Crystal Structures of Incommensurately Modulated Ln(PO3)3 (Ln=Tb-Yb) and Commensurate Gd(PO3)3 and Lu(PO3)3
Authors:Hoppe, Henning A.; Sedlmaier, Stefan J.
Journal:Inorganic Chemistry 46 3467-3474 (2007)
DOI:https://doi.org/10.1021/ic0616030
B-IncStrDB ID: qLtANQxiE5A Entry date: 2024-03-07 Last revision: 2024-03-07
dyp3o9
Chemical data
Common Name: dysprosium metaphosphat [ Help ]
Structural Formula Sum: Dy1 O9 P3 [ Help ]
Formula weight: 399.4 Da [ Help ]
Crystallographic data and experimental details
Crystal system: monoclinic [ Help ]
Space group name (H-M): Cc [ Help ]
Superspace group name: Cc(0β0)0 [ Help ]
Symmetry operations of the superspace group: (Show/hide table) [ Help ]
| Operation code | Operation in algebraic form |
|---|---|
| 1 | x1,x2,x3,x4 |
| 2 | x1,-x2,1/2+x3,-x4 |
| 3 | 1/2+x1,1/2+x2,x3,x4 |
| 4 | 1/2+x1,1/2-x2,1/2+x3,-x4 |
a: 14.174(3) Å [ Help ]
b: 6.7095(14) Å [ Help ]
c: 10.095(3) Å [ Help ]
α: 90 ° [ Help ]
β: 127.624(16) ° [ Help ]
γ: 90 ° [ Help ]
Volume: 760.3(4) Å3 [ Help ]
Modulation dimension: 1 [ Help ]
Measured independent wave vectors: (Show/hide table) [ Help ]
| Wave vector id | q_x | q_y | q_z |
|---|---|---|---|
| 1 | 0.00000 | 0.36400 | 0.00000 |
Z: 4 [ Help ]
Cell determination reflection Nb.: 2000 [ Help ]
θ(min) for cell determination: 2.65 ° [ Help ]
θ(max) for cell determination: 30.07 ° [ Help ]
Cell measurement temperature: 293 K [ Help ]
μ: 10.481 mm-1 [ Help ]
Absorption correction type: none [ Help ]
Minimum transmission factor: 1.000 [ Help ]
Maximum transmission factor: 1.000 [ Help ]
Refinement details
Total nb. of reflections: 6492 [ Help ]
Nb. of observed reflections: 1868 [ Help ]
Intense reflections threshold: I>3σ(I) [ Help ]
Refinement based on: Fsqd [ Help ]
R(obs): 0.0574 [ Help ]
wR(obs): 0.0707 [ Help ]
R(all): 0.1981 [ Help ]
wR(all): 0.0921 [ Help ]
S(all): 1.04 [ Help ]
S(obs): 1.54 [ Help ]
Nb. of reflections: 6492 [ Help ]
Nb. of parameters: 196 [ Help ]
Number of restraints: 32 [ Help ]
Weighting scheme: sigma [ Help ]
Weighting scheme remarks: w=1/σ2(I) [ Help ]
Δ/σ(max): 0.0247 [ Help ]
Δ/σ(mean): 0.0053 [ Help ]
Δρ(max): 0.64 e_Å-3 [ Help ]
Δρ(min): -0.66 e_Å-3 [ Help ]
Extinction method: JANA2000 [ Help ]
Extinction coefficient: 0.0081(5) [ Help ]
Absolute structure remarks: Flack H D (1983), Acta Cryst. A39, 876-881 [ Help ]
Flack parameter: 0.26(4) [ Help ]
Structural Information
Average Structure: (Show/hide table) [ Help ]
| Atom site label | Atom symbol | x | y | z | ADP type | Uiso/equiv | Symmetry multiplicity | Occupancy | Coords from (d)iffraction or (c)alculated | Coords restraints or constraints | Disordered cluster | Disordered group |
