CobaltMaghrebV1, Main, Exploration, bibRecord, 001469

Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O

Identifieur interne : 001469 ( Main/Exploration ); précédent : 001468; suivant : 001470

Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O

Auteurs : Slaheddine Kamoun [Tunisie] ; Amor Jouini [Tunisie]

Source :

Journal of Solid State Chemistry [ 0022-4596 ] ; 1990.

RBID : ISTEX:949BBF08BCB15E3E0AE89513899B48185632DCDA

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 PO 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, NH····O, POH····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.

Url:

https://api.istex.fr/document/949BBF08BCB15E3E0AE89513899B48185632DCDA/fulltext/pdf

DOI: 10.1016/0022-4596(90)90294-8

Affiliations:

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Le document en format XML

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<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 PO 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, NH····O, POH····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>
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Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O

Etude calorimétrique et structure cristalline du putrescinium monohydrogénomonophosphate dihydrate NH3(CH2)4NH3HPO42H2O

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Abstract

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