Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O
Identifieur interne : 001151 ( Istex/Corpus ); précédent : 001150; suivant : 001152Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O
Auteurs : Slaheddine Kamoun ; Amor JouiniSource :
- Journal of Solid State Chemistry [ 0022-4596 ] ; 1990.
Abstract
Abstract: Chemical preparation, calorimetric studies, and crystal structure are given for a new monophosphate. The putrescinium monohydrogen monophosphate dihydrate salt is monoclinic with the unit cell dimensions a = 6.541(1) Å, b = 16.648(3) Å, c = 9.175(1) Å, β = 95.74(1)°, V = 994.1(5) Å3, Dm = 1.498 Mgm−3, Dx = 1.484 Mgm−3, μ = 2.732 mm−1, space group P21 c with Z = 4. The structure was solved by the Patterson method and refined to a final value of 0.046 for 1732 observed independent reflections. The structure shows a layer arrangement perpendicular to the c axis: planes of the [HPO4]2− tetrahedra alternate with planes of the [(CH2)4(NH3)2]2+ dication. The zeolitic water molecules are located between these planes separated by a distance of 2.294 Å. The monohydrogen phosphate group is roughly tetrahedral with the symmetry 3m. The PO distances in this group range from 1.495(2) to 1.592(2) Å. The amino groups of putrescine are protonated. The putrescinium dication has an extensive all-trans configuration with a noncrystallographic inversion center. The cohesion and the stability of the atomic arrangement result from three kinds of hydrogen bonds, NH····O, POH····O(w), and O(W)H····O. The differential scanning calorimetric study shows that the dehydration of this salt occurs in two steps respectively at 105 and 121°C with a loss of one water molecule per step. The anhydrous salt undergoes four phase transitions respectively at temperatures of 133, 143, 159, and 165°C.
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DOI: 10.1016/0022-4596(90)90294-8
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<record><TEI wicri:istexFullTextTei="biblStruct"><teiHeader><fileDesc><titleStmt><title xml:lang="fr">Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O</title><author><name sortKey="Kamoun, Slaheddine" sort="Kamoun, Slaheddine" uniqKey="Kamoun S" first="Slaheddine" last="Kamoun">Slaheddine Kamoun</name><affiliation><mods:affiliation>Laboratoire de l'Etat Solide, Département de Chimie, Ecole Nationale d'Ingénieurs de Sfax, 3038 Sfax, Tunisie</mods:affiliation></affiliation></author><author><name sortKey="Jouini, Amor" sort="Jouini, Amor" uniqKey="Jouini A" first="Amor" last="Jouini">Amor Jouini</name><affiliation><mods:affiliation>Laboratoire de l'Etat Solide, Département de Chimie Faculté des Sciences de Monastir, 5000 Monastir, Tunisie</mods:affiliation></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">ISTEX</idno><idno type="RBID">ISTEX:949BBF08BCB15E3E0AE89513899B48185632DCDA</idno><date when="1990" year="1990">1990</date><idno type="doi">10.1016/0022-4596(90)90294-8</idno><idno type="url">https://api.istex.fr/document/949BBF08BCB15E3E0AE89513899B48185632DCDA/fulltext/pdf</idno><idno type="wicri:Area/Istex/Corpus">001151</idno><idno type="wicri:explorRef" wicri:stream="Istex" wicri:step="Corpus" wicri:corpus="ISTEX">001151</idno></publicationStmt><sourceDesc><biblStruct><analytic><title level="a" type="main" xml:lang="fr">Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O</title><author><name sortKey="Kamoun, Slaheddine" sort="Kamoun, Slaheddine" uniqKey="Kamoun S" first="Slaheddine" last="Kamoun">Slaheddine Kamoun</name><affiliation><mods:affiliation>Laboratoire de l'Etat Solide, Département de Chimie, Ecole Nationale d'Ingénieurs de Sfax, 3038 