C. Ben Nasr

Crystal Structure and Spectroscopic Studies of a New Organic Dihydrogenmonophosphate [2-NH2-6-CH3-C4H3N2O]2(H2PO4)2

Physicochemical properties of a new dihydrogenmonophosphate [2-NH 2 -6-CH 3 -C 4 H 3 N 2 O] 2 (H 2 PO 4 ) 2 are described on the basis of X-ray crystal structure investigation. This compound crystallizes in the triclinic space group P-1. The unit cell parameters are: a = 7.667(3) Å, b = 8.204(5) Å, c = 14.761(6) Å, α = 98.85(4)°, β = 99.23(3)°, γ = 90.50(4)°, V = 905.0 Å3, and Z = 2. The crystal structure was solved and refined to R = 0.037, using 4351 independent reflections. The atomic arrangement of this compound is built up by (H 2 PO 4 ) n n − chains. Each chain aggregates with organic molecules to form an open framework architecture through hydrogen bond interactions. The structure includes four types of hydrogen bonds. The first one, O─H─O, links the H 2 PO 4 groups to form (H 2 PO 4 ) n n − infinite inorganic chains parallel to the a axis. The three other types, O─H─O(carbonylic), N─H─O(carbonylic), and N─H─O, assemble the inorganic chains so as to build up a three-dimensional arrangement. This compound has also been investigated by IR, and solid-state 13 C and 31 P MAS NMR spectroscopies combined to ab initio calculations.

Synthesis, Structure, and Physicochemical Studies of Hexakis (5-Chloro-2,4-dimethoxyanilinium)cyclohexaphosphate Tetrahydrate

The physicochemical properties of a new organic cyclohexaphosphate, [5-Cl-2,4-(OCH3)2C6H2-NH3]6P6O18·4H2O, are discussed on the basis of an X-ray crystal structure investigation. This compound crystallizes in the monoclinic space group C2/c, with cell parameters a = 37.987(7) Å, b = 13.125(4) Å, c = 14.331(5) Å, β = 98.21(3)°, Z = 4, V = 7072(3) Å3. Its crystal structure is determined and refined to a final R = 0.058 for 5223 independent reflections. The atomic arrangement can be described as a layer organization built up by P6O18 ring anions and water molecules. Between these layers, the organic groups are located that form hydrogen bonds with oxygen atoms of P6O18 rings and water molecules. Intermolecular π–π stacking interactions between two neighboring organic cation rings help to establish the crystal packing. Solid 31P MAS-NMR spectroscopy is in agreement with X-ray structure. Ab initio calculations allow the attribution of the three phosphorus signals to the independent crystallographic sites. This compound is also characterized by thermal analysis and IR spectroscopy. Supplemental materials are available for this article. Go to the publishers online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.

The Synthesis and Characterization of 2-Amino-3-methylpyridinium Dihydrogenmonophosphate: (C6H9N2)H2PO4

A new crystal of 2-amino-3-methylpyridinium dihydrogenmonophosphate has been prepared and characterized by X-ray crystallography, thermal analysis, and impedance and NMR spectroscopies. This compound crystallizes in the triclinic space group P with a = 7.343(2) Å, b = 7.987(2) Å, c = 8.116(4) Å, α = 77,62(3)°, β = 77,74(3)°, γ = 87,03(2)°, V = 454.3 (3)Å3, and Z = 2. The crystal structure was solved and refined to R = 0.030 with 1602 independent reflections. The atomic arrangement can be described as (H2PO4 −)n polymeric chains anchoring the 2-amino-3-methylpyridinium cations through short hydrogen bonds. All ring atoms of the organic entity are coplanar. The exocyclic N atom is an electron receiving center, which is consistent with features of imino resonance evidenced by bond lengths and angles. Solid state 31P, 13C, and 15N CP-MAS-NMR spectroscopies are in agreement with the X-ray structure. Ab initio calculations allow the attribution of carbons and nitrogen to the independent crystallographic sites.

