Hydrothermal synthesis, structure determination, and solid-state NMR study of the first organically templated scandium phosphate
Identifieur interne : 00F202 ( Main/Repository ); précédent : 00F201; suivant : 00F203Hydrothermal synthesis, structure determination, and solid-state NMR study of the first organically templated scandium phosphate
Auteurs : RBID : Pascal:02-0453575Descripteurs français
- Pascal (Inist)
- Etude expérimentale, Préparation chimique, Synthèse hydrothermale, Scandium Hydrogénophosphate, Template, Matériau hybride, Structure ouverte, Dication organique, Composé aliphatique saturé, Diffraction RX, Structure cristalline, Structure moléculaire, Spectre RMN, Angle magique, Phosphore 31, Scandium 45, Hydrogène 1, Liaison hydrogène, 6166F, Ethylènediammonium.
English descriptors
- KwdEn :
- Chemical preparation, Crystal structure, Experimental study, Hybrid material, Hydrogen 1, Hydrogen bonds, Hydrothermal synthesis, Magic angle, Molecular structure, NMR spectra, Open framework, Organic dication, Phosphorus 31, Saturated aliphatic compound, Scandium 45, Scandium Acid phosphates, Template, XRD.
Abstract
Using the well-known chemical analogy 2SiIVO2 ↔ MIIIPO4, the first organically templated scandium phosphate was hydrothermally synthesized. Sc(HP04)2.0.5(N2C2H10) crystallizes in the monoclinic P2/n (no. 13) space group with lattice parameters a = 9.4088(2) Å, b = 9.0924(1) Å, c = 9.6884(2) Å, β = 117.252(1)°, V = 736.83(2) Å3, Z = 4. Its structure was solved by single-crystal X-ray diffraction and was already encountered with indium in place of scandium. It is composed of corner-sharing ScO6 octahedra and HPO4 tetrahedra whose connections ensure a three-dimensional framework exhibiting cages delimited by eight-membered windows where the ethylendiammonium cations are encapsulated. The local structure of the framework was characterized by 31P MAS, 45Sc MAS, and 3QMAS NMR spectroscopies. The interaction between the inorganic network and the template is probed using 1H-31P heteronuclear correlation NMR spectroscopy, which provided evidence for strong hydrogen bonds between the amino protons and the oxygen atoms of the inorganic network.
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en" level="a">Hydrothermal synthesis, structure determination, and solid-state NMR study of the first organically templated scandium phosphate</title><author><name sortKey="Riou, D" uniqKey="Riou D">D. Riou</name><affiliation wicri:level="3"><inist:fA14 i1="01"><s1>Institut Lavoisier UMR 8637, Université de Versailles-St. Quentin en Yvelines, 45 Avenue des Etats-Unis</s1><s2>78035 Versailles</s2><s3>FRA</s3><sZ>1 aut.</sZ></inist:fA14><country>France</country><placeName><region type="region" nuts="2">Île-de-France</region><settlement type="city">Versailles</settlement></placeName></affiliation></author><author><name sortKey="Fayon, F" uniqKey="Fayon F">F. Fayon</name><affiliation wicri:level="3"><inist:fA14 i1="02"><s1>Centre de Recherche sur les Matériaux à Haute Température CNRS, 1d Avenue de la recherche scientifique</s1><s2>45071 Orléans</s2><s3>FRA</s3><sZ>2 aut.</sZ><sZ>3 aut.</sZ></inist:fA14><country>France</country><placeName><region type="region" nuts="2">Région Centre</region><settlement type="city">Orléans</settlement></placeName></affiliation></author><author><name sortKey="Massiot, D" uniqKey="Massiot D">D. Massiot</name><affiliation wicri:level="3"><inist:fA14 i1="02"><s1>Centre de Recherche sur les Matériaux à Haute Température CNRS, 1d Avenue de la recherche scientifique</s1><s2>45071 Orléans</s2><s3>FRA</s3><sZ>2 aut.