Lanthanide(III)/Pyrimidine-4,6-dicarboxylate/Oxalate Extended Frameworks: A Detailed Study Based on the Lanthanide Contraction and Temperature Effects
Authors:Cepeda, Javier; Balda, Rolindes; Beobide, Garikoitz; Castillo, Oscar; Fernandez, Joaquin; Luque, Antonio; Perez-Yanez, Sonia; Roman, Pascual; Vallejo-Sanchez, Daniel
Journal:Inorganic Chemistry 50 8437-8451 (2011)
DOI:https://doi.org/10.1021/ic201013v
B-IncStrDB ID: 10382EoKH1L Entry date: 2015-02-19 Last revision: 2021-12-12
3-Ho
Chemical data
Full Name: poly-{[(mu-oxalato)bis(mu3-pyrimidine-4,6-dicarboxylato)-k2N,O:k2N',O':kO'')- tetraacuadiholmium(III)] - water (1/2.33)} [ Help ]
Formula moiety: C7 H6 Ho N2 O8, 2.33(H2O) [ Help ]
Structural Formula: C7 H6 Ho N2 O8, 2.33(H2O) [ Help ]
Structural Formula Sum: C7 H10.66 Ho N2 O10.33 [ Help ]
Formula weight: 453.04 Da [ Help ]
Crystallographic data and experimental details
Crystal system: monoclinic [ Help ]
Superspace group name: P21/n(α0γ)0s [ Help ]
a: 9.6219(3) Å [ Help ]
b: 15.8216(4) Å [ Help ]
c: 7.9375(2) Å [ Help ]
α: 90.0 ° [ Help ]
β: 96.625(3) ° [ Help ]
γ: 90.0 ° [ Help ]
Volume: 1200.3(1) Å3 [ Help ]
Modulation dimension: 1 [ Help ]
Z: 4 [ Help ]
Cell measurement temperature: 100.0(2) K [ Help ]
Cell determination reflection Nb.: 29616 [ Help ]
θ(min) for cell determination: 2.88 ° [ Help ]
θ(max) for cell determination: 30.07 ° [ Help ]
μ: 6.666 mm-1 [ Help ]
Absorption correction type: numerical [ Help ]
Absorption correction remarks: CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. [ Help ]
Minimum transmission factor: 0.246 [ Help ]
Maximum transmission factor: 0.615 [ Help ]
Symmetry operations of the superspace group: (Show/hide table) [ Help ]
| Operation code | Operation in algebraic form |
|---|---|
| 1 | x1,x2,x3,x4 |
| 2 | -x1+1/2,x2+1/2,-x3+1/2,-x4+1/2 |
| 3 | -x1,-x2,-x3,-x4 |
| 4 | x1+1/2,-x2+1/2,x3+1/2,x4+1/2 |
Measured independent wave vectors: (Show/hide table) [ Help ]
| Wave vector id | q_x | q_y | q_z |
|---|---|---|---|
| 1 | 0.0 | 0.0 | 0.33333 |
Refinement details
Total nb. of reflections: 10567 [ Help ]
Nb. of observed reflections: 5146 [ Help ]
Intense reflections threshold: I>3σ(I) [ Help ]
Refinement based on: F [ Help ]
Weighting scheme: sigma [ Help ]
Weighting scheme remarks: w=1/(σ2(F)+0.0001F2) [ Help ]
Refinement of hydrogen atoms: constr [ Help ]
Extinction method: none [ Help ]
Nb. of reflections: 10567 [ Help ]