Sfax, Tunisie</mods:affiliation></affiliation></author><author><name sortKey="Jouini, Amor" sort="Jouini, Amor" uniqKey="Jouini A" first="Amor" last="Jouini">Amor Jouini</name><affiliation><mods:affiliation>Laboratoire de l'Etat Solide, Département de Chimie Faculté des Sciences de Monastir, 5000 Monastir, Tunisie</mods:affiliation></affiliation></author></analytic><monogr></monogr><series><title level="j">Journal of Solid State Chemistry</title><title level="j" type="abbrev">YJSSC</title><idno type="ISSN">0022-4596</idno><imprint><publisher>ELSEVIER</publisher><date type="published" when="1990">1990</date><biblScope unit="volume">89</biblScope><biblScope unit="issue">1</biblScope><biblScope unit="page" from="67">67</biblScope><biblScope unit="page" to="74">74</biblScope></imprint><idno type="ISSN">0022-4596</idno></series><idno type="istex">949BBF08BCB15E3E0AE89513899B48185632DCDA</idno><idno type="DOI">10.1016/0022-4596(90)90294-8</idno><idno type="PII">0022-4596(90)90294-8</idno></biblStruct></sourceDesc><seriesStmt><idno type="ISSN">0022-4596</idno></seriesStmt></fileDesc><profileDesc><textClass></textClass><langUsage><language ident="fr">fr</language></langUsage></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">Abstract: Chemical preparation, calorimetric studies, and crystal structure are given for a new monophosphate. The putrescinium monohydrogen monophosphate dihydrate salt is monoclinic with the unit cell dimensions a = 6.541(1) Å, b = 16.648(3) Å, c = 9.175(1) Å, β = 95.74(1)°, V = 994.1(5) Å3, Dm = 1.498 Mgm−3, Dx = 1.484 Mgm−3, μ = 2.732 mm−1, space group P21 c with Z = 4. The structure was solved by the Patterson method and refined to a final value of 0.046 for 1732 observed independent reflections. The structure shows a layer arrangement perpendicular to the c axis: planes of the [HPO4]2− tetrahedra alternate with planes of the [(CH2)4(NH3)2]2+ dication. The zeolitic water molecules are located between these planes separated by a distance of 2.294 Å. The monohydrogen phosphate group is roughly tetrahedral with the symmetry 3m. The PO distances in this group range from 1.495(2) to 1.592(2) Å. The amino groups of putrescine are protonated. The putrescinium dication has an extensive all-trans configuration with a noncrystallographic inversion center. The cohesion and the stability of the atomic arrangement result from three kinds of hydrogen bonds, NH····O, POH····O(w), and O(W)H····O. The differential scanning calorimetric study shows that the dehydration of this salt occurs in two steps respectively at 105 and 121°C with a loss of one water molecule per step. The anhydrous salt undergoes four phase transitions respectively at temperatures of 133, 143, 159, and 165°C.</div></front></TEI><istex><corpusName>elsevier</corpusName><author><json:item><name>Slaheddine Kamoun</name><affiliations><json:string>Laboratoire de l'Etat Solide, Département de Chimie, Ecole Nationale d'Ingénieurs de Sfax, 3038 Sfax, Tunisie</json:string></affiliations></json:item><json:item><name>Amor Jouini</name><affiliations><json:string>Laboratoire de l'Etat Solide, Département de Chimie Faculté des Sciences de Monastir, 5000 Monastir, Tunisie</json:string></affiliations></json:item></author><language><json:string>fre</json:string></language><originalGenre><json:string>Full-length article</json:string></originalGenre><abstract>Chemical preparation, calorimetric studies, and crystal structure are given for a new monophosphate. The putrescinium monohydrogen monophosphate dihydrate salt is monoclinic with the unit cell dimensions a = 6.541(1) Å, b = 16.648(3) Å, c = 9.175(1) Å, β = 95.74(1)°, V = 994.1(5) Å3, Dm = 1.498 