</sZ><sZ>3 aut.</sZ></inist:fA14><country>France</country><placeName><region type="region" nuts="2">Région Centre</region><settlement type="city">Orléans</settlement></placeName></affiliation></author></titleStmt><publicationStmt><idno type="inist">02-0453575</idno><date when="2002">2002</date><idno type="stanalyst">PASCAL 02-0453575 INIST</idno><idno type="RBID">Pascal:02-0453575</idno><idno type="wicri:Area/Main/Corpus">00E935</idno><idno type="wicri:Area/Main/Repository">00F202</idno></publicationStmt><seriesStmt><idno type="ISSN">0897-4756</idno><title level="j" type="abbreviated">Chem. mater.</title><title level="j" type="main">Chemistry of materials</title></seriesStmt></fileDesc><profileDesc><textClass><keywords scheme="KwdEn" xml:lang="en"><term>Chemical preparation</term><term>Crystal structure</term><term>Experimental study</term><term>Hybrid material</term><term>Hydrogen 1</term><term>Hydrogen bonds</term><term>Hydrothermal synthesis</term><term>Magic angle</term><term>Molecular structure</term><term>NMR spectra</term><term>Open framework</term><term>Organic dication</term><term>Phosphorus 31</term><term>Saturated aliphatic compound</term><term>Scandium 45</term><term>Scandium Acid phosphates</term><term>Template</term><term>XRD</term></keywords><keywords scheme="Pascal" xml:lang="fr"><term>Etude expérimentale</term><term>Préparation chimique</term><term>Synthèse hydrothermale</term><term>Scandium Hydrogénophosphate</term><term>Template</term><term>Matériau hybride</term><term>Structure ouverte</term><term>Dication organique</term><term>Composé aliphatique saturé</term><term>Diffraction RX</term><term>Structure cristalline</term><term>Structure moléculaire</term><term>Spectre RMN</term><term>Angle magique</term><term>Phosphore 31</term><term>Scandium 45</term><term>Hydrogène 1</term><term>Liaison hydrogène</term><term>6166F</term><term>Ethylènediammonium</term></keywords></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">Using the well-known chemical analogy 2Si<sup>IV</sup>O<sub>2</sub> ↔ M<sup>III</sup>PO<sub>4</sub>, the first organically templated scandium phosphate was hydrothermally synthesized. Sc(HP04)<sub>2</sub>.0.5(N<sub>2</sub>C<sub>2</sub>H<sub>10</sub>) crystallizes in the monoclinic P2/n (no. 13) space group with lattice parameters a = 9.4088(2) Å, b = 9.0924(1) Å, c = 9.6884(2) Å, β = 117.252(1)°, V = 736.83(2) Å<sup>3</sup>, Z = 4. Its structure was solved by single-crystal X-ray diffraction and was already encountered with indium in place of scandium. It is composed of corner-sharing ScO<sub>6</sub> octahedra and HPO<sub>4</sub> tetrahedra whose connections ensure a three-dimensional framework exhibiting cages delimited by eight-membered windows where the ethylendiammonium cations are encapsulated. The local structure of the framework was characterized by <sup>31</sup>P MAS, <sup>45</sup>Sc MAS, and 3QMAS NMR spectroscopies. The interaction between the inorganic network and the template is probed using <sup>1</sup>H-<sup>31</sup>P heteronuclear correlation NMR spectroscopy, which provided evidence for strong hydrogen bonds between the amino protons and the oxygen atoms of the inorganic network.</div></front></TEI><inist><standard h6="B"><pA><fA01 i1="01" i2="1"><s0>0897-4756</s0></fA01><fA03 i2="1"><s0>Chem. mater.