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Title: An organically templated yttrium fluoride with a 'Super-Diamond' structure

Abstract

An organically templated yttrium fluoride has been prepared hydrothermally and characterised by X-ray powder diffraction. The crystal structure of [C{sub 3}N{sub 2}H{sub 12}]{sub 0.5}[Y{sub 3}F{sub 10}] may be regarded as a 'Super-Diamond' framework, space group Fd3-bar m, a=15.4817(1)A, where each carbon atom site of the diamond structure is replaced by a polyhedral [Y{sub 6}F{sub 8}F{sub 24/2}]{sup 2-} unit. The basic framework type is isostructural with the known phase (H{sub 3}O)[Yb{sub 3}F{sub 10}].H{sub 2}O. The novelty in the present case lies in the use of the organic structure-directing agent 1,3-diaminopropane.

Authors:
 [1];  [2]
  1. EaStChem, School of Chemistry, University of St. Andrews, St. Andrews, Fife KY16 9ST (United Kingdom)
  2. EaStChem, School of Chemistry, University of St. Andrews, St. Andrews, Fife KY16 9ST (United Kingdom), E-mail: pl@st-and.ac.uk
Publication Date:
OSTI Identifier:
21015645
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 180; Journal Issue: 1; Other Information: DOI: 10.1016/j.jssc.2006.09.032; PII: S0022-4596(06)00530-5; Copyright (c) 2006 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; CUBIC LATTICES; DIAMONDS; HYDROTHERMAL SYNTHESIS; SPACE GROUPS; X-RAY DIFFRACTION; YTTRIUM FLUORIDES

