Strukturen und thermische Zersetzung von enH2(H3O)[AlF6] und enH2[AlF5(H2O)]

Structures and Thermal Decomposition of enH₂(H₃O)[AlF₆] and enH₂[AlF₅(H₂O)] By precipitation with ethylene diamine (en) from a hydrofluoric acid solution of aluminium enH₂(H₃O)[AlF₆] is formed. It crystallizes in the orthorhombic space group Pnma, a = 1084.9(1), b = 1079.4(1), c = 682.0(1) pm, R = 0.032. H₃O⁺ cations and [AlF₆]^3– anions are connected via strong H bonds to layers which are further linked to a 3 D network by H bonds from the enH₂²⁺ cations. By recrystallization from water or precipitation from a less acid solution enH₂[AlF₅(H₂O)] is formed, which crystallizes monoclinic in the space group P2₁ (a = 660.0(1), b = 563.5(1), c = 994.4(2) pm, β = 98.44(3)°, R = 0.029). The [AlF₅(H₂O)]^2– anions are linked by strong O–H…F bonding to form ‘einer-double chains' interconnected again via the enH₂²⁺ cations to a 3 D framework. Thermoanalytical investigations show that enH₂[AlF₅(H₂O)], by loss of water above 150 °C, as well as enH₂(H₃O)[AlF₆], by loss of water and HF above 120 °C, transform to enH₂AlF₅. The subsequent decomposition goes over NH₄⁺ containing intermediates towards β-AlF₃. Before decomposition the oxonium fluoroaluminate reveals a reversible phase transition at 99 °C.     

Synthese,Kristallstrukturen und Magnetismus von (Hg6As4)[MoCl6]Cl, (Hg6As4)[TiCl6]Cl und (Hg6As4)[TiBr6]Br

Polycationic Hg–As Frameworks with Trapped Anions. II Synthesis, Crystal Structure, and Magnetism of (Hg₆As₄)[MoCl₆]Cl, (Hg₆As₄)[TiCl₆]Cl, and (Hg₆As₄)[TiBr₆]Br (Hg₆As₄)[MoCl₆]Cl is obtained by reaction of Hg₂Cl₂, Hg, As, and MoCl₄ in closed, evacuated glass ampoules in a temperature gradient 450 → 400 °C in form of dark red cubelike crystals. (Hg₆As₄)[TiCl₆]Cl and (Hg₆As₄)[TiBr₆]Br are also formed in closed, evacuated ampoules from Hg₂X₂ (X = Cl, Br), Hg, As, and Ti metal at 275 °C and 245 °C in form of dark green and black crystals, respectively. All three compounds are air and light sensitive. They crystallize isotypically (cubic, Pa 3, a = 1207.8(4) pm for (Hg₆As₄)[MoCl₆]Cl, a = 1209.4(3) pm for (Hg₆As₄)[TiCl₆]Cl, a = 1230.9(3) pm for (Hg₆As₄)[TiBr₆]Br, Z = 4). The structures consist of a three‐dimensionally connected Hg–As framework which is made up of As₂ groups (As–As distance averaged 242 pm) each connected via six Hg atoms to six neighbouring As₂ groups. There are two cavities of different size in the polycationic framework. The bigger cavity is filled with [MoCl₆]^3–, [TiCl₆]^3–, and [TiBr₆]^3– ions of nearly ideal octahedral shape, the smaller cavity with discrete halide ions. The magnetic properties of the two Ti containing compounds are in accordance with a d¹ paramagnetism. The temperature dependence and the magnitude of the magnetic moment can be interpreted with consideration of the spin‐orbit coupling. The so far known representatives of this structure type can be characterised by the ionic formula (Hg₆Y₄)⁴⁺[MX₆]^3–X^– (Y = As, Sb; M = Sb³⁺, Bi³⁺, Mo³⁺, Ti³⁺; X = Cl, Br).     

