41 results on '"Nasr, C."'
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2. Synthesis, crystal structure, vibrational, optical properties, and a theoretical study of a new Pb(II) complex with bis(1-methylpiperazine-1,4-diium): [C5H14N2]2PbCl6·3H2O.
- Author
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Mrad, Mohamed Lahbib, Belhajsalah, Souhir, Abdelbaky, Mohammed Said M., García-Granda, Sergio, Essalah, Khaled, and Ben Nasr, C.
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OPTICAL properties ,CRYSTAL structure ,X-ray powder diffraction ,X-ray photoelectron spectroscopy ,THERMAL analysis - Abstract
An investigation of the solid-state X-ray structure of the new organic–inorganic compound [C
5 H14 N2 ]2 PbCl6 ·3H2 O shows a layered organization of the (PbCl6 )4– anions, with (R2 NH2 )+ 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 [C5 H14 N2 ]2 PbCl6 ·3H2 O. [ABSTRACT FROM AUTHOR]- Published
- 2019
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3. Hirshfeld Surface Analysis, Crystal Structure and Spectroscopic Studies of a New Cu(II) Halocuprate Salt with Protonated N-Amino-Ethyl-Piperazine.
- Author
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El Glaoui, Maroua, El Glaoui, Maher, Jelsch, C., and Ben Nasr, C.
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ORTHORHOMBIC crystal system ,SINGLE crystals ,COPPER ions ,HYDROGEN bonding ,CRYSTAL structure - Abstract
(C
6 H18 N3 )4 [CuCl5 ]2 [CuCl4 ]3 ·1.42H2 O is prepared and characterized by various physicochemical techniques. The single crystal X-ray diffraction structural analysis reveals that the title compound belongs to the orthorhombic system with the space group Cmca. Its unit cell dimensions are: a = 24.286(2) Å, b = 14.3082(14) Å, c = 16.6160(16) Å, Z = 4, V = 5773.8(10) Å3 . Its crystal structure is determined and refined down to R = 0.024 and wR(F2 ) = 0.059. The structure contains three crystallographically independent Cu2+ ions coordinated to chlorine anions in various fashions. Cu1 is five-coordinated in a distorted square pyramidal fashion, while Cu2 and Cu3 are four-coordinated in square planar and distorted tetrahedral fashions, respectively. The entities are interconnected by means of the hydrogen bonding [O(W)-H...Cl, N-H...Cl, C-H...Cl and C-H...O(W)], forming a three-dimensional network. Intermolecular interactions are investigated by Hirshfeld surfaces and the contacts of the eight different chloride atoms are notably compared. The vibrational absorption bands are identified by infrared spectroscopy. The optical study is performed by UV-vis absorption. [ABSTRACT FROM AUTHOR]- Published
- 2018
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4. Crystal Structure, Magnetic Properties, and Electrical Characterization of a New Coordination Compound: [CuClO4(C4H6N2O)4H2O]ClO4(C4H6N2O)0.08.
- Author
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Ben Nasr, M., Kahlaoui, M., Ferenc, W., Cristovao, B., and Ben Nasr, C.
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CHEMICAL preparations industry ,CRYSTAL structure ,MOLECULAR structure ,MAGNETIC properties ,HYDROGEN bonding - Abstract
The chemical preparation and characterization of a novel coordination compound [CuClO
4 (C4 H6 N2 O)4H2 O]ClO4 (C4 H6 N2 O)0.08 is reported. The compound crystallizes in the monoclinic space group P21/c with lattice parameters a = 11.2678(5) Å, b = 12.8102(6) Å, c = 19.7250(8) Å, β = 100.3051(15)°, V = 2801.2(2) Å3 . The Cu(II) cation is six-coordinated in an elongated distorted octahedral fashion by four N atoms of four 3-amino-5-methylisoxazole ligands, one water oxygen atom, and one perchlorate oxygen atom. In the atomic arrangement, the coordinated and uncoordinated perchlorate anions are grouped in pairs to form anionic layers parallel to the (a, b) plane. A substantial number of H-bonding interactions leads to the formation of an intricate three-dimensional network. The vibrational absorption bands are identified by infrared spectroscopy and the electrical properties are studied by impedance spectroscopy. The DSC analysis agrees with the electrical conductivity results. Magnetic properties are also determined to characterize the complex. [ABSTRACT FROM AUTHOR]- Published
- 2018
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5. Synthesis, crystal structure and characterization of two new organic bismuthate(III) compounds: [CHO]BiX·2HO (X = Br, Cl).
- Author
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Aloui, Z., Ferretti, V., Abid, S., Rzaigui, M., and Nasr, C.
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CRYSTAL structure ,ORGANIC synthesis ,TRICLINIC crystal system ,CHEMICAL derivatives ,DIMERS ,ANIONS - Abstract
The synthesis and the structures of two new compounds with the general formula [CHNO]BiX·2HO (X = Br, Cl) are reported. They crystallize in the triclinic system and are isostructural. Crystal structures were solved and refined to R = 0.064, 0.048 and R = 0.15, 0.13 using 3392, 3679 independent reflections for the Cl and Br derivatives, respectively. The atomic arrangement can be described by inorganic chains along the [100] direction. These chains are themselves interconnected by means of N-H···X (X = Cl, Br) originating from the [CHNO] entities, to form three-dimensional network. The organic part consists of one organic cation which orients its two amine groups to the neighboring anions. The inorganic entity is made up of [BiX] dimers composed of two equivalent irregular octahedra sharing one edge. The oxygen atoms of the water molecules (OW) act as donor (O-H···X) and acceptor (N-H···O) of hydrogen bonds. The nature of the distortion of the inorganic polyhedra can be attributed to the stereoactivity of the Bi(III) lone electron pair. Raman and infrared spectra at room temperature were recorded in the 500-100 and 4000-400 cm frequency regions, respectively. This study confirms the presence of the organic cation [CHO] and the bioctahedron [BiX]. The calorimetric study shows that the title compound is stable until 384 K. [ABSTRACT FROM AUTHOR]
- Published
- 2015
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6. Synthesis and Characterization of Bis(4-methylbenzylammonium) Tetrachloridocadmate(II).
- Author
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Kefi, R., Zeller, M., Lefebvre, F., and Ben Nasr, C.
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CRYSTAL structure ,INORGANIC compounds ,ORGANIC compounds ,X-ray diffraction ,HYDROGEN bonding ,CRYSTALLOGRAPHY - Abstract
The crystal structure of the new inorganic-organic hybrid compound [4-CH
3 C6 H4 CH2 NH3 ]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]- Published
- 2011
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7. Synthesis, Structure, and Physicochemical Studies of Hexakis (5-Chloro-2,4-dimethoxyanilinium)cyclohexaphosphate Tetrahydrate.
- Author
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Salah, R. Bel Haj, Khedhiri, L., Nasr, C. Ben, Rzaigui, M., and Lefebvre, F.
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PHOSPHATES ,CRYSTALS ,X-ray crystallography ,HYDROGEN bonding ,NUCLEAR magnetic resonance spectroscopy ,X-ray diffraction - Abstract
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]
- Published
- 2010
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8. Structural and Physicochemical Studies of [2,3-(CH3)2C6H3NH3]4HP3O10.2H2O.
