Crystal Structure, 31 P, 13 C NMR, IR Spectroscopy Investigations and Thermal Behavior of Bis(diisopropylammonium) dihyd
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ORIGINAL PAPER
Crystal Structure, 31P, 13C NMR, IR Spectroscopy Investigations and Thermal Behavior of Bis(diisopropylammonium) dihydrogendiphosphate trihydrate L. Guelmami • A. Jouini
Received: 7 April 2012 / Accepted: 20 September 2012 / Published online: 9 October 2012 Ó Springer Science+Business Media New York 2012
Abstract Physicochemical properties of bis(diisopropylammonium) dihydrogendiphosphate trihydrate, (C6H16N)2 H2P2O73H2O are discussed on the basis of X-ray crystal structure investigation. It crystallizes in the monoclinic system with P21/n space group. Its unit cell dimensions ˚ , b = 15.045(2) A ˚ , c = 14.078(2) A ˚, are a = 12.152(1) A 3 ˚ b = 64.59(1) °, V = 2324.9(4) A , Z = 4. The structure has been solved using direct methods and refined to a reliability R factor 0.0465 for 4,255 reflections. Inorganic arrangement can be described as a three-dimensional infinite network. Organic cations are linked to the mineral entities by hydrogen bonds N–HO. The three-dimensional network of the anionic arrangement is thus consolidated. Thermal analysis reveals the presence of one type of water molecules. Solid state NMR and IR spectroscopies are reported. Keywords Organic-phosphate Crystal structure NMR solid TG–DTA DSC
report the synthesis, the crystal structure, the 31P, 13C solid state NMR, IR spectroscopic characteristics and the thermal behavior of bis(diisopropylammonium) dihydrogendiphosphate trihydrate, (C6H16N)2H2P2O73H2O (denoted as DIPAP).
Experimental Chemical Preparation Crystals of DIPAP were prepared in two steps. A concentrated solution of diphosphoric acid was first prepared by passing a solution of Na4P2O7 (0.5 g mL-1) through an ion exchange resin in its H-state (Amberlite IR 120). The diisopropylamine (C6H15N) was then carefully added drop wise to this aqueous solution to reach the stoichiometric ratio 1:2. Schematically the synthesis reaction is: H2 O H4 P2 O7 þ 2ðC6 H15 NÞ ! ðC6 H16 NÞ2 H2 P2 O7 3H2 O
Introduction In diphosphate chemistry the existence of [HP2O7]3-, [H2P2O7]2- and [H3P2O7]- anions has been well established. Such groups exhibit a characteristic in crystalline materials which is interconnection by very strong hydrogen bonds. They build infinite entities, chains [1], ribbons [2] or planes [3, 4], called macro anions. In the present work, we
L. Guelmami A. Jouini (&) Laboratoire de Chimie du Solide, De´partement de Chimie, Faculte´ des Sciences de Monastir, Universite´ de Monastir, 5019 Al Munastıˆr, Tunisia e-mail: [email protected]
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When most of the solution is evaporated, cube-shaped crystals appear deep down the vessels. The crystals obtained in this way are pure and stable under normal conditions of temperature and humidity. Crystal Data and Structure Determination The intensity data were collected at aroom temperature using an Enraf-Nonius CAD4 diffractometer with Mo(Ka) radiation. The cell parameters were determined from a least square refinement of 25 reflections measured at high angles (13–15°). Two standard reflections were periodic
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