Neue Oxonium-Bromochalkogenate(IV) — Darstellung,Struktur und Eigenschaften von [H3O][TeBr5] · 3C4H8O2 und [H3O]2[SeBr6]

New Oxonium Bromochalcogenates(IV) — Synthesis, Structure, and Properties of [H₃O][TeBr₅] · 3 C₄H₈O₂ and [H₃O]₂[SeBr₆] Dark red crystals of the composition [H₃O][TeBr₅] · 3 C₄H₈O₂ ( 1 ) were isolated from a saturated solution of TeBr₄ in 1,4-dioxane containing a small amount of water. In this compound (space group P2₁/m, a = 8.922(4) Å, b = 13.204(7) Å, c = 9.853(5) Å, β = 91.82(4)° at 150 K) a square pyramidal [TeBr₅]^? anion has been isolated for the first time. The coordination sphere of the anion is completed to a distorted octahedron by weak interaction with a dioxane molecule of the cationic system. The [H₃O]⁺ cations are connected to chains by dioxane molecules. At room temperature the compound is stable only in its mother liquor. Crystalline [H₃O]₂[SeBr₆] ( 2 ) (space group Fm3m, a = 10.421(1) Å at 170 K) is a bromoselenous acid of high symmetry. The [H₃O]⁺ ion is only weakly coordinated by Br atoms of the anion. The anions are isolated octahedral [SeBr₆]^2? units. The structure is isotypic to the K₂[PtCl₆] structure. Despite being a halogenochalcogen(IV) acid, 2 exhibits a remarkable thermal stability. Both oxonium compounds were characterized by single-crystal X-ray structure analyses. Vibrational spectra of 2 are reported.     

Synthese und Kristallstrukturen der Thiochloroantimonate(III) PPh4[Sb2SCl5] und (PPh4)2[Sb2SCl6] · CH3CN

Syntheses and Crystal Structures of the Thiochloroantimonates(III) PPh₄[Sb₂SCl₅] and (PPh₄)₂[Sb₂SCl₆]. CH₃CN (PPh₄)₂Sb₃Cl₁₁, obtained from Sb₂S₃, PPh₄Cl and HCl, reacts with Na₂S₄ in acetonitrile forming PPh₄[Sb₂SCl₅]. From this and Na₂S₄ or from (PPh₄)₂[Sb₂Cl₈] and Na₂S₄ or K₂S₅ in acetonitrile (PPh₄)₂[Sb₂SCl₆] · CH₃CN is obtained. Data obtained from the X-ray crystal structure determinations are: PPh₄[Sb₂SCl₅], monoclinic, space group P2₁/c, a = 1002.9(3), b = 1705.6(5), c = 1653.7(5) pm, β = 99.12(2)°, Z = 4, R = 0.068 for 1283 reflextions; (PPh₄)₂[Sb₂SCl₆] · CH₃CN, triclinic, space group P1 , a = 1287.8(7), b = 1343.6(9), c = 1696.5(9) pm, α = 69.82(5), β = 85.08(4), γ = 71.54(6)°, Z = 2, R = 0.059 for 6409 reflexions. In every anion two Sb atoms are linked via one sulfur and one ore two chloro atoms, respectively. Paris of [SbSCl₅]^? ions are associated via Sb …? S and Sb …? Cl contacts forming dimer units. In both compounds every Sb atom has a distorted octahedral coordination when the lone electron pair is included in the counting.     

Dithiolylium‐Chlorooxomolybdate(V): Synthese und Kristallstruktur von (C3Cl3S2)[MoOCl4] und (C3Cl3S2)[Mo2O2Cl7]

Dithiolylium Chlorooxomolybdates(V): Synthesis and Crystal Structure of (C₃Cl₃S₂)[MoOCl₄] and (C₃Cl₃S₂)[Mo₂O₂Cl₇] The reaction of 3, 4, 5‐Trichlor‐1, 2‐dithiolylium chloride with MoOCl₃ in dichlormethane under solvothermal conditions at 65 °C simultaneously yields the green tetrachlorooxomolybdate(V) (C₃Cl₃S₂)[MoOCl₄] and the yellow‐brown heptachlorodioxodimolybdate(V) (C₃Cl₃S₂)[Mo₂O₂Cl₇]. The crystal structures of both compounds contain nearly planar (C₃Cl₃S₂)⁺ ions with a S—S bond length of 203 pm. The discrete [MoOCl₄]^— ion in the structure of (C₃Cl₃S₂)[MoOCl₄] has the shape of a square pyramid with the oxygen atom at the apex. The molybdenum atom is displaced by 58 pm from the basal plane towards the oxygen atom. The [Mo₂O₂Cl₇]^— ion in the structure of (C₃Cl₃S₂)[Mo₂O₂Cl₇] has the form of a face‐sharing double octahedron. It is formally composed of a [MoOCl₄]^— ion and a MoOCl₃ molecule connected by one symmetrical and two unsymmetrical chloro bridges. The molybdenum atoms placed in the centers of such connected octahedra are 357 pm apart, indicating no Mo—Mo bond.     

