Synthetic, X-ray structural and protonation studies of CpCr(CO)2SPy and CpCr(CO)2SPym (SPy = C5 H4NS, SPym = C4H3N2S)

Victor Wee Lin Ng; Weng Kee Leong; Lip Lin Koh; Geok Kheng Tan; Lai Yoong Goh

doi:10.1016/j.jorganchem.2004.07.026

Synthetic, X-ray structural and protonation studies of CpCr(CO)₂SPy and CpCr(CO)₂SPym (SPy = C₅ H₄NS, SPym = C₄H₃N₂S)

Victor Wee Lin Ng, Weng Kee Leong, Lip Lin Koh, Geok Kheng Tan, Lai Yoong Goh^*

^*Corresponding author for this work

National University of Singapore

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

13 Citations (Scopus)

Abstract

The facile reaction of [CpCr(CO)₃]₂ (Cp = η₅-C₅H₅) (1) with one mole equivalent of 2.2′-dithiodipyridine ((C₅H₄NS) ₂ = (SPy)₂) at ambient temperature led to the isolation of dark brown crystalline solids of CpCr(CO)₂ (η²-SPy) (2) in ca. 72% yield. 2 undergoes quantitative conversion to CpCrCl₂(η¹-SPyH) (3) with HCl. The reaction 1 with one mole equivalent of 2-mercaptopyrimidine (C₄H₃N₂SH HSPym) at ambient temperature led to the isolation of reddish-brown crystalline solids of CpCr(CO)₂(η²-SPym) (4) and green solids of CpCr(CO)₃H (5) in yields of ca. 42% and 46%, respectively. Reaction of 4 with HCl and subsequent workup in acetonitrile resulted in the cleavage of the thiolate ligand, giving the 15-electron chromium(III) species CpCrCl₂(CH₃CN) (6) and free 2-mercaptopyrimidine. The complexes 2-4 have been determined by single X-ray diffraction analysis.

Original language	English
Pages (from-to)	3210-3217
Number of pages	8
Journal	Journal of Organometallic Chemistry
Volume	689
Issue number	20
DOIs	https://doi.org/10.1016/j.jorganchem.2004.07.026
Publication status	Published - Sept 29 2004
Externally published	Yes

ASJC Scopus Subject Areas

Biochemistry
Physical and Theoretical Chemistry
Organic Chemistry
Inorganic Chemistry
Materials Chemistry

Keywords

15-electron chromium(III) complexes
2-mercaptopyridine
2-mercaptopyrimidine
Cyclopentadienylchromium
X-ray crystal structures

Access to Document

10.1016/j.jorganchem.2004.07.026

Cite this

@article{c732e374a71e42ccb7e37e272ab7bc52,

title = "Synthetic, X-ray structural and protonation studies of CpCr(CO)2SPy and CpCr(CO)2SPym (SPy = C5 H4NS, SPym = C4H3N2S)",

abstract = "The facile reaction of [CpCr(CO)3]2 (Cp = η5-C5H5) (1) with one mole equivalent of 2.2′-dithiodipyridine ((C5H4NS) 2 = (SPy)2) at ambient temperature led to the isolation of dark brown crystalline solids of CpCr(CO)2 (η2-SPy) (2) in ca. 72% yield. 2 undergoes quantitative conversion to CpCrCl2(η1-SPyH) (3) with HCl. The reaction 1 with one mole equivalent of 2-mercaptopyrimidine (C4H3N2SH HSPym) at ambient temperature led to the isolation of reddish-brown crystalline solids of CpCr(CO)2(η2-SPym) (4) and green solids of CpCr(CO)3H (5) in yields of ca. 42% and 46%, respectively. Reaction of 4 with HCl and subsequent workup in acetonitrile resulted in the cleavage of the thiolate ligand, giving the 15-electron chromium(III) species CpCrCl2(CH3CN) (6) and free 2-mercaptopyrimidine. The complexes 2-4 have been determined by single X-ray diffraction analysis.",

keywords = "15-electron chromium(III) complexes, 2-mercaptopyridine, 2-mercaptopyrimidine, Cyclopentadienylchromium, X-ray crystal structures",

author = "Ng, {Victor Wee Lin} and Leong, {Weng Kee} and Koh, {Lip Lin} and Tan, {Geok Kheng} and Goh, {Lai Yoong}",

year = "2004",

month = sep,

day = "29",

doi = "10.1016/j.jorganchem.2004.07.026",

language = "English",

volume = "689",

pages = "3210--3217",

journal = "Journal of Organometallic Chemistry",

issn = "0022-328X",

publisher = "Elsevier",

number = "20",

}

TY - JOUR

T1 - Synthetic, X-ray structural and protonation studies of CpCr(CO)2SPy and CpCr(CO)2SPym (SPy = C5 H4NS, SPym = C4H3N2S)

AU - Ng, Victor Wee Lin

AU - Leong, Weng Kee

AU - Koh, Lip Lin

AU - Tan, Geok Kheng

AU - Goh, Lai Yoong

PY - 2004/9/29

Y1 - 2004/9/29

N2 - The facile reaction of [CpCr(CO)3]2 (Cp = η5-C5H5) (1) with one mole equivalent of 2.2′-dithiodipyridine ((C5H4NS) 2 = (SPy)2) at ambient temperature led to the isolation of dark brown crystalline solids of CpCr(CO)2 (η2-SPy) (2) in ca. 72% yield. 2 undergoes quantitative conversion to CpCrCl2(η1-SPyH) (3) with HCl. The reaction 1 with one mole equivalent of 2-mercaptopyrimidine (C4H3N2SH HSPym) at ambient temperature led to the isolation of reddish-brown crystalline solids of CpCr(CO)2(η2-SPym) (4) and green solids of CpCr(CO)3H (5) in yields of ca. 42% and 46%, respectively. Reaction of 4 with HCl and subsequent workup in acetonitrile resulted in the cleavage of the thiolate ligand, giving the 15-electron chromium(III) species CpCrCl2(CH3CN) (6) and free 2-mercaptopyrimidine. The complexes 2-4 have been determined by single X-ray diffraction analysis.

AB - The facile reaction of [CpCr(CO)3]2 (Cp = η5-C5H5) (1) with one mole equivalent of 2.2′-dithiodipyridine ((C5H4NS) 2 = (SPy)2) at ambient temperature led to the isolation of dark brown crystalline solids of CpCr(CO)2 (η2-SPy) (2) in ca. 72% yield. 2 undergoes quantitative conversion to CpCrCl2(η1-SPyH) (3) with HCl. The reaction 1 with one mole equivalent of 2-mercaptopyrimidine (C4H3N2SH HSPym) at ambient temperature led to the isolation of reddish-brown crystalline solids of CpCr(CO)2(η2-SPym) (4) and green solids of CpCr(CO)3H (5) in yields of ca. 42% and 46%, respectively. Reaction of 4 with HCl and subsequent workup in acetonitrile resulted in the cleavage of the thiolate ligand, giving the 15-electron chromium(III) species CpCrCl2(CH3CN) (6) and free 2-mercaptopyrimidine. The complexes 2-4 have been determined by single X-ray diffraction analysis.

KW - 15-electron chromium(III) complexes

KW - 2-mercaptopyridine

KW - 2-mercaptopyrimidine

KW - Cyclopentadienylchromium

KW - X-ray crystal structures

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