Mgm−3, Dx = 1.484 Mgm−3, μ = 2.732 mm−1, space group P21 c with Z = 4. The structure was solved by the Patterson method and refined to a final value of 0.046 for 1732 observed independent reflections. The structure shows a layer arrangement perpendicular to the c axis: planes of the [HPO4]2− tetrahedra alternate with planes of the [(CH2)4(NH3)2]2+ dication. The zeolitic water molecules are located between these planes separated by a distance of 2.294 Å. The monohydrogen phosphate group is roughly tetrahedral with the symmetry 3m. The PO distances in this group range from 1.495(2) to 1.592(2) Å. The amino groups of putrescine are protonated. The putrescinium dication has an extensive all-trans configuration with a noncrystallographic inversion center. The cohesion and the stability of the atomic arrangement result from three kinds of hydrogen bonds, NH····O, POH····O(w), and O(W)H····O. The differential scanning calorimetric study shows that the dehydration of this salt occurs in two steps respectively at 105 and 121°C with a loss of one water molecule per step. The anhydrous salt undergoes four phase transitions respectively at temperatures of 133, 143, 159, and 165°C.</abstract><qualityIndicators><score>5.086</score><pdfVersion>1.3</pdfVersion><pdfPageSize>504 x 720 pts</pdfPageSize><refBibsNative>true</refBibsNative><keywordCount>0</keywordCount><abstractCharCount>1487</abstractCharCount><pdfWordCount>2278</pdfWordCount><pdfCharCount>19896</pdfCharCount><pdfPageCount>8</pdfPageCount><abstractWordCount>234</abstractWordCount></qualityIndicators><title>Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O</title><pii><json:string>0022-4596(90)90294-8</json:string></pii><genre><json:string>research-article</json:string></genre><serie><language><json:string>unknown</json:string></language><title>(Present distributor: Kluwer, Academic Publishers, Dordrecht)</title></serie><host><volume>89</volume><pii><json:string>S0022-4596(00)X0336-2</json:string></pii><pages><last>74</last><first>67</first></pages><issn><json:string>0022-4596</json:string></issn><issue>1</issue><genre><json:string>journal</json:string></genre><language><json:string>unknown</json:string></language><title>Journal of Solid State Chemistry</title><publicationDate>1990</publicationDate></host><categories><wos><json:string>CHEMISTRY, INORGANIC & NUCLEAR</json:string><json:string>CHEMISTRY, PHYSICAL</json:string></wos></categories><publicationDate>1990</publicationDate><copyrightDate>1990</copyrightDate><doi><json:string>10.1016/0022-4596(90)90294-8</json:string></doi><id>949BBF08BCB15E3E0AE89513899B48185632DCDA</id><score>0.04617217</score><fulltext><json:item><original>true</original><mimetype>application/pdf</mimetype><extension>pdf</extension><uri>https://api.istex.fr/document/949BBF08BCB15E3E0AE89513899B48185632DCDA/fulltext/pdf</uri></json:item><json:item><original>false</original><mimetype>application/zip</mimetype><extension>zip</extension><uri>https://api.istex.fr/document/949BBF08BCB15E3E0AE89513899B48185632DCDA/fulltext/zip</uri></json:item><istex:fulltextTEI uri="https://api.istex.fr/document/949BBF08BCB15E3E0AE89513899B48185632DCDA/fulltext/tei"><teiHeader><fileDesc><titleStmt><title level="a" type="main" xml:lang="fr">Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O</title></titleStmt><publicationStmt><authority>ISTEX</authority><publisher>ELSEVIER</publisher><availability><p>ELSEVIER</p></availability><date>1990</date></publicationStmt><sourceDesc><biblStruct type="inbook"><analytic><title level="a" type="main" xml:lang="fr">Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O</title><author