Abstract　A　series　of　xylyl　(ortho,　meta,　and　para)　linked　N-ferrocenylmethylene-substituted　bis-imidazolium　salts　(3a-3c)　and　bis-benzimidazolium　salts　(4a-4c)　were　synthesized　and　structurally　characterized.　Their　binding　properties　for　anions　were　investigated　by　electrochemistry　and　1H　NMR　spectroscopy.　The　structure　of　3b,　3c,　4a　and　4b　were　confirmed　by　X-ray　crystallography.　As　expected,　all　salts　were　good　electrochemistry-signaling　receptors　for　several　anions　(F-,　AcO-,　HSO4-,　Cl-,　Br-　and　I-),　that　in　one　receptor　the　imidazolium/benzimidazolium　units　offer　binding　sites　for　anion　and　the　ferrocenyl　units　offer　electrochemistry　response　sites.　Furthermore,　the　results　showed　that　they　were　highly　selective　and　sensitive　to　F-　and　receptors　3b　and　4b　featuring　a　meta-xylene　spacer　were　more　effective　receptors　for　F-　compared　to　receptors　linked　by　an　orth　or　a　para-xylene　spacer.　1H　NMR　titrations　demonstrated　that　fluoride　ion　was　recognized　by　receptors　through　(C-H)+X-　hydrogen　bonds.　©　2015　Elsevier　B.V.