TY - JOUR
T1 - Synthesis, open-framework structure and thermal behaviour of ammonium tin oxalate, Sn2(NH4)2(C2O4) 3.3H2O
AU - Audebrand, Nathalie
AU - Vaillant, Marie Laure
AU - Auffrédic, Jean Paul
AU - Louër, Daniel
PY - 2001
Y1 - 2001
N2 - A new mixed ammonium tin oxalate trihydrate, Sn2(NH4)2(C2O4) 3.3H2O, has been prepared from evaporation of a solution of tin and ammonium oxalates. Its crystal structure has been solved from single-crystal diffraction data. The symmetry is orthorhombic, space group Pnma (No. 62), cell dimensions a = 15.1821(5) Å, b = 11.7506(2) Å, c = 10.8342(3) Å, and Z = 4. The structure consists of macroanionic layers built from [Sn(C2O4)3]2- groups. The SnO6 polyhedron can be described as a pseudo pentagonal bipyramid, with the lone pair of electrons presumably occupying one apex. The resulting framework displays holes in which the water molecules and ammonium groups are located. The thermal behaviour of the mixed ammonium tin oxalate has been investigated with temperature-dependent X-ray powder diffraction and conventional thermal analysis. The degradation process has been completely explained, as well as that of oxammite, a phase always obtained in the preparations. The thermal decomposition of oxammite leads to (NH4)2C2O4 and a new acid salt, NH4HC2O4. The mixed ammonium tin oxalate decomposes successively into the amorphous compounds, Sn2(NH4)2(C2O4) 3.H2O and Sn2(NH4)2(C2O4) 3, SnC2O4and, finally, cassiterite SnO2.
AB - A new mixed ammonium tin oxalate trihydrate, Sn2(NH4)2(C2O4) 3.3H2O, has been prepared from evaporation of a solution of tin and ammonium oxalates. Its crystal structure has been solved from single-crystal diffraction data. The symmetry is orthorhombic, space group Pnma (No. 62), cell dimensions a = 15.1821(5) Å, b = 11.7506(2) Å, c = 10.8342(3) Å, and Z = 4. The structure consists of macroanionic layers built from [Sn(C2O4)3]2- groups. The SnO6 polyhedron can be described as a pseudo pentagonal bipyramid, with the lone pair of electrons presumably occupying one apex. The resulting framework displays holes in which the water molecules and ammonium groups are located. The thermal behaviour of the mixed ammonium tin oxalate has been investigated with temperature-dependent X-ray powder diffraction and conventional thermal analysis. The degradation process has been completely explained, as well as that of oxammite, a phase always obtained in the preparations. The thermal decomposition of oxammite leads to (NH4)2C2O4 and a new acid salt, NH4HC2O4. The mixed ammonium tin oxalate decomposes successively into the amorphous compounds, Sn2(NH4)2(C2O4) 3.H2O and Sn2(NH4)2(C2O4) 3, SnC2O4and, finally, cassiterite SnO2.
KW - Ammonium tin oxalate
KW - Crystal structure
KW - Oxammite decomposition
KW - Synthesis
KW - Thermal behaviour
UR - http://www.scopus.com/inward/record.url?scp=0034977030&partnerID=8YFLogxK
U2 - 10.1016/S1293-2558(00)01148-1
DO - 10.1016/S1293-2558(00)01148-1
M3 - Article
AN - SCOPUS:0034977030
VL - 3
SP - 483
EP - 494
JO - Solid State Sciences
JF - Solid State Sciences
SN - 1293-2558
IS - 4
ER -