- Author
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Souissi, S., Smirani, W., Nasr, C. Ben, and Rzaigui, M.
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CATIONS ,PHOSPHATES ,ETHANES ,HYDROGEN bonding ,THERMAL analysis - Abstract
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]
- Published
- 2007
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9. Synthesis and Characterization of a New Cyclotriphosphate [C8H11NH3]3P3O9·3H2O.
- Author
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Mrad, M. L., Nasr, C. Ben, and Rzaigui, M.
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ORGANIC synthesis , *PHOSPHATES , *INFRARED spectroscopy , *X-ray diffraction , *THERMAL analysis , *ANIONS , *NUCLEAR magnetic resonance - Abstract
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]
- Published
- 2006
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10. The Synthesis and Characterization of 2-Amino-3-methylpyridinium Dihydrogenmonophosphate: (C 6 H 9 N 2 )H 2 PO 4.
- Author
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Oueslati, A., Touati, A., Nasr, C., and Lefebvre, F.
- Subjects
CRYSTALS ,CRYSTALLOGRAPHY ,THERMAL analysis ,HYDROGEN bonding ,ATOMS - Abstract
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]
- Published
- 2006
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11. Synthesis and Characterization of Two New Compounds: N(C 2 H 4 NH 3 ) 3 (H 2 TO 4 )(HTO 4 )·2H 2 O (T = P, As).
- Author
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Oueslati, J., Rayes, A., Ben Nasr, C., and Lefebvre, F.
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SALTS ,HYDROGEN ,ANIONS ,MOLECULES ,SPECTRUM analysis ,PHOSPHORUS ,CRYSTALLOGRAPHY - Abstract
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]
- Published
- 2006
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12. SYNTHESIS AND STRUCTURE CHARACTERIZATION OF PIPERAZINE-1,4-DIIUM TRIPHOSPHATE.
- Author
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Smirani, W., Nasr, C. Ben, and Rzaigui, M.
- Subjects
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PIPERAZINE , *PHOSPHATES , *NUCLEAR magnetic resonance , *NUCLEAR magnetic resonance spectroscopy , *X-ray diffraction - Abstract
[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]
- Published
- 2004
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13. Synthesis, crystal structure, vibrational spectroscopy, DFT, optical study and thermal analysis of a new stannate(IV) complex based on 2-ethyl-6-methylanilinium (C9H14N)2[SnCl6].
- Author
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Feddaoui, I., Abdelbaky, Mohammed S.M., García-Granda, S., Essalah, K., Ben Nasr, C., and Mrad, M.L.
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PHOTOLUMINESCENCE measurement , *THERMAL analysis , *CRYSTAL structure , *CRYSTAL optics , *X-ray photoelectron spectroscopy , *SPECTRUM analysis - Abstract
Abstract The new organic-inorganic compound, (C 9 H 14 N) 2 [SnCl 6 ], has been synthesized and characterized by single-crystal X-ray diffraction at room temperature. Structural analysis indicates that this compound crystallizes in the monoclinic system with C2/m space group. The N H⋯Cl hydrogen bonds between (C 9 H 14 N)+ cations and [SnCl 6 ]2- dianions contribute to the cohesion and the stability of the atomic arrangement. Hirshfeld surface analysis was used to investigate intermolecular interactions, as well 2D finger plots were conducted to reveal the contribution of these interactions in the crystal structure quantitatively. Furthermore, the room temperature Infrared (IR) spectrum of the title compound was analyzed on the basis of data found in the literature. The optical properties of the crystal were studied using optical absorption UV–visible and photoluminescence (PL) spectroscopy, which were investigated at room temperature exhibited one band at 237 nm and a photoluminescence emission at 407 nm. Experimental room-temperature X-ray studies were supported by theoretical methods using the DFT/B3LYP methods with the LanL2DZ basis set. The X-ray powder is in agreement with the X-ray structure. To determine molecular electrical transport properties we studied the energy difference between Occupied, HOMO, and Lowest Unoccupied, LUMO orbitals. Moreover, this compound was characterized by thermal analysis between 300 and 750 K and shows that the compound remains stable up to the temperature 383 K. Finally, X-ray photoelectron spectroscopy (XPS) analysis is reported to determine the degree of oxidation of tin in this compound and analyze the surface chemistry of (C 9 H 14 N) 2 [SnCl 6 ]. Graphical abstract Image 1 Highlights • The crystal structure is built by alternating organic and inorganic entities. • The optical properties were studied by UV–visible, photoluminescence and XPS study. • This compound was characterized by thermal analysis between 300 and 750 K. [ABSTRACT FROM AUTHOR]
- Published
- 2019
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14. Synthesis, crystal structure, physico-chemical characterization and theoretical study of a new Pb(II) complex [C10H22N2]3·PbCl5·3Cl·3H2O.
- Author
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Feddaoui, I., Abdelbaky, Mohammed S.M., García-Granda, Santiago, Essalah, K., Ben Nasr, C., and Mrad, M.L.
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HYDROGEN bonding , *CRYSTAL structure , *THERMAL analysis , *OPTICAL properties , *INTERMOLECULAR interactions , *PHASE transitions - Abstract
Abstract A novel hybrid material, [C 10 H 22 N 2 ] 3 ·PbCl 5 ·3Cl·3H 2 O, has been synthesized and its structure was determined by single-crystal X-ray diffraction. In the atomic arrangement, the different entities are held together through N H⋯Cl, O H⋯Cl and O H⋯O hydrogen bonds to form a three-dimensional network. Intermolecular interactions were investigated by Hirshfeld surfaces. The powder XRD data confirms the phase purity of the crystalline sample. The resulting IR spectrum calculated by the DFT/B3LYP/LanL2DZ method, is similar to the experimental spectrum allowing a good correlation between the experimental and theoretical wavenumbers. The optical properties in the UV–visible region have been explored by the UV–visible absorption. The photoluminescence (PL) spectroscopy, which was investigated at room temperature, exhibited one emission at 426 nm. Thermal analysis discloses a phase transition at 435 K and the decomposition of the sample starts from 554 K. Graphical abstract Image 1 Highlights • The entities [C 10 H 22 N 2 ]2+ and [PbCl 5 ]3- ions are interconnected by means of hydrogen bonding contacts, forming a three-dimensional network. • The vibrational frequencies were also predicted from the calculated intensities by DFT method. • The optical properties were studied by UV–visible absorption and photoluminescence study. • This compound was characterized by thermal analysis between 300 and 750 K. [ABSTRACT FROM AUTHOR]
- Published
- 2019
- Full Text
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15. Synthesis, crystal structure, vibrational, optical properties, thermal analysis and theoretical study of a new Sn(IV) complex (C5H14N2)2[SnCl6]2·5H2O.
- Author
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BelhajSalah, S., Abdelbaky, M.S.M., García-Granda, S., Essalah, K., Ben Nasr, C., and Mrad, M.L.