</s0></fA03><fA05><s2>14</s2></fA05><fA06><s2>5</s2></fA06><fA08 i1="01" i2="1" l="ENG"><s1>Hydrothermal synthesis, structure determination, and solid-state NMR study of the first organically templated scandium phosphate</s1></fA08><fA11 i1="01" i2="1"><s1>RIOU (D.)</s1></fA11><fA11 i1="02" i2="1"><s1>FAYON (F.)</s1></fA11><fA11 i1="03" i2="1"><s1>MASSIOT (D.)</s1></fA11><fA14 i1="01"><s1>Institut Lavoisier UMR 8637, Université de Versailles-St. Quentin en Yvelines, 45 Avenue des Etats-Unis</s1><s2>78035 Versailles</s2><s3>FRA</s3><sZ>1 aut.</sZ></fA14><fA14 i1="02"><s1>Centre de Recherche sur les Matériaux à Haute Température CNRS, 1d Avenue de la recherche scientifique</s1><s2>45071 Orléans</s2><s3>FRA</s3><sZ>2 aut.</sZ><sZ>3 aut.</sZ></fA14><fA20><s1>2416-2420</s1></fA20><fA21><s1>2002</s1></fA21><fA23 i1="01"><s0>ENG</s0></fA23><fA43 i1="01"><s1>INIST</s1><s2>21957</s2><s5>354000108334820700</s5></fA43><fA44><s0>0000</s0><s1>© 2002 INIST-CNRS. All rights reserved.</s1></fA44><fA45><s0>21 ref.</s0></fA45><fA47 i1="01" i2="1"><s0>02-0453575</s0></fA47><fA60><s1>P</s1></fA60><fA61><s0>A</s0></fA61><fA64 i1="01" i2="1"><s0>Chemistry of materials</s0></fA64><fA66 i1="01"><s0>USA</s0></fA66><fC01 i1="01" l="ENG"><s0>Using the well-known chemical analogy 2Si<sup>IV</sup>O<sub>2</sub> ↔ M<sup>III</sup>PO<sub>4</sub>, the first organically templated scandium phosphate was hydrothermally synthesized. Sc(HP04)<sub>2</sub>.0.5(N<sub>2</sub>C<sub>2</sub>H<sub>10</sub>) crystallizes in the monoclinic P2/n (no. 13) space group with lattice parameters a = 9.4088(2) Å, b = 9.0924(1) Å, c = 9.6884(2) Å, β = 117.252(1)°, V = 736.83(2) Å<sup>3</sup>, Z = 4. Its structure was solved by single-crystal X-ray diffraction and was already encountered with indium in place of scandium. It is composed of corner-sharing ScO<sub>6</sub> octahedra and HPO<sub>4</sub> tetrahedra whose connections ensure a three-dimensional framework exhibiting cages delimited by eight-membered windows where the ethylendiammonium cations are encapsulated. The local structure of the framework was characterized by <sup>31</sup>P MAS, <sup>45</sup>Sc MAS, and 3QMAS NMR spectroscopies. The interaction between the inorganic network and the template is probed using <sup>1</sup>H-<sup>31</sup>P heteronuclear correlation NMR spectroscopy, which provided evidence for strong hydrogen bonds between the amino protons and the oxygen atoms of the inorganic network.</s0></fC01><fC02 i1="01" i2="3"><s0>001B60A66F7</s0></fC02><fC03 i1="01" i2="3" l="FRE"><s0>Etude expérimentale</s0><s5>01</s5></fC03><fC03 i1="01" i2="3" l="ENG"><s0>Experimental study</s0><s5>01</s5></fC03><fC03 i1="02" i2="3" l="FRE"><s0>Préparation chimique</s0><s5>02</s5></fC03><fC03 i1="02" i2="3" l="ENG"><s0>Chemical preparation</s0><s5>02</s5></fC03><fC03 i1="03" i2="3" l="FRE"><s0>Synthèse hydrothermale</s0><s5>03</s5></fC03><fC03 i1="03" i2="3" l="ENG"><s0>Hydrothermal synthesis</s0><s5>03</s5></fC03><fC03 i1="04" i2="3" l="FRE"><s0>Scandium Hydrogénophosphate</s0><s2>NC</s2><s2>NA</s2><s5>08</s5></fC03><fC03 i1="04" i2="3" l="ENG"><s0>Scandium Acid phosphates</s0><s2>NC</s2><s2>NA</s2><s5>08</s5></fC03><fC03 i1="05" i2="3" l="FRE"><s0>Template</s0><s5>09</s5></fC03><fC03 i1="05" i2="3" l="ENG"><s0>Template</s0><s5>09</s5></fC03><fC03 i1="06" i2="X" l="FRE"><s0>Matériau hybride</s0><s5>10</s5></fC03><fC03 i1="06" i2="X" l="ENG"><s0>Hybrid material</s0><s5>10</s5></fC03><fC03 i1="06" i2="X" l="SPA"><s0>Material