skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: New rubidium zinc hydrogen phosphate, Rb{sub 2}Zn{sub 2}(HPO{sub 4}){sub 3}: Synthesis, crystal structure, and {sup 31}P single-crystal NMR

Abstract

A new rubidium zinc hydrogen phosphate, Rb{sub 2}Zn{sub 2}(HPO{sub 4}){sub 3}, is prepared by an unusual method utilizing long nucleation times. This material is crystallized from a gel with an initial composition of 1.0 ZnO/0.94 P{sub 2}O{sub 5}/0.96 Rb{sub 2}O/0.04 Li{sub 2}O/41 H{sub 2}O, while the phosphate concentration equals 1.6 M and pH = 3.5. The gel is placed in a sealed Pyrex flask at 52 C, and after 4.5 months crystallization of Rb{sub 2}Zn{sub 2}(HPO{sub 4}){sub 3} is noticed. This new crystalline compound has a three-dimensional framework structure built from spiral chains of alternating PO{sub 4} and ZnO{sub 4} tetrahedra connected pairwise and assembled by other PO{sub 4} tetrahedra, rubidium ions, and hydrogen bonds. The two rubidium ions, Rb(1) and Rb(2), have an exceptionally low number of oxygen contacts in the first coordination sphere, five and seven, respectively. Crystal data: monoclinic, P2{sub 1}/c (no. 14), a = 12.5880(4), b = 12.7170(8), c = 7.5827(8) {angstrom}, {beta} = 96.100(1){degree}, Z = 4. A single-crystal {sup 31}P NMR investigation of Rb{sub 2}Zn{sub 2}(HPO{sub 4}){sub 3} was performed employing a two-axis goniometer probe and reveals the presence of three chemically and six magnetically nonequivalent phosphorus sites, in accordance with the crystal structure.more » {sup 31}P chemical shielding anisotropies and isotropic chemical shifts ({minus}3.3(3), {minus}2.6(3), and 2.0(3) ppm) have been determined for the three phosphorus sites.« less

Authors:
; ; ;
Publication Date:
Research Org.:
Univ. of Southern Denmark, Odense (DK)
OSTI Identifier:
20075872
Resource Type:
Journal Article
Journal Name:
Inorganic Chemistry
Additional Journal Information:
Journal Volume: 39; Journal Issue: 10; Other Information: PBD: 15 May 2000; Journal ID: ISSN 0020-1669
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; RUBIDIUM COMPOUNDS; ZINC COMPOUNDS; PHOSPHATES; SYNTHESIS; CRYSTAL STRUCTURE; NUCLEAR MAGNETIC RESONANCE; PHOSPHORUS 31; MONOCRYSTALS

Citation Formats

Jensen, T.R., Hazell, R.G., Vosegaard, T., and Jakobsen, H.J. New rubidium zinc hydrogen phosphate, Rb{sub 2}Zn{sub 2}(HPO{sub 4}){sub 3}: Synthesis, crystal structure, and {sup 31}P single-crystal NMR. United States: N. p., 2000. Web. doi:10.1021/ic9906757.
Jensen, T.R., Hazell, R.G., Vosegaard, T., & Jakobsen, H.J. New rubidium zinc hydrogen phosphate, Rb{sub 2}Zn{sub 2}(HPO{sub 4}){sub 3}: Synthesis, crystal structure, and {sup 31}P single-crystal NMR. United States. doi:10.1021/ic9906757.
Jensen, T.R., Hazell, R.G., Vosegaard, T., and Jakobsen, H.J. Mon . "New rubidium zinc hydrogen phosphate, Rb{sub 2}Zn{sub 2}(HPO{sub 4}){sub 3}: Synthesis, crystal structure, and {sup 31}P single-crystal NMR". United States. doi:10.1021/ic9906757.
@article{osti_20075872,
title = {New rubidium zinc hydrogen phosphate, Rb{sub 2}Zn{sub 2}(HPO{sub 4}){sub 3}: Synthesis, crystal structure, and {sup 31}P single-crystal NMR},
author = {Jensen, T.R. and Hazell, R.G. and Vosegaard, T. and Jakobsen, H.J.},
abstractNote = {A new rubidium zinc hydrogen phosphate, Rb{sub 2}Zn{sub 2}(HPO{sub 4}){sub 3}, is prepared by an unusual method utilizing long nucleation times. This material is crystallized from a gel with an initial composition of 1.0 ZnO/0.94 P{sub 2}O{sub 5}/0.96 Rb{sub 2}O/0.04 Li{sub 2}O/41 H{sub 2}O, while the phosphate concentration equals 1.6 M and pH = 3.5. The gel is placed in a sealed Pyrex flask at 52 C, and after 4.5 months crystallization of Rb{sub 2}Zn{sub 2}(HPO{sub 4}){sub 3} is noticed. This new crystalline compound has a three-dimensional framework structure built from spiral chains of alternating PO{sub 4} and ZnO{sub 4} tetrahedra connected pairwise and assembled by other PO{sub 4} tetrahedra, rubidium ions, and hydrogen bonds. The two rubidium ions, Rb(1) and Rb(2), have an exceptionally low number of oxygen contacts in the first coordination sphere, five and seven, respectively. Crystal data: monoclinic, P2{sub 1}/c (no. 14), a = 12.5880(4), b = 12.7170(8), c = 7.5827(8) {angstrom}, {beta} = 96.100(1){degree}, Z = 4. A single-crystal {sup 31}P NMR investigation of Rb{sub 2}Zn{sub 2}(HPO{sub 4}){sub 3} was performed employing a two-axis goniometer probe and reveals the presence of three chemically and six magnetically nonequivalent phosphorus sites, in accordance with the crystal structure. {sup 31}P chemical shielding anisotropies and isotropic chemical shifts ({minus}3.3(3), {minus}2.6(3), and 2.0(3) ppm) have been determined for the three phosphorus sites.},
doi = {10.1021/ic9906757},
journal = {Inorganic Chemistry},
issn = {0020-1669},
number = 10,
volume = 39,
place = {United States},
year = {2000},
month = {5}
}