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Two new mononuclear complexes, [Cu2Cl1.23(NO3)0.77(Ampy)4(H2O)4](NO3)2·4H2O (I) and [CdI2(Ampy)2] (II) (Ampy = 4-amino-6-methoxypyrimidine) have been synthesized and characterized by single crystal X-ray diffraction studies (CCDC nos. 2023331 (I), 2023331 (II)) at 295 K for (I) and 100 K for (II). The structure of the Cu(II) complex shows that the Cu(II) central atom is five-coordinated with a distorted square pyramidal geometry. In compound (II) the Cd(II) cations are tetracoordinated with a distorted tetrahedral fashion. Intermolecular interactions were investigated by Hirshfeld surfaces. Electronic properties such as HOMO and LUMO energies were derived. [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]

• 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]

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]

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]

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]

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]

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]

1-Ethylpiperazinediium pentachloroantimonate (III) monohydrate, C 6 H 16 N 2 SbCl 5 ·H 2 O, has been synthesized by the reaction of antimony trioxide (Sb 2 O 3 ) and 1-ethylpiperazine in an aqueous solution of hydrochloric acid. The structure crystallizes in orthorhombic system, in the non-centrosymmetric space group Pca 2 1 and consists of isolated [C 6 H 16 N 2 ] 2+ cations, square pyramidal [SbCl 5 ] 2− anions and lattice water molecules. O H⋯Cl hydrogen bonds link the [SbCl 5 ] 2− anions and water molecules to form double chains stretching along the [101] direction. The chains in turn are linked to the organic cations via N H⋯Cl, C H⋯Cl, C H⋯O and N H⋯O hydrogen bonds to form a three-dimensional network. This structure presents an example of a general square pyramidal complex ion containing a stereo-chemically active lone pair of electrons. Solid state 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray structure, and vibrational absorption bands were identified by infrared spectroscopy. DFT calculations allowed the attribution of the NMR peaks and IR absorption bands. The interactions variability of the two independent cations and ten chloride atoms is analyzed via Hirshfeld surface analysis. [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 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]

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]

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]

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]