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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: 10162EQ1KcO Entry date: 2015-02-19 Last revision: 2022-01-02

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3-Gd

Chemical data

Full Name: poly-{[(mu-oxalato)bis(mu3-pyrimidine-4,6-dicarboxylato)-k2N,O:k2N',O':kO'')- tetraacuadigadolinium(III)] - water (1/2.33)} [ Help ]

Formula moiety: C7 H6 Gd N2 O8, 2.33(H2O) [ Help ]

Structural Formula: C7 H6 Gd N2 O8, 2.33(H2O) [ Help ]

Structural Formula Sum: C7 H10.66 Gd N2 O10.33 [ Help ]

Formula weight: 445.36 Da [ Help ]

Crystallographic data and experimental details

Crystal system: monoclinic [ Help ]

Superspace group name: P21/n(α0γ)0s [ Help ]

Symmetry operations of the superspace group: [ 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

a: 9.693(1) Å [ Help ]

b: 15.869(1) Å [ Help ]

c: 7.955(1) Å [ Help ]

α: 90 ° [ Help ]

β: 96.356(6) ° [ Help ]

γ: 90 ° [ Help ]

Volume: 1216.1(4) Å3 [ Help ]

Modulation dimension: 1 [ Help ]

Z: 4 [ Help ]

Cell measurement temperature: 100(2) K [ Help ]

Cell determination reflection Nb.: 36161 [ Help ]

θ(min) for cell determination: 2.87 ° [ Help ]

θ(max) for cell determination: 30.1 ° [ Help ]

Measured independent wave vectors: [ Help ]

Wave vector id q_x q_y q_z
1 0 0 0.33333

μ: 5.513 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: 0.435 [ Help ]

Maximum transmission factor: 0.818 [ Help ]

Refinement details

Total nb. of reflections: 10732 [ Help ]

Nb. of observed reflections: 6832 [ 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: 10732 [ Help ]

Nb. of parameters: 322 [ Help ]

R(obs): 0.0359 [ Help ]

wR(obs): 0.0417 [ Help ]

R(all): 0.0552 [ Help ]

wR(all): 0.043 [ Help ]

S(all): 1.47 [ Help ]

S(obs): 1.8 [ Help ]

Δ/σ(max): 0.0407 [ Help ]

Δ/σ(mean): 0.0017 [ Help ]

Δρ(max): 4.61 e_Å-3 [ Help ]

Δρ(min): -1.51 e_Å-3 [ Help ]

Structural Information

Average Structure: [ 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
Gd1 Gd 0.866108(14) 0.673077(9) 0.078551(17) Uani 0.00509(4) 4 1 d ? ? ?
O171 O 0.7058(2) 0.57072(13) -0.0483(3) Uani 0.0096(6) 4 1 d ? ? ?
O3w O 0.6283(3) 0.92543(16) 0.0416(3) Uani 0.0171(7) 4 1 d ? ? ?
O182 O 1.1105(2) 0.68917(13) 0.1491(3) Uani 0.009(6) 4 1 d ? ? ?
O21 O 0.9435(2) 0.53583(13) 0.188(3) Uani 0.009(6) 4 1 d ? ? ?
O181 O 0.687(2) 0.739(14) -0.1192(3) Uani 0.0091(6) 4 1 d ? ? ?
O2w O 0.8355(2) 0.81792(13) 0.1616(3) Uani 0.0124(6) 4 1 d ? ? ?
O23 O 0.9764(2) 0.59018(13) -0.1251(2) Uani 0.0083(6) 4 1 d ? ? ?
O1w O 0.8981(2) 0.67667(15) 0.3874(3) Uani 0.0126(6) 4 1 d ? ? ?
N11 N 0.623(2) 0.6715(16) 0.1884(3) Uani 0.0065(6) 4 1 d ? ? ?
N13 N 0.95(2) 0.7669(16) -0.1639(3) Uani 0.0065(6) 4 1 d ? ? ?
C16 C 0.5255(3) 0.63183(18) 0.0861(3) Uani 0.006(7) 4 1 d ? ? ?
C18 C 0.7042(3) 0.784(19) -0.2438(3) Uani 0.0064(7) 4 1 d ? ? ?
C15 C 0.3848(3) 0.64113(20) 0.1039(3) Uani 0.0076(8) 4 1 d ? ? ?
C14 C 0.3522(3) 0.69396(18) 0.2304(3) Uani 0.0061(7) 4 1 d ? ? ?
O4w O 0.7565(3) 0.57183(17) 0.5723(3) Uani 0.0244(9) 4 1 d ? ? ?
O172 O 0.4884(2) 0.55714(13) -0.1719(3) Uani 0.0102(6) 4 1 d ? ? ?
C17 C 0.5764(3) 0.58148(18) -0.057(3) Uani 0.006(7) 4 1 d ? ? ?
C12 C 1.0813(3) 0.7799(19) -0.1902(3) Uani 0.007(7) 4 1 d ? ? ?
C22 C 0.9907(3) 0.48451(19) 0.0901(3) Uani 0.0058(7) 4 1 d ? ? ?
H15 H 0.315038 0.612087 0.0314 Uiso 0.0075 4 1 d ? ? ?
H12 H 1.15293 0.751475 -0.117373 Uiso 0.0088 4 1 d ? ? ?
O5w O 0.5 0.5 0.5 Uani 0.0269(16) 2 0.5 d ? ? ?

