Search

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]

(C6H18N3)4[CuCl5]2[CuCl4]3·1.42H2O 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]

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]

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

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

Physicochemical properties of a new dihydrogenmonophosphate [2-NH2-6-CH3-C4H3N2O]2(H2PO4)2 are described on the basis of X-ray crystal structure investigation. This compound crystallizes in the triclinic space group P-1. The unit cell parameters are: a = 7.667(3) Å, b = 8.204(5) Å, c = 14.761(6) Å, α = 98.85(4)°, β = 99.23(3)°, γ = 90.50(4)°, V = 905.0 Å3, and Z = 2. The crystal structure was solved and refined to R = 0.037, using 4351 independent reflections. The atomic arrangement of this compound is built up by (H2PO4)nn - chains. Each chain aggregates with organic molecules to form an open framework architecture through hydrogen bond interactions. The structure includes four types of hydrogen bonds. The first one, O─H─O, links the H2PO4 groups to form (H2PO4)nn - infinite inorganic chains parallel to the a axis. The three other types, O─H─O(carbonylic), N─H─O(carbonylic), and N─H─O, assemble the inorganic chains so as to build up a three-dimensional arrangement. This compound has also been investigated by IR, and solid-state 13C and 31P MAS NMR spectroscopies combined to ab initio calculations. [ABSTRACT FROM AUTHOR]

Chemical preparation, crystal structure, thermal analysis, IR absorption, and NMR studies are given for a new hybrid organic-inorganic compound, the (2,6-dimethyanilinium) dihydrogenophosphate monohydrate [C8H12N]H2PO4·H2O. This compound crystallizes in a triclinic P=1 unit-cell, with a = 7.392(5) Å, b = 8.323(3) Å, c = 10.306(5) Å, α = 95.769 (4)°, β = 102.642 (3)°, γ = 113.498(2)°, V = 554.88(5) Å3, and Z = 2. Its crystal structure is determined and refined to R = 0.040 with 1942 independent reflections. The atomic arrangement can be described by inorganic layers built by H2PO4- anions, and H2O molecules with which the organic molecules perform different interactions to form a stable 3D network. Solid state 31P and 13C CP-MAS-NMR spectroscopies are in agreement with the X-ray structure. [ABSTRACT FROM AUTHOR]

Chemical preparation, crystal structure, and NMR spectroscopy of a new monophosphate with 2,3-dichloroanilinium cation are given. This new compound crystallizes in the monoclinic system, with the space group P21/n and the following parameters: a = 11.031 (6), b = 6.007(3), c = 15.227(2) Å β = 98.98(4), V = 996.73(3) Å3, and Z = 4. The crystal structure has been determined and refined to R = 0.048 and Rw = 0.1317 using 2030 independent reflections. The structure can be described as clusters that aggregate with six organic molecules, resulting in a (1 0 [image omitted]) two dimensional sheet, and formation of arrays in three dimensions, via various interactions (H-bonds, electrostatic, Van der Waals). In addition, C─Cl...π interactions are observed as a consequence of the chlorine atom being flanked by two phenyl rings of the neighboring molecules. The structure has also short intermolecular Cl...Cl interactions [type I, Cl...Cl = 3.380(1) Å, C─Cl...Cl' = 132.26°]. This compound has also been investigated by IR, thermal analysis, and solid-state 13C and 31P MAS NMR spectroscopy combined with Ab Initio calculations. [ABSTRACT FROM AUTHOR]

The crystal synthesis and structure of a new organic dihydrogenmophosphate [1-(2,3-(CH3)2-C6H3)C4H10N2]H2PO4 are reported. This compound crystallizes in the monoclinic P21/n with a = 7.545(2) Å, b = 26.315(4) Å, c = 7.798(6) Å, β = 115.01(4)°, V = 1403.0(1) Å3, and Z = 4. Crystal structure was solved and refined to R = 0.046, using 1981 independent reflections. It can be described by inorganic layers including the H2PO4- anions and the NH2+ ammonium groups parallel to (a, c) planes and situated at y = 1/4 and y = 3/4. The interlayer spacing is occupied by the organic molecules which perform different interactions around the 3D network cohesion. A characterization of this compound by solid-state 13C and 31P MAS NMR and ATG is also reported. [ABSTRACT FROM AUTHOR]

