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DOI: 10.1039/A806417B (Paper) Reference Section for: Chem. Commun., 1998, 2181-2182

A simple ladder tin phosphate and its layered relative

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S. Ayyappan, X. Bu and Anthony K. Cheetham

Abstract

A simple ladder tin phosphate built up of the 4-membered cyclic tecton, [Sn2P2O4], is described along with a related layered material.

References

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  6. (a) 2.06 g of tin(II) oxalate were dispersed in 10 ml of water and 1.8 g of 85 wt% H3PO4 were added to the mixture under continuous stirring. 2 g of DABCO were added to the above and stirred until homogeneous. The composition of the mixture was SnC2O4∶1.5H3PO4∶1.8DABCO∶45H2O. The mixture was heated initially at 150 °C for 2 days and finally at 180 °C for 2 days and the product contained large quantities of platelike single crystals; (b) 2.06 g of tin(II) oxalate, 2.81 ml of DEED, 5 ml of water and 5 ml of ethylene glycol were mixed together and stirred for 10 min. To this mixture 1.53 g of 85 wt% H3PO4 were added and the mixture homogenized and heated at 150 °C for 2 days. The final composition of the mixture was SnC2O4∶1.95DEED∶27.5H2O∶8glycol∶1.3H3PO4.
  7. (a) Crystal data for I: [C6N2H14]2+2[SnPO4]–·H2O, M= 559.4, monoclinic, space group C2/c, a= 18.539(2), b= 8.105(1), c= 10.203(1)Å, β= 98.9(2)°, V= 1514.4(1)Å3, Z= 4, Dc= 2.52 g cm–3, T= 298 K, µ(Mo-Kα)= 3.57 mm–1, R= 0.068, Rw= 0.076 for 717 data with F≥3σ(F); (b) Crystal data for II: [C6N2H18]2+2[SnPO4]–, M= 271.4, monoclinic, space group C2/m, a= 17.938(1), b= 4.883(1), c= 10.814(1)Å, β= 116.9(1)°, V= 844.3(1)Å 3 , Z= 2, Dc= 2.15 g cm–3, T= 298 K, µ(Mo-Kα)= 3.2 mm–1 , R= 0.057, Rw= 0.14 for 834 data with F≥2σ(F); two of the oxygens bonded to the phosphorous are disordered with a site occupancy factor of 0.5. CCDC 182/1004.
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