Nb. of parameters: 322 [ Help ]
R(obs): 0.0412 [ Help ]
wR(obs): 0.0428 [ Help ]
R(all): 0.0799 [ Help ]
wR(all): 0.0457 [ Help ]
S(all): 1.23 [ Help ]
S(obs): 1.68 [ Help ]
Δ/σ(max): 0.0398 [ Help ]
Δ/σ(mean): 0.0029 [ Help ]
Δρ(max): 4.21 e_Å-3 [ Help ]
Δρ(min): -2.37 e_Å-3 [ 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 |
|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Ho1 | Ho | 0.866924(17) | 0.672765(11) | 0.07276(2) | Uani | 0.00677(4) | 4 | 1.0 | d | ? | ? | ? |
| O171 | O | 0.7084(3) | 0.57069(16) | -0.0515(3) | Uani | 0.0109(7) | 4 | 1.0 | d | ? | ? | ? |
| O3w | O | 0.6298(3) | 0.9249(2) | 0.0407(4) | Uani | 0.0246(11) | 4 | 1.0 | d | ? | ? | ? |
| O182 | O | 1.1091(3) | 0.68988(16) | 0.1439(3) | Uani | 0.0109(7) | 4 | 1.0 | d | ? | ? | ? |
| O21 | O | 0.9436(3) | 0.53773(16) | 0.187(3) | Uani | 0.0111(8) | 4 | 1.0 | d | ? | ? | ? |
| O181 | O | 0.6874(3) | 0.73746(17) | -0.1236(3) | Uani | 0.0103(7) | 4 | 1.0 | d | ? | ? | ? |
| O2w | O | 0.84(3) | 0.8166(16) | 0.1517(3) | Uani | 0.014(8) | 4 | 1.0 | d | ? | ? | ? |
| O23 | O | 0.9774(3) | 0.58974(16) | -0.1273(3) | Uani | 0.0091(7) | 4 | 1.0 | d | ? | ? | ? |
| O1w | O | 0.8983(3) | 0.67869(18) | 0.3793(3) | Uani | 0.0144(8) | 4 | 1.0 | d | ? | ? | ? |
| N11 | N | 0.6257(3) | 0.67276(19) | 0.1828(3) | Uani | 0.0074(8) | 4 | 1.0 | d | ? | ? | ? |
| N13 | N | 0.9522(3) | 0.76502(19) | -0.1688(4) | Uani | 0.0085(8) | 4 | 1.0 | d | ? | ? | ? |
| C16 | C | 0.5271(3) | 0.6321(2) | 0.0819(4) | Uani | 0.0061(9) | 4 | 1.0 | d | ? | ? | ? |
| C18 | C | 0.7042(4) | 0.7829(2) | -0.2487(4) | Uani | 0.0071(9) | 4 | 1.0 | d | ? | ? | ? |
| C15 | C | 0.3862(3) | 0.6414(2) | 0.1005(4) | Uani | 0.0071(9) | 4 | 1.0 | d | ? | ? | ? |
| C14 | C | 0.3527(4) | 0.695(2) | 0.2253(4) | Uani | 0.0066(9) | 4 | 1.0 | d | ? | ? | ? |
| O4w | O | 0.7552(5) | 0.5744(2) | 0.5662(4) | Uani | 0.0306(14) | 4 | 1.0 | d | ? | ? | ? |
| O172 | O | 0.4886(3) | 0.55561(16) | -0.1752(3) | Uani | 0.0109(7) | 4 | 1.0 | d | ? | ? | ? |
| C17 | C | 0.5774(4) | 0.5811(2) | -0.0604(4) | Uani | 0.0067(9) | 4 | 1.0 | d | ? | ? | ? |
| C12 | C | 1.0845(4) | 0.778(2) | -0.1966(4) | Uani | 0.0099(10) | 4 | 1.0 | d | ? | ? | ? |
| C22 | C | 0.9901(3) | 0.485(2) | 0.0912(4) | Uani | 0.0065(9) | 4 | 1.0 | d | ? | ? | ? |
| H15 | H | 0.315038 | 0.612087 | 0.0314 | Uiso | 0.0075 | 4 | 1.0 | d | ? | ? | ? |
| H12 | H | 1.15293 | 0.751475 | -0.117373 | Uiso | 0.0088 | 4 | 1.0 | d | ? | ? | ? |
