Hydrogen Bonded Dimer N-(2-hydroxyethyl)-2-oxy-1-naphthaldimine and Its Oxo-vanadium(V) Complex

N-(2-hydroxyethyl)-2-oxy-1-naphthaldimine is a potential tridentate ligand prepared in a condensation reaction from 2-hydroxy-1- naphthaldehyde and 2-aminoethanol using catalytic amounts of triethylamine. Its vanadium(V) coordination compound was obtained by a template reaction from the methanol solution upon oxidation of VO2+ → VO3+ in air. Physico-chemical properties of both compounds were examined by thermogravimetric analysis, differential scanning calorimetry and FT IR spectroscopy. These results supplied some elements of structural information. Nevertheless, the entire stereochemistry of both the non-coordinated ligand and metal complex was elucidated by the X-ray structural determination. The ligand forms molecular complex by dimerization via intermolecular O–H⋅⋅⋅O hydrogen bonding. In the metal complex, four square pyramid basal plane coodination places are occupied by dinegative tridentate ligand ONO donor atoms and a methoxy group. All V–O bond distances are significantly different, depending on the nature of the functional group to wich oxygen atoms belong. The vanadium complex is an example of a fairly rare pentacoordinated square pyramidal VV species

2-{[(4-{[(2-Hy­droxy­phen­yl)(phen­yl)methyl­idene]amino}­phen­yl)imino](phen­yl)meth­yl}phenol

The title mol­ecule, C32H24N2O2, has a crystallographically imposed inversion centre and exists in the crystal as an enol–imine tautomer. The mol­ecular structure is stabilized by two strong intra­molecular O—H⋯N hydrogen bonds. The dihedral angles between the central benzene ring and the mean planes of the phenyl substituents are 59.99 (1) and 62.79 (2)°. In the crystal, the mol­ecules are arranged into (010) layers via C—H⋯π inter­actions

Controlling Solvate Formation of a Schiff Base by Combining Mechano-chemistry with Solution Synthesis

A Schiff base dicarboxylic acid (1) was prepared by condensation of 2-hydroxy-1-naphthaldehyde with 5-aminoisophthalic acid. Its solvates with pyridine (2a and 2b) and dimethylformamide (3) were prepared by liquid-assisted grinding and by conventional solvent-based methods. All products were characterised by FT-IR spectroscopy, thermogravimetric analysis and differential scanning calorimetry. The structures of 1, 2b and 3 were determined by single crystal X-ray diffraction. 1 was found to be a pure Schiff base, 2b a pyridine solvate and 3 a dimethylformamide solvate monohydrate. In all three structures, the Schiff base molecule appears to be present as the ketoamine tautomer.(doi: 10.5562/cca2111

Structural Investigation of Di-μ-chloro-bis[saccharinatopyridinemercury(II)] by X-ray Diffraction and FT IR Spectroscopy

The solid state structure of C12H9ClHgN2O3S2 was determined and the appropriate assignment of the CO and SO2 stretching vibrations in the FT IR spectrum was made. Two monomeric chlorosaccharinatopyridinemercury(II) moieties are joined together forming a di-chloro bridged dimmer by an inversion centre operation. The mercury atom is coordinated with two bridging chlorine and the pyridine and saccharinato nitrogen atoms in the shape of a heavily distorted tetrahedron. There is a significant difference between Hg1–Cl1 2.533(2) Å and Hg1–Cl1i 2.715(2) Å distances as well as between Hg1–N11 2.106(7) Å and Hg1–N21 2.209(7) Å bond lengths. The valence bond angles at the metal atom deviate significantly from the standard tetrahedral value, ranging from 86.23(7)° for Cl1–Hg1–Cl1i to 131.5(3)° for N11–Hg1–N21. Discrete molecules are linked together by weak intermolecular C–H⋅⋅⋅O attractions at distances less than 3.5 Å

The Crystal Structure and Conformation of bis(N-methyl-5-chlorosalicylideneiminato)nickel(II) and bis(N-ethyl-5-chlorosalicy lideneiminato)nickel(II)

The crystal structures of bis(N-methyl-5-chlorosalicylideneiminato) nickel(II) (A) and bis(N-ethyl-5-chlorosalicylideneiminato) nickel(II) (B) have been determined by X-ray structure analysis using heavy atom method and refined by fuU matrix leastsquares procedure to R values of 0.044 and 0.040 for (A) and (B), respectively. Both structures have molecular centre of symmetry and the nickel atom in a planar coordination. Molecules of both complex compounds have »stepped« conformation with distinct difference in the step heights: 0.121 and 0.702 A in (A) and (B), respectively. The Ni-O and Ni-N bond lengths are 1.818 and 1.924 A in (A), and \u271.830 and 1.916 A in (B)

Synthesis and Structure of N,N’-Butylene-N,N’-hexylenebis(2-oxy-1-naphthaldimine)

The title compounds were synthesized in the reaction of 2-hydroxy- 1-naphthaldehyde and corresponding aliphatic diamines. Standard TGA and DSC procedures were applied to characterize both compounds 1 and 2. The stereochemistry of the compounds in solid state was determined by the single crystal X-ray diffraction. Compound 1: C26H24N2O2, orthorhombic, space group Pbca, a = 8.142(2) Å, b = 9.097(3) Å, c = 28.812(8) Å, R = 0.032. Compound 2: C28H28N2O2, orthorhombic, space group Pbcn, a = 23.738(2) Å, b = 8.9933(8) Å, c = 10.4206(8) Å, R = 0.038. The molecules of both compounds 1 and 2 have an imposed centre of inversion in the middle of the aliphatic chain bridging two naphthaldimine moieties. The well known crystallographic D2h bond length pattern as well as quinoid effects were observed in the fused ring system in both cases. In both Schiff bases, the N−H⋅⋅⋅O type of intramolecular hydrogen bond was established. An additional intermolecular three-centre hydrogen bond links the molecules in 1