Abstract: A new organic templated metallophosphate, [Zn(H2PO4)2(HPO4)][C7H17N2] (denoted in the following ZnP-AMEP), has been synthesized hydrothermally using 2-aminomethyl,1-ethylpyrrolidine (AMEP) as a structure-directing agent. The structure, determined by single crystal X-ray diffraction, exhibits a parallel arrangement (along the direction) of infinite chains, built from (Zn2P2O12) four-membered rings sharing ZnO4 tetrahedra, interconnected together by strong hydrogen bonds to form a sheet-like architecture and with chains of extending along [100] at y =1/2 to form a 3D anionic network. To the best of our knowledge, the compound ZnP-AMEP represents the first organic templated metallophosphate in which the four-membered rings interact with chains of dihydrogenophosphate. Intra-chain and inter-chain P–OH⋯O hydrogen bonds help to establish the crystal packing and form apertures, wherein the amine molecules are located. Similarities and differences with other organic templated metallophosphates are briefly discussed for the title compound. Ab initio calculations allow the attribution of phosphorus and carbon solid-state NMR signals to the independent crystallographic sites and to the various atoms of the organic groups. Additional characterizations of the compound have also been performed by IR spectroscopy and TG–DTA analyses. [Copyright &y& Elsevier]

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]

Abstract: A new two-dimensional zinc phosphate, [Zn2.5(HPO4)2(PO4)][C6N2H10]·5H2O (denoted in the following as ZnP-2AMP), with alternating inorganic and organic layers has been synthesized hydrothermally using 2-aminomethylpyridine (2AMP) as the structure-directing agent. This compound represents the first structure with a Zn/P ratio of 5/6. The structure of this compound, determined by single crystal X-ray diffraction, consists of anionic parallel [Zn2.5(HPO4)2(PO4)(H2O)2]2− sheets built up from ZnO4, ZnO2(H2O)4, PO4 and HPO4, alternating with thick slabs of organic molecules (C6H10N2)2+ and water molecules, the octahedral ZnO2(H2O)4 being enclosed in each [4682122] cage. The organic cations are linked to the anionic sheets through hydrogen bonds. Solid-state 13C and 31P MAS NMR spectroscopies are in agreement with the X-ray structure. Ab initio calculations allow the partial attribution of phosphorus and carbon signals to the independent crystallographic sites and to the various atoms of the organic groups. Additional characterization of the compound has also been performed by IR spectroscopy and TG-DTA analyses. [Copyright &y& Elsevier]

Along a systematic study of open-framework materials aiming at producing new molecular sieves, we characterized a new zincophosphate Zn(HPO 4 )Cl[C 4 H 10 N]. It was synthesized under mild conditions (r.t.) in the presence of pyrrolidinium as an organic-structure directing agent. The structure of this compound, determinated by single crystal X-ray diffraction, consists of anionic parallel [Zn(HPO 4 )Cl] - sheets alternating with thick slabs of organic molecules (C 4 H 10 N) + . These latters are linked to the anionic sheets through hydrogen bonds. Zn(HPO 4 )Cl[C 4 H 10 N] crystallizes in the monoclinic system and the space group C2/c (No. 9) with cell parameters a = 24,83(9), b = 9,258(5), c = 8.778(3), β = 110,45(4), Z = 8, V = 1891.0(14) Åt 3 , R = 0.045, and R w = 0.07. Solid state 31 P and 13 C MAS NMR spectroscopies are in agreement with the X-ray structure. [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]

Abstract: Chemical preparation, crystal structure and NMR spectroscopy of a new organic cation p-phenylenediammonium monophosphate [p-NH3C6H4NH3][H2PO4]2 are presented. This new compound crystallizes in the orthorhombic system, with the space group Pnma and the following parameters: a =7.970 (2)Å; b =22.770 (7)Å; c =7.000 (7)Å, V =1270.3 (11)Å3, Z =4 and D x =1.590gcm−3. The crystal structure has been determined and refined to R =0.043 and R (w) =0.057 using 2623 independent reflections. The structural arrangement can be described as inorganic layers of (H8P4O16)4− units, parallel to (a, c) planes. The organic groups (p-H3NC6H4NH3)2+are anchored between the phosphoric layers to form a three-dimensional infinite network. This compound is also investigated by IR and solid-state 1H, 13C and 31P MAS NMR spectroscopies. The ab initio method is used in the calculation of chemical shifts. [Copyright &y& Elsevier]

