Citation:
LV Yang-Yang, YE Li-Wang, XU Zhi-Huang, CAO You-Jie, SU Gen-Bo, ZHUANG Xin-Xin. Structure, Growth and Characterization of Ammonium 5-Sulfosalicylic Acid Monohydrate Crystal[J]. Chinese Journal of Structural Chemistry,
2015, 34(3): 453-460.
doi:
10.14102/j.cnki.0254-5861.2011-0386
Structure, Growth and Characterization of Ammonium 5-Sulfosalicylic Acid Monohydrate Crystal
摘要:
Ammonium 5-sulfosalicylic acid monohydrate (NH4·C7H5O6S·H2O, ASSA) was synthesized and optical grade crystal with dimensions of 45mm×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 C7H11NO7S with formula weight 253.23. The crystal belongs to monoclinic space group P21/c with a=11.884(9), b=7.306(5), c=12.152(9)Å, β=104.851(13)°, V=1019.8(13)Å3, 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, IR 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.
English
Structure, Growth and Characterization of Ammonium 5-Sulfosalicylic Acid Monohydrate Crystal
Abstract:
Ammonium 5-sulfosalicylic acid monohydrate (NH4·C7H5O6S·H2O, ASSA) was synthesized and optical grade crystal with dimensions of 45mm×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 C7H11NO7S with formula weight 253.23. The crystal belongs to monoclinic space group P21/c with a=11.884(9), b=7.306(5), c=12.152(9)Å, β=104.851(13)°, V=1019.8(13)Å3, 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, IR 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.
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