The title complex [CuNaL(ClO~4)] of a Robson macrocycle with two different coordination compartments H~2L, derived from Schiff base condensation of 4-methyl-2, 6-diformylphenol and two kinds of diamine, has been synthesized in one template reaction. The complex has been characterized by UV-Vis, IR, ^1H NMR and ESR spectra. The ESR spectrum shows three peaks at g~x=1.987, g~y=2.168 and g~z=2.233, respectively. The complex crystallizes in the monoclinic crystal system, space group P2~1/n, with Z=4, a=0.9255(3), b=1.7689(2), c=1. 6055(2)nm, β=101.69(2)ⅲ, and V=2.574nm^3. The refinement converges with R=0.053 and R~w=0.065 for 2640 reflections with I≥3σ(I). The Cu(Ⅱ) and Na(I) ions reside at the 4- and 5-coordination compartments of the macrocycle, respectively. The coordination geometry around the copper atom is regarded as a planar square. But the sodium atom is also coordinated with one oxygen atom of a perchlorate anion on the axis. This geometry of six-coordinate sodium may be considered as a pentagonal pyramid. The distance between Cu and Na bridged by two phenolic oxygens is 0.3227(3)nm.

Key words: DINUCLEAR COMPLEX, SODIUM, COPPER, ETHANEDIAMINE, FORMYL, UNIT CELL, X-RAY DIFFRACTION ANALYSIS, CRYSTAL STRUCTURE