Crystal growth and characterization by X-ray diffraction and NMR spectroscopy of a new p-phenylenediamonium diphosphate [p-NH 3 C 6 H 4 NH 3 ] H 2 P 2 O 7 are reported. This compound crystallizes in a triclinic unit cell P1 with the parameters a = 7.130(3), b = 9.047(3), c = 9.350(2) Å, α = 133.44(2)°, β = 95.02(2)°, γ = 107.11(4)°, Z = 2, V = 514.3(15) Å 3 , and D x = 1.848 g.cm - 3 . The crystal structure has been solved and refined to R = 0.0273, using 3678 independent reflections. The atomic arrangement is build up by infinite ribbons of [H 2 P 2 O 7 ] 2- anions, extending along the a-direction at y = 1/2. Between these ribbons are located the p-phenylenediammonium entities, which form hydrogen bonds N─H...O with some external oxygen atoms of phosphoric groups. Crystallographic results are correlated with that of the solid state 13 C and 31 P MAS NMR spectroscopy. [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]

A new adduct 4-benzyl piperidinium dihydrogenphosphate monophosphoric acid [C 12 H 16 NH 2 ] 2 (H 2 PO 4 ) 2 H 3 PO 4 , has been prepared and analyzed by X-ray diffraction. This adduct compound cristallizes in the monoclinic system, with the acentric space group P2 1 and the following unit-cell parameters: a = 13.103(3), b = 8.737(4), c = 13.620(3) Å, β = 92.38(2)°, Z = 2, and V = 1557.8(7) Å[3]. The crystal structure has been solved and refined to R = 0.059 and R (w) = 0.069 using 3306 independent reflections. Its structure can be described as inorganic layers of H 3 PO 4 and H 2 PO 4 - entities separated by organic molecules. In this atomic arrangement, H-bonds between the different species play an important role in the tridimensionnel network cohesion. Solid-state 13 C and 31 P MAS NMR spectroscopies are in agreement with the X-ray structure. Ab initio calculations allow the attribution of phosphorus and carbon signals to the independent crystallographic sites and to the various atoms of the organic groups. [ABSTRACT FROM AUTHOR]

A new zincophosphate [H3N(CH2)2NH3]0.5Zn (HPO4)Cl, was obtained at room temperature from a starting mixture of ZnCl2, H3PO4, H2O, and ethylene-diamine. Its unit cell is tricline P-1 (No. 2) with parameters a = 7.709(2) Å, b = 8.479(2) Å c = 5.175(2) Å, α = 104.99(3), β = 107.41(4), γ = 87.34(2), Z = 2, and V = 311.6(2) ų. Its structure is resolved to R = 0.024, Rw = 0.037. The backbone of the title compound is a linear heteroanion built by PO4 and ZnO3Cl tetrahedra assembled to farm four member rings themselves interconnected by sharing common oxygen atoms. Hydrogen bonds O--H…O established between these chains connect them as to build infinite planes. The organic entities, located between these planes form the 3D cohesion through N--H…O or N--H…Cl hydrogen bonds. [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]

Chemical preparation and characterization by X-ray diffraction, IR, and NMR spectroscopies and thermal analysis of a new o-ethylphenylammonium triphosphate [2-C2H5C6H4NH3]3H2P3O10 are reported. This compound crystallizes in a monoclinic unit cell P21/n with the parameters: a=17.670(1)Å, b=8.558(8)Å, c=20.100(2) Å, β=100.39(6)°, Z=4, and V=2990(4) Å3. Crystal structure has been solved and refined to R=0.041 using 6857 independent reflections. In this atomic arrangement, layers built by H2P3O103- groups are developed along (1 0 -1) direction. Between these layers are located the o-ethylphenylammonium entities which form hydrogen bonds with some external oxygen atoms of phosphoric groups. [Copyright &y& Elsevier]

The new organic salt 2,5-di-tert-butylanilinuim chloride [C14H24N]Cl was obtained from an aqueous solution by slow evaporation at room temperature and characterized by various techniques, mainly crystal X-ray diffraction. This title compound crystallized in the monoclinic system with space group P21/c. The atomic arrangement can be described by hybrid pillars running along the c-axis. The crystal packing is stabilized by N–H...Cl and C–H...Cl hydrogen bonds to form a three-dimensional network. The intermolecular interactions were investigated by Hirshfeld surfaces and the associated 2D fingerprint plots. Furthermore, the vibrational absorption bands were identified by IR spectroscopy and were also calculated by density functional theory (DFT). The optical property of the crystal was studied using solid-state UV–visible and photoluminescence spectroscopy. The study also presents the results of the DTA thermal analysis. [ABSTRACT FROM AUTHOR]