híbrido</s0><s5>10</s5></fC03><fC03 i1="07" i2="X" l="FRE"><s0>Structure ouverte</s0><s5>11</s5></fC03><fC03 i1="07" i2="X" l="ENG"><s0>Open framework</s0><s5>11</s5></fC03><fC03 i1="07" i2="X" l="SPA"><s0>Estructura abierta</s0><s5>11</s5></fC03><fC03 i1="08" i2="X" l="FRE"><s0>Dication organique</s0><s5>13</s5></fC03><fC03 i1="08" i2="X" l="ENG"><s0>Organic dication</s0><s5>13</s5></fC03><fC03 i1="08" i2="X" l="SPA"><s0>Dicatión orgánico</s0><s5>13</s5></fC03><fC03 i1="09" i2="X" l="FRE"><s0>Composé aliphatique saturé</s0><s5>15</s5></fC03><fC03 i1="09" i2="X" l="ENG"><s0>Saturated aliphatic compound</s0><s5>15</s5></fC03><fC03 i1="09" i2="X" l="SPA"><s0>Compuesto alifático saturado</s0><s5>15</s5></fC03><fC03 i1="10" i2="3" l="FRE"><s0>Diffraction RX</s0><s5>16</s5></fC03><fC03 i1="10" i2="3" l="ENG"><s0>XRD</s0><s5>16</s5></fC03><fC03 i1="11" i2="3" l="FRE"><s0>Structure cristalline</s0><s5>17</s5></fC03><fC03 i1="11" i2="3" l="ENG"><s0>Crystal structure</s0><s5>17</s5></fC03><fC03 i1="12" i2="3" l="FRE"><s0>Structure moléculaire</s0><s5>18</s5></fC03><fC03 i1="12" i2="3" l="ENG"><s0>Molecular structure</s0><s5>18</s5></fC03><fC03 i1="13" i2="3" l="FRE"><s0>Spectre RMN</s0><s5>19</s5></fC03><fC03 i1="13" i2="3" l="ENG"><s0>NMR spectra</s0><s5>19</s5></fC03><fC03 i1="14" i2="X" l="FRE"><s0>Angle magique</s0><s5>20</s5></fC03><fC03 i1="14" i2="X" l="ENG"><s0>Magic angle</s0><s5>20</s5></fC03><fC03 i1="14" i2="X" l="SPA"><s0>Angulo mágico</s0><s5>20</s5></fC03><fC03 i1="15" i2="3" l="FRE"><s0>Phosphore 31</s0><s5>21</s5></fC03><fC03 i1="15" i2="3" l="ENG"><s0>Phosphorus 31</s0><s5>21</s5></fC03><fC03 i1="16" i2="3" l="FRE"><s0>Scandium 45</s0><s5>22</s5></fC03><fC03 i1="16" i2="3" l="ENG"><s0>Scandium 45</s0><s5>22</s5></fC03><fC03 i1="17" i2="3" l="FRE"><s0>Hydrogène 1</s0><s5>23</s5></fC03><fC03 i1="17" i2="3" l="ENG"><s0>Hydrogen 1</s0><s5>23</s5></fC03><fC03 i1="18" i2="3" l="FRE"><s0>Liaison hydrogène</s0><s5>24</s5></fC03><fC03 i1="18" i2="3" l="ENG"><s0>Hydrogen bonds</s0><s5>24</s5></fC03><fC03 i1="19" i2="3" l="FRE"><s0>6166F</s0><s2>PAC</s2><s4>INC</s4><s5>56</s5></fC03><fC03 i1="20" i2="3" l="FRE"><s0>Ethylènediammonium</s0><s2>NK</s2><s4>INC</s4><s5>92</s5></fC03><fC07 i1="01" i2="3" l="FRE"><s0>Composé minéral</s0><s5>04</s5></fC07><fC07 i1="01" i2="3" l="ENG"><s0>Inorganic compounds</s0><s5>04</s5></fC07><fC07 i1="02" i2="3" l="FRE"><s0>Phosphate</s0><s2>NA</s2><s5>05</s5></fC07><fC07 i1="02" i2="3" l="ENG"><s0>Phosphates</s0><s2>NA</s2><s5>05</s5></fC07><fC07 i1="03" i2="3" l="FRE"><s0>Métal transition complexe</s0><s5>06</s5></fC07><fC07 i1="03" i2="3" l="ENG"><s0>Transition element complexes</s0><s5>06</s5></fC07><fC07 i1="04" i2="3" l="FRE"><s0>Hydrogénophosphate</s0><s2>NA</s2><s5>07</s5></fC07><fC07 i1="04" i2="3" l="ENG"><s0>Acid phosphates</s0><s2>NA</s2><s5>07</s5></fC07><fC07 i1="05" i2="3" l="FRE"><s0>Composé organique</s0><s5>12</s5></fC07><fC07 i1="05" i2="3" l="ENG"><s0>Organic compounds</s0><s5>12</s5></fC07><fC07 i1="06" i2="X" l="FRE"><s0>Ammonium Composé organique</s0><s2>NC</s2><s2>NA</s2><s5>14</s5></fC07><fC07 i1="06" i2="X" l="ENG"><s0>Ammonium Organic compounds</s0><s2>NC</s2><s2>NA</s2><s5>14</s5></fC07><fC07 i1="06" i2="X" l="SPA"><s0>Amonio Compuesto orgánico</s0><s2>NC</s2><s2>NA</s2><s5>14</s5></fC07><fN21><s1>266</s1></fN21><fN82><s1>PSI</s1></fN82></pA></standard></inist></record>Pour manipuler ce document sous Unix (Dilib)
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