|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Dy1 | Dy | -0.4471 | 0.2490(4) | -0.247 | Uani | 0.0327(2) | 4 | 1 | d | . | . | . |
| P1 | P | -0.2869(7) | 0.8952(9) | -0.9010(8) | Uani | 0.025(3) | 4 | 1 | d | . | . | . |
| P2 | P | -0.1939(10) | 0.5845(3) | -0.9998(15) | Uani | 0.0324(15) | 4 | 1 | d | . | . | . |
| P3 | P | -0.0974(7) | 0.9022(10) | -1.0834(9) | Uani | 0.032(3) | 4 | 1 | d | . | . | . |
| O12 | O | -0.2402(12) | 0.705(2) | -0.9203(16) | Uani | 0.050(9) | 4 | 1 | d | . | . | . |
| O23 | O | -0.1951(7) | 0.733(2) | -1.1195(12) | Uani | 0.025(4) | 4 | 1 | d | . | . | . |
| O31 | O | -0.1659(14) | 1.024(3) | -1.238(2) | Uani | 0.102(11) | 4 | 1 | d | . | . | . |
| O101 | O | -0.3640(12) | 0.840(3) | -0.869(2) | Uani | 0.052(9) | 4 | 1 | d | . | . | . |
| O102 | O | -0.3247(15) | 1.022(2) | -1.0373(19) | Uani | 0.061(10) | 4 | 1 | d | . | . | . |
| O201 | O | -0.0958(14) | 0.470(2) | -0.894(2) | Uani | 0.035(9) | 4 | 1 | d | . | . | . |
| O202 | O | -0.3088(17) | 0.487(3) | -1.1328(18) | Uani | 0.093(9) | 4 | 1 | d | . | . | . |
| O301 | O | -0.0604(15) | 1.029(3) | -0.942(2) | Uani | 0.069(11) | 4 | 1 | d | . | . | . |
| O302 | O | 0.0018(13) | 0.822(2) | -1.091(2) | Uani | 0.065(9) | 4 | 1 | d | . | . | . |
ADP components: (Show/hide table) [ Help ]
| Atom site label | Atom site symbol | U11 | U22 | U33 | U12 | U13 | U23 |
|---|---|---|---|---|---|---|---|
| Dy1 | Dy | 0.0293(2) | 0.0352(3) | 0.0382(3) | 0.0029(4) | 0.02294(19) | 0.0047(3) |
| P1 | P | 0.019(3) | 0.035(3) | 0.012(2) | 0.003(2) | 0.006(2) | 0.006(2) |
| P2 | P | 0.0384(17) | 0.0240(14) | 0.0455(15) | 0.000(3) | 0.0311(12) | 0.001(4) |
| P3 | P | 0.028(3) | 0.039(4) | 0.029(3) | 0.005(3) | 0.018(2) | 0.011(3) |
| O12 | O | 0.037(11) | 0.054(9) | 0.031(7) | 0.028(7) | 0.008(7) | 0.002(5) |
| O23 | O | 0.015(4) | 0.035(6) | 0.024(4) | -0.006(5) | 0.011(3) | -0.008(5) |
| O31 | O | 0.067(15) | 0.123(11) | 0.051(6) | -0.041(10) | 0.003(9) | 0.057(7) |
| O101 | O | 0.027874 | 0.027874 | 0.027874 | 0 | 0.017016 | 0 |
| O102 | O | 0.025906 | 0.025906 | 0.025906 | 0 | 0.015815 | 0 |
| O201 | O | 0.018608 | 0.018608 | 0.018608 | 0 | 0.01136 | 0 |
| O202 | O | 0.067(10) | 0.126(14) | 0.028(6) | -0.026(9) | -0.001(6) | 0.016(7) |
| O301 | O | 0.055(10) | 0.086(13) | 0.098(12) | 0.023(8) | 0.063(10) | 0.011(9) |
| O302 | O | 0.059(9) | 0.036(9) | 0.064(8) | 0.001(7) | 0.018(7) | -0.003(7) |
Fourier Wave Vectors (explicit: q_x,q_y,q_z or coefficients: q_1,q_2,...): (Show/hide table) [ Help ]
| Wave vector code | q_x | q_y | q_z |
|---|---|---|---|
