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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]

Abstract: Chemical preparation, crystal structure, calorimetric and spectroscopic investigations (IR and RMN) are given for a new non-centrosymmetric organic-cation dihydrogen phosphate–arsenate [H2(C4H10N2)][H2(As, P)O4]2. This compound is triclinic P1 with the following unit-cell parameters: a =7.082(2)Å, b =7.796(1)Å, c =12.05(3)Å, α =95.37(2)°, β =98.38(3)°, γ =62.98(1)°, Z =2, V =586.2(1)Å3 and D x =1.836gcm−3. The crystal structure has been solved and refined to R =0.03 using 2328 independent reflections. The structure can be described as infinite (H2XO) n chains spreading parallel to the b direction. These chains are themselves interconnected by a set of NO hydrogen bonds generated by the organic entities, alternating with the chains. Solid-state 13C, 15N and 31P MAS NMR spectroscopies are in agreement with the X-ray structure. [Copyright &y& Elsevier]

The aim of encapsulation of 2,3-dimethylanilinium cation in (H2XO4)n polymeric anion chains is to build acentric frameworks that are efficient for non-linear optical (NLO) applications. The synthesis and structures of two new inorganic–organic NLO crystals with general formula (2,3-(CH3)2C6H3NH3)H2XO4 (X=P, As) are reported. The magnitude of their second harmonic generations (SHG) responses was found to be between the KDP and urea. They crystallize with monoclinic unit-cells and are isotopic. We have determined the structure of phosphoric salt. The following unit-cell parameters were found: a=8.866(3) Å, b=5.909(6) Å, c=10.644(5) Å, β=112.44(1)°, V=515.5(5) Å3 and DX=1.412 g cm-3. The space group is P21 with Z=2. The structure was refined with R=0.041 (Rw=0.057) for 1652 reflections with I≥3σ(I). It exhibits infinite (H2PO4)nn- chains. The organic groups (2,3-(CH3)2C6H3NH3)+ are anchored between adjacent polyanions through multiple hydrogen bonds. Chemical preparation, crystal structure, calorimetric and spectroscopic investigation are described. [Copyright &y& Elsevier]

Chemical preparation and characterization by X-ray diffraction, IR, and NMR spectroscopies and thermal analysis of a new o-ethylphenylammonium triphosphate [2-C2H5C6H4NH3]3H2P3O10 are reported. This compound crystallizes in a monoclinic unit cell P21/n with the parameters: a=17.670(1)Å, b=8.558(8)Å, c=20.100(2) Å, β=100.39(6)°, Z=4, and V=2990(4) Å3. Crystal structure has been solved and refined to R=0.041 using 6857 independent reflections. In this atomic arrangement, layers built by H2P3O103- groups are developed along (1 0 -1) direction. Between these layers are located the o-ethylphenylammonium entities which form hydrogen bonds with some external oxygen atoms of phosphoric groups. [Copyright &y& Elsevier]

A new layered zinc-phosphate Zn(HPO4)Cl·[H3N(CH2)6NH3]0.5 was synthesized in acidic conditions at room temperature. It crystallizes in monoclinic space group C2/c (No. 15) with the lattice parameters a=21.826(3) A˚, b=9.452(7) A˚, c=8.780(1) A˚, β=109.36(8)°, V=1708.83(1) A˚3, Z=8, R=0.036, Rw=0.047. The structure of this compound is determined by X-ray diffraction and characterized with IR, TGA-DTA/DSC and NMR. The structure consists of inorganic layers, built by PO4 and ZnO3Cl tetrahedra interconnected by common oxygen atoms. The organic entities, located between these layers, perform the 3D cohesion through N&z.sbnd;H···O or N&z.sbnd;H···Cl hydrogen bonds. [Copyright &y& Elsevier]

Chemical preparation, crystal structure, calorimetric studies and spectroscopic investigation are given for a new organic cation dihydrogenomonophosphate [3,5-(CH3O)2C6H3NH3]2(H2PO4)2. This compound is triclinic P1 with the following unit cell parameters: a=9.030(6) A˚, b=16.124(5) A˚, c=8.868(3) A˚, α=75.04(3)°, β=110.71(4)°, γ=104.61(1)°, Z=4, V=1148.0(1) A˚3, Z=2 and ρcal.=1.454 g cm−3. Crystal structure was solved and refined to R=0.04, 2752 independent reflections. The atomic arrangement can be described as inorganic layers of H2PO4− anions parallel to y=SHAPE="SOL" ALIGN="C" STYLE="S">12 planes, between which are located the organic groups. Solid-state 13C and 31P MAS-NMR spectroscopies are in agreement with the X-ray structure. Ab initio calculations allow the attribution of the phosphorous and carbon signals to the independent crystallographic sites and to the various atoms of the organic groups. [Copyright &y& Elsevier]

Abstract: Chemical preparation, crystal structure and NMR spectroscopy of a new organic cation 5-chloro(2,4-dimethoxy)anilinium monophosphate H2PO4 are given. This new compound crystallizes in the monoclinic system, with the space group P21/c and the following parameters: a =5.524(2)Å, b =9.303(2)Å, c =23.388(2)Å, β =90.66(4), V =1201.8(2)Å3, Z =4 and D x =1.573gcm−3. Crystal structure has been determined and refined to R =0.031 and R w =0.080 using 1702 independent reflections. Structure can be described as an infinite (H2PO4) n n− corrugated chains in the a-direction. The organic groups (5-Cl-2,4-(OCH3)2C6H2NH3)+ are anchored between adjacent polyanions through multiple hydrogen bonds. This compound is also investigated by IR, thermal, and solid-state, 13C, 31P MAS NMR spectroscopies. [Copyright &y& Elsevier]

Abstract: A chlorozincophosphate of the composition Zn(HPO4)Cl·[C4H10NO] has been synthesised under mild condition water medium in the presence of morpholine as organic template. Its unit cell is monoclinic P2 1/a with parameters a =8.655(6)Å, b =9.302(5)Å, c =12.180(5)Å, β =101.10(4)°, Z =4 and V =962.1(9)Å3. The structure was determinated by single crystal X-ray diffraction. The structure involves a network of ZnO3Cl and PO3(OH) tetrahedra forming macroanionic inorganic layers with four- and eight-membered rings. Charge balance is achieved by the protonated amine which is trapped in the interlayers space and interacts with the organic framework through hydrogen bonding. Solid state 31P and 13C MAS-NMR spectroscopies are in agreement with the X-ray structure. [Copyright &y& Elsevier]

Chemical preparation, crystal structure, calorimetric, and spectroscopic investigations are given for a new organic-cation dihydrogenomonophosphate, (4-C2H5C6H4NH3)H2PO4 in the solid state. This compound crystallizes in the orthorhombic space group Pbca with the following unit cell parameters: a=8.286(3) A˚, b=9.660(2) A˚, c=24.876(4) A˚, Z=8, V=1991.2(7) A˚3, and DX=1.442 g cm−3. Crystal structure was solved with a final R=0.054 for 3305 independent reflections. The atomic arrangement coaled described as H2PO4− layers between which are located the 4-ethylanilinium cations. [Copyright &y& Elsevier]