摘要
Ammonium 5-sulfosalicylic acid monohydrate (NH4·C7H5O6S·H2O, ASSA) was synthesized and optical grade crystal with dimensions of 45ram × 20mm × 18mm was obtained from aqueous solution by the cooling solution method. The crystal structure was confirmed by X-ray single-crystal diffraction method and the empirical composition is C7HIINO7S with formula weight 253.23. The crystal belongs to monoclinic space group P21/c with a = 1 1.884(9), b = 7.306(5), c = 12.152(9) A, β = 104.851(13)°, V= 1019.8(13) A3, Z = 4, Dc = 1.649 g/cm3,μ = 0.340 mm-1, F(000) =528, the final R= 0.0307 and wR= 0.0866 for 7494 observed reflections (I〉 2σ(I)), Elemental analysis, 1R and 1H-NMR spectrum were used to characterize the compound. Thermal analysis showed that one coordination water molecule was contained and dehydration temperature of ASSA crystal was 106℃. Optical transmission and fluorescence spectrum revealed that the ASSA crystal exhibited a strong absorption in ultraviolet region with the sharp absorption edge located at 340 nm and a significant blue fluorescent emission band at 442 nm.
Ammonium 5-sulfosalicylic acid monohydrate (NH4·C7H5O6S·H2O, ASSA) was synthesized and optical grade crystal with dimensions of 45ram × 20mm × 18mm was obtained from aqueous solution by the cooling solution method. The crystal structure was confirmed by X-ray single-crystal diffraction method and the empirical composition is C7HIINO7S with formula weight 253.23. The crystal belongs to monoclinic space group P21/c with a = 1 1.884(9), b = 7.306(5), c = 12.152(9) A, β = 104.851(13)°, V= 1019.8(13) A3, Z = 4, Dc = 1.649 g/cm3,μ = 0.340 mm-1, F(000) =528, the final R= 0.0307 and wR= 0.0866 for 7494 observed reflections (I〉 2σ(I)), Elemental analysis, 1R and 1H-NMR spectrum were used to characterize the compound. Thermal analysis showed that one coordination water molecule was contained and dehydration temperature of ASSA crystal was 106℃. Optical transmission and fluorescence spectrum revealed that the ASSA crystal exhibited a strong absorption in ultraviolet region with the sharp absorption edge located at 340 nm and a significant blue fluorescent emission band at 442 nm.
基金
carried out under the sponsorship and financial support from the Key Laboratory of Optoelectronic Materials Chemistry and Physics,Chinese Academy of Sciences