Rubidium-decaamidodichromat(III), Rb4Cr2(NH2)10 – Synthese und Kristallstruktur

Rubidium Decaamidodichromate(III), Rb₄Cr₂(NH₂)₁₀ – Synthesis and Crystal Structure The reaction of chromium(III) with rubidium amide in a molar ratio of Cr(NH₂)₃/RbNH₂ = 1 : 1.75 at 140 °C and p(NH₃) = 3 kbar in a high-pressure autoclave results after 90 days in dark violet crystals of Rb₄Cr₂(NH₂)₁₀. Structure determination was done by single crystal X-ray methods:Pna2₁ (No. 33), Z = 4, a = 12.244(3) Å, b = 6.727(1) Å, c = 19.775(5) Å, N(F²_o > 3σ(F²_o)) = 1046, N(Var.) = 94, R/R_w = 0,051/0,059&#TAB;The structure of Rb₄Cr₂(NH₂)₁₀ contains isolated, face-sharing N-octahedra around two Cr³⁺-ions giving [Cr(NH₂)₃(NH₂)_3/2]₂^3–. These are arranged to oneanother following the motif of a hexagonal closest packing. They are connected via Rb⁺- and one further amide ion not bound to Cr³⁺. The compound is characterized by thermoanalytical and IR-/Raman-spectroscopic measurements.     

Darstellung,spektroskopische Charakterisierung und Kristallstruktur von (CF3)2C(F)OH2+Sb2F11–

Preparation, Spectroscopic Characterization, and Crystal Structure of (CF₃)₂C(F)OH₂⁺Sb₂F₁₁^– Hexafluoroacetone, (CF₃)₂CO, reacts at –78 °C with the superacid HF/SbF₅ under formation of the primary oxonium salt, (CF₃)₂C(F)OH₂⁺Sb₂F₁₁^–, which is characterized by vibrational spectroscopy and NMR spectra. The salt crystallizes in the triclinic space group P1 with a = 817.9(1), b = 989.0(1), c = 1003.8(1) pm and 2 formula units per unit cell.     

Synthese und Kristallstruktur von LiAl[(P2O6)2]

Synthesis and Crystal Structure Determination of LiAl[(P₂O₆)₂] Single crystals of previously unknown LiAl[(P₂O₆)₂] have been obtained by reaction of Li₂CO₃, Al₂O₃ and H₃PO₄ (1:1:16) at 350°C. The title compound crystallizes in Pbcn (a = 1 244.54(1), b = 823.40(1), c = 892.46(1) pm; Z = 4). The least-squares refinement (with anisotropic temperature factors) was performed using 766 observed reflections yielding R = 0.029 and R(w) = 0.075. Four anion chains are running parallel to the shortest axis in the unit cell, the period of identity amounting to four. Aluminium is surrounded by an almost regular octahedron, lithium by a distorted tetrahedron of oxygen.     

Zur Synthese und Kristallstruktur von LiPdAlF6 und PdZrF6

Synthesis and Crystal Structure of LiPdAlF₆ and PdZrF₆ . For the first time single crystals of the new compounds LiPdAlF₆ and PdZrF₆ have been obtained. LiPdAlF₆ (blue) crystallizes trigonal, space group P3 1c—D (No. 163; LiCaAlF₆-type [2]), in an ordered structure variant of the Li₂[ZrF₆]-structure [3], with a=497.21(9) pm, c=914.0(9) pm and Z=2. PdZrF₆ (also blue) is isotypic with LiSbF₆ [4] and crystallizes trigonal-rhomboedric with a=552,3(1) pm, c=1 447,5(4) pm, space group R 3 —C (No. 148) and Z=3.     

