[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.
The title compound, C25H26Cl2FN3O4S, contains two bio-active moieties (thiobarbituric acid and fluoroquinolone). In the crystal, molecules are linked via C—H⋯O and C—H⋯F hydrogen bonds, forming two-dimensional slab-like networks lying parallel to the bc plane. The benzene ring substituted by F and Cl atoms and the 4-chlorobutyl group seem to be partly disordered, however attempts to model the disorder were unsuccessful.
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, (C7H10N)2[HgBr4], consists of one cation and one half-anion, bisected by a twofold rotation axis passing through the metal atom. The anion exhibits a distorted tetrahedral arrangement about the HgII atom. In the crystal, the cations and anions are linked by N—H⋯Br hydrogen-bonding interactions along . Cation–cation π–π stacking and Br⋯Br intermolecular interactions are absent.
The title salt, C20H26N3O2
+·Cl−, lies across a twofold crystallographic axis with the central N atom of the cation and the chloride anion sitting on this axis, Z′ = 0.5. There is an intramolecular hydrogen bond between the hydroxy H atom and the imino N atom. The chloride anion and the cation are connected into chains along the a axis by an N—H⋯Cl hydrogen bond. In the crystal, the chains are linked via C—H⋯Cl interactions forming two-dimensional networks lying parallel to (101).
In the title compound, (C8H12N)2[ZnBr4], the coordination geometry of the anion is approximately tetrahedral. The Zn—Br bond lengths range from 2.3901 (19) to 2.449 (2) Å and the Br—Zn—Br angles range from 107.09 (8) to 112.48 (8)°. In the crystal, each [ZnBr4]2− anion is connected to four cations through two N—H⋯Br and two C—H⋯Br hydrogen bonds, forming two-dimensional ⋯(cation)2⋯anion⋯(cation2)⋯ sheets parallel to the bc plane. Within each sheet, the anions are arranged in stacks with no significant inter-anion Br⋯Br interactions [the shortest being > 4.3 Å], while the cations are in chains, with weak π–π stacking interactions [centroid–centroid distance = 3.991 Å] between cations interacting with the same anion.
In the title salt, C6H10N2
2+·2Br−, the non-H atoms of the 3-methylpyridinium unit of the cation are almost coplanar (r.m.s. deviation = 0.0052 Å). In the crystal, the dications and Br anions are linked by a combination of six hydrogen bonds, viz. one Npy—H⋯Br, two C—H⋯Br and three H2N–H⋯Br, into supramolecular layers, parallel to the bc plane, composed of alternating R24(10) and R24(8) loops. Weak π–π interactions between cationic rings with centroid–centroid distances of 3.891 (2) Å are also observed.
In the title molecular salt, C10H10N2
2+·2Br−, the dihedral angle between the aromatic rings is 20.83 (14)° and the N—H groups have a transoid conformaton [N—C—C—N = 158.5 (3)°]. In the crystal, the cations are linked to the anions by two N—H⋯Br and five C—H⋯Br hydrogen bonds, generating corrugated sheets incorporating R
2(11) and two different R
2(12) loops. This structure was originally reported by Nakatsu et al. [Acta Cryst (1972), A28, S24], but no atomic coordinates are available.
The asymmetric unit of the title salt, C7H10N+·Br−, comprises two 2,6-dimethylpyridinium cations and two bromide anions. One cation and one anion are situated in general positions, while the other cation and the other anion lie on a crystallographic mirror plane parallel to (010). Each pair of ions interact via N—H⋯Br and C—H⋯Br hydrogen bonding, generating motifs depending on the cation and anion involved. Thus, the cation and the anion on the mirror plane generate infinite chains along the c axis, while the other ionic pair leads to sheets parallel to the ac plane. In the overall crystal packing, both motifs alternate along the b axis, with a single layer of the chain motif sandwiched between two double layers of the sheet motif. The sheets and chains are further connected via aryl π–π interactions [centroid–centroid distances = 3.690 (2) and 3.714 (2) Å], giving a three-dimensional network.
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 salt, C6H9N2
+·Br2I−, the cation is essentially planar (r.m.s. deviation = 0.0062 Å for the non-H atoms) while the anion is almost linear with a Br—I—Br angle of 177.67 (2)°. The crystal packing shows two anions and two cations connected via N—H⋯Br and (pyridine)N—H⋯Br hydrogen-bonding interactions, forming centrosymmetric tetramers with R44(16) ring motifs. Very weak offset aromatic π–π stacking interactions [centroid-centroid separation = 4.038 (4), slippage = 1.773 Å] also occur.
