Rhenium compounds

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Rhenium compounds are compounds formed by the transition metal rhenium (Re). Rhenium can form in many oxidation states, and compounds are known for every oxidation state from -3 to +7 except -2, although the oxidation states +7, +4, and +3 are the most common. [1] Rhenium is most available commercially as salts of perrhenate, including sodium and ammonium perrhenates. These are white, water-soluble compounds. [2] The tetrathioperrhenate anion [ReS4]− is possible. [3]

Contents

Chalcogenides

Oxides

Rhenium(VI) oxide has an appearance similar to that of copper. REO3.JPG
Rhenium(VI) oxide has an appearance similar to that of copper.

Rhenium(IV) oxide (or rhenium dioxide) is an oxide of rhenium, with the formula ReO2. This gray to black crystalline solid is a laboratory reagent that can be used as a catalyst. It adopts the rutile structure. It forms via comproportionation: [4]

2 Re2O7 + 3 Re → 7 ReO2

Single crystals are obtained by chemical transport, using iodine as the transporting agent. [5] At high temperatures it undergoes disproportionation. It forms perrhenates with alkaline hydrogen peroxide and oxidizing acids. [6] In molten sodium hydroxide it forms sodium rhenate. [7]

Rhenium(VI) oxide, or rhenium trioxide, is another oxide of rhenium. It is the only stable group 7 trioxide. It has an appearance somewhat like copper. It can be formed by reducing rhenium(VII) oxide with carbon monoxide at 200 °C or elemental rhenium at 400 °C. [8] Re2O7 can also be reduced with dioxane. [9] Rhenium trioxide crystallizes with a primitive cubic unit cell, with a lattice parameter of 3.742 Å (374.2 pm). The structure of ReO3 is similar to that of perovskite (ABO3), without the large A cation at the centre of the unit cell. Each rhenium center is surrounded by an octahedron defined by six oxygen centers. These octahedra share corners to form the 3-dimensional structure. The coordination number of O is 2, because each oxygen atom has 2 neighbouring Re atoms. [10]

Rhenium(VII) oxide, or rhenium heptoxide, is another oxide of rhenium. It is the anhydride form of perrhenic acid, and is the raw material for all rhenium compounds. [11] Solid Re2O7 consists of alternating octahedral and tetrahedral Re centres. Upon heating, the polymer cracks to give molecular (nonpolymeric) Re2O7. This molecular species closely resembles manganese heptoxide, consisting of a pair of ReO4 tetrahedra that share a vertex, i.e., O3Re–O–ReO3. [12]

Other chalcogenides

Rhenium disulfide is a sulfide with the formula ReS2. It has a layered structure where atoms are strongly bonded within each layer. The layers are held together by weak Van der Waals bonds, and can be easily peeled off from the bulk material. It is a two-dimensional (2D) group VII transition metal dichalcogenide (TMD). ReS2 was isolated down to monolayers which is only one unit cell in thickness for the first time in 2014. [13] ReS2 is found in nature as the mineral rheniite. [14] It can be synthesized from the reaction between rhenium and sulfur at 1000 °C, or the decomposition of rhenium(VII) sulfide at 1100 °C: [15]

Re + 2 S → ReS2
Re2S7 → 2 ReS2 + 3 S

Rhenium diselenide (ReSe2) also has a layered structure, although, contrary to the other dichalcogenides, rhenium ditelluride does not. [16] In addition, rhenium also forms a heptoxide, which can be produced by the direct reaction of those elements, or through the reaction of ReO4− and H2S in 4N HCl. [17]

Perrhenates

Sample of sodium perrhenate, NaReO4 NaReO4.JPG
Sample of sodium perrhenate, NaReO4

The perrhenate ion is the anion with the formula ReO−
4, or a compound containing this ion. The perrhenate anion is tetrahedral, being similar in size and shape to perchlorate and the valence isoelectronic permanganate. The perrhenate anion is stable over a broad pH range and can be precipitated from solutions with the use of organic cations. At normal pH, perrhenate exists as metaperrhenate (ReO−
4), but at high pH mesoperrhenate (ReO3−
5) forms. Perrhenate, like its conjugate acid perrhenic acid, features rhenium in the oxidation state of +7 with a d0 configuration. Solid perrhenate salts takes on the color of the cation. [18] These salts are prepared by oxidation of rhenium compounds with nitric acid followed by neutralization of the resulting perrhenic acid. [19] [20] [21] Addition of tetrabutylammonium chloride to aqueous solutions of sodium perrhenate gives tetrabutylammonium perrhenate, which is soluble in organic solvents. [22]

