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Good-quality single crystals of polydistrontiumdimalatepentahydrate, a two-dimensional porous metal-organic framework, were successively grown by gel diffusion technique. Sodium metasilicate was used for gel preparation. Single crystal X-ray diffraction analyses showed that the compound crystallizes in triclinic space group P-1. The functional groups present in the crystals were identified by Fourier transform-infrared analysis. Elemental, powder X-ray diffraction and UV-visible spectral analyses of the compound were also performed. Thermal stability of the grown crystals was analyzed by thermogravimetry. Dielectric analyses of the title compound were conducted at room temperature in the frequency range of 400 Hz–4 MHz.