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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: 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]

The present paper undertakes the study of [C 6 H 16 N 2 O]SbCl 5 which is a new hybrid compound. It is synthesized and characterized by single-crystal X-ray diffraction, thermal analysis, IR and solid state NMR spectroscopies. The centrosymmetric compound crystallizes in the monoclinic space group P2 1 /n, with the following unit cell parameters: a = 9.8519(2), b = 8.8345(2), c = 17.3087(4) Å, β = 102.3(1)° and Z = 4. The atomic arrangement shows an alternation of organic and inorganic entities. The cohesion between these entities is performed via N–H⋯Cl and O–H⋯Cl hydrogen bonding to form a three-dimensional network. The 13 C CP-MAS NMR spectrum is in agreement with the X-ray structure. Infrared and Raman spectra at room temperature are recorded in the 4000–400 and 500–100 cm −1 frequency regions respectively. This study confirms the presence of the organic cation [C 6 H 16 N 2 ] 2+ and of the [SbCl 5 ] 2− anion. DFT calculations allow the attribution of the carbon peaks to the different atoms. [ABSTRACT FROM AUTHOR]

The inorganic–organic hybrid compound (C 9 N 4 H 28 )Cd 7 (H 2 O) 2 Cl 18 · n H 2 O( n = 5.89) features an unusual cadmium chloride structure. The title complex adopts a layered structure consisting of double-chains and tetramers of [Cd ϕ 6 ] ( ϕ = Cl, O) octahedra. Crystallization water molecules and [C 9 H 28 N 4 ] 4+ tetracations are located in interstices of the successive corrugated layers. This compound has also been investigated by FT-IR and solid-state 13 C, 15 N CP-MAS and 2D 13 C-H NMR spectroscopies. [ABSTRACT FROM AUTHOR]

A new Cd(II) complex with the monodentate ligand 3-fluoroaniline, CdCl 2 (C 6 H 4 FNH 2 ) 2 , has been prepared and characterized by single crystal X-ray diffraction, solid state NMR, IR, Raman and UV–visible spectroscopies. In the complex, the Cd(II) ion is surrounded by four chlorine atoms and two nitrogen atoms, forming a chain of edge-charing octahedra spreading along the a -axis direction. These chains are interconnected via N H…Cl hydrogen bonds to form inorganic layers parallel to the (a, b) plane. The organic 3-fluorophenyl groups are inserted between these layers and are interconnected via C H…F hydrogen bonds to perform an infinite three-dimensional network. Intermolecular π–π stacking interactions between neighboring aromatic rings are also observed with a face-to-face distance of 3.6816 (4) Å. The 13 C and 19 F CP-MAS NMR spectra are in agreement with the X-ray structure. DFT calculations allow the attribution of the carbon peaks to the different atoms. The absorption bands of the Cd 2 Cl 4 N 2 units were identified by Raman spectroscopy. The solid-state UV–vis spectrum of the complex has been assigned to ligand and charge transfer transitions. [ABSTRACT FROM AUTHOR]

Abstract: Three binuclear Cu(II) and Ni(II) perchlorate complexes with the potentially bidentate ligand 2-amino-6-methylpyrimidin-4(1H)-one (AMPO) [Cu(AMPO)4][Cu(H2O)5](ClO4)4·6H2O (1), [Cu2(AMPO)4(H2O)3](ClO4)4·½H2O (2) and[Ni(AMPO)4][Ni(H2O)6](ClO4)4·5H2O (3), have been prepared and were characterized by single crystal X-ray diffraction, IR spectroscopy and elemental analysis. Structural and IR data indicate that the ligand is present in its tautomeric form protonated at nitrogen in position one and metal coordinated at position three. The basic coordination pattern of the AMPO coordinated metal cations in all three complexes is square planar by four pyrimidyl nitrogen atoms of four different AMPO ligands. The coordination sphere is augmented by weak M⋯O interactions between the metal centers and AMPO keto oxygen atoms. Bond valence calculations indicate the M⋯O interactions to be most pronounced for nickel compound (3), and least for copper complex (2). The structural and geometrical differences between compounds (1) and (3) on the one hand and compound (2) on the other can to a large part be traced back to the lack of available water in the crystallization solvent in (2) which starves the cation not coordinated to AMPO nitrogen atoms of water molecules to saturate its coordination sphere, thus forcing two of the AMPO ligands in (2) to act as a bridging ligands, while the other AMPO ligands in the three structures are mostly monodentate with the coordination mode of the AMPO ligand being completed by weak secondary chelating M⋯O interactions. [Copyright &y& Elsevier]