Halides

Rhenium can form at least four fluorides, of which rhenium heptafluoride is the most common. This is the only thermally stable metal heptafluoride. [23] It has a pentagonal bipyramidal structure similar to IF7, [24] and can be prepared by the direct reaction of the elements at 400 °C. [25] Combining this with additional rhenium metal at 300 °C in a pressure vessel would produce rhenium hexafluoride. [26] It is one of the seventeen known binary hexafluorides. Both of these fluorides have a very low melting point. [27] In addition to this, rhenium also forms a pentafluoride, which form yellow-green crystals, [28] and a tetrafluoride, which forms blue crystals. [29]

The most common rhenium chlorides are ReCl6, ReCl5, ReCl4, and ReCl3. [23] The structures of these compounds often feature extensive Re-Re bonding, which is characteristic of this metal in oxidation states lower than VII. Salts of [Re2Cl8]2− feature a quadruple metal-metal bond. Although the highest rhenium chloride features Re(VI), fluorine gives the d0 Re(VII) derivative rhenium heptafluoride. Rhenium(III) chloride (ReCl3 or sometimes written as Re3Cl9), is a dark-red hygroscopic solid that is insoluble in ordinary solvents. It can be prepared by the thermal decomposition of rhenium(V) chloride. It is an early example of a cluster compound with metal-metal bonds. [30] Rhenium(III) bromide also adopts the same structure, and is a black lustrous crystalline solid. [31] [32] It can be obtained by the direct reaction between rhenium metal and bromine at 500 °C under nitrogen: [33]

6 Re + 9 Br2 → 2 Re3Br9

Rhenium also forms two iodides, rhenium tetraiodide, which can be reduced from perrhenic acid with hydrogen iodide, and rhenium triiodide, which forms from the decomposition of this. [34] [35] Like tungsten and molybdenum, with which it shares chemical similarities, rhenium forms a variety of oxyhalides. The oxychlorides are most common, and include ReOCl4, ReOCl3.

Organometallic compounds

Dirhenium decacarbonyl is a common entry point to other rhenium carbonyls. The general patterns are similar to the related manganese carbonyls. It is possible to reduce this dimer with sodium amalgam to Na[Re(CO)5] with rhenium in the formal oxidation state −1. Bromination of dirhenium decacarbonyl gives bromopentacarbonylrhenium(I), [36] then reduced with zinc and acetic acid to pentacarbonylhydridorhenium: [37]

Re2(CO)10 + Br2 → 2 Re(CO)5Br
Re(CO)5Br + Zn + HOAc → Re(CO)5H + ZnBr(OAc)

Bromopentacarbonylrhenium(I) is readily decarbonylated. In refluxing water, it forms the triaquo cation: [38]

Re(CO)5Br + 3 H2O → [Re(CO)3(H2O)3]Br + 2 CO

With tetraethylammonium bromide Re(CO)5Br reacts to give the anionic tribromide: [39]

Re(CO)5Br + 2 NEt4Br → [NEt4]2[Re(CO)3Br3] + 2 CO
Structure of methylrhenium trioxide. Methylrhenium-trioxide-3D-balls.png
Structure of methylrhenium trioxide.

Rhenium forms a variety of alkyl and aryl derivatives, often with pi-donor coligands such as oxo groups. Well known is methylrhenium trioxide ("MTO"), CH3ReO3 a volatile, colourless solid, a rare example of a stable high-oxidation state metal alkyl complex. This compound has been used as a catalyst in some laboratory experiments. It can be prepared by many routes, a typical method is the reaction of Re2O7 and tetramethyltin: [40]

Re2O7 + (CH3)4Sn → CH3ReO3 + (CH3)3SnOReO3

Analogous alkyl and aryl derivatives are known. Although PhReO3 is unstable and decomposes at –30 °C, the corresponding sterically hindered mesityl and 2,6-xylyl derivatives (MesReO3 and 2,6-(CH3)2C6H3ReO3) are stable at room temperature. The electron poor 4-trifluoromethylphenylrhenium trioxide (4-CF3C6H4ReO3) is likewise relatively stable. [41] MTO and other organylrhenium trioxides catalyze oxidation reactions with hydrogen peroxide as well as olefin metathesis in the presence of a Lewis acid activator. [42] Terminal alkynes yield the corresponding acid or ester, internal alkynes yield diketones, and alkenes give epoxides. MTO also catalyses the conversion of aldehydes and diazoalkanes into an alkene. [43]

Rhenium is also able to make complexes with fullerene ligands such as Re2(PMe3)4H8(η2:η2C60).

