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Two two-dimensional coordination complexes, {[Cu 4 (BTM) 6 (OPA) 4 ] Á 4DMF Á 3H 2 O} n (1) and {[Cu(BDTM) (OH)](ClO 4 ) Á 2H 2 O} n (2) (BTM = bis(1,2,4-triazol-1-yl) methane, BDTM = bis(3,5-dimethyl-1,2,4-triazol-1-yl)methane, OPA 2-= ortho-phthalic dianion, DMF = N,N-dimethylformamide), were synthesized and structurally characterized. Each Cu(II) ion locates in a distorted square pyramidal geometry in 1, in which OPA 2-ligands bridge Cu 2? ions along a axis to form a magnetic transmission chain and BTM ligands act as flexible spacers to construct the twodimensional layer structure. In 2, each Cu 2? ion adopts tetra-coordination geometry to two hydroxyl groups and two triazolyl nitrogen atoms from two different BDTM ligands. Two hydroxyl groups bridge two Cu 2? ions to form a rhombic diamond, and four BDTM ligands connect four diamonds to form a 36-membered macrocyclic structure with large channels along a axis. Magnetic properties revealed that both OPA 2-and OH -mediate anti-ferromagnetic interactions between Cu 2? ions with J = -0.06(3) and -301.9(2) cm -1 for 1 and 2, respectively.