A. Oueslati

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.

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.

Crystal structure of 5-chloro-2-methylanilinium chloride hydrate, (ClC7H6NH3)Cl . H2O

H(l) 2a 0.0412 0.4851 0.1320 0.059 H(2) 2a 0.1675 0.3395 0.1240 0.059 H(3) 2a 0.2294 0.5261 0.1345 0.059 H(7) 2a 0.5339 0.3477 0.6358 0.057 H(8) 2a 0.3123 0.3899 0.7725 0.059 H(9) 2a -0.0504 0.4937 0.3624 0.048 H(4) 2a 0.4851 0.2833 0.2425 0.074 H(5) 2a 0.6324 0.3128 0.4009 0.074 H(6) 2a 0.5596 0.4780 0.2912 0.074 H(10) 2a -0.4659 0.1646 0.9596 0.098 H(ll) 2a -0.3295 0.2956 0.9651 0.098

Crystal structure of o-cyanoaniline hydrochloride, (NCC6H4NH3)Cl

C7H7CIN2, monoclinic, Clcl (no. 9), a = 5.658(5) A , b = 15.406(9) A, c = 8.234(8) k,ß = 93.18(9)°, V= 716.6 A, Ζ = 4, R f f f F ) = 0.020, wRxetfF) = 0.052, T= 293 K. Source of material Crystals of o-cyanoaniline hydrochloride (synonym 2-cyanoanilinium chloride) were prepared by dissolving of 5 mmol of purified 2-cyanoaniline in 10 mL of an ethanol-water solution Table 2. Atomic coordinates and displacement parameters (in Ä). * Correspondence author (e-mail: cherif.bennasr@fsb.rnu.tn) Atom Site X y ζ i/iso H(l) 4a -0.257(4) -0.204(1) -0.761(2) 0.029(5) H(2) 4a -0.384(4) -0.218(1) -0.916(3) 0.040(5) H(3) 4a -0.505(4) -0.200(1) -0.774(3) 0.038(5) H(7) 4a -0.006(4) 0.044(1) -1.026(2) 0.042(5) H(6) 4a -0.276(4) 0.141(2) -0.907(3) 0.049(6) H(5) 4a -0.599(4) 0.096(1) -0.773(2) 0.037(5) H(4) 4a -0.630(4) -0.058(1) -0.732(3) 0.039(5)