A novel open-framework zinc phosphate with intersecting helical channels

Abstract

A new open-framework zinc phosphate, possessing two interpenetrating 8-membered helical channels, has been synthesized under mild hydrothermal conditions.

References

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9. 0.407 g of ZnO was dispersed in 9 ml of water and 0.365 g of HCl and 0.98 g of 85 wt% of H₃PO₄ were added to the mixture and stirred for 10 min. To this mixture 0.516 g of diethylenetriamine (DETA) was added and the mixture homogenized, transferred into a Parr pressure bomb and heated initially at 150 °C for 5 days which resulted in the formation of a large number of needles. The final composition of the mixture was ZnO ∶ 2H₃PO₄∶ 2HCl ∶ DETA ∶ 80H₂O.
10. Crystal data for 1:[NH₃(CH₂)₂NH₂(CH₂)₂NH₃]³⁺[Zn₄(PO₄)₃(H- PO₄)]^3–· H₂O, M = 766.6(1), monoclinic, space group =P2₁(no. 4), a= 10.021(4), b= 8.286(3), c= 11.856(7)Å, β= 103.13(1)°, V= 958.7(7)ų, Z= 9, D_c= 2.655 g cm^–3, µ(Mo-Ka)= 5.37 mm^–1, Mo-Kαradiation, λ= 0.71073 Å, 1.76 < θ < 23.26°. Data collection was performed using a Siemens SMART-CCD diffractometer. A total of 4056 data were collected and were merged to give 2565 unique reflections of which 2217 were considered to be observed [I > 2σ(I)]. The structure was solved and refined using SHELXTL-PLUS package of program against |F²|. Final R= 0.054, R_w= 0.13, S(goodness of fit)= 0.838 were obtained for all the data and 289 parameters. The final Fourier map had a minimum and maximum of–0.880 and 0.897 e Å^–3, respectively. CCDC 182/1109.
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