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The crystal structure of the new inorganic-organic hybrid compound [4-CH3C6H4CH2NH3]3[CdCl4] has been determined by single crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group Pnma with lattice parameters a = 10.721(2), b = 33.986(6), c = 5.326(1) Å, β= 97.222(1)°, V = 1940.8(7) Å3, and Z = 4. The framework of the title compound is built upon layers parallel to (010) made up from corner-sharing CdCl6 octahedra. 4-Methylbenzylammonium cations are situated between the layers and connect them via an N-H… Cl hydrogen bonding network. The Cd atom is located on an inversion centre, and the coordination environment is described as distorted octahedral. Solid state 13C CP-MAS NMR spectroscopy is in agreement with the X-ray structure. DFT calculations allow the attribution of the carbon peaks to the independent crystallographic sites. Thermal analysis and infrared spectroscopy were also used to characterize the complex [ABSTRACT FROM AUTHOR]

The physicochemical properties of a new organic cyclohexaphosphate, [5-Cl-2,4-(OCH3)2C6H2-NH3]6P6O18·4H2O, are discussed on the basis of an X-ray crystal structure investigation. This compound crystallizes in the monoclinic space group C2/c, with cell parameters a = 37.987(7) Å, b = 13.125(4) Å, c = 14.331(5) Å, β = 98.21(3)°, Z = 4, V = 7072(3) Å3. Its crystal structure is determined and refined to a final R = 0.058 for 5223 independent reflections. The atomic arrangement can be described as a layer organization built up by P6O18 ring anions and water molecules. Between these layers, the organic groups are located that form hydrogen bonds with oxygen atoms of P6O18 rings and water molecules. Intermolecular π-π stacking interactions between two neighboring organic cation rings help to establish the crystal packing. Solid 31P MAS-NMR spectroscopy is in agreement with X-ray structure. Ab initio calculations allow the attribution of the three phosphorus signals to the independent crystallographic sites. This compound is also characterized by thermal analysis and IR spectroscopy. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. [ABSTRACT FROM AUTHOR]

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, 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]

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)Å 3 , 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 (H 2 PO 4 - ) 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 31 P, 13 C, and 15 N 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. [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]

(C 6 H 7 FN) 4 (Li) 2 (P 6 O 18 ) (H 2 O) 6 (I) , a new organic cyclohexaphosphate, has been synthesized and grown at room temperature by an acid/base reaction between H 6 P 6 O 18 and 2-fluoroaniline as an organic template. The crystal structure of (I) was solved by single crystal X-ray diffraction analysis and it was found that the material belongs to triclinic system with space group P-1 and refined R -factor of 0.0520. Adjacent P 6 O 18 rings are connected via corner-sharing by LiO 4 tetrahedra, generating anionic [Li 2 P 6 O 18 ·H 2 O] 4- layers parallel to the ( a , b ) plane. The 2-fluoro-anilinium cations are inserted in the interlayer space and interact with the inorganic framework through N H⋯O and O H⋯O hydrogen-bonding interactions. Additional stabilization is provided by strong N H⋯F and weak C H⋯O hydrogen bonds. Hirshfeld surface analysis reveals the nature of intermolecular contacts of the title compound and their enrichment ratio reveals if they are over-represented. The crystal packing is a combination of strong electrostatic attractive interactions and of weaker hydrophobic contacts. The title compound was further characterized by FT-IR and NMR spectroscopies. Crystal symmetry is confirmed by 31 P magic angle spinning NMR and the vibrational absorption bands were identified by infrared spectroscopy. Electrical conductivity was studied using impedance spectroscopy and results showed that the conductivity at 150 °C was equal to 4.93 × 10 −4  S cm −1 . It is therefore concluded that (C 6 H 7 FN) 4 (Li) 2 (P 6 O 18 ) (H 2 O) 6 can be further used in lithium batteries. [ABSTRACT FROM AUTHOR]

