The metavoltine problem: Relationships between metavoltine and Maus' salt

Scordari, Fernando; Vurro, Francesca; Menchetti, Silvio

doi:10.1007/bf01081304

Cited by 13 publications

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“…This study was undertaken to obtain a more complete crystal-chemical knowledge of a group of natural and synthetic compounds whose structures are based on [Fe]+(H20)aO(SO4)6] ~-units, as in metavoltine (Scordari, Vurro & Menchetti, 1975;Giacovazzo, Scordari, Todisco & Menchetti, 1976) and a-Maus's salt (Giacovazzo, Scordari & Menchetti, 1975). Blaas (1883) claimed that metavoltine from Madeni Zakh, Iran, and a-Maus's salt were very similar.…”

Section: Introductionmentioning

confidence: 99%

The structure of K₂(K_0.41,H₂O_0.59)₆Na_3.98H₃O_0.78 ⁺ X _0.68 ⁺(F_0.05 ²⁺,vacancy_0.95)Fe₆ ³⁺O₂(SO₄)₁₂.11.91H₂O: a compound related to metavoltine and α-Maus's salt

Scordari¹

1980

Acta Crystallogr Sect B

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Xo.6a (Feo.os,Do.95 AbstractA synthetic phase, obtained by complete evaporation at about 353K of an aqueous solution containing iron(III), hydrated sodium sulfates and potassium sulfate, has been found to be an interesting compound related to metavoltine, K2Na6(Fe2+,Cu,Zn)Fe3+O2 -(SO4)12.18H20 , and to a-Maus's salt, KsFe~ +-O(SO4) 6. 10H20. The occupancy coefficients lead to structure models in agreement with space group P1, although the structure of this compound has been solved in P3. Lattice parameters are a = b = 9.643, c = 18.018 A, and Z = 1. The crystal structure has been determined from X-ray data collected on an automated diffractometer by means of Patterson and Fourier syntheses. The least-squares refinement using 2542 observed reflections led to a conventional R value of 0.086 with isotropic temperature factors. Like metavoltine and a-Maus's salt, the present structure is based on [Fe]+(H20)30(SO4)6] 5-clusters which are essentially linked to each other by alkaline ions and hydrogen bonds. As in a-Maus's salt, some sites are statistically occupied by K atoms and water molecules forming rings around the trigonal axis, while as in metavoltine, one site is occupied by an Fe 2+ cation; this site appears to be much less occupied in the present salt.

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Section: Introductionmentioning

confidence: 99%

The structure of K₂(K_0.41,H₂O_0.59)₆Na_3.98H₃O_0.78 ⁺ X _0.68 ⁺(F_0.05 ²⁺,vacancy_0.95)Fe₆ ³⁺O₂(SO₄)₁₂.11.91H₂O: a compound related to metavoltine and α-Maus's salt

Scordari¹

1980

Acta Crystallogr Sect B

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“…This suppresses the hydrolytic polymerization and affords the opportunity to crystallize potential reaction intermediates. Indeed, the aqueous analogue of the Fe 3 subunit ([Fe 3 O(SO 4 ) 6 (H 2 O) 3 ] 5– ) exists both in natural mineral (e.g., carlsonite (Figure S5a) and metavoltine , (Figure S5b)) and synthetic structures (Maus’ salt (Figure S6)). This provides strong evidence that the relevant Fe(III) clusters do form in aqueous environments, and that the MeOH substitution for the bound waters does not dramatically bias this polynuclear assembly.…”

Section: Resultsmentioning

confidence: 99%

Stabilizing Reactive Fe(III) Clusters by Freeze-Dry/Solvent-Exchange To Benchmark Iron Hydrolysis Pathways

et al. 2019

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Isolating Fe(III) clusters from water without stabilizing ligands is significantly challenged by the high acidity of Fe3+-bound water, leading to uncontrolled precipitation of iron oxyhydroxides. Here we demonstrate a freeze-drying solvent-exchange method that enabled the isolation of a metastable Fe(III) sulfate decameric cluster formulated [Fe10O2(SO4)12(OCH3)2]·14CH3OH (Fe 10 ). Without stabilization by solvent-exchange, the aqueous species undergoes rapid conversion to the iron sulfate mineral schwertmannite. Monitoring the hydrolysis process from cluster intermediates to schertmannite by small-angle X-ray scattering, we observe the progression from Fe 10 to 37 Å soluble nanoparticles prior to the precipitation process. This condensation behavior of Fe 10 is further exploited to develop a simple laboratory synthesis of schwetmannite. In addition, we demonstrate the versatility of the freeze-drying solvent-exchange method by isolating Al(III), Zn(II), and Cd(II) substituted Fe(III) sulfate clusters. The freeze-drying solvent-exchange method provides a unique opportunity to isolate cluster intermediates and models to aid in our understanding of metal-ion hydrolysis processes in environmental, material science, and geological studies.

