The first characterization of dimeric lanthanide complex anion: synthesis and crystal structure of [NH(Et)3]2[Lu(L)4]2$6CH3OH

Two lanthanide complexes with acrylic acid ligand: [Ho(L)3(CH3OH)2]2$CH3OH$H2O (1) and [NH(Et)3]2[Lu(L)4]2$6CH3OH (2) (LZ(E)-3-(2-hydroxyl-phenyl)-acrylic acid) are studied. The crystal structure data for 1: C59H60Ho2O24, orthorhombic, Pbcn, aZ15.4289(12) A ° , bZ7.9585(6) A ° , cZ23.041(2) A ° , bZ99.657(2)8, ZZ4, R1Z0.0637, wR2Z0.0919; for 2: C27H30.50LaO13.75, triclinic, PK1, aZ13.3034(4) A ° , bZ13.3087(4) A ° , cZ14.5461(6) A ° , aZ85.932(2)8, bZ64.611(2)8, gZ81.595(2)8, ZZ2, R1Z0.0394, wR2Z0.0446. Two structure data were collected using graphite monochromated molybdenum Ka radiation and refined using full-matrix least square techniques on F2. Complex 2 is the first dimeric lanthanide complex anion. Two structures show dinuclear complexes with bismonodentate and bidentate chelate bridge modes of carboxylato ligand. Bidentate chelate coordination mode were also included in these two complexes. The smallest bridge angle of bidentate chelate carboxylato bridge (h3-O, 104.70(9)8) has been found for the first time. Complexes 1 and 2 act as supramolecular synthons assembled by 2D and 3D hydrogen bonding in the crystal lattices. q 2005 Elsevier B.V. All rights reserved