One of the first transition metal hydride complexes to be reported was (C5H5)2ReH. A variety of half-sandwich compounds have been prepared from (C5H5)Re(CO)3 and (C5Me5)Re(CO)3. Notable derivatives include the electron-precise oxide (C5Me5)ReO3 and (C5H5)2Re2(CO)4.

Pictures of rhenium compounds

See also

Related Research Articles

<span class="mw-page-title-main">Rhenium</span> Chemical element, symbol Re and atomic number 75

Rhenium is a chemical element; it has symbol Re and atomic number 75. It is a silvery-gray, heavy, third-row transition metal in group 7 of the periodic table. With an estimated average concentration of 1 part per billion (ppb), rhenium is one of the rarest elements in the Earth's crust. It has the third-highest melting point and second-highest boiling point of any element at 5869 K. It resembles manganese and technetium chemically and is mainly obtained as a by-product of the extraction and refinement of molybdenum and copper ores. It shows in its compounds a wide variety of oxidation states ranging from −1 to +7.

<span class="mw-page-title-main">Group 7 element</span> Group of chemical elements

Group 7, numbered by IUPAC nomenclature, is a group of elements in the periodic table. It contains manganese (Mn), technetium (Tc), rhenium (Re) and bohrium (Bh). This group lies in the d-block of the periodic table, and are hence transition metals. This group is sometimes called the manganese group or manganese family after its lightest member; however, the group itself has not acquired a trivial name because it belongs to the broader grouping of the transition metals.

Molybdenum trioxide describes a family of inorganic compounds with the formula MoO3(H2O)n where n = 0, 1, 2. The anhydrous compound is produced on the largest scale of any molybdenum compound since it is the main intermediate produced when molybdenum ores are purified. The anhydrous oxide is a precursor to molybdenum metal, an important alloying agent. It is also an important industrial catalyst. It is a yellow solid, although impure samples can appear blue or green.

<span class="mw-page-title-main">Perrhenic acid</span> Chemical compound

Perrhenic acid is the chemical compound with the formula Re2O7(H2O)2. It is obtained by evaporating aqueous solutions of Re2O7. Conventionally, perrhenic acid is considered to have the formula HReO4, and a species of this formula forms when rhenium(VII) oxide sublimes in the presence of water or steam. When a solution of Re2O7 is kept for a period of months, it breaks down and crystals of HReO4·H2O are formed, which contain tetrahedral ReO−4. For most purposes, perrhenic acid and rhenium(VII) oxide are used interchangeably. Rhenium can be dissolved in nitric or concentrated sulfuric acid to produce perrhenic acid.

<span class="mw-page-title-main">Ammonium perrhenate</span> Chemical compound

Ammonium perrhenate (APR) is the ammonium salt of perrhenic acid, NH4ReO4. It is the most common form in which rhenium is traded. It is a white salt; soluble in ethanol and water, and mildly soluble in NH4Cl. It was first described soon after the discovery of rhenium.

<span class="mw-page-title-main">Manganese heptoxide</span> Chemical compound

Manganese(VII) oxide (manganese heptoxide) is an inorganic compound with the formula Mn2O7. Manganese heptoxide is a volatile liquid with an oily consistency. It is a highly reactive and powerful oxidizer that reacts explosively with nearly any organic compound. It was first described in 1860. It is the acid anhydride of permanganic acid.

<span class="mw-page-title-main">Rhenium(VII) oxide</span> Chemical compound

Rhenium(VII) oxide is the inorganic compound with the formula Re2O7. This yellowish solid is the anhydride of HOReO3. Perrhenic acid, Re2O7·2H2O, is closely related to Re2O7. Re2O7 is the raw material for all rhenium compounds, being the volatile fraction obtained upon roasting the host ore.