Darstellung und Kristallstruktur von (CH3NH3)8[NdCl6][NdCl4(H2O)2]2Cl3

Preparation and Crystal Structure of (CH₃NH₃)₈[NdCl₆][NdCl₄(H₂0)₂]₂Cl₃ (CH₃NH₃)₈[NdCl₆][NdCl₄ (H₂O)₂]₂Cl₃ is for the first time prepared and investigated by X-ray, single crystal work. It crystallizes in the monoclinic system (space group C2/m, Z = 2) with a = 9.358(5), b = 17.424(9), c = 15.360(8) Å, β = 108.30(4)°. The structure contains besides isolated Cl^? ions distorted [NdCl₆]^3? octahedra and [NdCl₄(H₂O)₂]^? chains.     

Zur Kristallstruktur von La[AuF4]3, dem Anfangsglied der Reihe M[AuF4]3−xFx (x = 0, 0,5 und 1)

On the Crystal Structure of La[AuF₄]₃, the Final Link in the Series M[AuF₄]_3?xF_x (x = 0, 0.5 and 1) Yellow La(AuF₄)₃ was prepared for the first time in form of single crystals and investigated by X-ray methods. It crystallizes in space group R3 c-D (Nr. 167) with a = 1056.2(2) pm, c = 1633.7(8) pm, Z = 6.     

Benzodithiazolium‐Chlorooxomolybdate(V): Darstellung und Kristallstruktur von (C6H4NS2)[MoOCl4] und (C6H4NS2)[MoOCl4·H2O]

Benzodithiazolium Chlorooxomolybdate(V): Preparation and Crystal Structure of (C₆H₄NS₂)[MoOCl₄] and (C₆H₄NS₂)[MoOCl₄·H₂O] Red benzo‐1,3,2‐dithiazolium‐chlorooxomolybdate(V) (C₆H₄NS₂)[MoOCl₄] ( 1 ) was obtained by the reaction of benzo‐1,3,2‐dithiazoliumchloride and molybdenum(V)chloride oxide in dichlormethane under solvothermal conditions at 70 °C. In the presence of small amounts of concentrated hydrochloric acid the yellow compound (C₆H₄NS₂)[MoOCl₄·H₂O] ( 2 ) is formed under analogue conditions. Both crystal structures ( 1 : monoclinic, C2/c, a = 799.2(1), b = 2091.5(2), c = 791.5(1) pm, β = 102.2(1)°, Z = 4; 2 : monoclinic, Cc, a = 953.7(1), b = 2468.9(3), c = 608.1(1) pm, β = 112.5(1)°, Z = 4) contain the planar benzo‐1,3,2‐dithiazolium ion. Within the structure of 1 the molybdenum atoms in the [MoOCl₄]^? ions are coordinated in a square pyramidal fashion with an oxygen atom in apical position and the basal plane formed by chlorine atoms. The nitrogen atom of the cation, which bears a partial negativ charge, expands the coordination to a distorted octahedron. The structure therefore is made up of ionic pairs {(C₆H₄NS₂)⁺ [MoOCl₄]^?} with a Mo–N distance of 266 pm. 1 is paramagnetic with a magnetic moment of 1.7 B.M. corresponding to one unpaired electron per formula unit. In the structure of 2 the coordination of the [MoOCl₄]^? ion is expanded by the oxygen atom of a coordinating water molecule. The structure is dominated by hydrogen bonds between the oxygen atoms of the [MoOCl₄·H₂O]^? ions which cause the concatenation of the anions to infinite chains.     

NiH3IO6 · 6H2O — Kristallstruktur und Schwingungsspektren

NiH₃IO₆ · 6 H₂O — Crystal Structures and Vibrational Spectra The crystal structure of NiH₃IO₆ · 6 H₂O has been determined by X-ray single-crystal diffraction (Pc, Z = 2, a = 516.74(9), b = 981.5(2), c = 1052.5(2) pm, β = 116.496(8)°) on the basis of 4169 unique reflections (R = 1.96%). The structure is built up of distorted Ni(H₂O)₆²⁺ and H₃IO₆^2? octahedra linked by hydrogen bonding. IR and Raman spectra of both the title compound and isostructural MgH₃IO₆ · 6 H₂O as well as of deuterated specimens are given. There are up to 14 different OH(OD) modes in the spectra of isotopically dilute samples due to the 15 different hydrogen positions of the structure. The internal modes of the meridional H₃IO₆^2? ions (pseudo C_2v symmetry) are discussed with respect to that double T-shaped entity, which gives rise to only two instead of 3I? O, I? O(H), and OH stretches in the IR and Raman spectra, i.e. the same as for facial (C_3v) structured ions.     

