Synthesis and characterization of two new "pincer" complexes of zinc(II). The X-ray crystal structures of the five coordinate complexes [ZnCl2{η3-NN'N-2,6-(R2NCH2)2C5H3N}] (R = n-Bu or Me)

2000 ◽  
Vol 78 (12) ◽  
pp. 1620-1626 ◽  
Author(s):  
Ignacio del Río ◽  
Robert A Gossage ◽  
Milja S Hannu ◽  
Martin Lutz ◽  
Anthony L Spek ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
General Formula ◽  
Pincer Complexes ◽  
Synthesis And Characterization ◽  
Donor Ligand ◽  
X Ray ◽  
Ru Complex ◽  
Trigonal Bipyramidal

The potentially terdentate NN'N donor ligand 2,6-bis[di-(n-butyl)aminomethyl]pyridine (1) does not form a stable, isolable Ru complex using any standard Ru starting materials. This is in contrast to the dimethylamino derivative 2. In the presence of Zn metal as a reducing agent, the treatment of hydrated ruthenium trichloride with 2 leads instead to the isolation of a diamagnetic Zn(II) complex (3) of general formula [ZnCl2(1)]. Analysis of 3 (NMR, X-ray) reveals the complex to be a mononuclear Zn halide compound containing ligand 1 in an η3-NN'N bonding motif. The Zn atom is found to be five-coordinate and in a geometry best described as midway between trigonal bipyramidal and square pyramidal in structure. Similar experiments using 2 produce an analogous Zn species (4) which has likewise been fully characterized (NMR, X-ray) and found to be similar to 3 although the metal is in a distinctly square pyramidal environment. These compounds are viewed as relatives of the class of Zn "pybox" catalysts.Key words: pincer complexes, zinc(II) compounds, X-ray crystal structure.

The synthesis and characterization of the pendant-armed ligand N,N′-bis(2′-pyridylmethyl)-1,7-dithia-4,11-diazacyclotetradecane (L4) and crystal structures of L4 and the copper(II) complex [Cu(L4)](ClO4)2 — Crystal structure of the nickel(II) complex of N-(2′-pyridylmethyl)-1,4,7-trithia-11-azacyclotetradecane (L2), [Ni(L2)(CH3CN)](ClO4)2·CH3CN

2006 ◽  
Vol 84 (2) ◽  
pp. 187-195 ◽  
Author(s):  
B CM Chak ◽  
A McAuley
Keyword(s):  
Crystal Structure ◽  
Copper Ion ◽  
Esr Spectra ◽  
Synthesis And Characterization ◽  
Electrochemical Studies ◽  
High Dilution ◽  
Donor Ligand ◽  
X Ray ◽  
Distorted Octahedral

The synthesis and characterization of the mixed donor ligand N,N′-bis(2′-pyridylmethyl)-1,7-dithia-4,11-diazacyclotetradecane (L4) containing two pendant pyridine arms is described. The macrocycle formation involves reaction of N-tosylbis(2-bromoethyl)amine with N-tosylbis(3-mercaptopropyl)amine at high dilution followed by detosylation at the nitrogen atoms using LiAlH4 in view of the presence of the thioether groups. An X-ray study of the ligand shows the sulphur atoms lie exo to the macrocyclic ring. The nickel(II) and copper(II) complexes of L4 have been characterized and the X-ray structure of the Cu(II) ion exhibits a five-coordinate copper ion despite the presence of six available donor atoms. In the case of ligand N-(2-pyridylmethyl)-1,4,7-trithia-11-azacyclotetradecane (L2), with a single pendant N donor, the Ni(II) complex is distorted octahedral with a molecule of acetonitrile in the sixth site. Details of UV–vis, ESR spectra, and electrochemical studies on the complexes are presented.Key words: synthesis, pendant-armed, mixed donor S,N macrocycles, copper, nickel.

scholarly journals Arene Ruthenium Metalla-Assemblies with Anthracene Moieties for PDT Applications

Inorganics ◽  
2018 ◽  
Vol 6 (3) ◽  
pp. 97 ◽  
Author(s):  
Marie Gaschard ◽  
Farzaneh Nehzat ◽  
Thomas Cheminel ◽  
Bruno Therrien
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
General Formula ◽  
Structure Analysis ◽  
White Light ◽  
Light Irradiation ◽  
Synthesis And Characterization ◽  
X Ray

The synthesis and characterization of three metalla-rectangles of the general formula [Ru4(η6-p-cymene)4(μ4-clip)2(μ2-Lanthr)2][CF3SO3]4 (Lanthr: 9,10-bis(3,3’-ethynylpyridyl) anthracene; clip = oxa: oxalato; dobq: 2,5-dioxido-1,4-benzoquinonato; donq: 5,8-dioxido-1,4-naphthoquinonato) are presented. The molecular structure of the metalla-rectangle [Ru4(η6-p-cymene)4(μ4-oxa)2(μ2-Lanthr)2]4+ has been confirmed by the single-crystal X-ray structure analysis of [Ru4(η6-p-cymene)4(μ4-oxa)2(μ2-Lanthr)2][CF3SO3]4 · 4 acetone (A2 · 4 acetone), thus showing the anthracene moieties to be available for reaction with oxygen. While the formation of the endoperoxide form of Lanthr was observed in solution upon white light irradiation, the same reaction does not occur when Lanthr is part of the metalla-assemblies.

Darstellung und Charakterisierung von Rubidiumhydrogencyanamid/Synthesis and Characterization of Rubidium Hydrogen Cyanamide

1999 ◽  
Vol 54 (11) ◽  
pp. 1375-1378 ◽  
Author(s):  
Michael Becker ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Liquid Ammonia ◽  
Synthesis And Characterization ◽  
Hydrogen Cyanamide ◽  
X Ray ◽  
Bond Lengths

The synthesis of RbHCN2 was carried out by reaction of cyanamide with rubidium amide in liquid ammonia. The crystal structure has been determinedo by x-ray powder methods (orthorhombic, P21,21,21, a = 7.299(1), b = 9.435(1), c = 9.420(1) Å; Z = 8). The anion is slightly bent (174°) and exhibits two different bond lengths (C-N: 1.17, HN-C: 1.31 Å).

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