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An investigation of the solid-state X-ray structure of the new organic–inorganic compound [C5H14N2]2PbCl6·3H2O shows a layered organization of the (PbCl6)4– anions, with (R2NH2)+ groups and water molecules developed in the [001] plane at x = (2n + 1)/4. The crystal structure is stabilized by N − H···Cl, N − H···O, O − H···Cl, O − H···O, and C − H···Cl hydrogen bonds. The powder X-ray diffraction and X-ray photoelectron spectroscopic (XPS) analyses confirm the phase purity of the crystal sample. The intermolecular contacts are quantified using the Hirshfeld surfaces computational method. The major inter-contacts contributing to the Hirshfeld surfaces are H...Cl, H...H, and O...H. The vibrational modes were identified and assigned by IR and Raman spectroscopies. The optical properties were investigated by UV–visible and photoluminescence spectroscopic studies. The compound was characterized by thermal analysis to determine its thermal behavior with respect to the temperature. Finally, X-ray photoelectron spectroscopy analysis is reported for analyzing the surface chemistry of [C5H14N2]2PbCl6·3H2O. [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 organic cation triphosphate, [2,3-(CH3)2C6H3 NH3]4HP3O10.2H2O, are discussed on the basis of X-ray crystal structure investigation. This compound crystallizes in a triclinic unit cell P1 with the parameters: a = 11.963(6) Å, b = 9.858(6) Å, c = 16.205(7) Å, α = 95.50(4)°, β = 95.21(4)°, γ = 89.07(4)°, V = 1894.4(16) Å3, Z = 2, and Dx = 1.365 g.cm- 3. Crystal structure has been solved and refined to R = 0.074 using 3766 independent reflections. In this atomic arrangement, layers built by HP3O104 - groups are developed in (a, b) planes at z = 1/2. Between these layers the 2,3-dimethylphenylammonium entities are located, which form hydrogen bonds with some external atoms of the phosphoric groups. A characterization of this compound by solid-state 13C and 31P MAS NMR, IR spectroscopy and thermal analysis is also reported. [ABSTRACT FROM AUTHOR]

Among the various categories of phosphates, the number of organic cation cyclotriphosphates remains limited. In this work, we report the chemical preparation, crystal structure, thermal analysis, and spectroscopic investigations of a new cyclotriphosphate [C8H11NH3]3P3O9·3H2O. It is characterized by X-ray diffraction, infrared spectroscopy, nuclear magnetic resonance, and thermal analysis. This compound is a triclinic P unit cell with the following parameters: a = 13.949(4), b = 9.867(3), c = 14.180(2) Å, α = 92.22(2), β = 119.27(2), γ = 85.10(10)°, V = 1696.1(8) Å3, and Z = 2. Its structure has been determined and refined to R = 0.041 and Rw = 0.062, using 4527 independent reflections. The atomic arrangement can be described by corrugated thick layers built by [P3O9]3- anions, ammonium groups, and water molecules. The organic entities are located between these layers. H-bonds connecting the different species play an important role in the tridimensionnal network cohesion. This compound is also characterized by infrared spectroscopy, nuclear magnetic resonance, and thermal analysis. [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]

The synthesis and structures of two new compounds with the general formula N(C 2 H 4 NH 3 ) 3 (H 2 TO 4 )(HTO 4 )·2H 2 O (T = P, As) are reported. They crystallize with triclinic unit cells and are isotropic. We determined the structure of phosphate salt. The following unit cell parameters were found: a = 9.886(4), b = 9.308(2), c = 10.140(3) Å, a = 109.38(2), ß = 108.83(3), ? = 74.40(3)°, V = 819.2(5) Å 3 , and ? cal. = 1.537 g · cm -3 . The crystal structure was solved with a final R = 0.042 for 3748 with I > 3s I). The space group is P-1 and Z = 2. The atomic arrangement can be described as a three-dimensional network of hydrogen bonds made up from H n PO 4 3- n (n = 1, 2) anions and H 2 O molecules between which are trapped the tris(2-ammoniumethyl)amine cations. Solid-state 13 C and 31 P MAS-NMR spectroscopies are in agreement with X-ray structure. Ab initio calculations allow the attribution of the phosphorus signals to the independent crystallographic sites. [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]

A series of novel quinoxaline based bisspirooxindolo-pyrrolizidines were synthesized through 1,3-dipolar cycloaddition under ultrasonication with shorter reaction time and good yields. The compounds were well characterized by various spectroscopic methods and finally single crystal X-ray diffraction method (4c, 4d). DFT energy calculations confirm the regioselectivity due to enone umpolung effect. The in vitro anti-cancer activity of the synthesized compounds (4a–s) shows that the compounds 4g and 4q exhibited good anti-cancer activity with IC50 values14.51 ± 1.1 and 11.36 ± 0.23 µM against DU-145 prostate cancer cell line; and 16.78 ± 0.95 and 14.28 ± 0.64 µM against Hela cervical cancer cell lines when compared to the standard anti-cancer drug doxorubicin (1.75 ± 0.06 and 1.35 ± 0.09 µM). In silico molecular docking studies indicated that the synthesized compounds may serve as a potential lead for the further development of novel anti-cancer agents. [ABSTRACT FROM AUTHOR]

The synthesis and crystal structure of a new noncentosymmetric compound with the general formula: [C48H51N8O8S4](HPO4)H2PO4 are reported. The structure, determined by single-crystal X-ray diffraction at 150 K can be described as organic layers [C48H51N8O8S4]3+ parallel to the (a and c) plane between which the inorganic groups consisting of H2PO4 − and HPO4 2− entities are inserted as inorganic layers. In this atomic arrangement, H-bonds and Vander-Waals interactions between the different species play an important role in the tridimensional network cohesion. Solid-state 13C and 31P MAS NMR spectroscopies are in agreement with the X-ray structure. 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 PUBLISHER]

