Search

Physicochemical properties of a new dihydrogenmonophosphate [2-NH2-6-CH3-C4H3N2O]2(H2PO4)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 (H2PO4)nn - 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 H2PO4 groups to form (H2PO4)nn - 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 13C and 31P MAS NMR spectroscopies combined to ab initio calculations. [ABSTRACT FROM AUTHOR]

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 [C8H12N]H2PO4·H2O. 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) Å3, 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 H2PO4- anions, and H2O molecules with which the organic molecules perform different interactions to form a stable 3D network. Solid state 31P and 13C CP-MAS-NMR spectroscopies are in agreement with the X-ray structure. [ABSTRACT FROM AUTHOR]

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 [image omitted]) 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. [ABSTRACT FROM AUTHOR]

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. [ABSTRACT FROM AUTHOR]

Abstract: A new organic templated metallophosphate, [Zn(H2PO4)2(HPO4)][C7H17N2] (denoted in the following ZnP-AMEP), has been synthesized hydrothermally using 2-aminomethyl,1-ethylpyrrolidine (AMEP) as a structure-directing agent. The structure, determined by single crystal X-ray diffraction, exhibits a parallel arrangement (along the direction) of infinite chains, built from (Zn2P2O12) four-membered rings sharing ZnO4 tetrahedra, interconnected together by strong hydrogen bonds to form a sheet-like architecture and with chains of extending along [100] at y =1/2 to form a 3D anionic network. To the best of our knowledge, the compound ZnP-AMEP represents the first organic templated metallophosphate in which the four-membered rings interact with chains of dihydrogenophosphate. Intra-chain and inter-chain P–OH⋯O hydrogen bonds help to establish the crystal packing and form apertures, wherein the amine molecules are located. Similarities and differences with other organic templated metallophosphates are briefly discussed for the title compound. Ab initio calculations allow the attribution of phosphorus and carbon solid-state NMR signals to the independent crystallographic sites and to the various atoms of the organic groups. Additional characterizations of the compound have also been performed by IR spectroscopy and TG–DTA analyses. [Copyright &y& Elsevier]

Abstract: A new two-dimensional zinc phosphate, [Zn2.5(HPO4)2(PO4)][C6N2H10]·5H2O (denoted in the following as ZnP-2AMP), with alternating inorganic and organic layers has been synthesized hydrothermally using 2-aminomethylpyridine (2AMP) as the structure-directing agent. This compound represents the first structure with a Zn/P ratio of 5/6. The structure of this compound, determined by single crystal X-ray diffraction, consists of anionic parallel [Zn2.5(HPO4)2(PO4)(H2O)2]2− sheets built up from ZnO4, ZnO2(H2O)4, PO4 and HPO4, alternating with thick slabs of organic molecules (C6H10N2)2+ and water molecules, the octahedral ZnO2(H2O)4 being enclosed in each [4682122] cage. The organic cations are linked to the anionic sheets through hydrogen bonds. Solid-state 13C and 31P MAS NMR spectroscopies are in agreement with the X-ray structure. Ab initio calculations allow the partial attribution of phosphorus and carbon signals to the independent crystallographic sites and to the various atoms of the organic groups. Additional characterization of the compound has also been performed by IR spectroscopy and TG-DTA analyses. [Copyright &y& Elsevier]

Along a systematic study of open-framework materials aiming at producing new molecular sieves, we characterized a new zincophosphate Zn(HPO 4 )Cl[C 4 H 10 N]. It was synthesized under mild conditions (r.t.) in the presence of pyrrolidinium as an organic-structure directing agent. The structure of this compound, determinated by single crystal X-ray diffraction, consists of anionic parallel [Zn(HPO 4 )Cl] - sheets alternating with thick slabs of organic molecules (C 4 H 10 N) + . These latters are linked to the anionic sheets through hydrogen bonds. Zn(HPO 4 )Cl[C 4 H 10 N] crystallizes in the monoclinic system and the space group C2/c (No. 9) with cell parameters a = 24,83(9), b = 9,258(5), c = 8.778(3), β = 110,45(4), Z = 8, V = 1891.0(14) Åt 3 , R = 0.045, and R w = 0.07. Solid state 31 P and 13 C MAS NMR spectroscopies are in agreement with the X-ray structure. [ABSTRACT FROM AUTHOR]

