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CrystEngComm, 2009, 11, 2431 - 2440, DOI: 10.1039/b907874f
Synthesis of phenyl substituted bisphosphonates and crystal structures and characterization of Cd complexes of (dichloromethylene)bisphosphonic acid phenyl and alkyl ester derivatives
Jonna Jokiniemi, Jouko Vepsäläinen, Harri Nätkinniemi, Sirpa Peräniemi and Markku Ahlgrén
Two novel phenyl esters and partial phenyl esters of (dicloromethylene)bisphosphonic acid were synthesised. Three new layered Cd complexes of (dichloromethylene)bisphosphonic acid P,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
– 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/ 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.
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