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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]

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]

A new cyclohexaphosphate with the composition (C 6 H 7 ClN) 6 P 6 O 18 ·0.5(H 2 O) has been synthesized at room temperature in the presence of 4-chloroaniline as organic template and investigated by various physicochemical techniques. Its unit cell is triclinic P-1 with parameters a = 9.0054(8), b = 10.1053(9), c = 16.4454(14) Å, α = 100.476(7), β = 93.485(7), γ = 115.407(9) °, Z = 2 and V = 1313.0(2)Å 3 . The structure involves a network of inorganic parallel layers built up by P 6 O 18 6 − ring anions, NH 3 groups and water molecules. Charge balance is achieved by the protonated amine which is trapped in the interlayer space and interacts with the organic framework through strong hydrogen bonding. The 13 C, 15 N and 31 P 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]

The inorganic–organic hybrid compound (C 9 N 4 H 28 )Cd 7 (H 2 O) 2 Cl 18 · n H 2 O( n = 5.89) features an unusual cadmium chloride structure. The title complex adopts a layered structure consisting of double-chains and tetramers of [Cd ϕ 6 ] ( ϕ = Cl, O) octahedra. Crystallization water molecules and [C 9 H 28 N 4 ] 4+ tetracations are located in interstices of the successive corrugated layers. This compound has also been investigated by FT-IR and solid-state 13 C, 15 N CP-MAS and 2D 13 C-H NMR spectroscopies. [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]

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]

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]

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]

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]

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]

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]

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]

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]

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]

A new Cd(II) complex with the monodentate ligand 3-fluoroaniline, CdCl 2 (C 6 H 4 FNH 2 ) 2 , has been prepared and characterized by single crystal X-ray diffraction, solid state NMR, IR, Raman and UV–visible spectroscopies. In the complex, the Cd(II) ion is surrounded by four chlorine atoms and two nitrogen atoms, forming a chain of edge-charing octahedra spreading along the a -axis direction. These chains are interconnected via N H…Cl hydrogen bonds to form inorganic layers parallel to the (a, b) plane. The organic 3-fluorophenyl groups are inserted between these layers and are interconnected via C H…F hydrogen bonds to perform an infinite three-dimensional network. Intermolecular π–π stacking interactions between neighboring aromatic rings are also observed with a face-to-face distance of 3.6816 (4) Å. The 13 C and 19 F CP-MAS NMR spectra are in agreement with the X-ray structure. DFT calculations allow the attribution of the carbon peaks to the different atoms. The absorption bands of the Cd 2 Cl 4 N 2 units were identified by Raman spectroscopy. The solid-state UV–vis spectrum of the complex has been assigned to ligand and charge transfer transitions. [ABSTRACT FROM AUTHOR]

Synthesis and structures of two new isomeric organic amine perchlorate salts with the general formula (ClC 7 H 6 NH 3)ClO 4 ·H 2 O, 3-Cl-2-(CH 3)C 6 H 3 NH 3 ClO 4· H 2 O (I) and 5-Cl-2-(CH 3)C 6 H 3 NH 3 ClO 4· H 2 O (II) , are reported. They crystallize in the monoclinic system and are isostructural. In the crystal packing of these organic salts, ClO 4 − anions, water molecule and –NH 3 + groups have a layered organization around the z = 1/4 and z = 3/4 planes. The cations are linked to successive layers through hydrogen bonds to establish a three-dimensional network, involving the hydrogen atoms of the NH 3 groups. CP–MAS NMR, IR, UV–Visible spectroscopy and differential scanning calorimetry (DSC) were used to characterize these compounds. Image 1 • Structural study of two isostructural hydrates of isomeric organic amine perchlorates. • NMR signals are in full agreement with the crystallographic data. • DFT calculations allow the attribution of the experimental NMR lines. • Hirshfeld surface analysis was used to evaluate intermolecular contacts. • The electronic properties such as HOMO and LUMO energies were studied. [ABSTRACT FROM AUTHOR]