Synthesis and Crystal Structures of the Five-Coordinate Diorganotin(IV) Complex [Ph2Sn(L)]·DMF and its 5-Hydroxypyrazoline Ligand (H2L)

• Published in: Journal of chemical crystallography 2011-04, Vol.41 (4), p.528-532
• Main Authors: de Sousa, Gerimário F., Marques, Daniel R., Resck, Inês S., Sabino, José R.
• Format: Article
• Language: English
• Subjects: Chemistry; Chemistry and Materials Science; Crystallography and Scattering Methods; Inorganic Chemistry; Organometallic Chemistry; Original Paper; Physical Chemistry
• ISSN: 1074-1542; 1572-8854
• DOI: 10.1007/s10870-010-9914-4

A five-coordinate diorganotin(IV) complex [Ph 2 Sn(L)]·DMF and its ligand, 5-hydroxy-3-methyl-5-phenyl-( N 4 -phenylthiosemicarbazone)pyrazoline (H 2 L), were synthesized and characterized by elemental analysis, IR, NMR ( 1 H, 13 C) spectroscopies and X-ray crystallography techniques. Our studies revealed that H 2 L has formed as 5-hydroxy-4,5-dihydropyrazoline derivative in orthorhombic, Pbca space group with a  = 15.4330(3) Å, b  = 11.5427(2) Å, c  = 18.1440(3) Å whereas [Ph 2 Sn(L)]·DMF crystallizes with two independent molecules ( a and b ) in the asymmetric unit in triclinic system, P ī space group with a  = 9.2795(1) Å, b  = 15.8315(2) Å, c  = 19.9895(3) Å, α  = 100.855(1)°, β  = 92.985(1)°, γ  = 102.243(1)°. In molecule a , the central Sn(IV) atom adopts a distorted tetragonal–pyramidal (TTP) geometry with N2 atom at apical position, while in molecule b the Sn(IV) occupies the centre of a trigonal-bipyramid (TBP) with N2 atom of the ONS-tridentate ligand and both Ph groups occupying equatorial positions. One molecule of DMF (crystallization solvent) helps in stabilizing the crystal structure. Graphical Abstract