xml:id="author-1"><persName><forename type="first">Slaheddine</forename><surname>Kamoun</surname></persName><affiliation>Laboratoire de l'Etat Solide, Département de Chimie, Ecole Nationale d'Ingénieurs de Sfax, 3038 Sfax, Tunisie</affiliation></author><author xml:id="author-2"><persName><forename type="first">Amor</forename><surname>Jouini</surname></persName><affiliation>Laboratoire de l'Etat Solide, Département de Chimie Faculté des Sciences de Monastir, 5000 Monastir, Tunisie</affiliation></author></analytic><monogr><title level="j">Journal of Solid State Chemistry</title><title level="j" type="abbrev">YJSSC</title><idno type="pISSN">0022-4596</idno><idno type="PII">S0022-4596(00)X0336-2</idno><imprint><publisher>ELSEVIER</publisher><date type="published" when="1990"></date><biblScope unit="volume">89</biblScope><biblScope unit="issue">1</biblScope><biblScope unit="page" from="67">67</biblScope><biblScope unit="page" to="74">74</biblScope></imprint></monogr><idno type="istex">949BBF08BCB15E3E0AE89513899B48185632DCDA</idno><idno type="DOI">10.1016/0022-4596(90)90294-8</idno><idno type="PII">0022-4596(90)90294-8</idno></biblStruct></sourceDesc></fileDesc><profileDesc><creation><date>1990</date></creation><langUsage><language ident="fr">fr</language></langUsage><abstract xml:lang="en"><p>Abstract: Chemical preparation, calorimetric studies, and crystal structure are given for a new monophosphate. The putrescinium monohydrogen monophosphate dihydrate salt is monoclinic with the unit cell dimensions a = 6.541(1) Å, b = 16.648(3) Å, c = 9.175(1) Å, β = 95.74(1)°, V = 994.1(5) Å3, Dm = 1.498 Mgm−3, Dx = 1.484 Mgm−3, μ = 2.732 mm−1, space group P21 c with Z = 4. The structure was solved by the Patterson method and refined to a final value of 0.046 for 1732 observed independent reflections. The structure shows a layer arrangement perpendicular to the c axis: planes of the [HPO4]2− tetrahedra alternate with planes of the [(CH2)4(NH3)2]2+ dication. The zeolitic water molecules are located between these planes separated by a distance of 2.294 Å. The monohydrogen phosphate group is roughly tetrahedral with the symmetry 3m. The PO distances in this group range from 1.495(2) to 1.592(2) Å. The amino groups of putrescine are protonated. The putrescinium dication has an extensive all-trans configuration with a noncrystallographic inversion center. The cohesion and the stability of the atomic arrangement result from three kinds of hydrogen bonds, NH····O, POH····O(w), and O(W)H····O. The differential scanning calorimetric study shows that the dehydration of this salt occurs in two steps respectively at 105 and 121°C with a loss of one water molecule per step. The anhydrous salt undergoes four phase transitions respectively at temperatures of 133, 143, 159, and 165°C.</p></abstract></profileDesc><revisionDesc><change when="1990-05-29">Modified</change><change when="1990">Published</change></revisionDesc></teiHeader></istex:fulltextTEI><json:item><original>false</original><mimetype>text/plain</mimetype><extension>txt</extension><uri>https://api.istex.fr/document/949BBF08BCB15E3E0AE89513899B48185632DCDA/fulltext/txt</uri></json:item></fulltext><metadata><istex:metadataXml wicri:clean="Elsevier, elements deleted: tail"><istex:xmlDeclaration>version="1.0" encoding="utf-8"</istex:xmlDeclaration><istex:docType PUBLIC="-//ES//DTD journal article DTD version 4.5.2//EN//XML" URI="art452.dtd" name="istex:docType"></istex:docType><istex:document><converted-article version="4.5.2" docsubtype="fla" xml:lang="fr"><item-info><jid>YJSSC</jid><aid>90902948</aid><ce:pii>0022-4596(90)90294-8</ce:pii><ce:doi>10.1016/0022-4596(90)90294-8</ce:doi><ce:copyright