- Subjects
- *
CRYSTAL structure , *OPTICAL properties , *THERMAL analysis , *ORTHORHOMBIC crystal system , *X-ray diffraction , *HYDROGEN bonding , *INTERMOLECULAR interactions - Abstract
Abstract In this study, a new organic-inorganic hybrid metal compound (C 5 H 14 N 2) 2 [SnCl 6 ] 2 ·5H 2 O was crystallized at room temperature in the orthorhombic system (space group P2 1 2 1 2 1) where the structure is determined by single crystal X-ray diffraction analysis. The examination of the structure shows the cohesion and stability of the atomic arrangement result from the establishment of N—H⋯Cl, O(W)—H(W)⋯Cl, N—H⋯O(W) and O(W)—H(W)⋯O(W) hydrogen bonds between 1-methylpiperazine-1,4-diium (C 5 H 14 N 2)2+cations, isolated (SnCl 6)2– anions and water molecules to form organic and inorganic layers parallel to the (a, c) plane and alternate along the b-axis. Hirshfeld surface analysis was used to investigate intermolecular interactions, as well 2D fingerprint plots were conducted to reveal the contribution of these interactions in the crystal structure quantitatively. The solid phase FTIR and FT-Raman spectra of this compound have been recorded in the regions 400–4000 and 100–500 cm−1, respectively. The vibrational frequencies were also predicted from the calculated intensities by DFT method and were compared with the experimental frequencies, which yield good agreement between observed and calculated frequencies. Besides, the optical proprieties were investigated by UV-visible and photoluminescence spectroscopy studies in the region 200–700 nm and the electronic properties HOMO and LUMO energies were measured by TD-DFT approach. Moreover, this compound was characterized by thermal analysis between 300 and 500 K which revealing two phase transitions. Finally, X-ray photoelectron spectroscopy (XPS) analysis is reported to determine the degree of oxidation of tin in this compound and analyzing the surface chemistry of (C 5 H 14 N 2) 2 [SnCl 6 ] 2 ·5H 2 O. Graphical abstract Image 1 The different characterization techniques of (C 5 H 14 N 2) 2 [SnCl 6 ] 2 ·5H 2 O. Highlights • The crystal structure exhibits organic and inorganic layers parallel to the (a, c) plane and alternate along the b-axis. • The 3D Hirshfield surfaces and the associated 2D fingerprint plots were investigated for intermolecular interactions. • The vibrational frequencies were also predicted from the calculated intensities by DFT method and were compared with the experimental frequencies. • The optical properties were studied by UV–visible absorption, photoluminescence spectroscopy studies and XPS technique. • This compound was characterized by thermal analysis between 300 and 500. [ABSTRACT FROM AUTHOR]
- Published
- 2018
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16. Crystal structure, Hirshfeld surface analysis, thermal behavior and spectroscopic investigations of a new organic cyclohexaphosphate, (C10H15N2)4(Li)2(P6O18)(H2O)6.
- Author
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Khedhiri, L., Hamdi, A., Soudani, S., Kaminsky, W., Lefebvre, F., Jelsch, C., Wojtaś, M., and Ben Nasr, C.
- Subjects
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CRYSTAL structure , *THERMAL stability , *CYCLOHEXANOLS , *PHOSPHATES , *INORGANIC compounds - Abstract
The synthesis and the structure of (C 10 H 15 N 2 ) 4 (Li) 2 (P 6 O 18 )(H 2 O) 6 are described. This compound crystallizes in the triclinic system, with the centric space group P-1 and the following unit cell parameters: a = 9.7762(6), b = 10.2502(8), c = 15.2173(11) Å, α = 92.588(4), β = 98.855(4), γ = 115.724(4)°, Z = 2 and V = 1346.62(17) Å 3 . The crystal structure has been solved and refined to R = 0.0452 and Rw = 0.1121. [Li 2 (P 6 O 18 )(H 2 O)] 4- entities are associated by strong O H⋯O hydrogen bonds to form inorganic layers lying in the (a, b) plane. These layers are interconnected with the organic entities via N H⋯O and C H⋯O hydrogen bonds. In this atomic arrangement, H bonds between the different species play an important role in the three-dimensional network. The contacts enrichment ratios derived from the Hirshfeld surface analysis show that the crystal packing is stabilized by ionic bridges Li + … O, strong N/O H⋯O hydrogen bonds but also hydrophobic interactions between the two independant 1-phenylpiperazine-1,4-dium ligands. The Molecular Electrostatic Potential (MEP) maps and the HOMO and LUMO energy gaps of the new compound were computed. The title compound was further characterized by FT-IR and NMR spectroscopies. The crystal symmetry was confirmed by 31 P and 7 Li MAS NMR and the vibrational absorption bands were identified by infrared spectroscopy. The new compound was also characterized by thermal analysis to determine the thermal behavior. [ABSTRACT FROM AUTHOR]
- Published
- 2018
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17. Crystal Structure, Magnetic Properties, and Electrical Characterization of a New Coordination Compound: [CuClO4(C4H6N2O)4H2O]ClO4(C4H6N2O)0.08.
- Author
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Ben Nasr, M., Kahlaoui, M., Ferenc, W., Cristovao, B., and Ben Nasr, C.
- Subjects
- *
CHEMICAL preparations industry , *CRYSTAL structure , *MOLECULAR structure , *MAGNETIC properties , *HYDROGEN bonding - Abstract
The chemical preparation and characterization of a novel coordination compound [CuClO4(C4H6N2O)4H2O]ClO4(C4H6N2O)0.08 is reported. The compound crystallizes in the monoclinic space group P21/c with lattice parameters a = 11.2678(5) Å, b = 12.8102(6) Å, c = 19.7250(8) Å, β = 100.3051(15)°, V = 2801.2(2) Å3. The Cu(II) cation is six-coordinated in an elongated distorted octahedral fashion by four N atoms of four 3-amino-5-methylisoxazole ligands, one water oxygen atom, and one perchlorate oxygen atom. In the atomic arrangement, the coordinated and uncoordinated perchlorate anions are grouped in pairs to form anionic layers parallel to the (a, b) plane. A substantial number of H-bonding interactions leads to the formation of an intricate three-dimensional network. The vibrational absorption bands are identified by infrared spectroscopy and the electrical properties are studied by impedance spectroscopy. The DSC analysis agrees with the electrical conductivity results. Magnetic properties are also determined to characterize the complex. [ABSTRACT FROM AUTHOR]
- Published
- 2018
- Full Text
- View/download PDF
18. Crystal structure, quantum mechanical investigation, IR and NMR spectroscopy of two new organic salts: (C8H12NO)·[NO3] (I) and (C8H14N4)·[ClO4]2 (II).
- Author
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Bayar, I., Khedhiri, L., Soudani, S., Lefebvre, F., Pereira Da Silva, P.S., and Ben Nasr, C.
