Solvothermal reaction of lanthanide（Ⅲ） salts with fluorescein （2-（6-hydroxy3-oxo-3H-xanthen-9-yl）benzoic acid） led to a series of new coordination polymers {[Ln（C 20 H 11 O 5）（C 20 H 10 O 5）（H 2 O）]·DMF} n （Ln=Er,Eu,Gd,Tb,Tm,Yb）.The PXRD patterns of the complexes indicate they are isomorphous.The structure of complex {[Er（C 20 H 11 O 5）（C 20 H 10 O 5）（H 2 O）]·DMF} n has been determined by single-crystal X-ray diffraction,revealing a 2D framework in which DMF molecules were filled between the layers.The crystal structure belongs to the triclinic system,space group P1,with a=12.107（4）,b=12.232（4）,c=13.273（4）,α=68.005（7）,β=88.024（11）,γ=77.451（8）°,V=1776.7（9） 3,Z=2,D c=1.720 g/cm 3,μ=2.434 mm-1,F（000）=918,R int=0.0584,T=293（2） K,the final R=0.0621 and wR=0.1501.
Treatment of resorcin[4]arene tetracarboxylic acid 1 with triethylamine in the presence of Co（CH3COO）2·4H2O and 4,4 -bipyridine gave a co-crystallization 14-·4Et3NH＋（C32H20O164-·4Et3NH＋,Mr=1069.27） from ethanol and water.The compound was structurally determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21/n,with a=8.1763（18）,b=12.913（3）,c=28.724（7） ,β=97.574（4）o,V=3006.3（12） 3,Z=2,Dc=1.181 g/cm3,F（000）=1152,Rint=0.0275,T=293（2） K,μ=0.086 mm-1,the final R=0.0634 and wR = 0.1752 for 5082 observed reflections with I 〉 2σ（I）. The co-crystallization is very stable at room temperature. Possibly, a network of N-H…O（=C） plays an important role in the structure. Meanwhile, the compound emits a weak cyan luminescence with peak maximum band at 458 nm.
