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Title: Hydro(solvo)thermal synthesis and structural characterization of a new organically templated gallophosphate: [H{sub 3}N(CH{sub 2}){sub 2}NH{sub 3}]{sub 1/2}.[Ga{sub 5} (PO{sub 4}){sub 4}(OH){sub 4}]

Abstract

A new three-dimensional open-framework gallophosphate: [H{sub 3}N(CH{sub 2}){sub 2}NH{sub 3}]{sub 1/2}.[Ga{sub 5} (PO{sub 4}){sub 4}(OH){sub 4}] has been prepared by hydro(solvo)thermal synthesis in presence of ethylenediamine (en) as structure-directing agent. Its structure was determined by means of single-crystal X-ray diffraction analysis with the following crystal data: monoclinic space group C2/m, a=10.1604(9)A, b=12.0085(15)A, c=7.1892(7)A, {beta}=90.797(6){sup o}, V=877.08(16)A{sup 3}, Z=2, R{sub 1}=0.0264, wR{sub 2}=0.0764. The total numbers of measured reflections and unique reflections were 3508 and 1300, respectively. It is built up from a new secondary building unit (SBU) Ga{sub 4}P{sub 4}O{sub 20}(OH){sub 4}, in which Ga atoms exhibit distorted trigonal bipyramidal coordination and P atoms are in tetrahedral coordination. The SBU Ga{sub 4}P{sub 4}O{sub 20}(OH){sub 4} are linked into a layer by bridge oxygen atoms. The GaO{sub 4}(OH){sub 2} octahedra link the layers into a three-dimentional framework. Diprotonated ethylenediamine was found in the channel of the framework. The material was characterized by IR spectroscopy, {sup 1}H NMR spectra, thermogravimetric and differential thermal analyses and elemental analysis.

Authors:
 [1];  [1];  [1];  [1]
  1. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130023 (China)
Publication Date:
OSTI Identifier:
20725890
Resource Type:
Journal Article
Journal Name:
Journal of Solid State Chemistry
Additional Journal Information:
Journal Volume: 178; Journal Issue: 4; Other Information: DOI: 10.1016/j.jssc.2004.12.036; PII: S0022-4596(04)00673-5; Copyright (c) 2005 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA); Journal ID: ISSN 0022-4596
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; DIFFERENTIAL THERMAL ANALYSIS; GALLIUM PHOSPHATES; HYDROTHERMAL SYNTHESIS; LAYERS; MONOCLINIC LATTICES; MONOCRYSTALS; NMR SPECTRA; SPACE GROUPS; THERMAL GRAVIMETRIC ANALYSIS; X-RAY DIFFRACTION

Citation Formats

Lei, Yang, Guanghua, Li, Zhan, Shi, and Shouhua, Feng. Hydro(solvo)thermal synthesis and structural characterization of a new organically templated gallophosphate: [H{sub 3}N(CH{sub 2}){sub 2}NH{sub 3}]{sub 1/2}.[Ga{sub 5} (PO{sub 4}){sub 4}(OH){sub 4}]. United States: N. p., 2005. Web. doi:10.1016/j.jssc.2004.12.036.
Lei, Yang, Guanghua, Li, Zhan, Shi, & Shouhua, Feng. Hydro(solvo)thermal synthesis and structural characterization of a new organically templated gallophosphate: [H{sub 3}N(CH{sub 2}){sub 2}NH{sub 3}]{sub 1/2}.[Ga{sub 5} (PO{sub 4}){sub 4}(OH){sub 4}]. United States. https://doi.org/10.1016/j.jssc.2004.12.036
Lei, Yang, Guanghua, Li, Zhan, Shi, and Shouhua, Feng. Fri . "Hydro(solvo)thermal synthesis and structural characterization of a new organically templated gallophosphate: [H{sub 3}N(CH{sub 2}){sub 2}NH{sub 3}]{sub 1/2}.[Ga{sub 5} (PO{sub 4}){sub 4}(OH){sub 4}]". United States. https://doi.org/10.1016/j.jssc.2004.12.036.
@article{osti_20725890,
title = {Hydro(solvo)thermal synthesis and structural characterization of a new organically templated gallophosphate: [H{sub 3}N(CH{sub 2}){sub 2}NH{sub 3}]{sub 1/2}.[Ga{sub 5} (PO{sub 4}){sub 4}(OH){sub 4}]},
author = {Lei, Yang and Guanghua, Li and Zhan, Shi and Shouhua, Feng},
abstractNote = {A new three-dimensional open-framework gallophosphate: [H{sub 3}N(CH{sub 2}){sub 2}NH{sub 3}]{sub 1/2}.[Ga{sub 5} (PO{sub 4}){sub 4}(OH){sub 4}] has been prepared by hydro(solvo)thermal synthesis in presence of ethylenediamine (en) as structure-directing agent. Its structure was determined by means of single-crystal X-ray diffraction analysis with the following crystal data: monoclinic space group C2/m, a=10.1604(9)A, b=12.0085(15)A, c=7.1892(7)A, {beta}=90.797(6){sup o}, V=877.08(16)A{sup 3}, Z=2, R{sub 1}=0.0264, wR{sub 2}=0.0764. The total numbers of measured reflections and unique reflections were 3508 and 1300, respectively. It is built up from a new secondary building unit (SBU) Ga{sub 4}P{sub 4}O{sub 20}(OH){sub 4}, in which Ga atoms exhibit distorted trigonal bipyramidal coordination and P atoms are in tetrahedral coordination. The SBU Ga{sub 4}P{sub 4}O{sub 20}(OH){sub 4} are linked into a layer by bridge oxygen atoms. The GaO{sub 4}(OH){sub 2} octahedra link the layers into a three-dimentional framework. Diprotonated ethylenediamine was found in the channel of the framework. The material was characterized by IR spectroscopy, {sup 1}H NMR spectra, thermogravimetric and differential thermal analyses and elemental analysis.},
doi = {10.1016/j.jssc.2004.12.036},
url = {https://www.osti.gov/biblio/20725890}, journal = {Journal of Solid State Chemistry},
issn = {0022-4596},
number = 4,
volume = 178,
place = {United States},
year = {2005},
month = {4}
}