- Subjects
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AMMONIUM nitrate , *PERCHLORATES , *CRYSTAL structure , *INTERMOLECULAR interactions , *X-ray diffraction , *DENSITY functional theory - Abstract
Two new organic-inorganic hybrid materials, 4-methoxybenzylammonium nitrate, (C 8 H 12 NO)·[NO 3 ] (I) , and 2-(1-piperazinyl)pyrimidinium bis(perchlorate), (C 8 H 14 N 4 )·[ClO 4 ] 2 (II) , have been synthesized by an acid/base reaction at room temperature, their structures were determined by single crystal X-ray diffraction. Compound (I) crystallizes in the orthorhombic system and Pnma space group with a = 15.7908 (7), b = 6.8032 (3), c = 8.7091 (4) Å, V = 935.60 (7) Å 3 with Z = 4. Full-matrix least-squares refinement converged at R = 0.038 and w R ( F 2 ) = 0.115. Compound (II) belongs to the monoclinic system, space group P 2 1 / c with the following parameters: a = 10.798(2), b = 7.330(1), c = 21.186(2) Å, β = 120.641 (4)°, V = 1442.7 (3) Å 3 and Z = 4. The structure was refined to R = 0.044, w R ( F 2 ) = 0.132. In the structures of ( I ) and ( II ), the anionic and cationic entities are interconnected by hydrogen bonding contacts forming three-dimensional networks. Intermolecular interactions were investigated by Hirshfeld surfaces and the contacts of the four different chloride atoms in (II) were compared. The Molecular Electrostatic Potential (MEP) maps and the HOMO and LUMO energy gaps of both compounds were computed. The vibrational absorption bands were identified by infrared spectroscopy. These compounds were also investigated by solid-state 13 C, 35 Cl and 15 N NMR spectroscopy. DFT calculations allowed the attribution of the IR and NMR bands. [ABSTRACT FROM AUTHOR]
- Published
- 2018
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19. Crystal structure, quantum mechanical investigation, IR and NMR spectroscopy of two new organic perchlorates: (C6H18N3)·(ClO4)3H2O (I) and (C9H11N2)·ClO4(II).
- Author
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Bayar, I., Khedhiri, L., Soudani, S., Lefebvre, F., Ferretti, V., and Ben Nasr, C.
- Subjects
- *
CRYSTAL structure , *PERCHLORATES , *BENZIMIDAZOLE derivatives , *MONOCLINIC crystal system , *X-ray diffraction - Abstract
The reaction of perchloric acid with 1-(2-aminoethyl)piperazine or 5,6-dimethyl-benzimidazole results in the formation of 1-(2-amonioethyl)piperazine-1,4-dium triperchlorate hydrate (C 6 H 18 N 3 )·(ClO 4 ) 3 ·H 2 O (I) or 5,6-dimethyl-benzylimidazolium perchlorate (C 9 H 11 N 2 )·ClO 4 (II) . Both compounds were fully structurally characterized including single crystal X-ray diffraction analysis. Compound (I) crystallizes in the centrosymmetric triclinic space group P 1 ¯ with the lattice parameters a = 7.455 (2), b = 10.462 (2), c = 10.824 (2) Å, α = 80.832 (2), β = 88.243 (2), γ = 88.160 (2) °, Z = 2 and V = 832.77 (3) Å 3 . Compound (II) has been found to belong to the P 2 1 /c space group of the monoclinic system, with a = 7.590 (3), b = 9.266 (3), c = 16.503 (6) Å, β = 107.38 (2) °, V = 1107.69 (7) Å 3 and Z = 4. The structures of (I) and (II) consist of slightly distorted [ClO 4 ] - tetrahedra anions and 1-(2-amonioethyl)piperazine-1,4-dium trication (I) or 5,6-dimethyl-benzylimidazolium cations (II) and additionally a lattice water in (I) . The crystal structures of ( I) and ( II) exhibit complex three-dimensional networks of H-bonds connecting all their components. In the atomic arrangement of (I) , the ClO 4 − anions form corrugated chains, while in (II) the atomic arrangement exhibits wide pseudo-hexagonal channels of ClO 4 tetrahedra including the organic entities. The lattice water serves as a link between pairs of cations and pairs of anions via several O H⋯O and N-H⋯O interactions in compound (I) . The vibrational absorption bands were identified by infrared spectroscopy. These compounds were also investigated by solid-state 13 C, 35 Cl and 15 N NMR spectroscopy. DFT calculations allowed the attribution of the IR and NMR bands. Intermolecular interactions were investigated by Hirshfeld surfaces. Electronic properties such as HOMO and LUMO energies were derived. [ABSTRACT FROM AUTHOR]
- Published
- 2018
- Full Text
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20. Synthesis, crystal structure, vibrational and optical properties of a new Pb(II) complex (2-hydroxyethyl)piperazine-1,4-diium tetrachloroplombate(II) C6H16N2OPbCl4.
- Author
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Mrad, M.L., Feddaoui, I., Abdelbaky, M.S.M., García-Granda, S., and Ben Nasr, C.
- Subjects
- *
COMPLEX compounds synthesis , *LEAD compounds , *METAL complexes , *CRYSTAL structure , *OPTICAL properties of metals - Abstract
A novel hybrid material, C 6 H 16 N 2 OPbCl 4 , has been successfully synthesized in nitrogen atmosphere by slow evaporation at room temperature. The compound structure was determined by single-crystal X–ray diffraction and crystallizes in the triclinic space group P -1 ( a = 5.9926(2) Å, b = 10.3691(5) Å, c = 11.3558(4) Å, α = 111.755(4)°, β = 96.080(3)°, γ = 105.948(4)°, Z = 2) at 293 K. The structure is built up from anionic 1-D polymeric chains of PbCl 4 O octahedral extended along the ( b + c )-axis. These chains are interconnected by O H⋯Cl hydrogen bonds to form inorganic layers parallel to ( a, b + c ) plane. The organic layers are inserted between the inorganic ones and connect them through N H⋯Cl and C H⋯Cl hydrogen bonds to build a three dimensional network. To gain more information about intermolecular interaction we used Hirshfeld surfaces associated with 2D finger plots. The optical and PL properties of the compound were investigated in the solid state at room temperature and exhibited two bands at 250 and 290 nm and a photoluminescence emission at 529 nm. Raman and infrared spectra were used to gain more information for vibrational modes of the title compound. As for thermal analysis, DSC analysis shows that this compound is stable at temperature below melting point. Finally, XPS analysis is achieved for analyzing the surface chemistry of C 6 H 16 N 2 OPbCl 4 crystals. [ABSTRACT FROM AUTHOR]
- Published
- 2018
- Full Text
- View/download PDF
21. Synthesis, X-ray single crystal structure, likelihood of occurrence of intermolecular contacts, spectroscopic investigation and DFT quantum chemical calculations of zwitterionic complex: 1-Ethylpiperaziniumtrichlorozincate (II).
- Author
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Soudani, S., Jeanneau, E., Jelsch, C., Lefebvre, F., and Ben Nasr, C.
- Subjects
- *
ZWITTERIONS , *HYDROGEN bonding , *INTERMOLECULAR interactions , *ELECTRIC potential , *DENSITY functional theory , *QUANTUM chemistry - Abstract
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]
- Published
- 2017
- Full Text
- View/download PDF
22. Crystal and geometry-optimized structure, Hirshfeld surface analysis and physicochemical studies of a new Co(II) complex with the ligand 2-amino-6-methoxypyrimidine.
- Author
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Nbili, W., Soudani, S., Kaabi, K., Wojtaś, M., Ferretti, V., Lefebvre, F., Jelsch, C., and Ben Nasr, C.