type="unknown" year="1990"></ce:copyright></item-info><head><ce:title>Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH<ce:inf>3</ce:inf>(CH<ce:inf>2</ce:inf>)<ce:inf>4</ce:inf>NH<ce:inf>3</ce:inf>HPO<ce:inf>4</ce:inf>2H<ce:inf>2</ce:inf>O</ce:title><ce:author-group><ce:author><ce:given-name>Slaheddine</ce:given-name><ce:surname>Kamoun</ce:surname></ce:author><ce:affiliation><ce:textfn>Laboratoire de l'Etat Solide, Département de Chimie, Ecole Nationale d'Ingénieurs de Sfax, 3038 Sfax, Tunisie</ce:textfn></ce:affiliation></ce:author-group><ce:author-group><ce:author><ce:given-name>Amor</ce:given-name><ce:surname>Jouini</ce:surname></ce:author><ce:affiliation><ce:textfn>Laboratoire de l'Etat Solide, Département de Chimie Faculté des Sciences de Monastir, 5000 Monastir, Tunisie</ce:textfn></ce:affiliation></ce:author-group><ce:date-received day="12" month="3" year="1990"></ce:date-received><ce:date-revised day="29" month="5" year="1990"></ce:date-revised><ce:abstract xml:lang="en"><ce:section-title>Abstract</ce:section-title><ce:abstract-sec><ce:simple-para>Chemical preparation, calorimetric studies, and crystal structure are given for a new monophosphate. The putrescinium monohydrogen monophosphate dihydrate salt is monoclinic with the unit cell dimensions <ce:italic>a</ce:italic> = 6.541(1) Å, <ce:italic>b</ce:italic> = 16.648(3) Å, <ce:italic>c</ce:italic> = 9.175(1) Å, β = 95.74(1)°, <ce:italic>V</ce:italic> = 994.1(5) Å<ce:sup>3</ce:sup>, <ce:italic>D</ce:italic><ce:inf>m</ce:inf> = 1.498 Mgm<ce:sup>−3</ce:sup>, <ce:italic>D</ce:italic><ce:inf><ce:italic>x</ce:italic></ce:inf> = 1.484 Mgm<ce:sup>−3</ce:sup>, μ = 2.732 mm<ce:sup>−1</ce:sup>, space group <math altimg="si1.gif"><fr shape="sol"><nu>P2<inf>1</inf></nu><de>c</de></fr></math> with <ce:italic>Z</ce:italic> = 4. The structure was solved by the Patterson method and refined to a final value of 0.046 for 1732 observed independent reflections. The structure shows a layer arrangement perpendicular to the <math altimg="si2.gif"><ovl type="rarr">c</ovl></math> axis: planes of the [HPO<ce:inf>4</ce:inf>]<ce:sup>2−</ce:sup> tetrahedra alternate with planes of the [(CH<ce:inf>2</ce:inf>)<ce:inf>4</ce:inf>(NH<ce:inf>3</ce:inf>)<ce:inf>2</ce:inf>]<ce:sup>2+</ce:sup> dication. The zeolitic water molecules are located between these planes separated by a distance of 2.294 Å. The monohydrogen phosphate group is roughly tetrahedral with the symmetry 3<ce:italic>m</ce:italic>. The PO distances in this group range from 1.495(2) to 1.592(2) Å. The amino groups of putrescine are protonated. The putrescinium dication has an extensive all-<ce:italic>trans</ce:italic> configuration with a noncrystallographic inversion center. The cohesion and the stability of the atomic arrangement result from three kinds of hydrogen bonds, NH····O, POH····O(w), and O(W)H····O. The differential scanning calorimetric study shows that the dehydration of this salt occurs in two steps respectively at 105 and 121°C with a loss of one water molecule per step. The anhydrous salt undergoes four phase transitions respectively at temperatures of 133, 143, 159, and 165°C.