Synthesis and characterisation of mono- and dinuclear diethyldithiocarbamatonickel(II) organochalcogenide complexes

James Darkwa; Emmanuel Y. Osei-Twum; Luis A. Litorja

doi:10.1016/S0277-5387(98)00400-8

Synthesis and characterisation of mono- and dinuclear diethyldithiocarbamatonickel(II) organochalcogenide complexes

James Darkwa^*
, Emmanuel Y. Osei-Twum
, Luis A. Litorja

^*Corresponding author for this work

King Fahd University of Petroleum & Minerals

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

8 Scopus citations

Abstract

The reaction of Ni(dtc)(PR₃)Cl (dtc=diethyldithiocarbamate, R=Ph or Bu) with HSC₆H₄Cl-4 or HSCH₂C₆H₄Cl-4 and Et₃N gave two types of complex. For PPh₃, the products were [Ni(dtc)(μ-SC₆H₄Cl-4)]₂ (1) and [Ni(dtc)(μ-SCH₂C₆H₄Cl-4)]₂ (2); whilst PBu₃ gave Ni(dtc)(PBu₃)(SC₆H₄Cl-4) (3). The structure of freshly prepared 3 was determined to be monomeric, as indicated by X-ray diffraction studies. However, at room temperature in solution, 3 was observed to slowly convert to 1. Structural identification of 1 and 2 and similar dimers, and structural identification of 3 and analogous monomers, were investigated by mass spectrometry. Electron impact mass spectrometry (EIMS) failed to confirm the proposed structures due to extensive decomposition in the mass spectrometer. In the electron impact (EI) mode, all complexes invariably decomposed to Ni(dtc)₂; on the other hand, fast atom bombardment (FAB) ionisation gave the expected molecular ions for all compounds.

Original language	English
Pages (from-to)	1115-1122
Number of pages	8
Journal	Polyhedron
Volume	18
Issue number	8-9
DOIs	https://doi.org/10.1016/S0277-5387(98)00400-8
State	Published - 12 Mar 1999

Bibliographical note

Funding Information:
Financial support by the Foundation for Research Development, South Africa (JD) and the Research Institute, King Fahd University of Petroleum and Minerals is gratefully acknowledged. We thank A.E. Thage for her assistance with the synthesis. We are also grateful to Professor J.C.A. Boeyens and Ms. Leanne Cook, Structural Chemistry Department, University of the Witwatersrand, South Africa, for determining the crystal structure as a service.

Keywords

Crystal structure
Mass spectrometry
Nickel thiolato complexes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/S0277-5387(98)00400-8

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@article{a98de057889a488fa2fd9a14d5fdc32f,

title = "Synthesis and characterisation of mono- and dinuclear diethyldithiocarbamatonickel(II) organochalcogenide complexes",

abstract = "The reaction of Ni(dtc)(PR3)Cl (dtc=diethyldithiocarbamate, R=Ph or Bu) with HSC6H4Cl-4 or HSCH2C6H4Cl-4 and Et3N gave two types of complex. For PPh3, the products were [Ni(dtc)(μ-SC6H4Cl-4)]2 (1) and [Ni(dtc)(μ-SCH2C6H4Cl-4)]2 (2); whilst PBu3 gave Ni(dtc)(PBu3)(SC6H4Cl-4) (3). The structure of freshly prepared 3 was determined to be monomeric, as indicated by X-ray diffraction studies. However, at room temperature in solution, 3 was observed to slowly convert to 1. Structural identification of 1 and 2 and similar dimers, and structural identification of 3 and analogous monomers, were investigated by mass spectrometry. Electron impact mass spectrometry (EIMS) failed to confirm the proposed structures due to extensive decomposition in the mass spectrometer. In the electron impact (EI) mode, all complexes invariably decomposed to Ni(dtc)2; on the other hand, fast atom bombardment (FAB) ionisation gave the expected molecular ions for all compounds.",

keywords = "Crystal structure, Mass spectrometry, Nickel thiolato complexes",

author = "James Darkwa and Osei-Twum, \{Emmanuel Y.\} and Litorja, \{Luis A.\}",

note = "Funding Information: Financial support by the Foundation for Research Development, South Africa (JD) and the Research Institute, King Fahd University of Petroleum and Minerals is gratefully acknowledged. We thank A.E. Thage for her assistance with the synthesis. We are also grateful to Professor J.C.A. Boeyens and Ms. Leanne Cook, Structural Chemistry Department, University of the Witwatersrand, South Africa, for determining the crystal structure as a service.",

