Synthesis, spectral (FT-IR, 1 H, 13 C) studies, and crystal structure of [(2,6-CO 2 ) 2 C 5 H 3 NSnBu 2 (H 2 O)] 2 ·CHCl 3
Résumé
Abstract Di- n -butyltin(IV) 2,6-pyridinedicarboxylate [(2,6-CO 2 ) 2 C 5 H 3 NSnBu 2 (H 2 O)] 2 ·CHCl 3 , has been synthesized and characterized by elemental analyses, infrared and NMR ( 1 H and 13 C) spectroscopy, and single-crystal X-ray diffraction. The title complex crystallizes in the triclinic space group P 1 ‾ $P‾{1}$ ; with a = 9.2330(4), b = 10.4790(5), c = 20.2489(8) Å, α = 89.439(4), β = 87.492(3), γ = 85.888(4)°, V = 1951.96(15) Å 3 , and Z = 2. In this complex, the 2,6-pyridinedicarboxylate groups are tetradentate, chelating, and bridging ligands for the tin(IV) atoms. NMR spectra showed that the ligands bind to the tin(IV) center in the anionic (COO − ) form. In the asymmetric unit of the dimeric complex, the monomer is composed of an n -Bu 2 Sn unit bonded to one 2,6-pyridinedicarboxylate group through one nitrogen and two oxygen donor atoms. It is also coordinated by a water molecule. In the dimer formed by carboxylate bridging, a trans- heptacoordinated geometry around the tin(IV) atom is established. The chloroform molecule is connected to the dimer by C–H···O contacts. Compound exhibits extended O–H···O and C–H···O hydrogen bonding networks leading to a supramolecular layer topology.