Single crystals of holmium oxalate heptahydrate are grown by gel diffusion method using organic agar gel as a medium of growth. The crystals grow in the agar gel with hexagonal morphology having well defined habit faces Powder X-ray diffraction results show that the crystals belong to monoclinic system bearing the space group P2<sub>1</sub>/c with cell parameters; a = 12.197<img alt="" src="Edit_b4006270-e152-466e-8edf-e0a3c5d1a1b5.bmp" width="1" height="1" />Å <img alt="" align="left" src="Edit_b1e0a402-3daf-4259-b72d-cbce31e6dfe0.bmp" width="1" height="1" />, b = 11.714 , c = 6.479 , α = 90°, β = 120.12°, γ = 90°, V = 799.6Å <sup>3</sup>. Fourier transform Infrared spectrum of the crystals shows the presence of water and other associated functional groups. Thermogravimetric analysis support the presence of 7 H<sub>2</sub>O molecules associated with holmium oxalate crystal lattice. The thermal decomposition in the nitrogen atmosphere leads to the formation of holmium oxide as the final product