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“…Metavoltine was first described by Blass [23] from Madeni Zakh, Hormozgan, Iran, and its actual definition had been questioned, owing to the uncertain relationships with synthetic Maus' Salt [24,25]. Only the solution of the crystal structure of metavoltine by Giacovazzo et al [19] allowed for an accurate definition of this mineral.…”

Section: Scordariite and Metavoltine: A Comparisonmentioning

confidence: 99%

Crystal Chemistry of Sulfates from the Apuan Alps (Tuscany, Italy). V. Scordariite, K8(Fe3+0.67□0.33)[Fe3+3O(SO4)6(H2O)3]2(H2O)11: A New Metavoltine-Related Mineral

et al. 2019

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The new mineral species scordariite, K8(Fe3+0.67□0.33)[Fe3+3O(SO4)6(H2O)3]2(H2O)11, was discovered in the Monte Arsiccio mine, Apuan Alps, Tuscany, Italy. It occurs as pseudo-hexagonal tabular crystals, yellowish to brownish in color, up to 0.5 mm in size. Cleavage is perfect on {0001}. It is associated with giacovazzoite, krausite, gypsum, jarosite, alum-(K), and magnanelliite. Electron microprobe analyses give (wt %): SO3 47.31, Al2O3 0.66, Fe2O3 24.68, FeO 0.69, Na2O 0.52, K2O 17.36, H2Ocalc 15.06, total 106.28. The partitioning of Fe between Fe2+ and Fe3+ was based on Mössbauer spectroscopy. On the basis of 67 O atoms per formula unit, the empirical chemical formula is (K7.50Na0.34)Σ7.84(Fe3+6.29Al0.26Fe2+0.20)Σ6.75S12.02O50·17H2O. The ideal end-member formula can be written as K8(Fe3+0.67□0.33)[Fe3+3O(SO4)6(H2O)3]2(H2O)11. Scordariite is trigonal, space group R-3, with (hexagonal setting) a = 9.7583(12), c = 53.687(7) Å, V = 4427.4(12) Å3, Z = 3. The main diffraction lines of the observed X-ray powder pattern are [d(in Å), estimated visual intensity]: 8.3, strong; 6.6, medium; 3.777, medium; 3.299, medium; 3.189, medium; 2.884, strong. The crystal structure of scordariite has been refined using X-ray single-crystal data to a final R1 = 0.057 on the basis of 1980 reflections with Fo > 4σ(Fo) and 165 refined parameters. It can be described as a layered structure formed by three kinds of layers. As with other metavoltine-related minerals, scordariite is characterized by the occurrence of the [Fe3+3O(SO4)6(H2O)3]5− heteropolyhedral cluster.

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The metavoltine problem: Relationships between metavoltine and Maus' salt

Cited by 13 publications

References 3 publications

The structure of K₂(K_0.41,H₂O_0.59)₆Na_3.98H₃O_0.78 ⁺ X _0.68 ⁺(F_0.05 ²⁺,vacancy_0.95)Fe₆ ³⁺O₂(SO₄)₁₂.11.91H₂O: a compound related to metavoltine and α-Maus's salt

The structure of K₂(K_0.41,H₂O_0.59)₆Na_3.98H₃O_0.78 ⁺ X _0.68 ⁺(F_0.05 ²⁺,vacancy_0.95)Fe₆ ³⁺O₂(SO₄)₁₂.11.91H₂O: a compound related to metavoltine and α-Maus's salt

Stabilizing Reactive Fe(III) Clusters by Freeze-Dry/Solvent-Exchange To Benchmark Iron Hydrolysis Pathways

Crystal Chemistry of Sulfates from the Apuan Alps (Tuscany, Italy). V. Scordariite, K8(Fe3+0.67□0.33)[Fe3+3O(SO4)6(H2O)3]2(H2O)11: A New Metavoltine-Related Mineral

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The metavoltine problem: Relationships between metavoltine and Maus' salt

Cited by 13 publications

References 3 publications

The structure of K2(K0.41,H2O0.59)6Na3.98H3O0.78 + X 0.68 +(F0.05 2+,vacancy0.95)Fe6 3+O2(SO4)12.11.91H2O: a compound related to metavoltine and α-Maus's salt

The structure of K2(K0.41,H2O0.59)6Na3.98H3O0.78 + X 0.68 +(F0.05 2+,vacancy0.95)Fe6 3+O2(SO4)12.11.91H2O: a compound related to metavoltine and α-Maus's salt

Stabilizing Reactive Fe(III) Clusters by Freeze-Dry/Solvent-Exchange To Benchmark Iron Hydrolysis Pathways

Crystal Chemistry of Sulfates from the Apuan Alps (Tuscany, Italy). V. Scordariite, K8(Fe3+0.67□0.33)[Fe3+3O(SO4)6(H2O)3]2(H2O)11: A New Metavoltine-Related Mineral

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The structure of K₂(K_0.41,H₂O_0.59)₆Na_3.98H₃O_0.78 ⁺ X _0.68 ⁺(F_0.05 ²⁺,vacancy_0.95)Fe₆ ³⁺O₂(SO₄)₁₂.11.91H₂O: a compound related to metavoltine and α-Maus's salt

The structure of K₂(K_0.41,H₂O_0.59)₆Na_3.98H₃O_0.78 ⁺ X _0.68 ⁺(F_0.05 ²⁺,vacancy_0.95)Fe₆ ³⁺O₂(SO₄)₁₂.11.91H₂O: a compound related to metavoltine and α-Maus's salt