Contributions to the stereochemistry of zirconium oxysalts—part III: syntheses and crystal structures of M2+Zr(SO4)3 with M = Mg, Mn, Co, Ni, Zn and Cd, and a note on (Fe3+,2+,Zr)2(SO4)3 and Fe2(SO4)3

Giester, Gerald; Talla, Dominik; Wildner, Manfred

doi:10.1007/s00706-019-02496-2

Cited by 3 publications

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References 35 publications

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“…At the time we started our investigations of zirconium oxysalts [1], more than a dozen of purely inorganic zirconium sulfates, but no selenates or selenites had been structurally described in the literature. In the course of our studies [1][2][3] and present work, we were as yet able to synthesize and characterize seven zirconium sulfates as well as seven zirconium compounds containing [SeO 4 ] and/or [SeO 3 ] anions with interesting stereochemical properties. Currently, in continuation of our research program, the investigation of eight new zirconium oxysalts is in progress.…”

Section: Discussionmentioning

confidence: 97%

“…The presented work is part of long-term investigations on the crystal chemistry of zirconium oxysalts with (XO 4 ) 2− or (XO 3 ) 2− (X = S, Se) anions synthesized under mild-hydrothermal conditions below 250 °C. So far, the compounds Zr(SeO 4 ) 2 •H 2 O and Zr(SeO 4 ) 2 •4H 2 O [1], Zr(SeO 3 )(SeO 4 ), Zr 4 (SeO 3 )(SeO 4 ) 7 , and Zr 3 (SeO 3 )(SeO 4 ) 5 •2H 2 O [2], as well as M 2+ Zr(SO 4 ) 3 with M = Mg, Mn, Co, Ni, Zn and Cd, and (Fe 3+,2+ ,Zr) 2 (SO 4 ) 3 [3] were obtained and structurally characterized in detail. The present part IV of this series of studies deals with the two isotypic compounds Zr 2 (OH) 2 (XO 4 ) 3 •4H 2 O (X = S, Se), as well as with Zr(SO 4 ) 2 •4H 2 O and Zr(SeO 3 ) 2 .…”

Section: Introductionmentioning

confidence: 99%

“…Fig 3. Single polyhedral sheets in the structures of a Zr(SO 4 ) 2 •4H 2 O in a projection onto (001) compared to b 'monoclinic γ-Ce(SO 4 ) 2 •4H 2 O' according to[16] in a projection onto ( 2 0 1).…”

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Contributions to the stereochemistry of zirconium oxysalts—part IV: syntheses and crystal structures of Zr2(OH)2(XO4)3·4H2O (X = S, Se), Zr(SO4)2·4H2O, and Zr(SeO3)2

et al. 2022

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Zr2(OH)2(XO4)3·4H2O (X = S, Se), Zr(SO4)2·4H2O, and Zr(SeO3)2 were synthesized at low-hydrothermal conditions from mixtures of Zr2O2(CO3)(OH)2, the respective acids, and minor amounts of water. While Zr2(OH)2(XO4)3·4H2O (X = S, Se) and Zr(SO4)2·4H2O form crystals up to several tenths of a mm, Zr(SeO3)2 was mainly obtained as microcrystalline powder, single crystals rarely exceeded 10 μm in size. Samples were investigated by single-crystal X-ray techniques and in the case of Zr(SeO3)2 also by X-ray powder diffraction. The compounds Zr2(OH)2(XO4)3·4H2O (X = S, Se) crystallize in the Ce2(OH)2(SO4)3·4H2O structure type (C2/c, Z = 4, a = 13.034(2) / 13.308(3), b = 6.500(1) / 6.683(2), c = 15.056(3) / 15.383(4) Å, β = 96.27(1) / 96.81(1)°, V = 1267.9(4) / 1358.5(6) Å3 for X = S / Se, respectively). Tetragonal aniprisms Zr[8]O8 are edge-connected to dimers that share corners with XO4 tetrahedra forming a three-dimensional network. Zr(SO4)2·4H2O (Fddd, Z = 8, a = 5.498(1), b = 11.618(3), c = 25.893(6) Å, V = 1653.9(6) Å3) is isotypic with the respective selenate compound. Occasionally, pseudomerohedral twinning is observed, simulating a larger monoclinic C-centered unit cell. Again, tetragonal antiprisms Zr[8]O8 are formed; however, they are corner-linked with SO4 tetrahedra to Zr(SO4)2 layers interconnected solely by hydrogen bonds. Zr(SeO3)2 crystallizes in P21/c, Z = 2; a = 4.9724(3), b = 8.5992(5), c = 6.9447(3) Å, β = 110.128(3)°, V = 278.81(3) Å3 (unit cell from powder data) and belongs to the β-Sn(SeO3)2 structure type established further for Ti(SeO3)2 and Pb(SeO3)2. Isolated ZrO6 octahedra share corners with the selenite groups forming a three-dimensional network. Graphical abstract

