TY - JOUR
T1 - Synthesis and structural characterization of solid phases of the Sn(II) - Organophosphonate system
T2 - The 1-Dimensional [Sn(HO3PCH2PO3H)] · H2O and the 3-Dimensional [Sn2{O3PC(OH)(CH3)PO3}]
AU - Zapf, Pamela J.
AU - Rose, David J.
AU - Haushalter, Robert C.
AU - Zubieta, Jon
N1 - Funding Information:
The work at Syracuse University was supported by NSF Grant CHE 9318824.
PY - 1996/9/5
Y1 - 1996/9/5
N2 - The first Sn(II) - organophosphonate solid phases have been prepared and structurally characterized by single crystal X-ray diffraction. The one-dimensional species [Sn(HO3PCH2PO3H)] -H2O (1) was prepared conventionally from a mixture of SnCl2, CH2(PO3H2)2, and H2O in the mole ratio 1:2.9:8.17 kept at 4°C for 12 h. The three-dimensional phase [Sn2{O3PC(OH) (CH3)PO3}] (2) was prepared hydrothermally from a mixture of SnCl2, CH3C(OH)(PO3H)2, 1,4 diaminopropane · HCl, and H2O in the mole ratio 1:3.87:1.9:2215 with pH adjusted to 3.5 by addition of (CH3)4NOH, heated at 150°C for 135.5 h. Compound 1 consists of linear chains of {SnO3} pyramids bridged by (HO3PCH2PO3H)2- groups. The structure of 2 is a three-dimensional open framework. Crystal data: 1, triclinic P1 a = 4.8777(1) Å, b = 8.786(2) Å, c = 9.446(2) Å, α = 84.52(3)°, β = 78.78(3)°, γ = 74.39(3)°, V = 382.0(2) Å3, Z = 2, Dcalc = 2.701 g cm-3, structure solution and refinement based on 1059 reflections converged at R = 0.060; 2, monoclinic P21/c, a = 10.889(2) Å, b = 8.556(2) Å, c = 9.460(2) Å, β = 96.92(2)°, V = 874.9(4) Å3, Dcalc = 3.336 g cm-3, structure solution and refinement based on 1121 reflections, converged at R = 0.055.
AB - The first Sn(II) - organophosphonate solid phases have been prepared and structurally characterized by single crystal X-ray diffraction. The one-dimensional species [Sn(HO3PCH2PO3H)] -H2O (1) was prepared conventionally from a mixture of SnCl2, CH2(PO3H2)2, and H2O in the mole ratio 1:2.9:8.17 kept at 4°C for 12 h. The three-dimensional phase [Sn2{O3PC(OH) (CH3)PO3}] (2) was prepared hydrothermally from a mixture of SnCl2, CH3C(OH)(PO3H)2, 1,4 diaminopropane · HCl, and H2O in the mole ratio 1:3.87:1.9:2215 with pH adjusted to 3.5 by addition of (CH3)4NOH, heated at 150°C for 135.5 h. Compound 1 consists of linear chains of {SnO3} pyramids bridged by (HO3PCH2PO3H)2- groups. The structure of 2 is a three-dimensional open framework. Crystal data: 1, triclinic P1 a = 4.8777(1) Å, b = 8.786(2) Å, c = 9.446(2) Å, α = 84.52(3)°, β = 78.78(3)°, γ = 74.39(3)°, V = 382.0(2) Å3, Z = 2, Dcalc = 2.701 g cm-3, structure solution and refinement based on 1059 reflections converged at R = 0.060; 2, monoclinic P21/c, a = 10.889(2) Å, b = 8.556(2) Å, c = 9.460(2) Å, β = 96.92(2)°, V = 874.9(4) Å3, Dcalc = 3.336 g cm-3, structure solution and refinement based on 1121 reflections, converged at R = 0.055.
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U2 - 10.1006/jssc.1996.0283
DO - 10.1006/jssc.1996.0283
M3 - Article
AN - SCOPUS:0000623342
SN - 0022-4596
VL - 125
SP - 182
EP - 185
JO - Journal of Solid State Chemistry
JF - Journal of Solid State Chemistry
IS - 2
ER -