Citation Formats

Stephens, Nicholas F., and Lightfoot, Philip. An organically templated yttrium fluoride with a 'Super-Diamond' structure. United States: N. p., 2007. Web. doi:10.1016/j.jssc.2006.09.032.
Stephens, Nicholas F., & Lightfoot, Philip. An organically templated yttrium fluoride with a 'Super-Diamond' structure. United States. doi:10.1016/j.jssc.2006.09.032.
Stephens, Nicholas F., and Lightfoot, Philip. Mon . "An organically templated yttrium fluoride with a 'Super-Diamond' structure". United States. doi:10.1016/j.jssc.2006.09.032.
@article{osti_21015645,
title = {An organically templated yttrium fluoride with a 'Super-Diamond' structure},
author = {Stephens, Nicholas F. and Lightfoot, Philip},
abstractNote = {An organically templated yttrium fluoride has been prepared hydrothermally and characterised by X-ray powder diffraction. The crystal structure of [C{sub 3}N{sub 2}H{sub 12}]{sub 0.5}[Y{sub 3}F{sub 10}] may be regarded as a 'Super-Diamond' framework, space group Fd3-bar m, a=15.4817(1)A, where each carbon atom site of the diamond structure is replaced by a polyhedral [Y{sub 6}F{sub 8}F{sub 24/2}]{sup 2-} unit. The basic framework type is isostructural with the known phase (H{sub 3}O)[Yb{sub 3}F{sub 10}].H{sub 2}O. The novelty in the present case lies in the use of the organic structure-directing agent 1,3-diaminopropane.},
doi = {10.1016/j.jssc.2006.09.032},
journal = {Journal of Solid State Chemistry},
number = 1,
volume = 180,
place = {United States},
year = {Mon Jan 15 00:00:00 EST 2007},
month = {Mon Jan 15 00:00:00 EST 2007}
}
  • The utilization of the hydrothermal technique in combination with cationic organic templates has been extensively used in the synthesis of zeolites and molecular sieves. Here, the authors report the hydrothermal synthesis and single-crystal structure of (H{sub 3}N(CH{sub 2}){sub 3}NH{sub 3})[V{sub 4}O{sub 10}], a layered mixed-valence vanadium oxide with organic ammonium cations between the layers. 21 refs., 4 figs.
  • The authors discuss the synthesis and structural characterization of (VO){sub 2}(PO{sub 4}){sub 2}H{sub 2}PO{sub 4}{sm_bullet}N{sub 2}C{sub 2}H{sub 10}. The structure consists of V{sup IV}O{sub 6}, V{sup v}O{sub 6}, PO{sub 4}, and H{sub 2}PO{sub 4} polyhedra, connected via V-O-P bonds. 19 refs., 4 figs.
  • An astonishing variety of inorganic networks templated by organic species have been reported over the last 10 years. A great deal of attention has been paid to the structure-directing role of the organic species, and the structural effect of variously coordinated cations, for example distorted octahedral vanadium and pyramidal tin. Less exploratory work has been carried out on the anionic part of the inorganic network, and most groups reported so far (phosphate, germanate, etc.) invariably adopt tetrahedral coordination. The possibilities of incorporating the pyramidal [HP0{sub 3}]{sup 2{minus}} hydrogen phosphite group into extended structures templated by inorganic, alkaline earth cations wasmore » explored a few years ago. In this paper the authors report the synthesis, crystal structure, and some properties of (CN{sub 3}H{sub 6}){sub 4}{center_dot}Zn{sub 3}(SeO{sub 3}){sub 5}, the first organically-templated phase to contain the pyramidal selenite [SeO{sub 3}]{sup 2{minus}} anion.« less
  • The first organically templated neodymium sulfate has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction analysis. [C{sub 2}N{sub 2}H{sub 10}]{sub 1.5}[Nd(SO{sub 4}){sub 3}(H{sub 2}O)].2H{sub 2}O crystallizes in the monoclinic space group P2{sub 1}/c with crystal data a=6.5896(5)A, b=26.539(3)A, c=9.9889(8)A, {beta}=104.399(5){sup o}, V=1692.0(2)A{sup 3}, Z=4. Refinement gave R{sub 1}[I>2{sigma}(I)]=0.0471, and wR{sub 2}[I>2{sigma}(I)]=0.0899. The compound exhibits an infinite zigzag anionic layer structure, which consists of {l_brace}Nd(SO{sub 4}){sub 3}(H{sub 2}O){r_brace}{sup 3-} structural units connected together to form interesting eight-membered rings via corner-sharing and edge-sharing modes. The compound has the antiferromagnetic behavior and exhibits intense photoluminescence upon photo-excitation at 450nm.
  • Four scandium phosphate-based structures have been prepared hydrothermally in the presence of the primary diamines ethylenediamine and diaminobutane and the primary amine cyclohexylamine and characterised by single crystal and powder X-ray diffraction, {sup 31}P and {sup 45}Sc solid-state MAS NMR and chemical analysis. Charge balancing protons in the structures are located using bond valence sum calculations and postulated hydrogen bonding networks. Compound 1, [(H{sub 3}NC{sub 2}H{sub 4}NH{sub 3}){sub 3}][Sc{sub 3}(OH){sub 2}(PO{sub 4}){sub 2}(HPO{sub 4}){sub 3}(H{sub 2}PO{sub 4})], P1-bar , a=5.4334(6), b=8.5731(9), c=16.3022(18)A, {alpha}=79.732(4), {beta}=83.544(4), {gamma}=80.891(5){sup o}, Z=2, is built up of scandium phosphate ribbons, based on trimers of ScO{sub 6}more » octahedra linked by OH groups. These trimers are joined through phosphate groups bound through three oxygens, and are decorated by phosphate groups linked by a single oxygen atom. The ribbons are arranged parallel to the a-axis and linked one to another by fully protonated ethylenediammonium ions. Compounds 2, [(H{sub 3}NC{sub 4}H{sub 8}NH{sub 3}){sub 3}][(Sc(OH{sub 2})){sub 6}Sc{sub 2}(HPO{sub 4}){sub 12}(PO{sub 4}){sub 2}], P3-bar , a=13.8724(3), c=9.4351(11)A, Z=1, and 3, [(H{sub 3}NC{sub 4}H{sub 8}NH{sub 3}){sub 2}(H{sub 3}O)][Sc{sub 5}F{sub 4}(HPO{sub 4}){sub 8}], C2/m, a=12.8538(4), b=14.9106(4), c=10.1906(3)A, {beta}=101.17(9){sup o}, Z=2, were prepared using diaminobutane as the organic template in the absence and presence, respectively, of fluoride ions in the gel. Compound 2 has a pillared layered structure, in which ScO{sub 6} octahedra are linked by three vertices of hydrogenphosphate groups into sheets and the sheets pillared by ScO{sub 6} octahedra to give a three-dimensionally connected framework isostructural with a previously reported iron(III) hydrogenphosphate. The protonated diaminobutane molecules occupy cavities between the layers. Compound 3 has a layered structure in which isolated ScO{sub 6} octahedra and tetrameric arrangements of ScO{sub 4}F{sub 2} octahedra, the latter linked in squares through fluoride ions, are connected by phosphate tetrahedra that share two or three oxygens with scandium atoms. In this structure, the protonated diaminobutane molecules connect the layers, the -NH{sub 3}{sup +} groups fitting into recesses in the layers. Compound 4, [(C{sub 6}H{sub 11}NH{sub 3})][ScF(HPO{sub 4})(H{sub 2}PO{sub 4})], Pbca, a=7.650(3), b=12.867(5), c=26.339(11)A, Z=8, the first scandium phosphate to be prepared with a monoamine, is also a layered solid. In this case, the layers contain single chains of ScO{sub 4}F{sub 2} octahedra which share fluoride ions in trans positions. Phosphate tetrahedra bridge across scandiums via two of their four oxygens, both within the same chain and also to neighbouring chains to make up the layer. The protonated amine groups of the cyclohexylamine molecules achieve close contact with phosphates of the layer, while the cyclohexyl moieties, which are in the chair configuration, project into the interlayer space.« less