No abstract

Source of material [3,4]Dioxolebenzohydrazide (18.2 mg, 0.1 mmol) was dissolved in methanol (10 ml), then 3,5-dichloro-2-hydroxybenzaldehyde (19.2 mg, 0.1 mmol) was added slowly into the solution, and the mixture was stirred at room temperature for 3h.The resulting solution was left in air for af ew days, yielding colorless blockshaped crystals. Experimental details DiscussionHyrazone compounds have shown interesting structures and biological properties. Recently, agreat deal of hydrazone derivatives and their metal complexes have been reported [1][2][3][4][5]. As part of the ongoing investigation of the crystal structure of such compounds, the crystal structure of anew hydrazone compound is reported in this paper. The molecular structure of the title compound consists of a [3,4]dioxolebenzohydrazide and a3 ,5-dichloro-2-hydroxybenzylidene groups that are located on opposite sides of the C=N bond showing an E configuration. The dihedral angle between the two substituted benzene rings C1-C6 and C9-C14 is 4.5(2)°,indicating the molecule is nearly coplanar. The crystal structure involves an intramolecular O1−H1···N1 hydrogen bond. The methanol molecules are linked to the hydrazone molecules through intermolecular N2−H2···O5 and O5−H5···O2 hydrogen bonds. The bond lengths and angles are in good agreement with the corresponding values observed in the similar structures [6][7][8]. The torsion angles of C7−N1−N2−C8 and N1−N2−C8−C9 are 0.4(2) and 3.0(2)°,respectively.

Source of material [3,4]Dioxolebenzohydrazide (18.2 mg, 0.1 mmol) was dissolved in methanol (10 ml), then 2-chloro-5-nitrobenzaldehyde (18.6 mg, 0.1 mmol) was added slowly into the solution, and the mixture was stirred at room temperature for 3h.The resulting solution was left in air for afew days, yielding colorless block-shaped crystals. Experimental details

Source of materialAll the chemicals used were of AR grade. N,N-diethyl-1,2-diaminoethane (23.2 mg, 0.2 mmol) and 3-bromo-5-chlorosalicylaldehyde (47.0 mg, 0.2 mmol) were refluxed in 10 ml methanol for 30 min. To the above solution was added NaN 3 (6.5 mg, 0.1 mmol) and Co(NO 3 ) 2 · 6H 2 O (29.0 mg, 0.1 mmol) in 10 ml methanol. The mixture was refluxed for 1 h. The mixture was filtered after cooling to room temperature. After keeping the filtrate in air for 7 d, brown crystals were formed. Experimental detailsH2 was located from a Fourier difference map and refined isotropically, with NH distance restrained to 0.90(1) Å. Other H atoms were positioned geometrically and constrained as riding atoms, with CH distances of 0.93-0.97 Å, and U iso (H) set to 1.2 or 1.5 U eq (C). DiscussionThe condensation reaction of aromatic aldehydes with primary amines has been shown to offer an easy and inexpensive way of forming a variety of Schiff bases. These Schiff bases exhibit a wide range of biological activities and applications [1][2][3][4][5][6][7]. Cobalt is an important life-required element. Many cobalt complexes were prepared and structurally determined by single-crystal X-ray analysis [6][7][8]. We have reported the structure of a mononuclear Schiff base cobalt(III) complex [9] and a mononuclear Schiff base nickel(II) complex [10]. As an extension of the work, we synthesized a further Schiff base cobalt(III) complex. The asymmetric unit of the crystal structure of the title compound is composed of the cationic mononuclear complex molecule [Co(C 13 H 17 BrClN 2 O)(C 13 H 18 BrClN 2 O)(N 3 )] + and a nitrate anion. The Co(III) atom in the complex is coordinated by two Schiff base ligands and one azide ligand, forming an octahedral coordination. One Schiff base ligand coordinates to the metal through one phenolic O, one imine N, and one amine N atoms, while the other one coordinates to the metal through phenolic O and imine N atoms. The azide acts as a terminal ligand and coordinates to the metal through one terminal N atom. The CoO and CoN bond lengths are comparable to the values in other similar complexes [11,12]. The N3Co1N4 bond angle deviates from the ideal value of 90°by 3.9(2)°, which is due to the strain created by the five-membered chelate ring Co1/N3/C21/C22/N4.

The title compound, C21H22N2O3, was synthesized by the reaction of tert-butyl­hydrazine with phthalic anhydride and further O-benzoyl­ation of the resulting inter­mediate by 3,5-dimethyl­benzoyl chloride. Inter­molecular C—H⋯O=C inter­actions link the mol­ecules into layers.