Lower chlorides of zirconium and hafnium. Formation of stable monochlorides

Struss, Arthur W.; Corbett, John D.

doi:10.1021/ic50088a015

Cited by 43 publications

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“…Starting materials for all reactions were ZrCl and ZrCl4; earlier work2•4 has shown that ZrCl can easily be produced in bulk and is a far more facile reductant for tetrachloride than is the metal. All weighings and manipulation of the compounds were carried out in a drybox under nitrogen containing [6][7][8][9][10][11][12][13][14][15][16][17][18][19][20] ppm of water vapor.…”

Section: Methodsmentioning

confidence: 99%

The zirconium dichloride phase region. Synthesis, structure, and photoelectron spectral studies of 3R-ZrCl2, 6T-Zr1.05Cl2, and related phases

Cisar¹,

Corbett²,

Daake³

1979

Inorg. Chem.

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Section: Methodsmentioning

confidence: 99%

The zirconium dichloride phase region. Synthesis, structure, and photoelectron spectral studies of 3R-ZrCl2, 6T-Zr1.05Cl2, and related phases

Cisar¹,

Corbett²,

Daake³

1979

Inorg. Chem.

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“…Hafnium gives a slower reaction and a smaller yield, and the two monochlorides are evidently isostructural. 7 The novelty of the monochloride stoichiometry together with its metallic character prompted the present study. A parallel study on the synthesis of ZrCl by Troyanov and Tsirel'nikov8 yielded a similar result judging from the powder pattern.…”

Section: Introductionmentioning

confidence: 99%

Crystal structure of zirconium monochloride. A novel phase containing metal-metal bonded sheets

Adolphson¹,

Corbett²

1976

Inorg. Chem.

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112

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Monocrystals of ZrCl were obtained by the reaction of ZrCl4(g) with a large excess of electropolished Zr in a sealed tantalum tube under a 600-800 OC gradient for 24 days. Integrated diffraction data were secured on an automated diffractometer using Mo Ka radiation. Systematic absences among 203 observed reflections together with tuned diffraction data established a C-centered monoclinic cell with a = 5.943 (6), b = 3.419 (3), c = 9.087 (18) A, p = 102.5 (1)O, Z = 4. The structure was solved by standard Patterson and Fourier techniques to a conventional residual of 0.080 and R, = 0.087. The structure contains homoatomic layers sequenced C1-Zr-ZrC1 so as to generate four-layer sheets, the layers and sheets being geometrically close to cubic close packed along [OOl]. The result is found to be within experimental error of a higher symmetry trigonal cell ( Z = 6) with the rhombohedral space group R3m. The diffraction data were therefore converted, averaged, and refined utilizing 85 independent reflections, half as many positional parameters, and a = 3.424 (2), c = 26.57 (4) to give R = 0.071 and R, = 0.087. Distances are not statistically distinguishable in the two refinements; although the rhombohedral description is formally preferred, the real symmetry probably depends appreciably on the crystalline perfection in the [OOl] direction. Each zirconium atom has three neighbors in the adjacent sheet at 3.09 A (Pauling bond order of O S ) , six more in the same sheet at 3.42 A, and three chlorine atoms on the other side at 2.63 A. Weak chlorine-chlorine interactions between sheets at 3.61 A contrast with the strong metal-metal binding within the sheets; the former are presumably responsible for the graphitic properties and anisotropic conduction of the compound.

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“…The composition of their product varied between ZrClg g and ZrCl^ ^ depending on the extent of heat-treatment, Struss and Corbett (22) obtained somewhat larger yields by employing the more forcing conditions of a 12-day 600°/500° reaction in a weld-sealed tantalum container and, although analytical data were not given, their powder pattern was reportedly in excellent agreement with those of Dahl,et (15) and Watts (16) for ZrCl^.…”

mentioning

confidence: 54%

“…^Guinier intensities are from a microdensitometer film scan while Debye-Scherrer intensities were visually estimated, \ll observed reflections are within ±0.02° of 6 ^ for lattice parameters of a=3,S03l(3) and c=28.071(3). ^ased on a Debye-Scherrer film read and corrected for shrinkage by A.W, Struss and reported in an earlier publication (22).…”

Section: Interatomic Distances and Anglesmentioning

confidence: 99%

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Synthesis and characterization of some reduced zirconium halides

Daake¹

1977

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Daake, Richard Lynn, "Synthesis and characterization of some reduced zirconium halides " (1976). Retrospective Theses and Dissertations. 5736. http://lib.dr.iastate.edu/rtd/5736 INFORMATION TO USERSThis material was produced from a microfilm copy of the original document. While the most advanced technological means to photograph and reproduce this document have been used, the quality is heavily dependent upon the quality of the original submitted.The following explanation of techniques is provided to help you understand markings or patterns which may appear on this reproduction. 1.The sign or "target" for pages apparently lacking from the document photographed is "Missing PagB(s)". if it was possible to obtain the missing page(s) or section, they are spliced into the film along with adjacent pages. This may have necessitated cutting thru an image and duplicating adjacent pages to insure you complete continuity.2. When an image on the film is obliterated with a large round black mark, it is an indication that the photographer suspected that the copy may have moved during exposure and thus cause a blurred image. You will find a good image of the page in the adjacent frame.3. When a map, drawing or chart, etc., was part of the material being photographed the photographer followed a definite method in "sectioning" the material, it is customary to begin photoing at the upper left hand corner of a large sheet and to continue photoing from left to right in equal sections with a small overlap, if necessary, sectioning is continued again -beginning below the first row and continuing on until complete.4. The majority of users indicate that the textual content is of greatest value, however, a somewhat higher quality reproduction could be made from "photographs" if essential to the understanding of the dissertation. Silver prints of "'photographs" may be ordetsd aî aadiîionsi chargé by writing the Order Department, giving the catalog number, title, author and specific pages you wish reproduced.5. PLEASE NOTE: Some pages may have indistinct print. Filmed as received.

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Lower chlorides of zirconium and hafnium. Formation of stable monochlorides

Cited by 43 publications

References 0 publications

The zirconium dichloride phase region. Synthesis, structure, and photoelectron spectral studies of 3R-ZrCl2, 6T-Zr1.05Cl2, and related phases

The zirconium dichloride phase region. Synthesis, structure, and photoelectron spectral studies of 3R-ZrCl2, 6T-Zr1.05Cl2, and related phases

Crystal structure of zirconium monochloride. A novel phase containing metal-metal bonded sheets

Synthesis and characterization of some reduced zirconium halides

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