- Subjects
- *
CRYSTAL structure , *AQUEOUS solutions , *SINGLE crystals , *X-ray diffraction , *INTERMOLECULAR interactions , *THERMAL analysis - Abstract
The crystal structure of the new complex [Co(C 5 H 7 N 3 O) 2 (H 2 O) 4 ](NO 3 ) 2 ⋅4H 2 O synthesized in aqueous solution has been determined by single crystal X-ray diffraction. The compound crystallizes in the triclinic space group P 1 ¯ with lattice parameters: a = 7.3056(2), b = 8.4065(2), c = 10.4724(3) Å, α = 103.9470(19), β = 105.6600(14), γ = 91.1350(18)°, V = 598.54(3) Å 3 and Z = 1. The Co(II) central ion is in a slightly distorted octahedral coordination geometry formed by two nitrogen atoms of two 2-amino-6-methoxypyrimidine ligands and four oxygen atoms of coordinated water molecules. The crystal packing is stabilized by intermolecular O H⋯O, N H⋯O and C H⋯O hydrogen bonds which link the molecules into a three-dimensional network. Intermolecular interactions were investigated by Hirshfeld surfaces. Electronic properties such as HOMO and LUMO energies were derived. The vibrational absorption bands were identified by infrared spectroscopy. The compound was characterized by thermal analysis to determine its thermal behavior with respect to temperature. [ABSTRACT FROM AUTHOR]
- Published
- 2017
- Full Text
- View/download PDF
23. Crystal structure, vibrational and optical properties of a new Bi(III) halide complex: [C6H16N2]5Bi2Br10(BiBr6)2·2H2O.
- Author
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Essid, M., Aloui, Z., Ferretti, V., Lefebvre, F., and Nasr, C. Ben
- Subjects
- *
CRYSTAL structure , *CRYSTALLOGRAPHY , *ALLOTROPIC transition , *HALIDES , *CATIONS - Abstract
A new Bi(III) halide complex, [C 6 H 16 N 2 ] 5 Bi 2 Br 10 (BiBr 6 ) 2 ·2H 2 O has been synthesized at room temperature in the presence of 1,4-dimethylpiperazine by slow evaporation technique and characterized by physicochemical methods. It crystallizes in a triclinic centrosymmetric space group, P -1. The crystal lattice is composed of two types of anionic entities [Bi 2 Br 10 ] 4− and [BiBr 6 ] 3− surrounded by 1,4-dimethylpiperazine-1,4-diium cations and water molecules. The anionic part was found for the first time in halobismuthate(III) solid complexes. In the crystal, the components are linked by C-H…Br(Ow) and Ow-H…Br hydrogen bonds to built three-dimensional network. The vibrational absorption bands were identified by Infrared and Raman spectroscopy. The 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray structure. Intermolecular hydrogen bonding was investigated by means of the Hirshfeld surfaces. The percentages of hydrogen bonding interactions are analyzed by Fingerprint plots of Hirshfeld surface. The optical properties of this compound were studied by UV–Vis and luminescence spectroscopy. The DSC curve shows that this compound is stable below melting point. [ABSTRACT FROM AUTHOR]
- Published
- 2017
- Full Text
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24. Crystal structure, Hirshfeld surface analysis, quantum mechanical study and spectroscopic characterization of the non-centrosymmetric coordination compound bis(4-fluoroaniline)dichloridozincate.
- Author
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Ben Nasr, M., Soudani, S., Lefebvre, F., Jelsch, C., and Ben Nasr, C.
- Subjects
- *
ZINC compounds , *ANILINE , *CRYSTAL structure , *CHLORINE , *NITROGEN - Abstract
The Zn(II) complex with the monodentate ligand 4-fluoroaniline, ZnCl 2 (C 6 H 4 FNH 2 ) 2 , has been prepared and characterized by single crystal X-ray diffraction, solid state nuclear magnetic resonance, infrared spectroscopy and differential scanning calorimetry. The Zn(II) ion is tetracoordinated by two nitrogen atoms of two monodentate 4-fluoroaniline ligands and two chlorine atoms. In the molecular arrangement, the ZnCl 2 (C 6 H 4 FNH 2 ) 2 entities are interconnected via N H⋯Cl hydrogen bonds to form layers parallel to the ( a , b ) plane. The nature and proportion of contacts in the crystal packing were investigated through the Hirshfeld surfaces. The crystal is mainly maintained by electrostatic attractions Cl − … H N and by extensive hydrophobic contacts as revealed by the Hirshfeld 2D fingerprint plots and statistical analysis. The 13 C and 19 F CP-MAS NMR spectra are in agreement with the X-ray structure and confirm the phase purity of the crystalline sample. The vibrational absorption bands were identified by infrared spectroscopy. A calorimetric study shows that the title compound is stable until 262.5 °C. [ABSTRACT FROM AUTHOR]
- Published
- 2017
- Full Text
- View/download PDF
25. Synthesis, crystal structure, physico-chemical characterization of a new hybrid material, (2-hydroxyethyl)piperazine-1,4-diium hexachlorostannate(IV) monohydrate.
- Author
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Salah, S. Belhaj, da Silva, Pedro Sidónio Pereira, Lefebvre, F., Ben Nasr, C., Ammar, S., and Mrad, M.L.
- Subjects
- *
CRYSTAL structure , *HYDRATES , *INORGANIC compounds , *PIPERAZINE , *SINGLE crystals , *AQUEOUS solutions , *CHEMICAL synthesis - Abstract
The new organic-inorganic compound [C 6 H 16 N 2 O](SnCl 6 ).H 2 O was synthesized and single crystals were grown from an aqueous solution through these slow evaporation technique. The atomic arrangement can be described by organic-inorganic layers parallel to the (a, c) plane. These layers are connected via hydrogen bonds (O H⋯O and C H⋯Cl) to build a three dimensional arrangement. 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 and Raman scattering. DFT calculations allowed the attribution of the IR bands. The 3D Hirshfeld surfaces and the associated 2D fingerprint plots were investigated for intermolecular interactions. X-ray photoelectron spectroscopy analysis (XPS) is a technique for analyzing the surface chemistry of a compound. It was employed to measure the elemental composition and electronic state of the elements within a material. The DSC profile shows endothermic peaks centered at approximately 343, 370 and 552 K. [ABSTRACT FROM AUTHOR]
- Published
- 2017
- Full Text
- View/download PDF
26. Crystal structure, quantum mechanical study and spectroscopic studies of nitrate and perchlorate salts of 3-chloroaniline, [C6H7ClN]NO3 (I) and [C6H7ClN]ClO4 (II).
- Author
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Bayar, I., Khedhiri, L., Jeanneau, E., Lefebvre, F., and Ben Nasr, C.