A series of nitrogen‐doped TiO2 were prepared through a simple sol‐solvothermal method. The catalysts were characterized by BET, XRD, SEM‐EDS, Raman, XPS, FTIR, UV‐Vis, etc. The results show that N−TiO2 photocatalyst has a larger specific surface area, stable anatase phase, and narrow forbidden band energy (3.17–3.24 eV). The N‐doped TiO2 has more oxygen vacancies (OVs) than pure TiO2, as confirmed by results such as XPS and ESR. The photocatalytic evaluation results show that the decolorization of methyl orange reached 99.03 % over the 3 % N‐doped TiO2, which is 40 % higher than that of pure TiO2. Meanwhile, 3 % N‐doped TiO2 exhibited a faster MO mineralisation rate than TiO2. After repeatedly used for 5 times, the photocatalyst 3‐N−TiO2 still showed high activity in the degradation of MO. The improvement of the visible light performance of the N−TiO2 photocatalyst could be attributed to the introduction of N in TiO2 to generate new N 2p energy levels and rich OVs. [ABSTRACT FROM AUTHOR]

Slow evaporation, at ambient temperature, reaction has produced a novel polymeric mercury (II) hybrid, ethylpyrazinium-tridecachloro-mercurate(II) monohydrate (C6H9N2)[Hg6Cl13]·H2O. The atomic structure can be characterized as layers of [Hg6Cl13]– anions, water molecules, and nitrogen atoms linked by O–H...Cl hydrogen bonds, with the organic cations positioned among the inorganic layers and linked by N–H...O and C–H...Cl H-Bonds. Hydrogen bond strength and inter-contacts quantification were discussed using Hirshfeld surface analysis. It shows that 46.1% of the crystal structure's stability is due to hydrogen bonding interaction of type H...Cl/Cl...H. The SEM/EDX analyses were carried out. Through the use of infrared spectroscopy, the vibrational characteristics of the material were studied and the assignments were accomplished by help of DFT calculations. The electrical properties, such as HOMO and LUMO levels, have been described. Finally, TG–DTA analysis was used to investigate the thermal behavior. [ABSTRACT FROM AUTHOR]

A novel organic–inorganic hybrid compound, named (1-phenylpiperazinium) trihydrogen triphosphate, with the formula (C10H15N2)2H3P3O10 has been obtained by low speed of evaporation of a mixture of an alcoholic solution of 1-phenylpiperazine and triphosphoric acid H5P3O10 at room temperature after using the ion exchange chemical procedure. To carry out a detailed crystallographic structure analysis, single-crystal X-ray diffraction has been reported. In the molecular arrangement, the different entities are held together through N–H...O, O–H...O, and C-H...O hydrogen bonds, building up a three-dimensional packing. Powder X-ray diffraction analysis is acquired to confirm the purity of the product. The nature and the proportion of intermolecular interactions were investigated by Hirshfeld surface analysis. In order to support the experimental results, a density functional theory (DFT) calculation was performed, using the Becke-3-parameter-Lee–Yang–Parr (B3LYP) function with LANL2DZ basis set, and the data indicate much agreement between the experimental and the theoretical results. Thus, the physicochemical properties were studied employing a variety of techniques (FTIR, NMR, UV–visible, and photoluminescence). To get an insight of the possible employment of the present material in biology, cell viability assays were performed. [ABSTRACT FROM AUTHOR]

