| Popis: |
Two novel phenyl esters and partial phenyl esters of (dicloromethylene)bisphosphonic acid were synthesised. Three new layered Cd complexes of (dichloromethylene)bisphosphonic acidP,P-diphenyl, monophenyl and monoethyl esters were prepared. The complexes, [Cd3{(Cl2CP2O6Ph)2(H3COH)(H2O)5}(H2O)2]n (7), [{Cd(Cl2CP2O6Ph2)(H2O)3}(H2O)]n (8) and [{Cd1.5(Cl2CP2O6Et)(H2O)2}(C3H6O)0.5(H2O)4.5]n (9), were characterized by single crystal X-ray diffraction, IR spectroscopy, solid-state 31P- and 113Cd-CP/MAS NMR and elemental analysis. Also their thermal behaviour was investigated. Compound 7 consists of 1D chains with four independent octahedral Cd atoms joined by two L1 ligands, L1 = (Cl2CP2O6Ph)3−. The chains are connected into layers by phosphonate O atoms, and the adjacent layers are held together by face-to-face π–π stacking interactions. Compound 8 shows a new type of layered structure for metal bisphosphonates, where the L2 ligand, L2 = (Cl2CP2O6Ph2)2−, coordinates tridentately to three Cd2+ ions. Each CdO6 octahedron is connected to three CPO3 tetrahedra and each tetrahedron to three octahedra leading to a 2-D framework consisting of 12-membered cyclic cores. The layers are held together by edge-to-face CH/π interactions. In compound 9, the asymmetric unit contains two independent Cd2+ cations connected by L3 ligands, L3 = (Cl2CP2O6Et)3– and aqua ligands, to form a Cd–bisphosphonate layer. The layers are further interconnected into a 3-D supramolecular network by extensive hydrogen bonds. |
