metal centres exhibit a distorted square planar geometry, with the donor atoms of the chelated N,E ligands arranged trans with respect to each other. The orientation of the methyl moieties of the ligands with respect to each other and the square planar metal were varied, with the methyl moieties in [Pt(L3)2][PF6]2 (3b) having anti-geometry in the solid state while those of [M(L1)2][PF6]2 [M = Pd (1a), Pt (1b)] and [Pd(L3)2][PF6]2 (3a) show the methylselenoether groups to have syn-geometries with respect to themselves and the metal plane. All synthesised complexes were further characterised by elemental analysis, FT-IR spectroscopy and liquid secondary ionisation mass spectrometry (LSIMS) techniques.",
keywords = "Dicationic, Heteroleptic, Palladium, Plantinum, X-ray",
author = "Jones, {Roderick C.} and Gardiner, {Michael G.} and Skelton, {Brian W.} and Tolhurst, {Vicki Anne}",
year = "2018",
month = "12",
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journal = "Polyhedron",
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Synthesis and structural studies of dicationic Pd(II) and Pt(II) complexes of 2-(alkylchalcogenomethyl)pyridines, [M{NC5H4-2-(CH2ER)}2][PF6]2. / Jones, Roderick C.; Gardiner, Michael G.; Skelton, Brian W.; Tolhurst, Vicki Anne.

In: Polyhedron, Vol. 156, 01.12.2018, p. 291-296.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Synthesis and structural studies of dicationic Pd(II) and Pt(II) complexes of 2-(alkylchalcogenomethyl)pyridines, [M{NC5H4-2-(CH2ER)}2][PF6]2

AU - Jones, Roderick C.

AU - Gardiner, Michael G.

AU - Skelton, Brian W.

AU - Tolhurst, Vicki Anne

PY - 2018/12/1

Y1 - 2018/12/1

N2 - Six novel dicationic complexes of the formula [ML2][PF6]2, were prepared from the reaction of MCl2 (M = Pd, Pt) with two equivalents of Tl[PF6] in acetonitrile (MeCN), followed by addition of two equivalents of 2-(alkylchalcogenomethyl)pyridine (N,E) ligands (L) [L = 2-(methylthiomethyl)pyridine (L1), 2-(phenylthiomethyl)pyridine (L2), 2-(methylselenomethyl)pyridine (L3)] at room temperature. Structures of the synthesised complexes [M(L1)2][PF6]2 [M = Pd (1a), Pt (1b)] and [M(L3)2][PF6]2 [M = Pd (3a), Pt (3b)] were characterised by single crystal X-ray diffraction studies, illustrating they crystallise in the triclinic crystal system in the space group P1¯. The metal centres exhibit a distorted square planar geometry, with the donor atoms of the chelated N,E ligands arranged trans with respect to each other. The orientation of the methyl moieties of the ligands with respect to each other and the square planar metal were varied, with the methyl moieties in [Pt(L3)2][PF6]2 (3b) having anti-geometry in the solid state while those of [M(L1)2][PF6]2 [M = Pd (1a), Pt (1b)] and [Pd(L3)2][PF6]2 (3a) show the methylselenoether groups to have syn-geometries with respect to themselves and the metal plane. All synthesised complexes were further characterised by elemental analysis, FT-IR spectroscopy and liquid secondary ionisation mass spectrometry (LSIMS) techniques.

AB - Six novel dicationic complexes of the formula [ML2][PF6]2, were prepared from the reaction of MCl2 (M = Pd, Pt) with two equivalents of Tl[PF6] in acetonitrile (MeCN), followed by addition of two equivalents of 2-(alkylchalcogenomethyl)pyridine (N,E) ligands (L) [L = 2-(methylthiomethyl)pyridine (L1), 2-(phenylthiomethyl)pyridine (L2), 2-(methylselenomethyl)pyridine (L3)] at room temperature. Structures of the synthesised complexes [M(L1)2][PF6]2 [M = Pd (1a), Pt (1b)] and [M(L3)2][PF6]2 [M = Pd (3a), Pt (3b)] were characterised by single crystal X-ray diffraction studies, illustrating they crystallise in the triclinic crystal system in the space group P1¯. The metal centres exhibit a distorted square planar geometry, with the donor atoms of the chelated N,E ligands arranged trans with respect to each other. The orientation of the methyl moieties of the ligands with respect to each other and the square planar metal were varied, with the methyl moieties in [Pt(L3)2][PF6]2 (3b) having anti-geometry in the solid state while those of [M(L1)2][PF6]2 [M = Pd (1a), Pt (1b)] and [Pd(L3)2][PF6]2 (3a) show the methylselenoether groups to have syn-geometries with respect to themselves and the metal plane. All synthesised complexes were further characterised by elemental analysis, FT-IR spectroscopy and liquid secondary ionisation mass spectrometry (LSIMS) techniques.

KW - Dicationic

KW - Heteroleptic

KW - Palladium

KW - Plantinum

KW - X-ray

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U2 - 10.1016/j.poly.2018.09.058

DO - 10.1016/j.poly.2018.09.058

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