| O5w | O | 0.5 | 0.5 | 0.5 | Uani | 0.021(2) | 2 | 0.5 | d | ? | ? | ? |
ADP components: (Show/hide table) [ Help ]
| Atom site label | Atom site symbol | U11 | U22 | U33 | U12 | U13 | U23 |
|---|---|---|---|---|---|---|---|
| Ho1 | Ho | 0.00379(7) | 0.00879(8) | 0.00762(8) | 0.0008(8) | 0.00019(5) | -0.00052(8) |
| O171 | O | 0.0062(12) | 0.0124(14) | 0.0143(13) | -0.0016(11) | 0.0017(10) | -0.0025(10) |
| O3w | O | 0.015(17) | 0.037(2) | 0.0199(18) | 0.0121(17) | -0.0065(15) | -0.014(16) |
| O182 | O | 0.004(11) | 0.0168(15) | 0.0117(12) | -0.0001(10) | -0.0003(10) | -0.0025(10) |
| O21 | O | 0.0115(13) | 0.0123(14) | 0.0095(12) | 0.0054(11) | 0.0018(10) | 0.0009(10) |
| O181 | O | 0.0054(11) | 0.0154(14) | 0.0099(12) | -0.0009(11) | -0.0002(10) | 0.0032(10) |
| O2w | O | 0.0152(13) | 0.0101(14) | 0.0161(14) | 0.0007(11) | -0.0003(11) | -0.0034(10) |
| O23 | O | 0.0089(12) | 0.0098(13) | 0.0084(11) | 0.0003(10) | 0.0002(10) | 0.0012(10) |
| O1w | O | 0.0116(13) | 0.0236(16) | 0.0076(12) | 0.004(13) | -0.0012(10) | -0.0071(12) |
| N11 | N | 0.006(13) | 0.0092(13) | 0.0071(12) | -0.0008(13) | 0.0013(10) | 0.0026(12) |
| N13 | N | 0.0079(14) | 0.009(15) | 0.0088(14) | 0.0004(12) | 0.002(12) | -0.001(11) |
| C16 | C | 0.0079(15) | 0.0043(16) | 0.0063(15) | 0.0012(13) | 0.0011(13) | 0.0019(12) |
| C18 | C | 0.0079(15) | 0.0069(17) | 0.0067(15) | 0.0013(13) | 0.0016(13) | -0.0038(12) |
| C15 | C | 0.0072(16) | 0.0081(15) | 0.0054(16) | -0.0016(13) | -0.0018(13) | 0.0012(12) |
| C14 | C | 0.0074(15) | 0.0057(16) | 0.0067(15) | -0.0017(12) | 0.0011(13) | 0.0036(12) |
| O4w | O | 0.031(3) | 0.039(2) | 0.022(2) | -0.009(2) | 0.0026(19) | -0.0036(17) |
| O172 | O | 0.0091(12) | 0.0131(13) | 0.0102(12) | 0.0013(10) | -0.0004(10) | -0.0014(10) |
| C17 | C | 0.0089(16) | 0.0051(16) | 0.0071(15) | 0.0004(13) | 0.0044(13) | 0.0019(12) |
| C12 | C | 0.0069(16) | 0.0109(18) | 0.0114(16) | 0.0011(14) | -0.0002(14) | 0.0003(14) |
| C22 | C | 0.0021(14) | 0.0095(17) | 0.0079(15) | -0.0004(13) | 0.0002(13) | 0.0001(13) |
| O5w | O | 0.025(4) | 0.024(3) | 0.016(3) | 0.002(3) | 0.009(3) | -0.005(2) |
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 | 0.0 | 0.0 | 0.33333 |
Occupation crenel coefficients: (Show/hide table) [ Help ]
| Atom site label | Center (x0) | Width |
|---|---|---|
| O5w | 0.0 | 0.5 |