A new (C8H12N)2SnCl6.2H2O was isolated from a slow evaporation reaction at ambient temperature. The title compound crystallizes in the triclinic/P 1 ¯ space group, as determined by X-ray diffraction (XRD). The anions [SnCl6]2−and the H2O molecules are connected via O–H...Cl H–bonds to build up inorganic sheets extending on the plane (a, b) at z = 0 and the (C8H12N)+ cations are inserted between two successive layers and connect them through multiple H-bonds to make an infinite 3D structure. The intermolecular interactions were fully characterized using the Hirshfeld surface analysis, while the associated 2D fingerprints plots were generated to understand their contribution in building the solid-state architecture within the structure. Powder XRD was used to verify the purity of the crystalline sample phase. FT-IR and CP-MAS 13C NMR spectroscopy were used to investigate the vibrational modes and NMR characteristics. Moreover, the optical properties were investigated. The DFT calculations were utilized to explain these findings and determine the gap energy using the HOMO and LUMO energies. In addition, the XPS analysis was reported to analyze the surface chemistry. Finally, the thermal analysis by TG/DTA were performed, to determine its thermal behavior. [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]

Abstract: The synthesis and structure of a new adduct with the [2-NH2-6-CH3- C4H3N2O]2HPO4 formula is described. This compound crystallizes in the triclinic space group . The unit cell parameters are: a =7.679(1)Å, b =9.883(2)Å, c =10.217(3)Å, α =83.36(2)°, β =79.48(5)°, γ =80.34(4)°, V =748.7(1)Å3, and Z =2. The crystal structure was solved and refined to R =0.037, using 2241 independent reflections. The atomic arrangement of this compound is built up by (H4P2O8)2− dimers. Each dimer aggregates with organic molecules to form an open framework architecture like through hydrogen bond interactions. Solid-state 13C and 31P MAS NMR spectroscopies are in agreement with the X-ray structure. [Copyright &y& Elsevier]

Abstract: A chlorozincophosphate of the composition Zn(HPO4)Cl·[C4H10NO] has been synthesised under mild condition water medium in the presence of morpholine as organic template. Its unit cell is monoclinic P2 1/a with parameters a =8.655(6)Å, b =9.302(5)Å, c =12.180(5)Å, β =101.10(4)°, Z =4 and V =962.1(9)Å3. The structure was determinated by single crystal X-ray diffraction. The structure involves a network of ZnO3Cl and PO3(OH) tetrahedra forming macroanionic inorganic layers with four- and eight-membered rings. Charge balance is achieved by the protonated amine which is trapped in the interlayers space and interacts with the organic framework through hydrogen bonding. Solid state 31P and 13C MAS-NMR spectroscopies are in agreement with the X-ray structure. [Copyright &y& Elsevier]

Chemical preparation, crystal structure, calorimetric, and spectroscopic investigations are given for a new organic-cation dihydrogenomonophosphate, (4-C2H5C6H4NH3)H2PO4 in the solid state. This compound crystallizes in the orthorhombic space group Pbca with the following unit cell parameters: a=8.286(3) A˚, b=9.660(2) A˚, c=24.876(4) A˚, Z=8, V=1991.2(7) A˚3, and DX=1.442 g cm−3. Crystal structure was solved with a final R=0.054 for 3305 independent reflections. The atomic arrangement coaled described as H2PO4− layers between which are located the 4-ethylanilinium cations. [Copyright &y& Elsevier]

The new organic–inorganic hybrid material (C6H7N2S)2[SbCl4]Cl was synthesized by slow evaporation method and characterized by single-crystal X-ray diffraction, infrared absorption, Hirshfeld surface analysis, optical absorption and photoluminescence measurements. The Centro symmetric compound crystallizes in the triclinic system of space group P 1 ¯ with two formula units cell (Z = 2).The crystal structure is composed of a discrete [SbCl4]− anion and two isolated chloride Cl− anions which carried the same negative charge to balance the total charge of this compound surrounded by the 4 pyridiniumethioamide cations. Organic and inorganic parts which are linked by means of hydrogen bonding contacts N–H···Cl with N···Cl length are varied in the range of 3.221–3.456 Å to form a Zero-dimensional network. The infrared study performed at room temperature charge in the 4000–400 cm−1 frequency regions confirms the existence of the organic cation [C6H7N2S]+ and that of the [SbCl4]− anion. The Photoluminescence spectrum exhibits a broad and strong band of luminescence located at 1.95 eV (635 nm), which can be even observed with the naked eye at room temperature and is due to exaction emission. The various intermolecular interactions of the two independent cations and six chloride atoms were examined via Hirshfeld surface analysis. [ABSTRACT FROM AUTHOR]

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]

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]

