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New mixed crystals of K2Mg0.78Mn0.22(SO4)2.6H2O (KMMS) were synthesized and grown from an equimolar mixture of the Tutton's salt K2Mg(SO4)2.6H2O and MnSO4 by slow evaporation of the aqueous solution at room temperature. Crystal composition as determined by single crystal XRD analysis reveals that it belongs to the monoclinic system with P21/c space group and cell parameter values are, a=        The coexistence of magnesium and manganese ions in the mixed crystal is confirmed by single crystal XRD analysis, atomic absorption spectroscopy, inductively coupled plasma and energy dispersive X-ray spectroscopy. Slight variations are observed in FT-IR and XRD of pure and mixed crystals. The surface morphology of the mixed crystal is studied by scanning electron microscopy. Thermogravimetric and differential thermal analysis curves show the purity of the substance. Large full width at half maximum value of diffraction curves in high resolution X-ray diffraction spectroscopy reveals the presence of misorientation in the lattice blocks because of the Mn(II)incorporation.