Oxochloride Complexes of Rhenium

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We have been unable t o prepare TcCI, by the method published previously even though our reaction between Tc and CI, gave products which appeared the same. Tc0,CI and TcOCI, have been prepared and fully characterized for the first time.11 a ete impossible de preparer TcCI, par la methode precedemment publiee, m@me si la reaction entre Tc et CI, conduit a des produits qui semblent les m&mes. Les composes Tc0,CI et TcOCI, ont ete prepares et caracterises sans ambigui'tt pour la premiire fois.

Section: Introductionmentioning

confidence: 77%

Technetium Chlorides and Oxochlorides

Guest¹,

Lock²

1972

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“…The band at 906 cm-' corresponds t o a linear Re-0-Re asyinmetric stretch (1 1) and is observed at the same frequency for ReO,. Similarly a band at -370 cnl-I has been assigned to an Re-C1 stretch for ReOC1, (12). The bands in the 460-497 cm-' region are too high for trans~tions except those associated with the -0-Re-0-Resystem.…”

Section: Resultsmentioning

confidence: 99%

Oxodichlororhenium(IV), ReOCl₂

Frais¹,

Howard-Lock²,

Lock³

1973

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The preparation and some physical and chemical properties of ReOCI, are described.On dCcrit la prkparation ainsi que quelques propri Can. J Chem . 51. 828 (1973) Introduction Until recently only two oxochlorides of rhenium have been clearly established, namely ReOCl, and Re03Cl (1). Very recently there have been reports of ReOCI, (2) and the mixed complexes Re03Cl-ReOCl, (3) and Re,03C1,-(ReO,Cl), (4). We now report the existence of yet another simple oxochloride, namely oxodichlororhenium(IV), ReOCI,. ExperimentsRhenium and chlorine analyses were performed by the neutron activation method described previously (5). Infrared spectra were recorded for solid samples ground into a mull with Nujol. The Nujol had been dried by refluxing with phosphorus pentoxide followed by vacuum distillation. The mull samples were mounted between potassium bromide plates and spectra were recorded on Perkin-Elmer 337, 521, and 301 spectrometers. Raman emission was excited by 10 mW of radiation from a He-Ne laser 0,6328 A), and spectra were recorded with a Coderg PHO double monochromator with photoelectric detection. X-Ray diffraction photographs of powdered samples were recorded on a Debye-Scherrer camera. Samples were sealed inside fused quartz tubes and nickel-filtered CuKcc radiation was used for recording the photographs. Line intensities were measured from the photographs with a Joyce-Loebl microdensitometer. ReOC12 was prepared by a number of different chemical reactions. Typical reaction conditions are described below unless changes in the conditions made significant differences in the distribution of products, in which case different runs are described. Analysi~ and Identification of Prod~lctsFor qualitative identification of products only infrared spectroscopy (volatile materials) or X-ray diffraction (involatile n~aterials) was used. Combination of these techniques with quantitative analysis (see below) applied to pure and known "impure" samples (i.e. mixtures of known composition) has shown that infrared spectroscopy could identify as little as 5% of an impurity (and in many cases < 1%) while X-ray diffraction could detect as little as 5% of impurity in a single substance and 10% in a ' T o whom correspondence should be addressed.CtCs physiques et chimiques de ReOC1,.[Traduit par le journal] mixture of two compounds. For X-ray diffraction it is possible that large quantities of an amorphous product were present but we have no other evidence for this in any of our experiments. For each type of reaction reported below many runs were made (typically 5-10) and in most runs attempts were made not only to separate volatile and involatile products, but to separate the products into individual components. This was hard to do for volatile products, but for involatile products was achieved by hand-picking crystals. Parts of both volatile and involatile samples were examined by X-ray and infrared techniques to confirm that only the expected products were present. For quantitative analysis of a reaction, the nature of the products ...

“…Gas samples were contained in a heated gas cell with silver chloride windows (3). Solution samples were prepared in the manner described previously (4) and were contained in standard solution cells with potassium bromide windows. Raman spectra were excited by the 6328 A line of a helium-neon laser and were recorded on a Czerny-Turner-type Spex laser Raman recording spectrograph, which contained a double monochromator.…”

Section: Methodsmentioning

confidence: 99%

“…Preparation and Purificalion of Starting Materials Powdered rhenium metal, rhenium trioxide, rhenium oxotetrachloride, oxygen, and chlorine were obtained and purified as described previously (4). Rhenium heptoxide was prepared from vacuum dried rhenium metal and dry oxygen using a method similar to that of Melaven et al ( 9 , but using a modified apparatus (Fig.…”

Section: Methodsmentioning

confidence: 99%

The Preparation, Physical Properties, and Structure of Oxotetrachloroaquorhenium(VI), ReOCl₄(OH₂)

Frais¹,

Lock²

1972

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Oxotetrachloroaquorhenium(VI), ReOC1,-H,O, has been prepared and characterized for the first time by analysis, infrared spectroscopy and single crystal X-ray diffraction. The crystals were orthorhombic, a = 10.834(8), b = 11.089(8), c = 5.51 7(4) A, Pn2,a, Z = 4. Intensity data were recorded by integrating film methods and measured with a Joyce-Loebl microdensitometer, and 624 observable of the 704 measured independent reflections were given non-zero weight in the final cycle of full matrix least-squares refinement where R, = 0.0572 and R, = 0.0687., The molecular structure is based on a very distorted octahedron with a stron ly