Hydrothermal synthesis and structural characterization of the three-dimensional framework solids (NH4) [V2(OH) (PO4)2(H2O)] · H2O and Rb6[(Mo9V3O6) (PO4)10(H2PO4)3(OH) 9] · 8.5H2O

Victoria Soghomonian; Linda A. Meyer; Robert C. Haushalter; Jon Zubieta

doi:10.1016/s0020-1693(97)06081-7

Hydrothermal synthesis and structural characterization of the three-dimensional framework solids (NH₄) [V₂(OH) (PO₄)₂(H₂O)] · H₂O and Rb₆[(Mo₉V₃O₆) (PO₄)₁₀(H₂PO₄)₃(OH) ₉] · 8.5H₂O

Victoria Soghomonian, Linda A. Meyer, Robert C. Haushalter, Jon Zubieta

Department of Chemistry

Research output: Contribution to journal › Article › peer-review

15 Scopus citations

Abstract

Hydrothermal synthesis has been employed to prepared two three-dimensional, open-framework solids with tetranuclear metal oxide cores. The reaction of VCl₄, H₃PO₄, 1,3-diaminopropane and H₂O in the mole ratio 1:7.4:8.6:1004 at 200°C for 87 h yielded (NH₄) [V₂(OH) (PO₄)₂(H₂O)] · H₂O (1·H₂O), while the reaction of Rb₂MoO₄, Rb₂V₂O₆, vanadium metal, U-Bu₄NBr, H₃PO₄ and H₂O in the mole ratio 2:1.1:1:1:145:392 at 240°C for 48 h produced Rb₆[(Mo₉V₃O₆)(PO₄) ₁₀(H₂PO₄)₃(OH)₉] · 8.5H₂O (2·8.5H₂O). The structure of 1·H₂O is constructed from tetranuclear units of edge-and corner-sharing V (III) octahedra linked into a three-dimensional framework through phosphate tetrahedra. Compound 2·8.5H₂O exhibits structurally distinct tetranuclear units of edge-and corner-sharing Mo(V) and Mo(III)/V(III) octahedra linked through phosphate tetrahedra into a open-framework solid with hexagonal channels. Both 1·H₂O and 2·8.5H₂O exhibit microporosity as evidenced by Type I water sorption isotherms. Crystal data: H₈O₁₂P₂V₂ (1·H₂O), monoclinic P2₁/n, a=9.803(2), b=9.688(2), c=9.858(2) Å, β=102.91(3)°, V=912.6(3) Å³; structure solution and refinement converged at 0.0448 for 1481 reflections. H₃₂O_75.5P₁₃V₃Mo₉Rb ₆ (2·8.5H₂O), hexagonal P6₃/m, a=16.563(2), c=12.534(3) Å, V=2977.8(7) Å³; R=0.0570 for 3022 reflections.

Original language	English (US)
Pages (from-to)	122-129
Number of pages	8
Journal	Inorganica Chimica Acta
Volume	275-276
DOIs	https://doi.org/10.1016/s0020-1693(97)06081-7
State	Published - Jul 1 1998

Keywords

Crystal structures
Oxovanadium compounds
Phosphate compounds
Three-dimensional compounds

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

Access to Document

10.1016/s0020-1693(97)06081-7

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Hydrothermal synthesis and structural characterization of the three-dimensional framework solids (NH₄) [V₂(OH) (PO₄)₂(H₂O)] · H₂O and Rb₆[(Mo₉V₃O₆) (PO₄)₁₀(H₂PO₄)₃(OH) ₉] · 8.5H₂O. / Soghomonian, Victoria; Meyer, Linda A.; Haushalter, Robert C. et al.
In: Inorganica Chimica Acta, Vol. 275-276, 01.07.1998, p. 122-129.

Research output: Contribution to journal › Article › peer-review

@article{7aa3e0fbb5f947b4b2d2176f3dcae335,

title = "Hydrothermal synthesis and structural characterization of the three-dimensional framework solids (NH4) [V2(OH) (PO4)2(H2O)] · H2O and Rb6[(Mo9V3O6) (PO4)10(H2PO4)3(OH) 9] · 8.5H2O",

abstract = "Hydrothermal synthesis has been employed to prepared two three-dimensional, open-framework solids with tetranuclear metal oxide cores. The reaction of VCl4, H3PO4, 1,3-diaminopropane and H2O in the mole ratio 1:7.4:8.6:1004 at 200°C for 87 h yielded (NH4) [V2(OH) (PO4)2(H2O)] · H2O (1·H2O), while the reaction of Rb2MoO4, Rb2V2O6, vanadium metal, U-Bu4NBr, H3PO4 and H2O in the mole ratio 2:1.1:1:1:145:392 at 240°C for 48 h produced Rb6[(Mo9V3O6)(PO4) 10(H2PO4)3(OH)9] · 8.5H2O (2·8.5H2O). The structure of 1·H2O is constructed from tetranuclear units of edge-and corner-sharing V (III) octahedra linked into a three-dimensional framework through phosphate tetrahedra. Compound 2·8.5H2O exhibits structurally distinct tetranuclear units of edge-and corner-sharing Mo(V) and Mo(III)/V(III) octahedra linked through phosphate tetrahedra into a open-framework solid with hexagonal channels. Both 1·H2O and 2·8.5H2O exhibit microporosity as evidenced by Type I water sorption isotherms. Crystal data: H8O12P2V2 (1·H2O), monoclinic P21/n, a=9.803(2), b=9.688(2), c=9.858(2) {\AA}, β=102.91(3)°, V=912.6(3) {\AA}3; structure solution and refinement converged at 0.0448 for 1481 reflections. H32O75.5P13V3Mo9Rb 6 (2·8.5H2O), hexagonal P63/m, a=16.563(2), c=12.534(3) {\AA}, V=2977.8(7) {\AA}3; R=0.0570 for 3022 reflections.",