In the title salt, 2C7H10N+·IBr2
−·Br−, each of the anions, viz. [IBr2]− and Br−, lie on a twofold axis. The IBr2
− anion is almost linear, with a Br—I—Br angle of 178.25 (3)°. The cation is essentially planar (r.m.s. deviation = 0.0067 Å). In the crystal, each Br− anion links two cations via N—H⋯Br⋯H—N hydrogen-bonding interactions.
The asymmetric unit of the title compound, (C5H6Br2N3)2[SnBr6], contains one cation and one half-anion in which the Sn atom is located on a crystallographic centre of inversion and is in a quasi-octahedral geometry. The crystal structure is assembled via hydrogen-bonding interactions of two kinds, N(pyridine/amine)—H⋯Br—Sn, along with C—Br⋯Br—Sn interactions [3.4925 (19) Å]. The cations are involved in π–π stacking, which adds an extra supramolecularity as it presents a strong case of offset-face-to-face motifs [centroid–centroid distance = 3.577 (3) Å]. The intermolecular hydrogen bonds, short Br⋯Br interactions and π–π stacking result in the formation of a three-dimensional supramolecular architecture.
The asymmetric unit of the title compound, (C5H8N2)[HgBr4]·H2O, consists of one cation, one anion and one water molecule. The anion exhibits a distorted tetrahedral arrangement about the Hg atom. The crystal structure contains alternating sheets of cations (in the ac plane) and stacks of anions. Several strong hydrogen-bonding interactions (pyN—H⋯Br and C—H⋯Br; py is pyridine), along with O—H⋯Br interactions, connect the sheets of cations to the stacks of anions. Cation–cation π–π stacking is also present (C⋯C distances in the range 3.424–3.865 Å). The shortest Br⋯Br distance is 3.9527 (9) Å.
The asymmetric unit of the title compound, (C5H5BrN)2[SnBr6], contains one cation and one half-anion. The [SnBr6]2− anion is located on an inversion center and forms a quasi-regular octahedral arrangement. The crystal structure consists of two-dimensional supramolecular layers assembled via hydrogen-bonding interactions of N—H⋯Br—Sn [D⋯A = 3.375 (13)–3.562 (13) Å and D—H⋯A = 127–142°, along with C—Br⋯Br synthons [3.667 (2) and 3.778 (3) Å]. These layers are parallel to the bc plane and built up from anions interacting extensively with the six surrounding cations.
In the crystal structure of the title compound, (C6H9N2)2[CuBr4], the geometry around the Cu atom is intermediate between tetrahedral (Td) and square planar (D4h). Each [CuBr4]2− anion is connected non-symmetrically to four surrounding cations through N—H⋯X (pyridine and amine proton) hydrogen bonds, forming chains of the ladder-type running parallel to the crystallographic b axis. These layers are further connected by means of offset face-to-face interactions (parallel to the a axis), giving a three-dimensional network. Cation π–π stacking [centroid separations of 3.69 (9) and 3.71 (1) Å] and Br⋯aryl interactions [3.72 (2) and 4.04 (6) Å] are present in the crystal structure. There are no intermolecular Br⋯Br interactions.
The asymmetric unit of the title compound, (C5H5BrN)2[SnCl6], contains one cation and one half-anion. The [SnCl6]2− anion is located on an inversion center and forms a quasi-regular octahedral arrangement. Hydrogen-bonding interactions of two kinds, viz. N—H⋯Cl—Sn and C—H⋯Cl—Sn, along with Cl⋯Br interactions [3.4393 (15) Å], connect the ions in the crystal structure into two-dimensional supramolecular arrays. These supramolecular arrays are arranged in layers approximately parallel to (110) built up from anions interacting with six symmetry-related surrounding cations.
In the crystal structure of the title compound, (C7H10N)2[CoBr4], the [CoBr4]2− anion is connected to two cations through N—H⋯Br and H2C—H⋯Br hydrogen bonds to form two-dimensional cation–anion–cation layers normal to the crystallographic b axis. Interactions of the π–π type are absent between cations in the stacks [centroid–centroid separation = 5.01 (5) Å]. Significant intermolecular Br–aryl interactions are present in the structure, especially an unusually short Br–ring centroid interaction of 3.78 (1) Å. The coordination geometry of the anion is approximately tetrahedral and a twofold rotation axis passes through the Co atom.
In the title compound, C18H16N4O2, the central six-membered ring has a boat conformation.