Lithiumtriamidostannat(II), Li[Sn(NH2)3] – Synthese und Kristallstruktur

Lithium Triamidostannate(II), Li[Sn(NH₂)₃] – Synthesis and Crystal Structure Rusty-red glistening, transparent crystals of Li[Sn(NH₂)₃] were obtained by reaction of metallic lithium with tetraphenyl tin in liquid ammonia at 110 °C. The structure was determined from X-ray single-crystal diffractometer data: Space group P 2₁/n, Z = 4, a = 8.0419(9) Å, b = 7.1718(8) Å, c = 8.5085(7) Å, β = 90.763(8)°, R₁ (F _o ≥ 4σ(F _o)) = 2.8%, wR₂ (F ≥ 2σ(F )) = 5.3%, N(F ≥ 2σ(F )) = 1932, N(Var.) = 65. The crystal structure contains trigonal pyramidal complex anions [Sn(NH₂)₃]^– with tin at the apex, which are connected to layers of sequence A B A B … by lithium in tetrahedra-double units [Li(NH₂)_2/2(NH₂)₂]₂.     

Synthese und Kristallstruktur von Ba2ScCl7, ein Bariumchlorid-hexachloroscandat(III), Ba2Cl[ScCl6]

Synthesis and Crystal Structure of Ba₂ScCl₇, a Barium Chloride Hexachloroscandate(III), Ba₂Cl[ScCl₆] Colourless single crystals of Ba₂ScCl₇ are obtained from a 1 : 1 molar mixture of BaCl₂ and ScCl₃. It crystallizes with the non-centrosymmetric monoclinic space group P2₁ with a = 688,88(7), b = 1349,4(1), c = 1207,4(1), β = 94,93(1)° in a new structure that contains isolated [ScCl₆] octahedra and one ‘‘lonesome”︁”︁ chloride ligand according to Ba₂Cl[ScCl₆].     

Synthese,Kristallstruktur und spektroskopische Charakterisierung von Tetraphosphorhexaoxiddiselenid P4O6Se2

Synthesis, Crystal Structure, and Spectroscopic Characterization of Tetraphosphorus Hexaoxide Diselenide P₄O₆Se₂ P₄O₆Se₂ has been prepared by photochemical selenation of P₄O₆ with red selenium in CS₂ in presence of catalytical amounts of iodine. Isolation and single crystal growth were performed by fractional crystallization and subsequent sublimation. The compound crystallizes in the monoclinic space group P2₁/c (Nr. 14) with a = 11.473(2); b = 6.536(1); c = 11.796(2) Å; β = 90.06(1)°; Z = 4; R₁ = 0.030; wR² = 0.073. Within the limits of experimental error, the P₄O₆Se₂ molecules exhibit C_2v symmetry in the crystal. Bond lengths and angles within the molecule as well as the arrangement of the molecules within the crystal are discussed; IR-, Raman-, and ³¹P solution NMR data are reported.     

Synthese und Kristallstruktur von [Fe(MeCN)6][Fe2OCl6]

Synthesis and Crystal Structure of [Fe(MeCN)₆][Fe₂OCl₆] [Fe(MeCN)₆][Fe₂OCl₆] ( 2 ) is obtained by passing dry air through a solution of FeCl₂ in acetonitrile in almost quantitative yield. 2 crystallises in the trigonal space group R 3 [a = b = 12.121(1), c = 29.875(6) Å, Z = 6]. The oxygen atom in the Fe₂OCl₆ anion occupies the 3 position and causes therefore an Fe–O–Fe angle of 180°. The refinement in the triclinic space group P1 leads to a slightly bent arrangement of the Fe–O–Fe fragment.     

