The layered zirconium [N-(phosphonomethyl)iminodiacetic acid-phosphate] Zr(HPO4)1.34[O3PCH2N- (CH2CO2H)2]0.66·H2O can only be prepared in the series of the zirconium phosphonate-phosphates Zr(HPO4)2-x [O3PCH2N(CH...The layered zirconium [N-(phosphonomethyl)iminodiacetic acid-phosphate] Zr(HPO4)1.34[O3PCH2N- (CH2CO2H)2]0.66·H2O can only be prepared in the series of the zirconium phosphonate-phosphates Zr(HPO4)2-x [O3PCH2N(CH2CO2H)2]x·H2O (ZPPMIDA) by the reaction of zirconium oxychloride with phosphonic acid and H2O3PCH2N(CH2CO2H)2 in the designed x range of 0 < x < 2, which had been monitored by using the phosphorus integration value ratio of HPO42- and [O3PCH2N(CH2CO2H)2]2- group in the 31P MAS NMR spectra. After intercala- tion of n-butyl amine, the 31P chemical shift of HPO42- group at - 8.0￣- 10.0 ppm moved to 6.0 ppm with a change of 14.0￣16.0 ppm and that of [O3PCH2N(CH2CO2H)2]2- group at - 29.1 ppm changed only 0.5 ppm. Due to the pil- lared effect of [O3PCH2N(CH2CO2H)2]2- groups on the interlayer spacing, intercalated amines such as n-butylamine, n-hexyl amine and n-octyl amine easily reacted with HPO42- group in ZPPMIDA (x=0.66) rather than that in α- ZrP, and carboxylic group (-CO2H) in ZPPMIDA (x=0.66).展开更多
A new molybdophosphate, (NH3CH2CH2NH3)2Mo5O15(HPO4)2 has been synthesized under hydrothermal conditions and structurally characterized by single crystal X ray diffractions. The compound crystallizes in the monoclinic,...A new molybdophosphate, (NH3CH2CH2NH3)2Mo5O15(HPO4)2 has been synthesized under hydrothermal conditions and structurally characterized by single crystal X ray diffractions. The compound crystallizes in the monoclinic, space group C2/c, a=1.7633(2)nm, b=1.00122(11) nm, c=1.37624(13)nm, β=96.974(5)°, V=2.4117(5)nm3, Z=4, Dc=2.853g·cm-3, μ(MoKα)=2.766mm-1, F(000)=1992. The structure contains the isolated polyanions of [Mo5O15(HPO4)2]4- units around which the portonated ethylenediamine ions are pos itioned. By hydrogen bond interactions the polyanions are interconnected to form a three dimensional network. Other characterizations by powder XRD, IR and thermal analysis are also described. CCDC: 206321.展开更多
文摘The layered zirconium [N-(phosphonomethyl)iminodiacetic acid-phosphate] Zr(HPO4)1.34[O3PCH2N- (CH2CO2H)2]0.66·H2O can only be prepared in the series of the zirconium phosphonate-phosphates Zr(HPO4)2-x [O3PCH2N(CH2CO2H)2]x·H2O (ZPPMIDA) by the reaction of zirconium oxychloride with phosphonic acid and H2O3PCH2N(CH2CO2H)2 in the designed x range of 0 < x < 2, which had been monitored by using the phosphorus integration value ratio of HPO42- and [O3PCH2N(CH2CO2H)2]2- group in the 31P MAS NMR spectra. After intercala- tion of n-butyl amine, the 31P chemical shift of HPO42- group at - 8.0￣- 10.0 ppm moved to 6.0 ppm with a change of 14.0￣16.0 ppm and that of [O3PCH2N(CH2CO2H)2]2- group at - 29.1 ppm changed only 0.5 ppm. Due to the pil- lared effect of [O3PCH2N(CH2CO2H)2]2- groups on the interlayer spacing, intercalated amines such as n-butylamine, n-hexyl amine and n-octyl amine easily reacted with HPO42- group in ZPPMIDA (x=0.66) rather than that in α- ZrP, and carboxylic group (-CO2H) in ZPPMIDA (x=0.66).
文摘A new molybdophosphate, (NH3CH2CH2NH3)2Mo5O15(HPO4)2 has been synthesized under hydrothermal conditions and structurally characterized by single crystal X ray diffractions. The compound crystallizes in the monoclinic, space group C2/c, a=1.7633(2)nm, b=1.00122(11) nm, c=1.37624(13)nm, β=96.974(5)°, V=2.4117(5)nm3, Z=4, Dc=2.853g·cm-3, μ(MoKα)=2.766mm-1, F(000)=1992. The structure contains the isolated polyanions of [Mo5O15(HPO4)2]4- units around which the portonated ethylenediamine ions are pos itioned. By hydrogen bond interactions the polyanions are interconnected to form a three dimensional network. Other characterizations by powder XRD, IR and thermal analysis are also described. CCDC: 206321.
