Synthesis and characterization of technetium(V) 8-quinolinolates. X-ray crystal structure of cis-chlorobis(2-methyl-8-quinolinolato)oxotechnetium(V)

Journal Article · Wed Sep 12 00:00:00 EDT 1984 · Inorg. Chem.; (United States)

DOI:https://doi.org/10.1021/ic00187a013· OSTI ID:6319030

Wilcox, B E; Heeg, M J; Deutsch, E

Technetium(V) complexes of 8-quinolinolates of the form TcOL/sub 2/X (L = 8-quinolinolate and its 5,7-dichloro, 5,7-dibromo, 5-nitro, and 2-methyl derivatives; X = Cl, Br) have been synthesized and characterized. These neutral species precipitate from methanol after reaction of the quinolinolate ligand with TcOX/sub 4//sup -/. High performance liquid chromatography analyses of the complexes show that the halide ligand of cis-TcO(8-quinolinolate)/sub 2/X is susceptible to solvolysis in methanol, forming what is believed to be TcOL/sub 2/(OCH/sub 3/); when X is Cl, the specific first-order rate constant governing this process is 1 X 10/sup -4/s/sup -1/ (25/sup 0/C, no ionic strength, in methanol). A single-crystal X-ray structure determination shows that the chlorobis(2-methyl-8-quinolinolato)oxotechnetium(V) complex, TcO(CH/sub 3/C/sub 9/H/sub 5/NO)/sub 2/Cl, formula weight 467, has a distorted-octahedral coordination geometry, with the chloro and oxo ligands in a cis configuration. A oxo-induced structural trans effect characteristic of M=O moieties is manifested in a lengthening of the Tc-O bond trans to the yl oxygen and a displacement of the Tc atom out of the mean equatorial plane. This complex crystallizes in the triclinic centrosymmetric space group P anti-1 with a = 7.693 (2) A, b = 9.337 (2) A, c = 12.739 (3) A, ..cap alpha.. = 86.52 (2)/sup 0/, ..beta.. = 85.99 (2)/sup 0/, ..gamma.. = 84.12 (2)/sup 0/, and V = 907 (2) A/sup 3/, with Z = 2, for 2882 observed reflections with I/sub 0/ greater than or equal to 2sigma(I). Structural aspects of metal complexes containing 8-quinolinolate ligands are discussed. 32 references, 4 figures, 6 tables.

• Research Organization: Univ. of Cincinnati, OH
• OSTI ID: 6319030
• Journal Information: Inorg. Chem.; (United States), Vol. 23:19
• Country of Publication: United States
• Language: English

Related Subjects

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY
37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
TECHNETIUM COMPLEXES
STRUCTURAL CHEMICAL ANALYSIS
SYNTHESIS
BOND ANGLE
BOND LENGTHS
BROMINE COMPOUNDS
CORRELATIONS
CRYSTAL STRUCTURE
DATA ANALYSIS
EXPERIMENTAL DATA
HETEROCYCLIC COMPOUNDS
LATTICE PARAMETERS
LEAST SQUARE FIT
LIGANDS
LIQUID COLUMN CHROMATOGRAPHY
MATHEMATICAL MODELS
MOLECULAR STRUCTURE
MONOCRYSTALS
NITRO COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
OXYGEN COMPOUNDS
STABILITY
TECHNETIUM CHLORIDES
TRICLINIC LATTICES
X-RAY DIFFRACTION
CHLORIDES
CHLORINE COMPOUNDS
CHROMATOGRAPHY
COHERENT SCATTERING
COMPLEXES
CRYSTAL LATTICES
CRYSTALS
DATA
DIFFRACTION
DIMENSIONS
HALIDES
HALOGEN COMPOUNDS
INFORMATION
LENGTH
MAXIMUM-LIKELIHOOD FIT
NUMERICAL DATA
NUMERICAL SOLUTION
ORGANIC COMPOUNDS
REFRACTORY METAL COMPOUNDS
SCATTERING
SEPARATION PROCESSES
TECHNETIUM COMPOUNDS
TRANSITION ELEMENT COMPLEXES
TRANSITION ELEMENT COMPOUNDS
400702* - Radiochemistry & Nuclear Chemistry- Properties of Radioactive Materials
400301 - Organic Chemistry- Chemical & Physicochemical Properties- (-1987)