- Subjects
- *
CRYSTAL structure , *NITRATES , *PERCHLORATES , *CHLOROANILINE , *TEMPERATURE effect , *QUANTUM chemistry - Abstract
Two new organic-inorganic hybrid compounds, 3-chloroanilinium nitrate (I) and 3-chloanilinium perchlorate (II) , have been synthesized by an acid/base reaction at room temperature in the presence of 3-chloroaniline as an organic-structure directing agent and their structures were determined by single crystal X-ray diffraction. Compound I , [C 6 H 7 ClN]NO 3 , crystallizes in the orthorhombic space group Pbca with a = 10.4137(16), b = 9.6232(11), c = 16.059(2) Å, V = 1609.3(4) and z = 8. Full-matrix least-squares refinement converged at R = 0.041 and Rw = 0.121. Compound II , [C 6 H 7 ClN]ClO 4 , belongs to the monoclinic system, space group P 21/ n with the following parameters: a = 10.684(2), b = 7.2667(12), c = 12.229(2) Å, β = 104.27(2)°, V = 920.1(3) and z = 4. The structure was refined to R = 0.054 and Rw = 0.102. Both salts form anionic parallel layers alternating with thick slabs of [C 6 H 7 NCl] + organic molecules. Charge balance is achieved by the protonated amine which interacts with the inorganic framework through hydrogen bonding. Solid-state 13 C CP-MAS NMR spectroscopy is in agreement with the X-ray structures. Ab initio calculations allow the partial attribution of carbon signals to the various atoms of the organic groups. Electronic properties such as HOMO and LUMO energies were studied by Quantum mechanical evaluation by using the B3LYP/6-31+G* method. [ABSTRACT FROM AUTHOR]
- Published
- 2017
- Full Text
- View/download PDF
27. A Hirshfeld surface analysis, crystal structure and infrared characterization of a new organic cyclohexaphosphate, (C8H12N)4(Li)2(P6O18)(H2O)6.
- Author
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Khedhiri, L., Ferretti, V., Jelsch, C., Rzaigui, M., and Ben Nasr, C.
- Subjects
- *
CRYSTAL structure , *SURFACE analysis , *PHOSPHATES , *SINGLE crystals , *CHEMICAL reactions , *TEMPERATURE effect - Abstract
Single crystals of a new organic cyclohexaphosphate (C 8 H 12 N) 4 (Li) 2 (P 6 O 18 )(H 2 O) 6 prepared by an acid/base reaction between cyclohexaphosphoric acid H 6 P 6 O 18 and 2,6-dimethylaniline, have been successfully grown by slow evaporation technique at room temperature. This compound was characterized using X-ray diffraction (XRD) and FT-IR spectroscopy. The results show that the title compound was phased with a triclinic structure and P-1 space group. The crystal structure was solved by using 5203 independent reflections with a final R value of 0.031. The P 6 O 18 ring is centrosymmetrical. Its main geometrical features are those commonly observed in others cyclohexaphosphates. The atomic arrangement of this compound can be described by an organization in a three-dimensional framework, built up from alternated organic and inorganic species. Adjacent P 6 O 18 rings are linked via corner-sharing by LiO 4 tetrahedra, generating anionic [Li 2 (P 6 O 18 )(H 2 O)] 4- layers parallel to (110). Charge balance is achieved by the protonated amine which is trapped in the interlayer space and interacts with the organic framework through strong and medium hydrogen bonding. An extensive network of N H⋯O and O H⋯O hydrogen-bonding interactions link the components into a three-dimensional network and additional stabilization is provided by weak C H⋯O hydrogen bonds. Intermolecular interactions were investigated by Hirshfeld surfaces. The vibrational absorption bands were identified by infrared spectroscopy. The stretching modes of P 6 O 18 ring and band assignments are described. [ABSTRACT FROM AUTHOR]
- Published
- 2017
- Full Text
- View/download PDF
28. Synthesis and characterization of two organic cation hydrogensulfates: 1-(2,5-dimethylphenyl)piperazine-1,4-diium bis(hydrogensulfate) monohydrate (SI) and 1-(2,3-dimethylphenyl)piperazine-1,4-diium bis(hydrogensulfate) (SII).
- Author
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Arbi, M., Khedhiri, L., Wojtaś, M., Jeanneau, E., Lefebvre, F., and Ben Nasr, C.
- Subjects
- *
SULFATES , *THERMAL analysis , *X-ray diffraction , *ANIONS , *PIPERAZINE , *NUCLEAR magnetic resonance spectroscopy - Abstract
Treatment of 1-(2,5-dimethylphenyl)piperazine and 1-(2,3-dimethylphenyl)piperazine with H 2 SO 4 in 2:1 molar ratio at RT affords the corresponding sulfate salts [C 12 H 20 N 2 ][HSO 4 ] 2 ·H 2 O (SI) and [C 12 H 20 N 2 ][HSO 4 ] 2 (SII). These compounds have been characterized by X-ray diffraction, thermal analysis and spectroscopic investigations (IR and NMR). In the atomic arrangement of (SI) the HSO 4 − anions are associated by pairs linked to the water molecules forming corrugated ribbons, while in the (SII) structure, the pairs of the HSO 4 − anions form corrugated chains. Solid-state 13 C and 15 N CP-MAS NMR spectroscopies are in agreement with the X-ray structure. The vibrational absorption bands were identified by infrared spectroscopy. NMR peaks were attributed with the aid of DFT calculations. The electronic properties such as HOMO and LUMO energies were determined. [ABSTRACT FROM AUTHOR]
- Published
- 2017
- Full Text
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29. Synthesis, structure and physicochemical characterization of the hybrid material [C6H16N2O]2 SnCl6·2Cl·2H2O.
- Author
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Belhaj Salah, S., Pereira da Silva, P.S., Lefebvre, F., Ben Nasr, C., Ammar, S., and Mrad, M.L.
- Subjects
- *
CRYSTAL structure , *SURFACE analysis , *TIN chlorides , *UNIT cell , *SPACE groups , *INTERMOLECULAR interactions - Abstract
The current study reports the chemical preparation, crystal structure, Hirshfeld surface analysis and spectroscopic characterization of the novel compound [C 6 H 16 N 2 O] 2 SnCl 6 ·2Cl·2H 2 O. This compound crystallizes in the triclinic system (space group P − 1, Z = 1) with the following unit cell dimensions: a = 7.9764(9), b = 8.2703(9), c = 12.1103(14)Å, α = 84.469(6), β = 75.679(6), and γ = 64.066(5)°. The structure was solved using 3093 independent reflections down to R = 0.020. The atomic arrangement shows alternation of organic and inorganic entities. The cohesion between these entities is ensured by N H…Cl and O H…Cl hydrogen bonds that build a three-dimensional network. The 3D Hirshfeld surfaces and the associated 2D fingerprint plots were investigated for intermolecular interactions. 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 IR and NMR bands. X-ray powder, XPS and UV spectrum have been carried out. The DSC profile shows that the title material exhibits dehydration at 339 K. [ABSTRACT FROM AUTHOR]
- Published
- 2017
- Full Text
- View/download PDF
30. Crystal structure, Hirshfeld surface and spectroscopic studies of the noncentrosymmetric Bi(III) halide complex: [C8H12N]3BiCl6.
