[NiCl2(C14H12N2)(H2O)] complex has been synthesized from nickel chloride hexahydrate (NiCl2·6H2O) and 2,9-dimethyl-1,10-phenanthroline (dmphen) as N,N-bidentate ligand. The synthesized complex was characterized by elemental analysis, infrared (IR) spectroscopy, ultraviolet-visible (UV-vis) spectroscopy and differential thermal/thermogravimetric analysis (TG/DTA). The complex was further confirmed by single crystal X-ray diffraction (XRD) as triclinic with space group P-1. The desired complex, subjected to thermal decomposition at low temperature of 400 ºC in an open atmosphere, revealed a novel and facile synthesis of pure NiO nanoparticles with uniform spherical particle; the structure of the NiO nanoparticles product was elucidated on the basis of Fourier transform infrared (FT-IR), UV-vis spectroscopy, TG/DTA, XRD, scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDXS) and transmission electron microscopy (TEM).
nickel(II) complex; thermal decomposition; 2,9-dimethyl-1,10-phenanthroline; nanoparticles
There are two independent molecules in the asymmetric unit of the title compound, C12H9ClN2OS, a Schiff base derived from hydrazide, in which the dihedral angles between the thiophene and benzene rings are 3.6 (3) and 7.3 (3)°. In the crystal, the two independent molecules are arranged about an approximate non-crystallographic inversion center and are connected by two N—H⋯O hydrogen bonds. Weak C—H⋯Cl contacts are also present. Conversely, there are neither significant aromatic stacking interactions nor contacts involving S atoms.
In the title racemic Schiff base ligand, C20H20Cl2N2, which was prepared by the condensation of 2-chlorobenzaldehyde and cyclohexane-1,2-diamine, the cyclohexane ring adopts a chair conformation and the dihedral angle between the aromatic rings of the 2-chlorophenyl substituent groups is 62.52 (8)°. In the structure, there are two short intramolecular methine C—H⋯Cl interactions [C⋯Cl = 3.066 (2) and 3.076 (3) Å], and in the crystal there are also weak intermolecular aromatic C—H⋯Cl [3.464 (3), 3.553 (3) and 3.600 (3) Å] and Cl⋯Cl [3.557 (3) and 3.891 (3) Å] contacts.
In the title compound, C15H14O3, the dihedral angle between the benzene rings is 75.85 (7)°. In the crystal, centrosymmetrically related molecules are weakly associated through pairs of interactions between a benzene ring and an O atom of the ester group [ring centroid⋯O = 3.952 (7) Å], and through pairs of interactions between the other benzene ring and an O atom of the phenoxy group [ring centroid⋯O = 3.912 (7) Å], giving chains extending along .
In the title compound, C14H16N4, the six-membered hexahydropyrimidine ring adopts a chair conformation. In the crystal, one of the two pyrimidine N atoms engages in N—H⋯N hydrogen bonding with one of the pyridine N atoms, generating a helical chain running along the c axis. The helical pitch is the length of the c axis.
The title compound, [HgCl2(C14H12N2)], consists of one 2,9-dimethyl-1,10-phenanthroline (dmphen) ligand chelating the HgII ion and two chloride ligands coordinating to the HgII ion, forming a distorted tetrahedral environment. The dmphen ligand is nearly planar (r.m.s. deviation = 0.0225 Å). The dihedral angle between the normal to the plane defined by the HgII atom and the two Cl atoms and the normal to the plane of the dmphen ring is 81.8 (1)°.
The asymmetric unit of the title compound, [Hg(SCN)2(C14H12N2)], contains two complex molecules in which the HgII atoms are both four-coordinated in a distorted tetrahedral configuration by two N atoms from a chelating 2,9-dimethyl-1,10-phenanthroline ligand and by two S atoms from two thiocyanate anions. The 1,10-phenanthroline ligand is slightly folded for one complex, the dihedral angle between the pyridine planes being 5.3 (1)°. In contrast it is nearly planar [0.5 (1)°] as it complexes with the other HgII atom. The thiocyanate ligands are virtually linear and the S atom is bonded to HgII with N⋯S—Hg angles ranging from 99.3 (1) to 103.5 (1)°. Despite the presence of six aromatic rings in the asymmetric unit, there are no significant intermolecular π–π contacts between phenanthroline ligands as the centroid–centroid distance of the closest contact between six-membered rings is 4.11 (1) A°.