The synthesis and the X-ray structure of the Zn(II) zwitterionic complex:1-ethylpiperaziniumtrichlorozincate (II) are described. In the atomic arrangement, the ZnCl 3 N entities, grouped in pairs, are deployed along the b -axis to form layers. The organic entities are inserted between these layers through N H⋯Cl and C H⋯Cl hydrogen bonds to form infinite three-dimensional network. The 3D Hirshfeld surfaces were investigated for intermolecular interactions. The optimized geometry, Mulliken charge distribution, molecular electrostatic potential (MEP) maps and thermodynamic properties have been calculated using the Lee-Yang-Parr correlation functional B3LYP with the LanL2DZ basis set. The HOMO and LUMO energy gap and chemical reactivity parameters were made. The 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray crystal structure. The vibrational absorption bands were identified by infrared spectroscopy. DFT calculations allowed the attribution of the NMR peaks and of the IR bands. [ABSTRACT FROM AUTHOR]

The synthesis, crystal structure and spectroscopic characterization of a new chlorocadmate template by the 1-(2-hydroxyethyl)piperazine ligand are reported. In the atomic arrangement, the CdCl 5 O entities are deployed in corrugated rows along the a -axis at y = 1/4 and y = 3/4 to form layers parallel to the ( a,b ) plane. In these crystals, piperazinediium cations are in a chair conformation and are inserted between these layers through N H⋯Cl, C H⋯Cl, O H⋯Cl and N H⋯O hydrogen bonds to form infinite three-dimensional network. Investigation of intermolecular interactions and crystal packing via Hirshfeld surface analysis reveals that H⋯Cl and C H⋯H C intermolecular interactions are the most abundant contacts of the organic cation in the crystal packing. The crystal contacts enrichments reveals that, the Cd ++ … Cl − salt bridges, the Cd⋯O complexation and O H⋯Cl- and N H⋯Cl-strong H-bonds are the driving forces in the packing formation. The presence of twelve independent chloride anions and four organic cation in the asymmetric unit allowed comparing their contact propensities. The 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray structure. Additional characterization of this compound has also been performed by IR spectroscopy. [ABSTRACT FROM AUTHOR]

A novel organic–inorganic hybrid material, C 6 H 15 N 2 CdCl 3 .H 2 O, was synthesized, and its structure was determined at room temperature in the monoclinic space group P2 1 / n with the following parameters: a = 10.3829 (17), b = 7.7459 (12), c = 14.905 (2) Å, β = 98.801 (15), and Z = 4. Its crystal structure is characterized by one-dimensional polymeric chains of edge-sharing CdCl 5 N distorted octahedra. These chains are linked to the water molecules via O H … Cl hydrogen bonds to form layers parallel to the ( b , a + c ) plane. The crystal structure was stabilized by an extensive network of N H … Cl, O H … Cl and N H … O hydrogen bonds. The differential scanning calorimetry (DSC) reveals that the title compound is stable until 101.6 °C. The optimized geometry parameters, normal mode frequencies, and corresponding vibrational assignments of the present compound were theoretically examined by DFT/B3LYP method with the Lanl2dz basis set. The FT-IR spectrum of the polycrystalline sample was examined and compared to the calculated spectrum. The calculated results showed that the optimized geometry could well reproduce the crystal structure and that the theoretical vibrational frequency values were in good agreement with their experimental counterparts. [ABSTRACT FROM AUTHOR]

The chemical preparation, crystal structure, Hirshfeld surface analysis and spectroscopic characterization of the novel cadmium (II) 4-hydroxy-1-methylpiperidine complex, Cd 4 Cl 10 (C 6 H 14 NO) 2 ·2H 2 O, have been reported. The atomic arrangement can be described as built up by an anionic framework, formed by edge sharing CdCl 6 and CdCl 5 O octahedral linear chains spreading along the a -axis. These chains are interconnected by water molecules via O–H⋯Cl and O–H⋯O hydrogen bonds to form layers parallel to (011) plane. The organic cations are inserted between layers through C–H⋯Cl hydrogen bonds. Investigation of intermolecular interactions and crystal packing via Hirshfeld surface analysis reveals that the H C ⋯Cl and H C ⋯H C intermolecular interactions are the most abundant contacts of the organic cation in the crystal packing. The statistical analysis of crystal contacts reveals the driving forces in the packing formation. The 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray structure. The vibrational absorption bands were identified by infrared spectroscopy. DFT calculations allowed the attribution of the NMR peaks and of the IR bands. [ABSTRACT FROM AUTHOR]