Synthesis and Structure Characterization of Piperazine-1,4-diium Triphosphate

[C 4 N 2 H 12 ] 2 HP 3 O 10 · H 2 O, a new hydrate organic cation monohydrogeno-triphosphate, has been synthesized and characterized by X-ray diffraction, IR spectroscopy, mass angle spinning (MAS), NMR, and thermal analysis. The title compound crystallizes in a monoclinic unit cell with a = 11.072(5), b = 12.324(2), c = 13.122(5) Å, β = 93.85(5)°, Z = 4, V = 1787(1) Å 3 , and a noncentrosymmetric space group P2 1 (no. 4). Crystal structure is determined and refined to R = 0.057 using 4262 independent reflections. The atomic arrangement can be described as a typical layers organization. Layers built by HP 3 O 10 4− anions and water molecules are parallel to the (a, b) planes. Between these layers the piperazinium cations, which form hydrogen bonds with oxygen atoms of the triphosphate anion, are located.

Crystal Structure, (31P, 13C) MAS-NMR, IR Spectroscopy and Thermal Investigations of 2,6-Dimethylanilinium Dihydrogenmonophosphate Monohydrate

Chemical preparation, crystal structure, thermal analysis, IR absorption, and NMR studies are given for a new hybrid organic-inorganic compound, the (2,6-dimethyanilinium) dihydrogenophosphate monohydrate [C 8 H 12 N]H 2 PO 4 ·H 2 O. This compound crystallizes in a triclinic P=1 unit-cell, with a = 7.392(5) Å, b = 8.323(3) Å, c = 10.306(5) Å, α = 95.769 (4)°, β = 102.642 (3)°, γ = 113.498(2)°, V = 554.88(5) Å 3 , and Z = 2. Its crystal structure is determined and refined to R = 0.040 with 1942 independent reflections. The atomic arrangement can be described by inorganic layers built by H 2 PO 4 − anions, and H 2 O molecules with which the organic molecules perform different interactions to form a stable 3D network. Solid state 31 P and 13 C CP-MAS-NMR spectroscopies are in agreement with the X-ray structure.

Crystal Structure and Spectroscopic Studies of a New Organic Dihydrogenmonophosphate [1-(2,3-(CH3)2-C6H3)C4H10N2]H2PO4

The crystal synthesis and structure of a new organic dihydrogenmophosphate [1-(2,3-(CH3)2-C6H3)C4H10N2]H2PO4 are reported. This compound crystallizes in the monoclinic P21/n with a = 7.545(2) Å, b = 26.315(4) Å, c = 7.798(6) Å, β = 115.01(4)°, V = 1403.0(1) Å3, and Z = 4. Crystal structure was solved and refined to R = 0.046, using 1981 independent reflections. It can be described by inorganic layers including the H2PO4 − anions and the NH2 + ammonium groups parallel to (a, c) planes and situated at y = 1/4 and y = 3/4. The interlayer spacing is occupied by the organic molecules which perform different interactions around the 3D network cohesion. A characterization of this compound by solid-state 13C and 31P MAS NMR and ATG is also reported.

Synthesis, Crystal Structure, and NMR Spectroscopy of a New P-Phenylenediamonium Diphosphate [p-NH3C6H4NH3]H2P2O7

Crystal growth and characterization by X-ray diffraction and NMR spectroscopy of a new p-phenylenediamonium diphosphate [p-NH3 C 6 H 4 NH 3]H 2 P 2 O 7 are reported. This compound crystallizes in a triclinic unit cell P1 with the parameters a = 7.130(3), b = 9.047(3), c = 9.350(2) Å, α = 133.44(2)°, β = 95.02(2)°, γ = 107.11(4)°, Z = 2, V = 514.3(15) Å3, and D x = 1.848 g.cm− 3. The crystal structure has been solved and refined to R = 0.0273, using 3678 independent reflections. The atomic arrangement is build up by infinite ribbons of [H2 P 2 O 7] 2− anions, extending along the a-direction at y = 1/2. Between these ribbons are located the p-phenylenediammonium entities, which form hydrogen bonds N─H…O with some external oxygen atoms of phosphoric groups. Crystallographic results are correlated with that of the solid state 13C and 31P MAS NMR spectroscopy.

