Synthesis, Crystal structure of hepta (pyridinium) bis (hexachlorobismuthate (III)) nitrate [C5H6N]7(BiCl6)2(NO3)

An hepta (pyridinium) bis (hexachlorobismuthate (III)) nitrate, (C5H6N)7(BiCl6)2(NO3) crystallizes at room temperature in the monoclinic system, space group P21/n, with the following unit-cell parameters: a = 9.555(1) Å, b = 16.847(1) Å, c = 32.522(1) Å, β = 94.37° , V = 5219.8 Å3 and four molecules per unit cell. Its crystal structure was determined and refined down to R1 = 0.0504, wR2 = 0.0667. The structure of the title compound, (C5H6N)7(BiCl6)2(NO3) consists of seven monoprotonated pyridinium (C5H6N)+ cations, two independent octahedron [BiCl6]3- and an isolated NO3- anion. These entities are linked together through N-H.....Cl and N-H.....O hydrogen bonds, originating from the (C5H6N)+ groups and the isolated anion of nitrate to forming a three dimensional network

Synthesis, Crystal Structure and Vibrational Properties of bis (N-benzylmethylammonium) Pentachlorobismuthate (III)

The [C8H12N]2 BiCl5 compound crystallised in the triclinic system with space group  P-1  with a = 9,833(4),                     b = 10,044(7), c = 12,225(7) Ã…, a= 78.82(4), β = 75,42(4), g= 76.89°(5)  and Z = 2. The average density value, Ïx = 1.518 g.cm-3  is in agreement with the calculated one, Ïx = 1.494 g.cm-3. The atomic arrangement can be described as an alternation of organic and inorganic layers. The anionic layer is built up of octahedral [Bi2Cl10]-4. The organic layers are arranged in sandwich between the anionic ones. The crystal packing is governed by means of the ionic N–H---Cl hydrogen bonds, forming a three dimensional network. The nature of the distortion of the inorganic polyhedra has been studied and can be attributed to the stereo activity of the Bi(III) lone electron pair. The infrared and Raman spectra was recorded in the 4000–400 cm-1 frequency region

Crystal structure and phase transition in the compound [C6H17N3]TlCl5.2H2O

The title compound 1-(2-ammonium-ethyl) piperaziniumpentachlorothallate (III) dihydrate crystallizes in the monoclinic system with space group Cm. The unit cell dimensions are: a = 12.786(5), b = 12.021(5), c = 10.566(5) Ã…, β = 93.469(5) °, with Z = 4. Its crystal structure was determined and refined down to R = 0.045. The structure of this compound consists of 1-(2-ammonium-éthyl) pipéraziniumcations and [Tl2Cl10]4- dimers. The arylammoniumcations are located between anions and connected to the halogen atoms by N-H…Cl hydrogen bonds. One phase transition at T = 320 K is detected and studied by differential scanning calorimetry, dielectric and impedance spectroscopy measurements. The evolution of the dielectric constant and dissipation factor as a function of temperature revealed the transition characterized by a strong jump in the conductivity plot.Â

catena-Poly[N,N,N′,N′-tetramethylethylendiammonium [[tetrabromidoantimonate(III)]-μ-bromido] hemihydrate]

The asymmetric unit of the title compound {(C6H18N2)2[Sb2Br10]·H2O}n, consists of two tetramethylethylendiammonium cations that are located on centres of inversion, as well as one tetramethylethylendiammonium cation, one water molecule, one distorted octahedral [SbBr6]3−anion and one bisphenoidal [SbBr4]− anion in general positions. The [SbBr6]3− and [SbBr4]− anions are linked together by two long Sb—Br bonds of 3.2709 (8) and 3.5447 (7) Å into {[Sb2Br10]4−}n chains along [001]. One of the three tetramethylethylendiammonium cations is disordered and was refined using a split model (occupancy ratio 0.58:0.42). The cations and the water molecule are connected to the {[Sb2Br10]4−}n polymeric anions by weak N—H ...Br and O(water)—H ...Br hydrogen bonding

Crystal structure and investigation of phase transitions in hexa (2 amino-indolinium) dodecachlorobithallate(III) and quinolinium tetrachlorothallate(III)

International audienceTwo new thallium containing salts with different aryl ammonium cations have been prepared and characterized by X-ray crystallography, infrared spectroscopy and dielectric measurements. The salt [C8N2H8](6)Tl2Cl12 (1) crystallizes in the monoclinic system with space group Pn. The unit cell dimensions are: a = 15.120(5), b = 11.825(5), c = 17.167(5) angstrom, beta = 104.460(5)degrees with Z = 2, D-calcd = 1.818 g cm(-3), R = 0.0369. The structure consists of 2 amino-indo-linium cations and monomeric TICl63- anions. The TICl63- has a strongly octahedral geometry presenting five short and one long (T11-C113 = 2.739(5) and T12-C126 = 2.684(5) angstrom) Tl-Cl bonds. The presence of multiple hydrogen bonds is considered to be responsible for the octahedral distortion. However, the second compound [C9H8N]TlCl4 (2) crystallizes in the Pna2(1) orthorhombic space group, with a = 9.253(1), b = 9.799(1), c = 14.558(2) angstrom, Z = 4, D-calcd = 2.397 g cm(-3), R = 0.0608. The structure of the quinolinium tetrachlorothallate(III) is characterized by tetracoordinate thallium, forming a regular tetrahedral TlCl4 with Tl-Cl distances between 2.366(2) and 2.451(3) angstrom. The structure consists of quinolinium cations separating chains of TlCl4- tetrahedra, these chains being perpendicular to the c axis. Infrared spectra confirm the presence of the organic cations. Differential scanning calorimetry study was carried out. Electrical measurements were performed to discuss the mechanism of the phase transition

