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Two new macrocyclic complexes with C-methyl substituents on the framework,namely, [CuL](ClO4)2 (L = 5,12-dimethyl- 1,8-dihydroxyethyl- 1,3,6,8,10,13-hexaazacyclotetradecane) 1 and [NiL](ClO4)2 2, have been synthesized and structurally characterized through X-ray diffraction analysis. Also, crystal structure of [CuL1](ClO4)2 (L1 = 1,8-dimethyl- 1,3,6,8,10,13- hexaazacyclotetradecane) 3 has been determined. Crystal data for 1: C14H32C12CuN6O10, Mr = 578.90,monoclinic, P21In, a = 8.3529(11), b = 10.8105(17), c = 13.3709(17) A, β = 105.189(10)°, V =1165.2(3) A3, Z = 2, Dc = 1.650 g/cm3, F(000) = 602, λ(MoKα) = 0.71073 A,μ = 1.229 mm-1, R =0.0474 and wR = 0.0895 for 2771 observed reflections (I ＞ 2σ(I)). Crystal data for 2:C14H32C12N6NiO10, Mr = 574.07, monoclinic, P21/c, a = 8.3636(12), b = 12.997(2), c = 10.764(2) A,β = 99.31 (2)°, V = 1154.7(3) A3, Z = 2, Dc = 1.651 g/cm3, F(000) = 600, λ(MoKα) = 0.71073 A,μ =1.134 mm-1, R = 0.0380 and wR = 0.0796 for 2670 observed reflections (I ＞ 2σ(Ⅰ)). Crystal data for 3. C10H26Cl2CuN6O8, Mr = 492.81, monoclinic, P21/n, a = 8.4860(17), b = 8.6320(17), c = 12.662(3)A, β = 103.40(3)°, V = 902.2(3) A3, Z = 2, Dc = 1.814 g/cm3, F(000) = 510, λ(MoKα) = 0.71073 A,μ = 1.562 mm - 1, R = 0.0505 and wR = 0. 1 061 for 1967 observed reflections (I ＞ 2σ(Ⅰ)). Complexes 1 and 2 are isostructural with the metal ions situated at the inversion center. Hydrogen bonds between O atoms of pendant and perchlorate anion give rise to a two-dimensional supramolecular layer. The Cu(Ⅱ) ions of compounds 1 and 3 adopt distorted axially-elongated octahedral coordinate geometry, and the nickel(Ⅱ) ion in complex 2 is four-coordinated with a square-planar configuration.