A heteronuclear CuII–LuIII complex (systematic name: {6,6′‐diethoxy‐2,2′‐[ethane‐1,2‐diylbis(nitrilomethylidyne)]diphenolato}trinitratolutetium(III)copper(II)), [CuLu(C20H22N2O4)(NO3)3], with the hexadentate Schiff base compartmental ligand N,N′‐ethylenebis(3‐ethoxysalicylaldiimine) (H2L), has been synthesized and structurally characterized. The Cu and Lu atoms are doubly bridged by two phenolate O atoms afforded by the Schiff base ligand. No classical intermolecular hydrogen bonds are found. Some weak O⋯Cu and C—H⋯O interactions generate a two‐dimensional zigzag sheet.
Tetrathiol 1,2,4,5-(HSCH 2 ) 4 C 6 H 2 reacted with Fe 3 (CO) 12 and Et 3 N followed by treatment of the intermediate µ- CO-containing 10) generated in situ from the initially formed tetraanion 7. Similarly, the triplebutterfly complexes [(µ-Ph 2 P)Fe 2 (CO) 6 ] 2 [Fe 2 (CO) 6 ][(µ-SCH 2 ) 4 C] (14) and [(µ-σ,π-CH 2 CHdCH 2 )Fe 2 (CO) 6 ] 2 -[Fe 2 (CO) 6 ][(µ-SCH 2 ) 4 C] (16) were produced by reaction of Ph 2 PCl or CH 2 dCHCH 2 Br with the µ-CO- 12) generated initially by reaction of tetrathiol C(CH 2 SH) 4 with Fe 3 (CO) 12 and Et 3 N. The double-butterfly complex [Fe 2 (CO) 6 ] 2 [(µ-SCH 2 ) 4 C] (15) derived in situ from dianion 13 was also isolated as a minor product along with major products 14 and 15. All the new complexes 9, 11, and 14-16 were characterized by elemental analysis and IR and NMR spectroscopy, as well as by X-ray crystallography for 9, 11, 14, and 15.
The molecule of the title compound, C13H9ClN3O, is roughly planar and displays a trans configuration with respect to the C=N double bond. The dihedral angle between the benzene and pyridine rings is 4.8 (3)°. The crystal structure is stabilized by intermolecular N—H...N hydrogen bonds.
Key indicators: single-crystal X-ray study; T = 293 K; mean (C-C) = 0.004 Å; R factor = 0.022; wR factor = 0.048; data-to-parameter ratio = 17.0.A heteronuclear Cu II -Sm III complex (systematic name:has been synthesized and structurally characterized. The Cu and Sm atoms are doubly bridged by two phenolate O atoms provided by the Schiff base ligand. The coordination of the Cu atom is square planar, formed by two imine N and two phenolate O atoms. The Sm III atom has a decacoordination environment, formed by the phenolate O atoms, two ethoxy O atoms and two O atoms each from the three nitrates. No classical intermolecular hydrogen bonds are found. Some weak C-HÁ Á ÁO and OÁ Á ÁCu interactions [OÁ Á ÁCu = 3.167 (4) Å ] generate a two-dimensional zigzag sheet. Experimental Crystal data [CuSm(C 20 H 22 N 2 O 4 )(NO 3 ) 3 ] M r = 754.32 Orthorhombic, P2 1 2 1 2 1 a = 8.6208 (8) Å b = 13.8333 (13) Å c = 21.151 (2) Å V = 2522.4 (4) Å 3 Z = 4 Mo K radiation = 3.23 mm À1 T = 293 (2) K 0.28 Â 0.17 Â 0.15 mm Data collection Bruker APEXII area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2004) T min = 0.533, T max = 0.622 19177 measured reflections 6184 independent reflections 5236 reflections with I > 2(I) R int = 0.024
In the title hydroxyurea derivative, C15H14F2N2O2, the dihedral angle between the two benzene rings is 48.64 (19)°. The urea group forms dihedral angles of 48.1 (2) and 79.2 (2)° with the two benzene rings. In the crystal, inversion dimers linked by pairs of N—H⋯O hydrogen bonds occur, and further N—H⋯O links lead to chains of molecules.
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