Synthese,Kristallstruktur und thermischer Abbau von Mg(H2O)6[B12H12] · 6 H2O

Synthesis, Crystal Structure, and Thermal Decomposition of Mg(H₂O)₆[B₁₂H₁₂] · 6 H₂O By reaction of an aqueous solution of the free acid (H₃O)₂[B₁₂H₁₂] with MgCO₃ and subsequent isothermic evaporation of the resulting solution to dryness, colourless, bead‐shaped single crystals of the dodecahydrate of magnesium dodecahydro closo‐dodecaborate Mg(H₂O)₆[B₁₂H₁₂] · 6 H₂O (cubic, F4₁32; a = 1643.21(9) pm, Z = 8) emerge. The crystal structure is best described as a NaTl‐type arrangement in which the centers of gravity of the quasi‐icosahedral [B₁₂H₁₂]^2— anions (d(B—B) = 178—180 pm, d(B—H) = 109 pm) occupy the positions of Tl^— while the Mg²⁺ cations occupy the Na⁺ positions. A direct coordinative influence of the [B₁₂H₁₂]^2— units at the Mg²⁺ cations is however not noticeable. The latter are octahedrally coordinated by six water molecules forming isolated hexaaqua complex cations [Mg(H₂O)₆]²⁺ (d(Mg—O) = 206 pm, 6×). In addition, six “zeolitic” water molecules are located in the crystal structure for the formation of a strong O—H^δ+···^δ—O‐hydrogen bridge‐bonding system. The evidence of weak B—H^δ—···^δ+H—O‐hydrogen bonds between water molecules and anionic [B₁₂H₁₂]^2— clusters is also considered. Investigations on the dodecahydrate Mg[B₁₂H₁₂] · 12 H₂O (≡ Mg(H₂O)₆[B₁₂H₁₂] · 6 H₂O) by DTA/TG measurements showed that its dehydration takes place in two steps within a temperature range of 71 and 76 °C as well as at 202 °C, respectively. Thermal treatment eventually leads to the anhydrous magnesium dodecahydro closo‐dodecaborate Mg[B₁₂H₁₂].     

Ein neues Oxophosphat (IV/III)-Anion – Darstellung und Kristallstruktur von Na6P4O10 · 2 H2O

A New Oxophosphate (IV/III) Anion – Preparation and Crystal Structure of Na₆P₄O₁₀ · 2 H₂O A new oxophosphate anion, P₄O₁₀^6?, was obtained by cleavage and simultaneous oxidation of the cyclo-hexaphosphate(III) anion in a solution of aqueous ammonia and ethanol. With sodium it forms a salt with the composition Na₆P₄O₁₀ · 2 H₂O. The crystal structure has been determined by single crystal X-ray diffraction (3 745 diffractometer data), the cell constants were obtained from X-ray powder data, space group P1 ; a = 6.004(1), b = 6.173(2), c = 11.496(2) Å, α = 99.26(2)°, β = 95.92(2)°, γ = 117.63(2)°, Z = 1, R = 0.044. The backbone of the anion is formed by phosphorus atoms directly bonded to each other. The coordination of each phosphorus atom is completed to four by oxygene. The resulting oxidation numbers are +III for the inner phosphorus atoms and +IV for the terminal phosphorus atoms. The site symmetry of the anion is approximately C_2h. Based on a ³¹P-NMR spectra of a solution the coupling constants of the AA ‘BB’ system were determined.     

Synthese,Kristallstruktur und thermischer Abbau von Cs1,5[Re3I3Cl7,5(H2O)1,5]

Synthesis, Crystal Structure and Thermal Behaviour of Cs_1,5[Re₃I₃Cl_7,5(H₂O)_1,5] Dark brown tetrahedra of Cs_1,5[Re₃I₃Cl_7,5(H₂O)_1,5] crystallize on slow cooling of a hot saturated solution of ReI₃ and CsCl in conc. hydrochlorid acid. The crystal structure (cubic, P4 3m (No. 215), a = 1241.06(3)pm, V_m = 287.8(1) cm³mol^?1, Z = 4, R = 0.067, R_w = 0.037) is built up from isolated building units [Re₃I₃Cl_7,5(H₂O)_1,5]^1,5? with statistical distribution of chloride ions and water molecules in the in plane, terminal positions. Consistent with the result based on the X-ray analysis, the IR-spectrum shows one band for the OH stretching frequencies of the water molecules coordinated to the Re₃ triangle at 3240 cm^?1. The anions are arranged in the fashion of a cubic closest packing with the cesium ions occupying all octahedral and one quarter of the tetrahedral interstices. Temperature-dependent Guinier-Simon photographs in connection with DTA/TG investigations reveal that Cs_1,5[Re₃I₃Cl_7,5(H₂O)_1,5] releases water at 190°C accompanied with a structural transition and the dehydration product decomposes at 370°C to Cs₂ReCl_6?xI_x, Re₃I_3+yCl_6?y and rhenium metal.