- Author
-
Essid, M., Aloui, Z., Ferretti, V., Abid, S., Lefebvre, F., Rzaigui, M., and Nasr, C. Ben
- Subjects
- *
CRYSTAL structure , *POLYTYPIC transformations , *CRYSTALLOGRAPHY , *HALIDES , *SPECTRUM analysis - Abstract
A new organic–inorganic hybrid material with the formula [C 8 H 12 N] 3 BiCl 6 has been synthesized and characterized by spectroscopic techniques and single crystal X-ray structure determination. This compound crystallizes in the non-centrosymmetric space group Pna 2 1 of the orthorhombic system with crystallographic parameters a = 25.5620(2), b = 16.7170(5), c = 7.8840(4) Å, V = 3369.0(2) Å 3 and Z = 4. Its structure consists of discrete [BiCl 6 ] 3− anions, showing the distorted octahedral geometry, surrounded by three crystallographically independent 2-phenylethylammonium cations. The crystal packing is governed by the formation of a number of N–H⋯Cl hydrogen bonds arranged in a three-dimensional network. Crystal structure analysis supported with the Hirshfeld surface and fingerprint plots enabled the identification of the significant intermolecular interactions. The 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray structure. The optical properties of [C 8 H 12 N] 3 BiCl 6 were investigated by UV–Vis and luminescence spectroscopy. The differential scanning calorimetry (DSC) revealed that the title compound is stable up to 210 °C. [ABSTRACT FROM AUTHOR]
- Published
- 2017
- Full Text
- View/download PDF
31. Structural, crystal structure, Hirshfeld surface analysis and physicochemical studies of a new chlorocadmate template by 1-(2-hydroxyethyl)piperazine.
- Author
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Soudani, S., Jeanneau, E., Jelsch, C., Lefebvre, F., and Ben Nasr, C.
- Subjects
- *
PIPERAZINE , *CRYSTAL structure , *CHEMICAL templates , *SURFACE chemistry , *HYDROGEN bonding - Abstract
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]
- Published
- 2016
- Full Text
- View/download PDF
32. Synthesis, crystal structure, and spectroscopic studies of organic–inorganic hybrid material: [C7H10NO]2BiBr5.
- Author
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Aloui, Z., Ferretti, V., Abid, S., Lefebvre, F., Rzaigui, M., and Ben Nasr, C.
- Subjects
- *
CRYSTAL structure , *ORGANIC compounds , *BISMUTH compounds , *CHEMICAL synthesis , *SINGLE crystals , *X-ray diffraction , *TEMPERATURE effect - Abstract
A novel organic–inorganic hybrid compound, 2-methoxyanilinium pentabromobismuthate(III), [C 7 H 10 NO] 2 BiBr 5 , was synthesized and its structure determined by means of single crystal X-ray diffraction studies at room temperature. The molecule crystallizes in the orthorhombic C222 1 space group with cell parameters a = 11.8870(4), b = 23.4775(8), c = 8.1232(3) Å , V = 2267.0(1) Å 3 and four molecules in the unit cell. The structure of the title compound is built up from one-dimensional [BiBr 5 ] 2n− n polyanionic zig-zag chains composed of deformed BiBr 6 octahedra share Br(2) apex and 2-methoxyanilinium cations. The assignment of the vibrational bands was based on comparison with vibrational mode frequencies of homologous compounds. Theoretical calculations were performed using density functional theory (DFT) for studying the vibrational spectrum of the investigated molecule in its ground state. The 13 C CP-MAS NMR spectrum is in agreement with the X-ray structure. [ABSTRACT FROM AUTHOR]
- Published
- 2016
- Full Text
- View/download PDF
33. A Hirshfeld surface analysis, crystal structure and physicochemical studies of zwitterionic complex: 1-(2-hydroxyethyl)piperaziniumtrichlorozincate (II).
- Author
-
Soudani, S., Jeanneau, E., Jelsch, C., Lefebvre, F., and Ben Nasr, C.
- Subjects
- *
SURFACE analysis , *CRYSTAL structure , *POLYZWITTERIONS , *HYDROXYETHYL starch , *INFRARED spectroscopy - Abstract
The synthesis, crystal structure and spectroscopic characterization of the novel 1-(2-hydroxyethyl)piperaziniumtrichlorozincate(II) zwitterionic complex are reported. In the atomic arrangement, the ZnCl 3 N entities, grouped in pairs, are deployed in rows along the a -axis to form layers parallel to the ( a , c ) plane. The organic molecules 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 networks. Intermolecular interactions were investigated by Hirshfeld surfaces. 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]
- Published
- 2016
- Full Text
- View/download PDF
34. Synthesis, structural characterization, Hirshfeld surface analysis and spectroscopic studies of cadmium (II) chloride complex with 4-hydroxy-1-methylpiperidine.
- Author
-
Soudani, S., Ferretti, V., Jelsch, C., Lefebvre, F., and Nasr, C. Ben
- Subjects
- *
CADMIUM chloride , *SURFACE analysis , *HYDROGEN bonding , *CRYSTAL structure , *INTERMOLECULAR interactions - Abstract
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]
- Published
- 2016
- Full Text
- View/download PDF
35. Synthesis, structural and vibrational investigation for Tetrakis(2,6-diethylanilinium) decabromodibismuthate(III) hexahydrate [C10H16N]4Bi2Br10·6H2O.
- Author
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Aloui, Z., Ferretti, V., Abid, S., Lefebvre, F., Rzaigui, M., and Ben Nasr, C.
- Subjects
- *
CATIONS , *ELECTRONS , *DENSITY functional theory , *ELECTRIC distortion , *INFRARED spectroscopy - Abstract
The new organic–inorganic compound, Tetrakis(2,6-diethylanilinium) decabromodibismuthate(III) hexahydrate, has been synthesized and characterized by single-crystal X-ray diffraction at room temperature. It crystallizes in the monoclinic system (P2 1 /c space group). The structure consists of discrete dinuclear [Bi 2 Br 10 ] 4− anions, [C 10 H 16 N] + cations and water molecules. The organic part consists of two organic cations which orient their two amine groups to the neighboring anions. The inorganic entity is made up by [Bi 2 Br 10 ] 4− dimers composed of two equivalent irregular octahedra sharing one edge. The water molecules are sandwiched between the [Bi 2 Br 10 ] 4− anions and the neighboring [C 10 H 16 N] + cations. The crystal packing is governed by N(O)–H⋯Br and N–H⋯O W hydrogen bonds and π−π interactions to built a three dimensional network. The nature of the inorganic polyhedra distortion, which can be attributed to the stereo-activity of the Bi(III) lone electron pair, has been studied. The infrared and NMR spectra were calculated by Density Functional Theory (DFT) using the B3LYP method with the 6–311++G** basis set. A good consistency was found between the calculated and experimental data. The vibrational absorption bands were identified by infrared spectroscopy. [ABSTRACT FROM AUTHOR]
- Published
- 2016
- Full Text
- View/download PDF
36. Structural and spectroscopic studies of bis(2-amino-6-methylpyrimidinium-4-(1H)-one) aquapentachloridoindate(III) monohydrate.
- Author
-
Nbili, W., Kaabi, K., Ferretti, V., Lefebvre, F., and Ben Nasr, C.
