M.L. Mrad

Crystal Structure, Spectroscopic and Thermal Investigations of a New 4-Ammonio-2,2,6,6-tetramethylpiperidinium Tetrachlorozincate(II)

The new complex of Zn(II) with 4-ammino-2,2,6,6-tetramethylpiperidine, [C9H22N2]ZnCl4, has been prepared and characterized by various physicochemical studies. This compound crystallizes in the monoclinic system, with the space group P21/c and the following cell parameters: a = 9.8682(7), b = 7.5164(5), c = 21.019(2) A, β = 99.003 (7)°, V = 1539.8(2) A3 and Z = 4. The crystal structure was solved and refined to R = 0.024 using 3070 reflections. The atomic arrangement can be described by slightly distorted tetrahedral ZnCl42- anions and 4-ammmonio-2,2,6,6-tetramethylpiperidinium cations holding together by different interactions. The four chlorine atoms of the ZnCl42- tetrahedron are acting as acceptors of hydrogen bonds. The crystal packing is influenced by cation-to-anion N-H…Cl and C-H…Cl hydrogen bonds leading to open framework architecture.

4-Ammonio-2,2,6,6-tetra­methyl­piperidinium bis­(dihydrogen phosphate) monohydrate

In the crystal structure of the title compound, C9H22N2 2+·2H2PO4 −·H2O, the H2PO4 − anions are hydrogen bonded to each other, forming a ribbon parallel to the b axis. The water molecules connect these ribbons via O—H⋯O hydrogen bonds. The organic cations are attached to the dihydrogen phosphate anions and water molecules through N—H⋯O and C—H⋯O hydrogen bonds, forming an infinite three-dimensional network.

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.

Physico-Chemical Studies of Tris (adamantan-1-aminium) Hexachlorostannate (IV) Chloride Monohydrate

The structural characteristics of organic ammonium salts of the hexahalogenostannates (IV) with a general formula (R-NH 3)3SnX 6 have not yet been studied extensively. In the course of investigating these types of materials, the title compound, a double salt of adamantan-1aminium chloride and hexahalogenostannate (IV), with the formula (C 10 H18 N) 3[SnCl 6]Cl·H 2O, was crystallized. Its asymmetric unit contains three independent cations of protonated adamantan-1-amine, one chloride anion, one Hexachlorostannate (IV) ion and a hydrate water molecule. The atomic arrangement can be described as inorganic SnCl 6 2- units isolated from each other by the organic cations, the chloride anions and the cocrystallized water molecules. The compound exhibits bifurcated and simple hydrogenbonding interactions between the ammonium groups, the water molecules and the chlorine atoms, with little variation in the hydrogen-bonding interactions. The 119 Sn, 13 C and 15 N CPMAS NMR spectra are in agreement with the X-ray structure.

Bis(adamantan-1-aminium) hydrogen phosphate fumaric acid sesquisolvate

The asymmetric unit of the title compound, 2C10H18N+·HPO4 2−·1.5C4H4O4, contains two adamantan-1-aminium cations, one hydrogen phosphate anion, and one and a half molecules of fumaric acid, one of which exhibits crystallographic inversion symmetry. Each HPO4 2− anion is hydrogen bonded, via all of its O atoms, to four NH3 + groups of the adamantan-1-aminium cations, forming chains along [100]. These chains are, in turn, interconnected via a set of O—H⋯O hydrogen bonds involving the fumaric acid solvent molecules, forming layers parallel to (001). Weak C—H⋯O interactions lead to a consolidation of the three-dimensional set-up.

4-Acetamido-anilinium nitrate monohydrate.

In the title hydrated salt, C8H11N2O+·NO3 −·H2O, the N—C bond distances [1.349 (2) and 1.413 (2) Å] along with the sum of the angles (359.88°) around the acetamide N atom clearly indicate that the heteroatom has an sp 2 character. The ammonium group is involved in a total of three N—H⋯O hydrogen bonds, two of these are with a water molecule, which forms two O—H⋯O hydrogen bonds. All these hydrogen bonds link the ionic units and the water molecule into infinite planar layers parallel to (100). The remaining two N—H⋯O interactions in which the ammoniun group is involved link these layers into an infinite three-dimensional network.

Tris(5-amino-1H-1,2,4-triazol-4-ium) dihydrogenphosphate hydrogen­phosphate trihydrate

In the crystal structure of the title molecular salt, 3C2H5N4 +·HPO4 2−·H2PO4 −·3H2O, the phosphate-based framework is built upon layers parallel to (010) made up from the H2PO4 − and HPO4 2− anions and water molecules, which are interconnected through O—H⋯O hydrogen bonds. The organic cations are located between the phosphate–water layers and are connected to them via N—H⋯O hydrogen bonds. The bond-length features are consistent with an imino resonance form for the exocyclic amino group, as is commonly found for a C—N single bond involving sp 2-hybridized C and N atoms.

2-Chloro­benzene-1,4-diaminium bis­(dihydrogenphosphate)

The asymmetric unit of the title salt, C6H9ClN2 2+·2H2PO4 −, contains two dihydrogenphosphate anions and one 2-chlorobenzene-1,4-diaminium dication. The H2PO4 − anions are interconnected through strong O—H⋯O hydrogen bonds to form two-dimensional infinite layers parallel to (001). The organic entities are anchored to the inorganic layers through N—H⋯O hydrogen bonds, and through weak C—Cl⋯O halogen bonds [3.159 (2) Å, 140.48 (7)°]. No π–π stacking interactions between neighboring aromatic rings or C—H⋯π interactions towards them are observed. Minor disorder is observed for the Cl atom and one hydroxy group [minor-component occupancy = 3.29 (9)%].

1-(2-Ammonio-eth-yl)piperazin-1,4-diium dihydrogeno-phosphate monohydrogeno-phosphate.

The structure of the title compound, C6H18N3·HPO4·H2PO4, is characterized by two kinds of inorganic chains running along the a-axis direction. The first one is composed of HPO4 2− anions, while the second one is built up by H2PO4 − anions. Both types of chains are held together by O—H⋯O hydrogen bonds. The organic cations are attached to these chains through N—H⋯O and C—H⋯O hydrogen bonds. The piperazin-1,4-diium ring adopts a chair conformation.

Crystalline and Molecular Structure of Hexaaqua-1,3-diammoniumpropane Cobalt(II) Nitrate, Co(H2O) 6 [C3H12N2] (NO3)4

Chemical preparation and x-ray characterization of a new compound hexaaqua-1,3-diammoniumpropane cobalt(II) nitrate, Co(H2O) 6 [C3H12N2] (NO3)4 are reported. This mixed organo-mineral compound crystallizes in the orthorhombic system with Cmcm space group. The unit cell dimensions are: a = 10.795(7), b = 11.969(4), c = 14.685(5) A, Z = 4 and V = 1897.5(12) A3. The structure was solved using the direct method and refined to reliability R-factor of 0.036 using 2554 independent reflections. In this atomic arrangement the different species built a three-dimensional network.