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X-ray structural studies of some group VIII compounds with catalytic implications

Author: Douglas Allen Sullivan
Publisher: 1975.
Dissertation: Thesis--University of Florida.
Edition/Format:   Thesis/dissertation : Thesis/dissertation : Biography : Manuscript   Archival Material : EnglishView all editions and formats
Database:WorldCat
Summary:
X-ray structural investigations of compounds containing Group VIII metal atoms are presented. The compounds studied illustrate interatomic interactions which may be of importance in catalytic processes. The structures of metal-containing compounds were solved by locating the heavy atoms in Patterson functions and locating the remaining atoms in Fourier syntheses. The direct method of symbolic addition was used in  Read more...
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Additional Physical Format: Online version:
Sullivan, Douglas Allen, 1945-
X-ray structural studies of some group VIII compounds with catalytic implications.
1975
(OCoLC)820089878
Material Type: Biography, Thesis/dissertation, Manuscript
Document Type: Book, Archival Material
All Authors / Contributors: Douglas Allen Sullivan
OCLC Number: 2670311
Notes: Typescript.
Vita.
Description: xiii, 237 leaves : ill. ; 28 cm.
Responsibility: by Douglas Allen Sullivan.

Abstract:

X-ray structural investigations of compounds containing Group VIII metal atoms are presented. The compounds studied illustrate interatomic interactions which may be of importance in catalytic processes. The structures of metal-containing compounds were solved by locating the heavy atoms in Patterson functions and locating the remaining atoms in Fourier syntheses. The direct method of symbolic addition was used in the one, all light-atom case presented. Trial structures were refined by the method of least-squares.The crystal structure of trans -chloro (dimethylglyoximato) (dimethylglyoxime) (4-chloroaniline) cobalt (III) illustrates an unusual ligand-induced proton shift. Both neutral and dianionic dimethylglyoxime groups are found in the complex and the 4-chloroaniline ligand is oriented over the dianionic dimethylglyoxime. The structure of trans-bis (dimethylxiglyoximato) bis (4-chloroaniline) cobalt (III) chloride shows that complex to contain two monoatomic dimethylglyoxime ligands and the 4-chloroaniline ligands to be skewed relative to the diglyoxime ligands. The crystal structure of trans-chlorobis (diphenylglyoximato) {4-chloroaniline) cobalt- (III) is described. Trends in the structures of these compounds and in the previously reported structures of similar compounds are discussed. Ultraviolet and infrared spectra of these compounds are given. The synthesis of a novel chelating ligand capable of binding two metal ions is described. The characterizations, including crystal structures, of its protonated forin, 1,4-dihydrazinophthalazinebis (2-pyridiniuracarboxaldimine) nitrate dihydrate, and of a nickel complex, y-chlorotetraaqua . ,4- dihydrazinophthalazinebis (2-pyridinecarboxaldimine) dinickel- (II) chloride dihydrate, are presented. The planar ligand is shown to bind tv/o nickel ions with a separation of 3. COS o (1) A. A chloride ion occupies a bridging site in the plane of the nickel atoms and the ligand. The magnetic moment per nickel atom of the chloride bridged complex was deteinnined to be 2.74 B.M. at 40°C. The plausibility of structurally similar complexes mimicking the nitrogen-fixing enzyme nitrogenase is also discussed. The X-ray crystal structures of 1- (ir-cyclopentadienyl) - l-triphenylphosphine-2 ,3,4, 5-tetrakis (pentaf luorophenyl) cobaltole and 1- (Tr-cyclopentadienyl) -1-triphenylphosphine- 2 ,3, 4 , 5-tetrakis (pentaf luorophenyl) rhodole are reported. These compounds are viewed as stabilized intermediates in the catalyzed cyclization of acetylenes. In each case the metal atom forms a metallocyclo by a-bonding to the terminal carbons of a butadiene-like fragment. The ir-bonding in the metallocycle appears to be dclocalized.

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