year = "1999",

month = mar,

day = "12",

doi = "10.1016/S0277-5387(98)00400-8",

language = "English",

volume = "18",

pages = "1115--1122",

journal = "Polyhedron",

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number = "8-9",

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TY - JOUR

T1 - Synthesis and characterisation of mono- and dinuclear diethyldithiocarbamatonickel(II) organochalcogenide complexes

AU - Darkwa, James

AU - Osei-Twum, Emmanuel Y.

AU - Litorja, Luis A.

N1 - Funding Information: Financial support by the Foundation for Research Development, South Africa (JD) and the Research Institute, King Fahd University of Petroleum and Minerals is gratefully acknowledged. We thank A.E. Thage for her assistance with the synthesis. We are also grateful to Professor J.C.A. Boeyens and Ms. Leanne Cook, Structural Chemistry Department, University of the Witwatersrand, South Africa, for determining the crystal structure as a service.

PY - 1999/3/12

Y1 - 1999/3/12

N2 - The reaction of Ni(dtc)(PR3)Cl (dtc=diethyldithiocarbamate, R=Ph or Bu) with HSC6H4Cl-4 or HSCH2C6H4Cl-4 and Et3N gave two types of complex. For PPh3, the products were [Ni(dtc)(μ-SC6H4Cl-4)]2 (1) and [Ni(dtc)(μ-SCH2C6H4Cl-4)]2 (2); whilst PBu3 gave Ni(dtc)(PBu3)(SC6H4Cl-4) (3). The structure of freshly prepared 3 was determined to be monomeric, as indicated by X-ray diffraction studies. However, at room temperature in solution, 3 was observed to slowly convert to 1. Structural identification of 1 and 2 and similar dimers, and structural identification of 3 and analogous monomers, were investigated by mass spectrometry. Electron impact mass spectrometry (EIMS) failed to confirm the proposed structures due to extensive decomposition in the mass spectrometer. In the electron impact (EI) mode, all complexes invariably decomposed to Ni(dtc)2; on the other hand, fast atom bombardment (FAB) ionisation gave the expected molecular ions for all compounds.

AB - The reaction of Ni(dtc)(PR3)Cl (dtc=diethyldithiocarbamate, R=Ph or Bu) with HSC6H4Cl-4 or HSCH2C6H4Cl-4 and Et3N gave two types of complex. For PPh3, the products were [Ni(dtc)(μ-SC6H4Cl-4)]2 (1) and [Ni(dtc)(μ-SCH2C6H4Cl-4)]2 (2); whilst PBu3 gave Ni(dtc)(PBu3)(SC6H4Cl-4) (3). The structure of freshly prepared 3 was determined to be monomeric, as indicated by X-ray diffraction studies. However, at room temperature in solution, 3 was observed to slowly convert to 1. Structural identification of 1 and 2 and similar dimers, and structural identification of 3 and analogous monomers, were investigated by mass spectrometry. Electron impact mass spectrometry (EIMS) failed to confirm the proposed structures due to extensive decomposition in the mass spectrometer. In the electron impact (EI) mode, all complexes invariably decomposed to Ni(dtc)2; on the other hand, fast atom bombardment (FAB) ionisation gave the expected molecular ions for all compounds.

KW - Crystal structure

KW - Mass spectrometry

KW - Nickel thiolato complexes

UR - https://www.scopus.com/pages/publications/0038927479

U2 - 10.1016/S0277-5387(98)00400-8

DO - 10.1016/S0277-5387(98)00400-8

M3 - Article

AN - SCOPUS:0038927479

SN - 0277-5387

VL - 18

SP - 1115

EP - 1122

JO - Polyhedron

JF - Polyhedron

IS - 8-9

ER -

Synthesis and characterisation of mono- and dinuclear diethyldithiocarbamatonickel(II) organochalcogenide complexes

Abstract

Bibliographical note

Keywords

ASJC Scopus subject areas

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