keywords = "Crystal structures, Oxovanadium compounds, Phosphate compounds, Three-dimensional compounds",

author = "Victoria Soghomonian and Meyer, {Linda A.} and Haushalter, {Robert C.} and Jon Zubieta",

year = "1998",

month = jul,

day = "1",

doi = "10.1016/s0020-1693(97)06081-7",

language = "English (US)",

volume = "275-276",

pages = "122--129",

journal = "Inorganica Chimica Acta",

issn = "0020-1693",

publisher = "Elsevier",

}

TY - JOUR

T1 - Hydrothermal synthesis and structural characterization of the three-dimensional framework solids (NH4) [V2(OH) (PO4)2(H2O)] · H2O and Rb6[(Mo9V3O6) (PO4)10(H2PO4)3(OH) 9] · 8.5H2O

AU - Soghomonian, Victoria

AU - Meyer, Linda A.

AU - Haushalter, Robert C.

AU - Zubieta, Jon

PY - 1998/7/1

Y1 - 1998/7/1

N2 - Hydrothermal synthesis has been employed to prepared two three-dimensional, open-framework solids with tetranuclear metal oxide cores. The reaction of VCl4, H3PO4, 1,3-diaminopropane and H2O in the mole ratio 1:7.4:8.6:1004 at 200°C for 87 h yielded (NH4) [V2(OH) (PO4)2(H2O)] · H2O (1·H2O), while the reaction of Rb2MoO4, Rb2V2O6, vanadium metal, U-Bu4NBr, H3PO4 and H2O in the mole ratio 2:1.1:1:1:145:392 at 240°C for 48 h produced Rb6[(Mo9V3O6)(PO4) 10(H2PO4)3(OH)9] · 8.5H2O (2·8.5H2O). The structure of 1·H2O is constructed from tetranuclear units of edge-and corner-sharing V (III) octahedra linked into a three-dimensional framework through phosphate tetrahedra. Compound 2·8.5H2O exhibits structurally distinct tetranuclear units of edge-and corner-sharing Mo(V) and Mo(III)/V(III) octahedra linked through phosphate tetrahedra into a open-framework solid with hexagonal channels. Both 1·H2O and 2·8.5H2O exhibit microporosity as evidenced by Type I water sorption isotherms. Crystal data: H8O12P2V2 (1·H2O), monoclinic P21/n, a=9.803(2), b=9.688(2), c=9.858(2) Å, β=102.91(3)°, V=912.6(3) Å3; structure solution and refinement converged at 0.0448 for 1481 reflections. H32O75.5P13V3Mo9Rb 6 (2·8.5H2O), hexagonal P63/m, a=16.563(2), c=12.534(3) Å, V=2977.8(7) Å3; R=0.0570 for 3022 reflections.

AB - Hydrothermal synthesis has been employed to prepared two three-dimensional, open-framework solids with tetranuclear metal oxide cores. The reaction of VCl4, H3PO4, 1,3-diaminopropane and H2O in the mole ratio 1:7.4:8.6:1004 at 200°C for 87 h yielded (NH4) [V2(OH) (PO4)2(H2O)] · H2O (1·H2O), while the reaction of Rb2MoO4, Rb2V2O6, vanadium metal, U-Bu4NBr, H3PO4 and H2O in the mole ratio 2:1.1:1:1:145:392 at 240°C for 48 h produced Rb6[(Mo9V3O6)(PO4) 10(H2PO4)3(OH)9] · 8.5H2O (2·8.5H2O). The structure of 1·H2O is constructed from tetranuclear units of edge-and corner-sharing V (III) octahedra linked into a three-dimensional framework through phosphate tetrahedra. Compound 2·8.5H2O exhibits structurally distinct tetranuclear units of edge-and corner-sharing Mo(V) and Mo(III)/V(III) octahedra linked through phosphate tetrahedra into a open-framework solid with hexagonal channels. Both 1·H2O and 2·8.5H2O exhibit microporosity as evidenced by Type I water sorption isotherms. Crystal data: H8O12P2V2 (1·H2O), monoclinic P21/n, a=9.803(2), b=9.688(2), c=9.858(2) Å, β=102.91(3)°, V=912.6(3) Å3; structure solution and refinement converged at 0.0448 for 1481 reflections. H32O75.5P13V3Mo9Rb 6 (2·8.5H2O), hexagonal P63/m, a=16.563(2), c=12.534(3) Å, V=2977.8(7) Å3; R=0.0570 for 3022 reflections.

KW - Crystal structures

KW - Oxovanadium compounds

KW - Phosphate compounds

KW - Three-dimensional compounds

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JO - Inorganica Chimica Acta

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