</ce:simple-para></ce:abstract-sec></ce:abstract></head></converted-article></istex:document></istex:metadataXml><mods version="3.6"><titleInfo lang="fr"><title>Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O</title></titleInfo><titleInfo type="alternative" lang="fr" contentType="CDATA"><title>Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH</title></titleInfo><name type="personal"><namePart type="given">Slaheddine</namePart><namePart type="family">Kamoun</namePart><affiliation>Laboratoire de l'Etat Solide, Département de Chimie, Ecole Nationale d'Ingénieurs de Sfax, 3038 Sfax, Tunisie</affiliation><role><roleTerm type="text">author</roleTerm></role></name><name type="personal"><namePart type="given">Amor</namePart><namePart type="family">Jouini</namePart><affiliation>Laboratoire de l'Etat Solide, Département de Chimie Faculté des Sciences de Monastir, 5000 Monastir, Tunisie</affiliation><role><roleTerm type="text">author</roleTerm></role></name><typeOfResource>text</typeOfResource><genre type="research-article" displayLabel="Full-length article"></genre><originInfo><publisher>ELSEVIER</publisher><dateIssued encoding="w3cdtf">1990</dateIssued><dateModified encoding="w3cdtf">1990-05-29</dateModified><copyrightDate encoding="w3cdtf">1990</copyrightDate></originInfo><language><languageTerm type="code" authority="iso639-2b">fre</languageTerm><languageTerm type="code" authority="rfc3066">fr</languageTerm></language><physicalDescription><internetMediaType>text/html</internetMediaType></physicalDescription><abstract lang="en">Abstract: Chemical preparation, calorimetric studies, and crystal structure are given for a new monophosphate. The putrescinium monohydrogen monophosphate dihydrate salt is monoclinic with the unit cell dimensions a = 6.541(1) Å, b = 16.648(3) Å, c = 9.175(1) Å, β = 95.74(1)°, V = 994.1(5) Å3, Dm = 1.498 Mgm−3, Dx = 1.484 Mgm−3, μ = 2.732 mm−1, space group P21 c with Z = 4. The structure was solved by the Patterson method and refined to a final value of 0.046 for 1732 observed independent reflections. The structure shows a layer arrangement perpendicular to the c axis: planes of the [HPO4]2− tetrahedra alternate with planes of the [(CH2)4(NH3)2]2+ dication. The zeolitic water molecules are located between these planes separated by a distance of 2.294 Å. The monohydrogen phosphate group is roughly tetrahedral with the symmetry 3m. The PO distances in this group range from 1.495(2) to 1.592(2) Å. The amino groups of putrescine are protonated. The putrescinium dication has an extensive all-trans configuration with a noncrystallographic inversion center. The cohesion and the stability of the atomic arrangement result from three kinds of hydrogen bonds, NH····O, POH····O(w), and O(W)H····O. The differential scanning calorimetric study shows that the dehydration of this salt occurs in two steps respectively at 105 and 121°C with a loss of one water molecule per step. The anhydrous salt undergoes four phase transitions respectively at temperatures of 133, 143, 159, and 165°C.</abstract><relatedItem type="host"><titleInfo><title>Journal of Solid State Chemistry</title></titleInfo><titleInfo type="abbreviated"><title>YJSSC</title></titleInfo><genre type="journal">journal</genre><originInfo><dateIssued encoding="w3cdtf">199011</dateIssued></originInfo><identifier type="ISSN">0022-4596</identifier><identifier type="PII">S0022-4596(00)X0336-2</identifier><part><date>199011</date><detail type="volume"><number>89</number><caption>vol.</caption></detail><detail type="issue"><number>1</number><caption>no.</caption></detail><extent unit="issue pages"><start>1</start><end>226</end></extent><extent unit="pages"><start>67</start><end>74</end></extent></part></relatedItem><identifier type="istex">949BBF08BCB15E3E0AE89513899B48185632DCDA</identifier><identifier type="DOI">10.1016/0022-4596(90)90294-8</identifier><identifier type="PII">0022-4596(90)90294-8</identifier><recordInfo><recordContentSource>ELSEVIER</recordContentSource></recordInfo></mods></metadata></istex></record>Pour manipuler ce document sous Unix (Dilib)
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