Crystal structure and phase transition of the quinolinium tetrabromothallate(III)

International audienceThe salt quinolinium tetrabromothallate(III) is orthorhombic Pna2(1) with the following unit cell dimensions: a = 9.582(2), b = 10.0210(19), c = 14.916(2) angstrom, Z = 4. The structure was solved by Patterson methods and refined to a final R-value of 0.0452 for 2043 observed reflections. The examination of the structure shows quinolinium cations separating chains of tetrahedral TlBr4-, these chains are perpendicular to the c axis. Infrared spectra confirms the presence of the organic cations, differential scanning calorimetry reveals a transition at T = 406 K. Electrical measurements and X-ray powder diffraction were performed to discuss the mechanism of the phase transition

Synthesis and characterization of a new organic-inorganic hybrid material based on antimony

In the current research work, a new organic–inorganic hybrid compound of the formula [C3H5N2S] SbCl4 was successfully synthesized and characterized, where C3H5N2S stands for the cation of 2-aminothiazole. The synthesis was carried out by slow evaporation of raw materials and colourless good-quality crystals were obtained. The single crystal X-ray diffraction analysis of the crystals demonstrated a 0-dimension structure consisting of Sb2Cl8 dimers separated by 2-aminothiazolecations. The cohesion and stabilization between these entities is performed via N-H···Cl hydrogen bonds. The samples were characterized also by Powder X-ray Diffraction (PXRD) analysis. The functional groups in the complex were confirmed by Fourier transform IR (FT-IR) and Fourier transform Raman (FT-Raman) spectroscopies. Thermogravimetric analysis (TGA) was performed to examine the phase transition, degradation and thermal stability of the material. Optical absorption measurements revealed two absorption bands located at 263 and 234 nm (4.7 and 5.3 eV). The Nuclear Magnetic Resonance (NMR) spectrum goes in good consistency with the X-ray structure.We acknowledge the financial support from the Ministry of Higher Education, Scientific Research of Tunisia and Spanish Ministerio de Ciencia e Innovación (PID2020-113558RB-C41) and Red CrysFact (Red2018-102574-T (AEI/MCI)) are acknowledged.Peer reviewe

Structural characterization, Hirshfeld surface analysis, vibrational (FT-IR and Raman) and optical properties of the tris (4-Bromo-N, N-dimethylanilinium) hexachlorobismuthate (III)

A novel interesting hybrid organic-inorganic compound with the formula [C8H11BrN]3BiCl6. Tris(4-Bromo-N, N-dimethylanilinium) hexachlorobismuthate (III) was grown by the slow evaporation technique at ambient temperature. It is structurally characterized by vibrational spectroscopy, Hirshfeld surface analyses, Solid state 13C NMR, UV-Visible absorption and photoluminescence measurements. A preliminary single crystal X-ray diffraction study revealed that the title compound crystallizes in the non-centrosymmetric (space group P212121) with crystallographic parameters: a = 9.2820(3) Å,b = 13.7960(5) Å, c = 27.4298(12) Å, v = 3512.5(2) Å3 with Z = 4. The Crystal structure composed of discrete [BiCl6]3- anions surrounded by three [C8H11BrN]+cations, which are connected via N-H⋯Cl and C-H⋯Cl hydrogen bonds arranged in a three dimensional network. The Hirshfeld surface analysis associated with 2D fingerprint plots were used to visualize and explore the significant intermolecular interactions in the crystal structure quantitatively.13C Nuclear Magnetic Resonance (NMR) spectrum is in agreement with the X-ray structure. Furthermore, the optical absorption and photoluminescence measurements, exhibit a strong purple photoluminescence emission located at 2.92 eV and observed at room temperature.This work is support by the “Department of Chemistry, Faculty of Sciences of Sfax, University of Sfax, BP 1171, 3038 Sfax, Tunisia”, Spanish MINECO (MAT2016-78155-C2-1-R) and Gobierno del Principado de Asturias (GRUPIN-ID2018-170)

alpha- to beta-[C6H4(NH3)(2)](2)Bi2I10 reversible solid-state transition, thermochromic and optical studies in the p-phenylenediamine-based iodobismuthate(III) material

International audiencealpha-[C6H4(NH3)(2)](2)Bi2I10, which is a new material containing low-dimensional iodobismuthate anions, was synthesized and through its single crystal X-ray diffraction measurements, was proven to crystallize at room temperature in the centrosymmetric space group P2(1)/c. It consists of a p-phenylenediammonium dication and a discrete (0-D) anion built up of edge-sharing bioctahedron. Due to the hydrogen bonds and the interatomic distances (Bi-I, I center dot center dot center dot I and pi-pi) changes, alpha-phase was transformed into the corresponding centrosymmetric beta-phase, beta-[C6H4(NH3)(2)](2)Bi2I10, through a single-crystal to single-crystal transformation occurring upon cooling to -28/-26 degrees C. Below the transition temperature, beta-[C6H4(NH3)(2)](2)Bi2I10 crystallizes in the monoclinic system, centrosymmetric space group P2(1)/n. Besides, the optical transmission measurements on alpha-[C6H4(NH3)(2)](2)Bi2I10 thin films have revealed two absorption bands at 2.47 and 3.01 eV. Finally, two room temperature photoluminescence emissions attributed to excitons radiative recombinations confined within the bioctahedra Bi2I104-, were observed in the red spectral range at 1.9 and 2.05 eV energy