Synthesis and X-ray diffraction structures of novel half-sandwich Os(ii)-and Ru(ii)-hydroxamate complexes

Attila J. Godó, A. Bényei, Brian Duff, Denise A. Egan, P. Buglyó

Research output: Contribution to journalArticle

14 Citations (Scopus)

Abstract

Novel water soluble half-sandwich complexes of the general formulae [M(η 6-p-cym)(ha)] 2(CF 3SO 3) 2, [M(η 6-p-cym)(ha)Cl] or [M(η 6-p-cym) (ha)(py)]X (M = Os, Ru; ha = hydroxamate; py = pyridine; X = Cl - or CF 3SO 3 -), incorporating metal-containing entities and hydroxamates both with potential anti-proliferative features, were prepared and characterized by elemental analysis, spectroscopy (NMR, IR) and ESI mass spectrometry. The X-ray crystal structure of [Ru(η 6-p-cym) (μ-meaha)] 2(CF 3SO 3) 2 (5), [Os(η 6-p-cym)(meaha)Cl] (6), [Ru(η 6-p-cym)(phebha) Cl], (9), [Ru(η 6-p-cym)(bha)(py)](CF 3SO 3) (12) and [Ru(η 6-p-cym)(phebha)(py)](CF 3SO 3) (14), 6 is the first published structure of an organometallic Os(ii)-hydroxamate reported. The effect of size differences of the metal ions, the steric demand of the R C and R N substituents at the hydroxamate group and the type of the monodentate ligand co-present in the stoichiometry, along with the binding architecture of the half-sandwich metal(ii) hydroxamate complexes are discussed. A novel dinuclear, dihydroxo bridged complex [Os(η 6-p-cym)(py)(μ-OH)] 2(CF 3SO 3) 2 (16) is prepared and characterized by X-ray crystallography. Unexpected formation of a dinuclear oxo bridged Os II/Os VI complex [{Os(η 6-p-cym)(meaha)} (μ-O){Os(O)(meaha) 2}]Cl (17) occurs, and the crystal and molecular structure has been determined by X-ray method. Complexes 1, 5-8, 10 and 14 were tested for their in vitro cytotoxicity, using human-derived ovarian cancer cell lines (A2780 and A2780 cisR), and showed no anti-proliferative effect in the concentration range (0-200 μM) studied.

Original languageEnglish
Pages (from-to)1486-1495
Number of pages10
JournalRSC Advances
Volume2
Issue number4
DOIs
Publication statusPublished - Feb 21 2012

Fingerprint

Crystal structure
Metals
X ray diffraction
X rays
X ray crystallography
Organometallics
Cytotoxicity
Stoichiometry
Pyridine
Molecular structure
Nuclear magnetic resonance spectroscopy
Mass spectrometry
Metal ions
Ligands
Cells
Water
Chemical analysis
pyridine

ASJC Scopus subject areas

  • Chemical Engineering(all)
  • Chemistry(all)

Cite this

Synthesis and X-ray diffraction structures of novel half-sandwich Os(ii)-and Ru(ii)-hydroxamate complexes. / Godó, Attila J.; Bényei, A.; Duff, Brian; Egan, Denise A.; Buglyó, P.

In: RSC Advances, Vol. 2, No. 4, 21.02.2012, p. 1486-1495.

Research output: Contribution to journalArticle

@article{3a9b9aaa5bb543e2b27f25ecb1bd5e1b,
title = "Synthesis and X-ray diffraction structures of novel half-sandwich Os(ii)-and Ru(ii)-hydroxamate complexes",
abstract = "Novel water soluble half-sandwich complexes of the general formulae [M(η 6-p-cym)(ha)] 2(CF 3SO 3) 2, [M(η 6-p-cym)(ha)Cl] or [M(η 6-p-cym) (ha)(py)]X (M = Os, Ru; ha = hydroxamate; py = pyridine; X = Cl - or CF 3SO 3 -), incorporating metal-containing entities and hydroxamates both with potential anti-proliferative features, were prepared and characterized by elemental analysis, spectroscopy (NMR, IR) and ESI mass spectrometry. The X-ray crystal structure of [Ru(η 6-p-cym) (μ-meaha)] 2(CF 3SO 3) 2 (5), [Os(η 6-p-cym)(meaha)Cl] (6), [Ru(η 6-p-cym)(phebha) Cl], (9), [Ru(η 6-p-cym)(bha)(py)](CF 3SO 3) (12) and [Ru(η 6-p-cym)(phebha)(py)](CF 3SO 3) (14), 6 is the first published structure of an organometallic Os(ii)-hydroxamate reported. The effect of size differences of the metal ions, the steric demand of the R C and R N substituents at the hydroxamate group and the type of the monodentate ligand co-present in the stoichiometry, along with the binding architecture of the half-sandwich metal(ii) hydroxamate complexes are discussed. A novel dinuclear, dihydroxo bridged complex [Os(η 6-p-cym)(py)(μ-OH)] 2(CF 3SO 3) 2 (16) is prepared and characterized by X-ray crystallography. Unexpected formation of a dinuclear oxo bridged Os II/Os VI complex [{Os(η 6-p-cym)(meaha)} (μ-O){Os(O)(meaha) 2}]Cl (17) occurs, and the crystal and molecular structure has been determined by X-ray method. Complexes 1, 5-8, 10 and 14 were tested for their in vitro cytotoxicity, using human-derived ovarian cancer cell lines (A2780 and A2780 cisR), and showed no anti-proliferative effect in the concentration range (0-200 μM) studied.",
author = "God{\'o}, {Attila J.} and A. B{\'e}nyei and Brian Duff and Egan, {Denise A.} and P. Bugly{\'o}",
year = "2012",
month = "2",
day = "21",
doi = "10.1039/c1ra00998b",
language = "English",
volume = "2",
pages = "1486--1495",
journal = "RSC Advances",
issn = "2046-2069",
publisher = "Royal Society of Chemistry",
number = "4",

}

TY - JOUR

T1 - Synthesis and X-ray diffraction structures of novel half-sandwich Os(ii)-and Ru(ii)-hydroxamate complexes

AU - Godó, Attila J.