In the title compound, [PdCl2(C26H24P2)]·C2H6OS, the PdII atom adopts a distorted cis-PdCl2P2 square-planar coordination geometry. The five-membered chelate ring adopts an envelope conformation with a methylene C atom in the flap position. The S and C atoms of the dimethyl sulfoxide (DMSO) solvent molecule are disordered over two sets of sites in a 0.8976 (18):0.1024 (18) ratio. The DMSO O atom accepts three C—H⋯O hydrogen bonds from an adjacent complex molecule.
In the molecule of the title compound, C16H20N4, the 1,3-diazinane ring adopts a chair conformation and the dihedral angle formed by the pyridine rings is 78.64 (8)°. The molecular conformation is stabilized by an intramolecular C—H⋯N hydrogen bond, forming an S(6) ring motif. In the crystal, centrosymmetrically related molecules are linked into dimers by pairs of N—H⋯N hydrogen bonds, generating rings of R
2(10) graph-set motif.
In the title compound, [RuCl2(C6H14N2)(C28H28P2)]·CH2Cl2, the RuII ion is coordinated in a slightly distorted octahedral environment, formed by two cis-oriented chloride ligands, two cis P atoms of a 1,4-bis(diphenylphosphanyl)butane ligand and two cis-chelating N atoms of a bidentate cyclohexane-1,2-diamine ligand. In the crystal, pairs of molecules form inversion dimers via N—H⋯Cl hydrogen bonds. In addition, intramolecular N—H⋯Cl and weak C—H⋯Cl, C—H⋯N, N—H⋯π and C—H⋯π hydrogen bonds are observed. One of the Cl atoms of the solvent molecule is disordered over two sites with refined occupancies of 0.62 (1) and 0.38 (1).
Novel hybrid xerogel materials were synthesized by a sol-gel procedure. n-octadecyltriethoxysilane was co-condensed with and without different cross-linkers using Q0 and T0 mono-functionalized organosilanes in the presence of n-hexadecylamine with different hydroxyl silica functional groups at the surface. These polymer networks have shown new properties, for example, a high degree of cross-linking and hydrolysis. Two different synthesis steps were carried out: simple self-assembly followed by sol-gel transition and precipitation of homogenous sols. Due to the lack of solubility of these materials, the compositions of the new materials were determined by infrared spectroscopy, 13C and 29Si CP/MAS NMR spectroscopy and scanning electron microscopy.
sol-gel; solid state NMR; cross-linkers; stationary phases
In the title complex, [CdBr2(C14H12N2)], the CdII ion is tetracoordinated by two N atoms of the bidentate 2,9-dimethyl-1,10-phenanthroline ligand and two bromide ions in a substantially distorted CdN2Br2 tetrahedral geometry. In the crystal, inversion dimers linked by pairs of weak C—H⋯Br bonds generate R
2(14) loops. Aromatic π–π stacking [shortest centroid–centroid separation = 3.633 (2) Å] interactions occur within, and also link, the dimers into chains propagating parallel to .
In the title compound, [CdI2(C14H12N2)], the molecule sits on a crystallographic twofold axis. The coordination sphere of the CdII atom is built of two symmetry-equivalent N atoms of one 2,9-dimethyl-1,10-phenanthroline (dmphen) ligand and two symmetry-equivalent I atoms, thus forming a distorted tetrahedral geometry. Inversion-related molecules interact along the c-axis direction by π–π stacking interactions between the phenanthroline ring systems, with centroid–centroid distances of 3.707 (9) and 3.597 (10) Å.
In the title compound, [RuCl2(C5H14N2)(C18H15P)2], the RuII atom is six-coordinated, forming a slightly distorted octahedral geometry, with two chloride ions in an axial arrangement, and two P atoms of two triphenylphosphane and two chelating N atoms of the bidentate 2,2-dimethylpropane-1,3-diamine ligand located in the equatorial plane. The average Ru—P, Ru—N and Ru—Cl bond lengths are 2.325 (18), 2.1845 (7) and 2.4123 (12) Å, respectively.
In the title Schiff base, C18H14N4O, the amido –NH– unit is connected to one of the two pyridyl N atoms at an N(—H)⋯N distance of 2.624 (2) Å. The molecular packing features an intermolecular C—H⋯N R
2(6) hydrogen-bonding ring motif.