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Section: Discussionmentioning

confidence: 97%

Section: Introductionmentioning

confidence: 99%

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Contributions to the stereochemistry of zirconium oxysalts—part IV: syntheses and crystal structures of Zr2(OH)2(XO4)3·4H2O (X = S, Se), Zr(SO4)2·4H2O, and Zr(SeO3)2

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Contributions to the stereochemistry of zirconium oxysalts—part V: syntheses and crystal structures of MZr(SeO4)3 (M = Mg, Mn, Co, Ni, Zn, Cd) and Li2Zr(XO4)3 (X = S, Se)

Giester

Wildner

2022

Monatsh Chem

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The new compounds M2+Zr(SeO4)3 (M2+ = Mg, Mn, Co, Ni, Zn, Cd) and Li2Zr(XO4)3 (X = S, Se) were synthesized at 220 °C by reaction of Zr2O2(CO3)(OH)2 with hydroxides or carbonates of M / Li and the respective acids H2SeO4/H2SO4. They form crystals up to several tenths of a mm and were investigated by single crystal X-ray diffraction. The framework structures of these selenates can be deduced from that of monoclinic Fe2(SO4)3 in space group P21/n, which is characterized by two types of isolated Fe3+O6 octahedra, corner-linked with three different sulfate groups: ferric iron is substituted in 1:1 ratio by Zr4+ and M2+ as already known for isotypic MZr(SO4)3 representatives. In the case of Li2Zr(XO4)3 members, one additional lithium atom occupies a tetrahedral vacancy of the Fe2(SO4)3 architecture. Graphical abstract

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CuSeO4 and Cu(SeO3OH)2·6H2O, two novel copper–selenium(VI) oxysalts

2023

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The two new copper(II) salts Cu(SeO4) and Cu(SeO3OH)2•6H2O were synthesized at lowtemperature hydrothermal conditions (220 °C), and room temperature, respectively. Their atomic arrangements were studied based on single-crystal X-ray investigations [P21/n, a = 4.823(1), b = 8.957(2), c = 6.953(1) Å, β = 94.82(1)° Z = 4; P -1, a = 6.133(1), b = 6.303(1), c = 8.648(2) Å, α = 70.45(1), β = 84.60(1), γ = 73.44(1)°, Z = 1]. Cu(SeO4) adopts the MnAsO4 structure type. It exhibits structural as well as topological relations with two formerly known isochemical compounds. They crystallize in the structure type ZnSO4 (mineral name zincosite, Pnma) respectively NiSO4 (Cmcm). The two minerals dravertite, CuMg(SO4)2, and hermannjahnite, CuZn(SO4)2, are isotypic with CuSeO4-P21/n; interestingly, also α-NaCu(PO4) belongs to this structure type: some rotation of the XO4 group allows a supplementary position for the Na atom.-Cu(SeO3OH)2•6H2O represents a new structure type. The protonated selenate group shows an extended Se-Oh bond distance (1.695 Å) as compared to the other Se-O bonds (1.614 to 1.626 Å). One OH dipole of the three independent H2O molecules represents a rather free hydrogen bond. For the other H atoms, the O-H•••O lengths vary from 2.585 to 2.799 Å. Interestingly, the distance Ow7•••Ow7 of only 2.791 Å does not represent an edge in a coordination polyhedron and it is not preliminary involved in the hydrogen bond scheme. All Cu 2+ ions in the two title compounds are in a pronounced [4+2] coordination. The Cu 2+[4+2] atoms in Cu(SeO4) are linked to chains along [100]; in Cu(SeO3OH)2•6H2O they are not connected among each other. Keywords Cu(II) oxysalt • selenate(VI) • selenate (protonated) • topology • Cu(SeO4) • Cu(SeO3OH)2•6H2O

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Contributions to the stereochemistry of zirconium oxysalts—part III: syntheses and crystal structures of M2+Zr(SO4)3 with M = Mg, Mn, Co, Ni, Zn and Cd, and a note on (Fe3+,2+,Zr)2(SO4)3 and Fe2(SO4)3

Cited by 3 publications

References 35 publications

Contributions to the stereochemistry of zirconium oxysalts—part IV: syntheses and crystal structures of Zr2(OH)2(XO4)3·4H2O (X = S, Se), Zr(SO4)2·4H2O, and Zr(SeO3)2

Contributions to the stereochemistry of zirconium oxysalts—part IV: syntheses and crystal structures of Zr2(OH)2(XO4)3·4H2O (X = S, Se), Zr(SO4)2·4H2O, and Zr(SeO3)2

Contributions to the stereochemistry of zirconium oxysalts—part V: syntheses and crystal structures of MZr(SeO4)3 (M = Mg, Mn, Co, Ni, Zn, Cd) and Li2Zr(XO4)3 (X = S, Se)

CuSeO4 and Cu(SeO3OH)2·6H2O, two novel copper–selenium(VI) oxysalts

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