Nanosized titania has promising application in the field of photocatalysis, optical coating and solar cell. Metal alkoxides based sol-gel methodology is one of the established & extensively used route for the preparation of nano-titania. In present work, nanosized titania have been prepared through sol-gel transformation of synthesised and chemically modified metal complex using titanium(IV) isopropoxide (TTIP). Modifications of metal alkoxides with chelating ligands result in the controlled condensation of TTIP. Metal complexes of TTIP were chemically modified by various schiffs bases. Phase of nano-sized titania was confirmed by X-ray diffraction and Fourier transform infrared spectroscopy. Shape, size and surface morphology were examined using scanning electron microscopy and high-resolution transmission electron micsroscopy. Elemental composition was investigated by energy disperse X-ray analysis. The absorption spectra and thus optical band gap were determined using Ultraviolet and visible spectroscopy. [ABSTRACT FROM AUTHOR]

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]

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]

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

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]

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]

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]

Three samples of copper sulfide Cu2S thin film were deposited on polyimide substrate by spray pyrolysis using deposition temperature of 400°C and deposition time of about 45 min. One of the samples was left as deposited, another was heat treated, while the third was laser treated. The structural, surface morphological, optical, mechanical, and electrical properties of the films were investigated. X-ray diffraction (XRD) analysis showed that the copper sulfide films were close to copper-rich phase (Cu2S). Increased crystallite size after heat and laser treatment was confirmed by XRD analysis and scanning electron microscopy. Vickers hardness measurements showed that the samples’ hardness values were enhanced with increasing crystallite size, representing an inverse Hall-Petch (H-P) effect. The calculated optical bandgap of the treated films was lower than that of the deposited film. Finally, it was found that both heat and laser treatment enhanced the physical properties of the sprayed Cu2S films on polyimide substrate for use in solar energy applications. [ABSTRACT FROM AUTHOR]

A novel photocatalyst ZnBiErO4 was firstly synthesized by solid-state reaction method and its structural and photocatalytic properties were analyzed by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy and UV-Vis diffuse reflectance. The results demonstrated that ZnBiErO4 crystallized with tetragonal crystal structure with space group I41/A. The lattice parameters for ZnBiErO4 were proved to be a = b = 10.255738 Å and c = 9.938888 Å. The band gap of ZnBiErO4 was estimated to be about 1.69 eV. Compared with nitrogen doped TiO2, ZnBiErO4 showed excellent photocatalytic activities for degrading methyl blue during visible light irradiation. The photocatalytic degradation of methyl blue with ZnBiErO4 or N-doped TiO2 as catalyst followed the first-order reaction kinetics. Moreover, the apparent first-order rate constant of ZnBiErO4 or N-doped TiO2 was 0.01607 min−1 or 0.00435 min−1. The reduction of total organic carbon, formation of inorganic products, such as SO42− and NO3− and the evolution of CO2 revealed the continuous mineralization of methyl blue during the photocatalytic process. ZnBiErO4 photocatalyst had great potential to purify textile industry wastewater. [ABSTRACT FROM AUTHOR]

A novel hybrid compound, bis(4-methylanilinium)hexachlorostannate(IV) monohydrate, formulated as (C 7 H 10 N) 2 [SnCl 6 ]·H 2 O, has been prepared and characterized by powder and single crystal X-ray diffraction (XRD), Hirshfeld surface analysis, infrared spectroscopy (IR), optical study, differential thermal analysis(DTA) and X-ray photoelectron spectroscopy analysis (XPS). The title compound crystallizes in the monoclinic space group P 2 1 / c with a = 13.093(1)Å, b = 7.093(6)Å, c = 24.152(2)Å, β = 98.536(4)⁰ and V = 2218.4(4) Å 3 . Their crystal structure exhibits alternating inorganic layers parallel to the ( ab ) plane at z = n/2. The different entities, [SnCl 6 ] 2- , organic cations and water molecules, are connected via hydrogen bonds to form a three-dimensional network. The powder XRD data confirms the phase purity of the crystalline sample. The intermolecular interactions were investigated by Hirshfeld surfaces. The vibrational absorption bands were identified by IR spectroscopy and have been discussed. The optical properties of the crystal were studied by using optical absorption, UV–visible absorption and photoluminescence spectroscopy studies. The compound was also characterized by DTA to determine its thermal behavior with respect to the temperature. Finally, XPS technique is reported for analyzing the surface chemistry of this compound. [ABSTRACT FROM AUTHOR]

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]

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]

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]