- Subjects
- *
HYDRATE analysis , *CRYSTALLIZATION , *DENSITY functional theory , *CRYSTAL structure , *NUCLEAR magnetic resonance spectroscopy - Abstract
Physico-chemical properties of a new organic indate(III) (C 5 H 8 N 3 O) 2 [InCl 5 (H 2 O)].H 2 O are discussed on the basis of its X-ray crystal structure investigation. The asymmetric unit includes two independent 2-amino-6-methylpyrimidinium-4-(1 H )-one cations, one aquapentachloridoindate dianion, and one crystallization water molecule. The In III ion is in a slightly distorted octahedral coordination geometry. In the crystal structure, the dimeric species formed by two metal complexes and two water molecules are connected to the 2-amino-6-methylpyrimidin-4-1 H )-one cations through N–H⋯Cl hydrogen bonds to build 2D sheets parallel to the (b, a + c) plane. 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 attributions of NMR signals and of the IR bands. [ABSTRACT FROM AUTHOR]
- Published
- 2015
- Full Text
- View/download PDF
37. Crystal structure, Hirshfeld surface analysis, quantum mechanical study and spectroscopic studies of noncentrosymmetric (S)nicotiniumtrichloridozincate monohydrate complex.
- Author
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Soudani, S., Ferretti, V., Jelsch, C., Lefebvre, F., and Ben Nasr, C.
- Subjects
- *
CRYSTAL structure , *SURFACE analysis , *QUANTUM mechanics , *MECHANICS (Physics) , *CRYSTALLOGRAPHY - Abstract
The chemical preparation, crystal structure and spectroscopic characterization of the novel noncentrosymmetric (S)nicotiniumtrichloridozincate monohydrate complex are reported. The atomic arrangement can be described as built up by chains of ZnNCl 3 tetrahedra and water molecules, interconnected via O–H…Cl hydrogen bonds. The organic entities are inserted between these chains through C–H…Cl and N–H…Cl hydrogen bonds. The 3D Hirshfeld surfaces and the associated 2D fingerprint plots were investigated for intermolecular interactions. 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. [ABSTRACT FROM AUTHOR]
- Published
- 2015
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38. Synthesis, crystal structure and vibrational spectroscopic analysis of tetrakis(5-amino-1-H-1,2,4-triazol-4-ium) decachlorodibismuthate(III):[C2H5N4]4Bi2Cl10.
- Author
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Aloui, Z., Ferretti, V., Abid, S., Lefebvre, F., Rzaigui, M., and Nasr, C. Ben
- Subjects
- *
CHEMICAL synthesis , *CRYSTAL structure , *VIBRATIONAL spectra , *MONOCLINIC crystal system , *SPACE groups , *ANION analysis - Abstract
Physico-chemical properties of a new organic bismuthate(III), [C 2 H 5 N 4 ] 4 Bi 2 Cl 10 are discussed on the basis of X-ray crystal structure investigation. This compound crystallizes in the monoclinic space group C 2/ c , with a = 16.3622(3), b = 12.7941(2), c = 14.8178(2) Å, β = 98.5660(10)°, V = 3067.35(8) Å 3 and Z = 4. The crystal structure consists of discrete binuclear [Bi 2 Cl 10 ] 4− anions and 3-amino-1-H-1,2,4-triazolium cations. The crystal packing is governed by strong N H⋯N and weak N H⋯Cl hydrogen bonds and Π–Π stacking interactions to form three-dimensional network. The 13 C CP-MAS NMR spectrum is in agreement with the X-ray structure. The infrared study confirms the presence of the organic cation [C 2 H 5 N 4 ] + . The vibrational absorption bands were identified by infrared spectroscopy and DFT calculations allowed their attribution. [ABSTRACT FROM AUTHOR]
- Published
- 2015
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39. Synthesis, crystal structure and characterization of a new organic–inorganic hybrid material: [C6H16N2O]SbCl5.
- Author
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Aloui, Z., Ferretti, V., Abid, S., Rzaigui, M., Lefebvre, F., and Ben Nasr, C.
- Subjects
- *
CRYSTAL structure , *CHEMICAL synthesis , *X-ray diffraction , *NUCLEAR magnetic resonance spectroscopy , *CRYSTALLIZATION , *RAMAN spectroscopy , *MOLECULAR structure - Abstract
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]
- Published
- 2015
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40. Synthesis, crystal structure and antibacterial studies of 2,4,6-trimetoxybenzaldehyde based dihydropyrimidine derivatives.
- Author
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Huseynzada, A.E., Jelsch, C., Akhundzada, H.N., Soudani, S., Nasr, C. Ben, Doria, F., Hasanova, U.A., Freccero, M., Gakhramanova, Z., Ganbarov, K., and Najafov, B.
- Subjects
- *
CRYSTAL structure , *CONFORMATIONAL analysis , *MOLECULAR crystals , *SURFACE analysis , *AMMONIUM nitrate , *SILVER nanoparticles , *MAGNETIC nanoparticles - Abstract
• New dihydropyrimidines. • Conformational analysis. • Hirshfeld surface analysis. We report herein the synthesis of new derivatives of dihydropyrimidine on the basis of 2,4,6-trimetoxybenzaldehyde , which was further regioselectively oxidized in the presence of cerium ammonium nitrate (CAN) with the formation of 5-acetyl-6-methyl-4-(2,4,6-trimethoxyphenyl)pyrimidin-2(1H)-one. The structures of both novel compounds were investigated by NMR, mass spectroscopy methods. The structure of the dihydropyrimidine compound 4 was also investigated by X-ray single crystal diffraction method. In order to understand the molecular interactions in its crystal packing, the Hirshfeld surface and contacts enrichment analyses were performed. Biological activities of the synthesized compounds were studied against gram-negative A. baumanii, E. coli, P. aeruginosa and K. pneumoniae and gram-positive S. aureus bacteria. [Display omitted] [ABSTRACT FROM AUTHOR]
- Published
- 2021
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41. Synthesis, crystal structure and antibacterial properties of 6-methyl-2-oxo-4-(quinolin-2-yl)-1,2,3,4-tetrahydropyrimidine-5-carboxylate.
- Author
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Huseynzada, A.E., Jelsch, C., Akhundzada, H.N., Soudani, S., Ben Nasr, C., Doria, F., Hasanova, U.A., and Freccero, M.
- Subjects
- *
CRYSTAL structure , *SURFACE analysis , *HYDROGEN bonding , *SINGLE crystals , *MOLECULAR interactions , *STACKING interactions - Abstract
The synthesis and investigation of a new biologically active derivative of dihydropyrimidine are reported. The structure of the synthesized compound was investigated by X-ray single crystal diffraction method. In order to understand the molecular interactions, the Hirshfeld surface and contacts enrichment analyses were performed. The crystal packing is mainly stabilized by strong N–H⋯O hydrogen bonds and aromatic cycle stacking. Among the different types of oxygen atoms, the most electronegative had the highest propensity to form H-bonds. Biological activity of the synthesized compound was studied against E.coli , P. aeruginosa and S. aureus bacteria. Image 1 • New Biginelli compound. • Conformational analysis. • Hirshfeld surface analysis. [ABSTRACT FROM AUTHOR]
- Published
- 2020
- Full Text
- View/download PDF
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