Two novel metal-organic frameworks (MOFs) [Cu 3 (C 7 H 2 NO 5 ) 2 ] n 3 3nH 2 O (1) and [CuAg 2 (C 7 H 3 NO 5 ) 2 ] n (2) were obtained by the hydrothermal reaction. Complex 1 exhibits a three-dimensional (3,6)-connected anatase topology with the Schl€ afli symbol (4 2 .6) 2 (4 4 .6 2 .8 8 .10), while complex 2 displays a two-dimensional (3,6)-connected TiS 2 related net topology with the Schl€ afli symbol (4 3 ) 2 (4 6 .6 6 .8 3 ). The optical studies show that 1 and 2 both have good third-order nonlinear optical and luminescent properties.