Abstract: Chemical preparation, crystal structure and NMR spectroscopy of a new organic cation p-phenylenediammonium monophosphate [p-NH3C6H4NH3][H2PO4]2 are presented. This new compound crystallizes in the orthorhombic system, with the space group Pnma and the following parameters: a =7.970 (2)Å; b =22.770 (7)Å; c =7.000 (7)Å, V =1270.3 (11)Å3, Z =4 and D x =1.590gcm−3. The crystal structure has been determined and refined to R =0.043 and R (w) =0.057 using 2623 independent reflections. The structural arrangement can be described as inorganic layers of (H8P4O16)4− units, parallel to (a, c) planes. The organic groups (p-H3NC6H4NH3)2+are anchored between the phosphoric layers to form a three-dimensional infinite network. This compound is also investigated by IR and solid-state 1H, 13C and 31P MAS NMR spectroscopies. The ab initio method is used in the calculation of chemical shifts. [Copyright &y& Elsevier]

Crystal growth and characterization by X-ray diffraction and NMR spectroscopy of a new p-phenylenediamonium diphosphate [p-NH 3 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) Å 3 , 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 [H 2 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 13 C and 31 P MAS NMR spectroscopy. [ABSTRACT FROM AUTHOR]

A new adduct 4-benzyl piperidinium dihydrogenphosphate monophosphoric acid [C 12 H 16 NH 2 ] 2 (H 2 PO 4 ) 2 H 3 PO 4 , has been prepared and analyzed by X-ray diffraction. This adduct compound cristallizes in the monoclinic system, with the acentric space group P2 1 and the following unit-cell parameters: a = 13.103(3), b = 8.737(4), c = 13.620(3) Å, β = 92.38(2)°, Z = 2, and V = 1557.8(7) Å[3]. The crystal structure has been solved and refined to R = 0.059 and R (w) = 0.069 using 3306 independent reflections. Its structure can be described as inorganic layers of H 3 PO 4 and H 2 PO 4 - entities separated by organic molecules. In this atomic arrangement, H-bonds between the different species play an important role in the tridimensionnel network cohesion. Solid-state 13 C and 31 P MAS NMR spectroscopies are in agreement with the X-ray structure. Ab initio calculations allow the attribution of phosphorus and carbon signals to the independent crystallographic sites and to the various atoms of the organic groups. [ABSTRACT FROM AUTHOR]

A new zincophosphate [H3N(CH2)2NH3]0.5Zn (HPO4)Cl, was obtained at room temperature from a starting mixture of ZnCl2, H3PO4, H2O, and ethylene-diamine. Its unit cell is tricline P-1 (No. 2) with parameters a = 7.709(2) Å, b = 8.479(2) Å c = 5.175(2) Å, α = 104.99(3), β = 107.41(4), γ = 87.34(2), Z = 2, and V = 311.6(2) ų. Its structure is resolved to R = 0.024, Rw = 0.037. The backbone of the title compound is a linear heteroanion built by PO4 and ZnO3Cl tetrahedra assembled to farm four member rings themselves interconnected by sharing common oxygen atoms. Hydrogen bonds O--H…O established between these chains connect them as to build infinite planes. The organic entities, located between these planes form the 3D cohesion through N--H…O or N--H…Cl hydrogen bonds. [ABSTRACT FROM AUTHOR]

[C4N2H12]2HP3O10·H2O, 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)Å3, and a noncentrosymmetric space group P21(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 HP3O104-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. [ABSTRACT FROM AUTHOR]

Abstract: The synthesis and structure of a new adduct with the [2-NH2-6-CH3- C4H3N2O]2HPO4 formula is described. This compound crystallizes in the triclinic space group . The unit cell parameters are: a =7.679(1)Å, b =9.883(2)Å, c =10.217(3)Å, α =83.36(2)°, β =79.48(5)°, γ =80.34(4)°, V =748.7(1)Å3, and Z =2. The crystal structure was solved and refined to R =0.037, using 2241 independent reflections. The atomic arrangement of this compound is built up by (H4P2O8)2− dimers. Each dimer aggregates with organic molecules to form an open framework architecture like through hydrogen bond interactions. Solid-state 13C and 31P MAS NMR spectroscopies are in agreement with the X-ray structure. [Copyright &y& Elsevier]