Definition of the displacive (translational) Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Displacement axis | Wave vector code |
|---|---|---|---|
| Ho1x1 | Ho1 | x | 1 |
| Ho1y1 | Ho1 | y | 1 |
| Ho1z1 | Ho1 | z | 1 |
| O171x1 | O171 | x | 1 |
| O171y1 | O171 | y | 1 |
| O171z1 | O171 | z | 1 |
| O3wx1 | O3w | x | 1 |
| O3wy1 | O3w | y | 1 |
| O3wz1 | O3w | z | 1 |
| O182x1 | O182 | x | 1 |
| O182y1 | O182 | y | 1 |
| O182z1 | O182 | z | 1 |
| O21x1 | O21 | x | 1 |
| O21y1 | O21 | y | 1 |
| O21z1 | O21 | z | 1 |
| O181x1 | O181 | x | 1 |
| O181y1 | O181 | y | 1 |
| O181z1 | O181 | z | 1 |
| O2wx1 | O2w | x | 1 |
| O2wy1 | O2w | y | 1 |
| O2wz1 | O2w | z | 1 |
| O23x1 | O23 | x | 1 |
| O23y1 | O23 | y | 1 |
| O23z1 | O23 | z | 1 |
| O1wx1 | O1w | x | 1 |
| O1wy1 | O1w | y | 1 |
| O1wz1 | O1w | z | 1 |
| N11x1 | N11 | x | 1 |
| N11y1 | N11 | y | 1 |
| N11z1 | N11 | z | 1 |
| N13x1 | N13 | x | 1 |
| N13y1 | N13 | y | 1 |
| N13z1 | N13 | z | 1 |
| C16x1 | C16 | x | 1 |
| C16y1 | C16 | y | 1 |
| C16z1 | C16 | z | 1 |
| C18x1 | C18 | x | 1 |
| C18y1 | C18 | y | 1 |
| C18z1 | C18 | z | 1 |
| C15x1 | C15 | x | 1 |
| C15y1 | C15 | y | 1 |
| C15z1 | C15 | z | 1 |
| C14x1 | C14 | x | 1 |
| C14y1 | C14 | y | 1 |
| C14z1 | C14 | z | 1 |
| O4wx1 | O4w | x | 1 |
| O4wy1 | O4w | y | 1 |
| O4wz1 | O4w | z | 1 |
| O172x1 | O172 | x | 1 |
| O172y1 | O172 | y | 1 |
| O172z1 | O172 | z | 1 |
| C17x1 | C17 | x | 1 |
| C17y1 | C17 | y | 1 |
| C17z1 | C17 | z | 1 |
| C12x1 | C12 | x | 1 |
| C12y1 | C12 | y | 1 |
| C12z1 | C12 | z | 1 |
| C22x1 | C22 | x | 1 |
| C22y1 | C22 | y | 1 |
| C22z1 | C22 | z | 1 |
| H15x1 | H15 | x | 1 |
| H15y1 | H15 | y | 1 |
| H15z1 | H15 | z | 1 |
| H12x1 | H12 | x | 1 |
| H12y1 | H12 | y | 1 |
| H12z1 | H12 | z | 1 |
| O5wx1 | O5w | x | 1 |
| O5wy1 | O5w | y | 1 |
| O5wz1 | O5w | z | 1 |
Displacive (translational) Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| Ho1x1 | 0.00226(4) | 0.00077(5) |
| Ho1y1 | 0.003416(19) | -0.008299(17) |
| Ho1z1 | -0.00662(4) | -0.00511(5) |
| O171x1 | 0.0034(6) | -0.0011(6) |
| O171y1 | -0.0004(3) | -0.0091(3) |
| O171z1 | -0.0045(7) | -0.0008(7) |
| O3wx1 | 0.0025(7) | -0.0143(6) |
| O3wy1 | 0.0054(3) | -0.0268(3) |
| O3wz1 | -0.0056(7) | 0.0274(7) |
| O182x1 | 0.0028(6) | 0.0015(6) |
| O182y1 | 0.0043(3) | -0.0041(3) |
| O182z1 | -0.0085(6) | -0.0067(6) |
| O21x1 | 0.0068(6) | 0.0062(6) |
| O21y1 | 0.0075(3) | -0.0048(3) |
| O21z1 | 0.0031(6) | -0.0033(6) |
| O181x1 | 0.0006(6) | -0.0005(6) |