Rhenium trioxide or rhenium(VI) oxide is an inorganic compound with the formula ReO3. It is a red solid with a metallic lustre that resembles copper in appearance. It is the only stable trioxide of the Group 7 elements (Mn, Tc, Re).

<span class="mw-page-title-main">Sodium perrhenate</span> Chemical compound

Sodium perrhenate (also known as sodium rhenate(VII)) is the inorganic compound with the formula NaReO4. It is a white salt that is soluble in water. It is a common precursor to other rhenium compounds. Its structure resembles that of sodium perchlorate and sodium permanganate.

<span class="mw-page-title-main">Bromopentacarbonylrhenium(I)</span> Chemical compound

Bromopentacarbonylrhenium(I) is an inorganic compound of rhenium, commonly used for the syntheses of other rhenium complexes.

<span class="mw-page-title-main">Dirhenium decacarbonyl</span> Chemical compound

Dirhenium decacarbonyl is the inorganic compound with the chemical formula Re2(CO)10. Commercially available, it is used as a starting point for the synthesis of many rhenium carbonyl complexes. It was first reported in 1941 by Walter Hieber, who prepared it by reductive carbonylation of rhenium. The compound consists of a pair of square pyramidal Re(CO)5 units joined via a Re-Re bond, which produces a homoleptic carbonyl complex.

<span class="mw-page-title-main">Potassium nonahydridorhenate</span> Chemical compound

Potassium nonahydridorhenate(VII) is an inorganic compound having the formula K2[ReH9]. This colourless salt is soluble in water but only poorly soluble in most alcohols. This salt contains the nonahydridorhenate(VII) anion, [ReH9]2−, which is a rare example of a coordination complex bearing only hydride ligands.

<span class="mw-page-title-main">Methylrhenium trioxide</span> Chemical compound

Methylrhenium trioxide, also known as methyltrioxorhenium(VII), is an organometallic compound with the formula CH3−ReO3. It is a volatile, colourless solid that has been used as a catalyst in some laboratory experiments. In this compound, rhenium has a tetrahedral coordination geometry with one methyl and three oxo ligands. The oxidation state of rhenium is +7.

<span class="mw-page-title-main">Oxotrichlorobis(triphenylphosphine)rhenium(V)</span> Chemical compound

Oxotrichlorobis(triphenylphosphine)rhenium(V) is the chemical compound with the formula ReOCl3(PPh3)2. This yellow, air-stable solid is a precursor to a variety of other rhenium complexes. In this diamagnetic compound, Re has an octahedral coordination environment with one oxo, three chloro and two mutually trans triphenylphosphine ligands. The oxidation state of rhenium is +5 and its configuration is d2.

<span class="mw-page-title-main">Rhenium(IV) oxide</span> Chemical compound

Rhenium(IV) oxide or rhenium dioxide is the inorganic compound with the formula ReO2. This gray to black crystalline solid is a laboratory reagent that can be used as a catalyst. It adopts the rutile structure.

The perrhenate ion is the anion with the formula ReO−
4, or a compound containing this ion. The perrhenate anion is tetrahedral, being similar in size and shape to perchlorate and the valence isoelectronic permanganate. The perrhenate anion is stable over a broad pH range and can be precipitated from solutions with the use of organic cations. At normal pH, perrhenate exists as metaperrhenate, but at high pH mesoperrhenate forms. Perrhenate, like its conjugate acid perrhenic acid, features rhenium in the oxidation state of +7 with a d0 configuration. Solid perrhenate salts takes on the color of the cation.

Organorhenium chemistry describes the compounds with Re−C bonds. Because rhenium is a rare element, relatively few applications exist, but the area has been a rich source of concepts and a few useful catalysts.

<span class="mw-page-title-main">Chromyl fluoride</span> Chemical compound

Chromyl fluoride is an inorganic compound with the formula CrO2F2. It is a violet-red colored crystalline solid that melts to an orange-red liquid.

<span class="mw-page-title-main">Rhenium trioxide chloride</span> Chemical compound

Rhenium trioxide chloride is an inorganic compound with the formula ReO3Cl. It is a colorless, distillable, diamagnetic liquid. It is a rhenium oxychloride. The material is used as a reagent in the preparation of rhenium compounds.

Rhenium trioxynitrate, also known as rhenium(VII) trioxide nitrate, is a chemical compound with the formula ReO3NO3. It is a white solid that readily hydrolyzes in moist air.

References

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