| 1 | 0.00000 | 0.36400 | 0.00000 |
Definition of the displacive (translational) Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Displacement axis | Wave vector code |
|---|---|---|---|
| Dy1x1 | Dy1 | x | 1 |
| Dy1y1 | Dy1 | y | 1 |
| Dy1z1 | Dy1 | z | 1 |
| P1x1 | P1 | x | 1 |
| P1y1 | P1 | y | 1 |
| P1z1 | P1 | z | 1 |
| P2x1 | P2 | x | 1 |
| P2y1 | P2 | y | 1 |
| P2z1 | P2 | z | 1 |
| P3x1 | P3 | x | 1 |
| P3y1 | P3 | y | 1 |
| P3z1 | P3 | z | 1 |
| O12x1 | O12 | x | 1 |
| O12y1 | O12 | y | 1 |
| O12z1 | O12 | z | 1 |
| O23x1 | O23 | x | 1 |
| O23y1 | O23 | y | 1 |
| O23z1 | O23 | z | 1 |
| O31x1 | O31 | x | 1 |
| O31y1 | O31 | y | 1 |
| O31z1 | O31 | z | 1 |
| O101x1 | O101 | x | 1 |
| O101y1 | O101 | y | 1 |
| O101z1 | O101 | z | 1 |
| O102x1 | O102 | x | 1 |
| O102y1 | O102 | y | 1 |
| O102z1 | O102 | z | 1 |
| O201x1 | O201 | x | 1 |
| O201y1 | O201 | y | 1 |
| O201z1 | O201 | z | 1 |
| O202x1 | O202 | x | 1 |
| O202y1 | O202 | y | 1 |
| O202z1 | O202 | z | 1 |
| O301x1 | O301 | x | 1 |
| O301y1 | O301 | y | 1 |
| O301z1 | O301 | z | 1 |
| O302x1 | O302 | x | 1 |
| O302y1 | O302 | y | 1 |
| O302z1 | O302 | z | 1 |
Displacive (translational) Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| Dy1x1 | 0.00165(10) | -0.0012(3) |
| Dy1y1 | -0.03247(10) | -0.0025(6) |
| Dy1z1 | 0.02178(12) | 0.0000(5) |
| P1x1 | 0.0147(5) | -0.0201(6) |
| P1y1 | -0.0142(9) | 0.0155(11) |
| P1z1 | 0.0234(6) | -0.0215(9) |
| P2x1 | -0.0067(5) | -0.0127(5) |
| P2y1 | 0.0048(12) | -0.0161(11) |
| P2z1 | -0.0040(6) | 0.0125(7) |
| P3x1 | 0.0123(5) | -0.0080(7) |
| P3y1 | 0.0105(10) | -0.0382(12) |
| P3z1 | 0.0126(7) | 0.0010(9) |
| O12x1 | -0.0223(8) | -0.0319(9) |
| O12y1 | -0.0185(13) | 0.0048(12) |
| O12z1 | -0.0206(11) | -0.0216(11) |
| O23x1 | -0.0108(8) | -0.0115(9) |
| O23y1 | 0.0249(12) | -0.0388(14) |
| O23z1 | -0.0069(11) | -0.0012(11) |
| O31x1 | 0.0290(6) | 0.0081(8) |
| O31y1 | 0.0302(17) | -0.0304(17) |
| O31z1 | 0.0166(11) | 0.0060(13) |
| O101x1 | 0.0223(12) | -0.0339(11) |
| O101y1 | 0.014(2) | 0.037(2) |
| O101z1 | 0.0458(17) | -0.0414(19) |
| O102x1 | 0.0122(14) | -0.0001(13) |
| O102y1 | -0.007(2) | 0.023(2) |
| O102z1 | 0.0313(17) | -0.0012(17) |
| O201x1 | 0.0046(8) | -0.0195(8) |
| O201y1 | 0.0395(16) | -0.0262(18) |
| O201z1 | 0.0217(15) | 0.0332(14) |
| O202x1 | 0.0041(7) | -0.0122(9) |
| O202y1 | -0.0370(19) | -0.011(2) |
| O202z1 | 0.0035(18) | 0.0098(18) |
| O301x1 | 0.0133(15) | -0.0007(15) |
| O301y1 | 0.028(3) | -0.030(3) |
| O301z1 | 0.008(2) | 0.005(2) |
| O302x1 | 0.0148(12) | -0.0124(12) |
| O302y1 | -0.032(2) | -0.043(2) |
| O302z1 | 0.0352(17) | -0.005(2) |