Structural and Physicochemical Studies of [2,3-(CH3)2C6H3NH3]4HP3O10.2H2O

Physicochemical properties of a new organic cation triphosphate, [2,3-(CH3)2C6H3 NH3]4HP3O10.2H2O, are discussed on the basis of X-ray crystal structure investigation. This compound crystallizes in a triclinic unit cell P1 with the parameters: a = 11.963(6) Å, b = 9.858(6) Å, c = 16.205(7) Å, α = 95.50(4)°, β = 95.21(4)°, γ = 89.07(4)°, V = 1894.4(16) Å3, Z = 2, and D x = 1.365 g.cm− 3. Crystal structure has been solved and refined to R = 0.074 using 3766 independent reflections. In this atomic arrangement, layers built by HP3O10 4 − groups are developed in (a, b) planes at z = 1/2. Between these layers the 2,3-dimethylphenylammonium entities are located, which form hydrogen bonds with some external atoms of the phosphoric groups. A characterization of this compound by solid-state 13C and 31P MAS NMR, IR spectroscopy and thermal analysis is also reported.

Synthesis and Characterization of a New Monophosphate (C6H6NCl2)(H2PO4) with an Interesting Chlorine-Mediated Framework

Chemical preparation, crystal structure, and NMR spectroscopy of a new monophosphate with 2,3-dichloroanilinium cation are given. This new compound crystallizes in the monoclinic system, with the space group P21/n and the following parameters: a = 11.031 (6), b = 6.007(3), c = 15.227(2) Å β = 98.98(4), V = 996.73(3) Å3, and Z = 4. The crystal structure has been determined and refined to R = 0.048 and Rw = 0.1317 using 2030 independent reflections. The structure can be described as clusters that aggregate with six organic molecules, resulting in a (1 0 ) two dimensional sheet, and formation of arrays in three dimensions, via various interactions (H-bonds, electrostatic, Van der Waals). In addition, C─Cl…π interactions are observed as a consequence of the chlorine atom being flanked by two phenyl rings of the neighboring molecules. The structure has also short intermolecular Cl…Cl interactions [type I, Cl…Cl = 3.380(1) Å, C─Cl…Cl′ = 132.26°]. This compound has also been investigated by IR, thermal analysis, and solid-state 13C and 31P MAS NMR spectroscopy combined with Ab Initio calculations.

Synthesis and Characterization of Two New Compounds: N(C2H4NH3)3(H2TO4)(HTO4)·2H2O (T = P, As)

The synthesis and structures of two new compounds with the general formula N(C2H4NH3)3(H2TO4)(HTO4)·2H2O (T = P, As) are reported. They crystallize with triclinic unit cells and are isotropic. We determined the structure of phosphate salt. The following unit cell parameters were found: a = 9.886(4), b = 9.308(2), c = 10.140(3) Å, α = 109.38(2), β = 108.83(3), γ = 74.40(3)°, V = 819.2(5) Å3, and ρcal. = 1.537 g · cm−3. The crystal structure was solved with a final R = 0.042 for 3748 with I > 3σ I). The space group is P-1 and Z = 2. The atomic arrangement can be described as a three-dimensional network of hydrogen bonds made up from HnPO4 3−n (n = 1, 2) anions and H 2 O molecules between which are trapped the tris(2-ammoniumethyl)amine cations. Solid-state 13C and 31P MAS-NMR spectroscopies are in agreement with X-ray structure. Ab initio calculations allow the attribution of the phosphorus signals to the independent crystallographic sites.