| O181y1 | -0.0028(3) | -0.0103(3) |
| O181z1 | -0.0073(7) | -0.0018(6) |
| O2wx1 | -0.0026(7) | 0.0056(7) |
| O2wy1 | 0.0049(3) | -0.0068(3) |
| O2wz1 | -0.0103(6) | -0.0063(7) |
| O23x1 | 0.0059(6) | -0.0003(6) |
| O23y1 | -0.0035(3) | -0.0075(3) |
| O23z1 | -0.0044(6) | -0.0023(6) |
| O1wx1 | 0.0032(7) | 0.0051(7) |
| O1wy1 | 0.0123(3) | -0.0007(3) |
| O1wz1 | -0.0053(6) | -0.0065(6) |
| N11x1 | 0.0028(8) | 0.0029(8) |
| N11y1 | 0.0013(3) | -0.0065(3) |
| N11z1 | 0.0001(8) | -0.0025(8) |
| N13x1 | -0.0005(8) | -0.0027(7) |
| N13y1 | -0.0006(3) | -0.0057(3) |
| N13z1 | -0.0067(8) | -0.0001(8) |
| C16x1 | 0.0018(9) | 0.0009(8) |
| C16y1 | 0.0012(4) | -0.0058(4) |
| C16z1 | -0.0019(9) | -0.0048(8) |
| C18x1 | -0.003(9) | -0.0015(9) |
| C18y1 | 0.0007(4) | -0.0055(4) |
| C18z1 | -0.0007(9) | 0.0053(9) |
| C15x1 | 0.0026(9) | 0.0013(8) |
| C15y1 | 0.001(4) | -0.0059(4) |
| C15z1 | -0.0041(9) | -0.0058(8) |
| C14x1 | 0.0019(8) | 0.0003(8) |
| C14y1 | 0.0007(4) | -0.0056(4) |
| C14z1 | 0.0025(8) | -0.004(8) |
| O4wx1 | 0.0071(7) | 0.0633(6) |
| O4wy1 | 0.007(4) | -0.0184(4) |
| O4wz1 | -0.0229(7) | -0.0094(7) |
| O172x1 | 0.0012(6) | -0.0016(6) |
| O172y1 | -0.0012(3) | -0.0064(3) |
| O172z1 | -0.0037(7) | -0.0013(6) |
| C17x1 | 0.004(9) | 0.0001(9) |
| C17y1 | -0.0004(4) | -0.0078(4) |
| C17z1 | -0.0034(9) | -0.0041(9) |
| C12x1 | -0.0013(9) | -0.0024(9) |
| C12y1 | 0.0003(4) | -0.0075(4) |
| C12z1 | -0.005(10) | 0.0008(9) |
| C22x1 | -0.0002(9) | 0.0041(8) |
| C22y1 | 0.0032(4) | -0.0079(4) |
| C22z1 | 0.002(9) | -0.0038(9) |
| H15x1 | 0.0022 | -0.0002 |
| H15y1 | 0.0026 | -0.0061 |
| H15z1 | -0.0108 | -0.0082 |
| H12x1 | 0.0006 | -0.0016 |
| H12y1 | 0.0017 | -0.0114 |
| H12z1 | -0.0082 | -0.0017 |
| O5wx1 | 0.0 | 0.0625(11) |
| O5wy1 | 0.0 | 0.0579(6) |
| O5wz1 | 0.0 | -0.0249(11) |
Definition of the ADP Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Tensor element | Wave vector code |
|---|---|---|---|
| Ho1U111 | Ho1 | U11 | 1 |
| Ho1U221 | Ho1 | U22 | 1 |
| Ho1U331 | Ho1 | U33 | 1 |
| Ho1U121 | Ho1 | U12 | 1 |
| Ho1U131 | Ho1 | U13 | 1 |
| Ho1U231 | Ho1 | U23 | 1 |
ADP Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| Ho1U111 | -0.0003(2) | 0.00059(18) |
| Ho1U221 | -0.00514(15) | 0.00155(15) |
| Ho1U331 | -0.0023(16) | -0.00013(15) |
| Ho1U121 | -1.0e-05(10) | -0.00048(12) |
| Ho1U131 | -0.00018(16) | -0.00091(14) |
| Ho1U231 | 0.00102(10) | -0.00582(12) |