Single crystals of 4-methylbenzylammonium sulfate were grown in an aqueous solution at room temperature. The grown compound is characterized by spectroscopic, thermal, and dielectric studies and its structure was determined by single-crystal X-ray diffraction analysis. Its crystal structure is described as a three-dimensional network where the sulfate anions (HSO4−) are interconnected through H-bonds to form anionic layers between which the 4-methylbenzylammonium cations are located. The hydrogen bonding network connecting the different components is given. Hirshfeld surface analysis was performed to visualize, explore and quantify intermolecular interactions in the crystal lattice. This analysis revealed the presence of H…C/H…C, C…O/O…C intermolecular interactions and O…O, H…H short contacts in the crystal. X-ray, structural and electrical results are correlated. The kind of the observed conduction is protonic by translocation. Differential scanning calorimetry (DSC) shows that this material presents a reversible phase transition at 390 K, confirmed by the dielectric permittivity study. [ABSTRACT FROM AUTHOR]

By employing 2-(4-methoxyphenyl)-1H-imidazole-4,5-dicarboxylic acid (p-MOPhH3IDC) to react with Cd(II), Zn(II) and Sr(II) ions, four polymers, [Cd(p-MOPhHIDC)(2,2′-bipy)]n(2,2′-bipy = 2,2′-bipyridine) (1), [Zn0.5(p-MOPhH2IDC)·H2O]n(2), {[Cd4(p-MOPhHIDC)4(C2H5OH)2(H2O)2]·4C2H5OH·2H2O}n(3) and {[Sr2(H2MOPhIDC)2(C8H4O4)(H2O)6]·6H2O}n(4) have been solvothermally synthesised and structurally characterised by single-crystal X-ray diffraction. Polymer1is a chain with 2,2′-bipy appending in the same side. Polymer2is a 2D rhombus grid structure. The π⋯π interactions between the aromatic groups supply the additional stabilisation for the solid-state structures of1and2. Polymer3shows a 3D framework bearing 1D open channels. Polymer4exhibits a 2D latticed plane. The thermal and photoluminescence properties of1–4have been investigated as well. Four polymers constructed by substituted imidazole dicarboxylates have been afforded and structurally characterized by single-crystal X-ray diffraction. Their thermal properties have been investigated. [ABSTRACT FROM AUTHOR]

A new adduct bis-(2-amino-3-benzyloxypyridinium) selenate monohydrate, [C12H13N2O]2SeO4.H2O, has been synthesized by slow evaporation at room temperature using 2-amino-3-benzyloxypyridine as the structure-directing agent. The structure, determined by single-crystal X-ray diffraction at 298 K, can be described as organic-inorganic tunnels with different forms built by infinite inorganic chains parallel to the c axis and connected to the organic cations. In this atomic arrangement, hydrogen bonds and van der Waals interactions between the different species play an important role in the tri-dimensional network cohesion. Solid-state13C and77Se MAS NMR spectroscopy results are in agreement with the X-ray structure. [Supplementary materials are available for this article. Go to the publisher's online edition ofPhosphorus, Sulfer, and Silicon and the Related Elementsfor the following free supplemental files:Additional figures and tables.] [ABSTRACT FROM AUTHOR]

A novel cadmium cyclohexaphosphate (C5H14N2)2Cd2Cl2P6O18.4H2O has been prepared and characterized by single-crystal X-ray diffraction, infrared and Raman spectroscopies, thermogravimetric analysis, and cyclic voltammetry. The structure consists of vertex linked of CdO5Cl octahedral and P6O18rings assembled into a two-dimensional macroanionic layers. Organic double-protonated homopiperazine cations are located between these layers and interact with the framework both electrostatically and via hydrogen bonds of N–H···O(Cl). [Supplemental materials are available for this article. Go to the publisher's onlineedition ofPhosphorus, Sulfur, and Silicon and the Related Elementsto view the following free supplemental files: Additional figures] [ABSTRACT FROM PUBLISHER]

An orthophosphoric hybrid material was successfully prepared by a hydrothermal reaction at 110 °C. A single crystal X-ray structure, thermal behavior, IR, and NMR spectroscopy investigations are given for a new organic cation bis dihydrogenomonophosphate C7H12N2[H2PO4]2.1/2H2O. The latter has been synthesized hydrothermally using 2,4-diaminotoluene (DAT) and orthophosphoric acid. The atomic arrangement can be described as inorganic sheets alternating with inorganic-organic layers. The organic group C7H12N+ 2 is located between inorganic groups to build multiple hydrogen bonds to ensure the three-dimensional cohesion network. The thermal behavior and IR, NMR and impedance spectroscopy studies are discussed for the powder samples of this compound. 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]

A new adduct 3-ammoniumphenyl sulfone dihydrogenphosphate phosphoric acid, [C12H14N2O2S](H2PO4)2H3PO4, has been synthesized by slow evaporation at room temperature using 3-aminophenyl sulfone as the structure-directing agent. The structure, determined by single-crystal X-ray diffraction at 293 K, can be described as inorganic layers built by H2PO4 − groups and H3PO4 molecules, parallel to the (a, c) planes at y = 0.5, between which molecules of the organic group [C12H14N2O2S]2+ are inserted. In this atomic arrangement, hydrogen bonds and van der Waals interactions between the different species play an important role in the tri-dimensional network cohesion. Solid-state 13C and 31P MAS NMR spectroscopies are in agreement with the X-ray structure. [Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements for the following free supplemental resource: Tables S1 and S2. Figures S1 and S2.] GRAPHICAL ABSTRACT [ABSTRACT FROM AUTHOR]