AU - Bényei, A.

AU - Duff, Brian

AU - Egan, Denise A.

AU - Buglyó, P.

PY - 2012/2/21

Y1 - 2012/2/21

N2 - Novel water soluble half-sandwich complexes of the general formulae [M(η 6-p-cym)(ha)] 2(CF 3SO 3) 2, [M(η 6-p-cym)(ha)Cl] or [M(η 6-p-cym) (ha)(py)]X (M = Os, Ru; ha = hydroxamate; py = pyridine; X = Cl - or CF 3SO 3 -), incorporating metal-containing entities and hydroxamates both with potential anti-proliferative features, were prepared and characterized by elemental analysis, spectroscopy (NMR, IR) and ESI mass spectrometry. The X-ray crystal structure of [Ru(η 6-p-cym) (μ-meaha)] 2(CF 3SO 3) 2 (5), [Os(η 6-p-cym)(meaha)Cl] (6), [Ru(η 6-p-cym)(phebha) Cl], (9), [Ru(η 6-p-cym)(bha)(py)](CF 3SO 3) (12) and [Ru(η 6-p-cym)(phebha)(py)](CF 3SO 3) (14), 6 is the first published structure of an organometallic Os(ii)-hydroxamate reported. The effect of size differences of the metal ions, the steric demand of the R C and R N substituents at the hydroxamate group and the type of the monodentate ligand co-present in the stoichiometry, along with the binding architecture of the half-sandwich metal(ii) hydroxamate complexes are discussed. A novel dinuclear, dihydroxo bridged complex [Os(η 6-p-cym)(py)(μ-OH)] 2(CF 3SO 3) 2 (16) is prepared and characterized by X-ray crystallography. Unexpected formation of a dinuclear oxo bridged Os II/Os VI complex [{Os(η 6-p-cym)(meaha)} (μ-O){Os(O)(meaha) 2}]Cl (17) occurs, and the crystal and molecular structure has been determined by X-ray method. Complexes 1, 5-8, 10 and 14 were tested for their in vitro cytotoxicity, using human-derived ovarian cancer cell lines (A2780 and A2780 cisR), and showed no anti-proliferative effect in the concentration range (0-200 μM) studied.

AB - Novel water soluble half-sandwich complexes of the general formulae [M(η 6-p-cym)(ha)] 2(CF 3SO 3) 2, [M(η 6-p-cym)(ha)Cl] or [M(η 6-p-cym) (ha)(py)]X (M = Os, Ru; ha = hydroxamate; py = pyridine; X = Cl - or CF 3SO 3 -), incorporating metal-containing entities and hydroxamates both with potential anti-proliferative features, were prepared and characterized by elemental analysis, spectroscopy (NMR, IR) and ESI mass spectrometry. The X-ray crystal structure of [Ru(η 6-p-cym) (μ-meaha)] 2(CF 3SO 3) 2 (5), [Os(η 6-p-cym)(meaha)Cl] (6), [Ru(η 6-p-cym)(phebha) Cl], (9), [Ru(η 6-p-cym)(bha)(py)](CF 3SO 3) (12) and [Ru(η 6-p-cym)(phebha)(py)](CF 3SO 3) (14), 6 is the first published structure of an organometallic Os(ii)-hydroxamate reported. The effect of size differences of the metal ions, the steric demand of the R C and R N substituents at the hydroxamate group and the type of the monodentate ligand co-present in the stoichiometry, along with the binding architecture of the half-sandwich metal(ii) hydroxamate complexes are discussed. A novel dinuclear, dihydroxo bridged complex [Os(η 6-p-cym)(py)(μ-OH)] 2(CF 3SO 3) 2 (16) is prepared and characterized by X-ray crystallography. Unexpected formation of a dinuclear oxo bridged Os II/Os VI complex [{Os(η 6-p-cym)(meaha)} (μ-O){Os(O)(meaha) 2}]Cl (17) occurs, and the crystal and molecular structure has been determined by X-ray method. Complexes 1, 5-8, 10 and 14 were tested for their in vitro cytotoxicity, using human-derived ovarian cancer cell lines (A2780 and A2780 cisR), and showed no anti-proliferative effect in the concentration range (0-200 μM) studied.

UR - http://www.scopus.com/inward/record.url?scp=84859143549&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=84859143549&partnerID=8YFLogxK

U2 - 10.1039/c1ra00998b

DO - 10.1039/c1ra00998b

M3 - Article

VL - 2

SP - 1486

EP - 1495

JO - RSC Advances

JF - RSC Advances

SN - 2046-2069

IS - 4

ER -