ADP components: [ Help ]

Atom site label Atom site symbol U11 U22 U33 U12 U13 U23
Gd1 Gd 0.00257(6) 0.00763(7) 0.00524(6) 0.0006(6) 0.00117(5) -0.00047(6)
O171 O 0.0051(10) 0.0106(11) 0.0135(10) -0.0001(8) 0.0031(9) -0.0025(9)
O3w O 0.0132(12) 0.0234(13) 0.0142(11) 0.0062(10) -0.0014(10) -0.0073(11)
O182 O 0.0045(9) 0.0138(12) 0.0089(9) -0.0004(8) 0.0011(8) -0.0009(8)
O21 O 0.0107(10) 0.0095(11) 0.0073(9) 0.0036(8) 0.0032(8) 0(8)
O181 O 0.0049(9) 0.0148(11) 0.0077(9) -0.0006(8) 0.0015(8) 0.0028(9)
O2w O 0.0134(11) 0.0098(11) 0.014(10) 0.0016(9) 0.002(9) -0.0034(9)
O23 O 0.0085(10) 0.0104(11) 0.0064(9) 0.0011(8) 0.002(8) 0.0015(8)
O1w O 0.0128(11) 0.0187(12) 0.0061(9) 0.0049(10) 0.0002(8) -0.0043(10)
N11 N 0.0049(10) 0.0082(11) 0.0065(10) -0.001(10) 0.0011(9) 0.0014(10)
N13 N 0.0047(11) 0.0074(12) 0.0076(10) 0.0002(9) 0.0013(9) -0.0014(9)
C16 C 0.0066(12) 0.0064(14) 0.0051(11) -0.0003(10) 0.002(10) 0.0007(11)
C18 C 0.0052(12) 0.0079(14) 0.0066(12) 0.0004(10) 0.0023(10) -0.0033(11)
C15 C 0.0056(13) 0.0088(13) 0.0082(13) -0.0004(11) 0.0003(11) 0.0012(11)
C14 C 0.0047(12) 0.008(14) 0.0061(11) 0.0005(10) 0.0026(10) 0.0037(10)
O4w O 0.0246(17) 0.0305(15) 0.0181(13) -0.003(12) 0.002(13) -0.0015(12)
O172 O 0.009(10) 0.0114(11) 0.0099(9) 0.0011(8) -0.0001(8) -0.002(8)
C17 C 0.007(13) 0.0044(13) 0.007(12) 0.0005(10) 0.0032(11) 0.0019(11)
C12 C 0.0043(12) 0.0102(14) 0.0068(12) 0.0003(11) 0.0012(10) 0.0002(11)
C22 C 0.0023(11) 0.0092(14) 0.0057(11) -0.0006(10) -0.0001(10) -0.0002(11)
O5w O 0.028(3) 0.03(3) 0.024(2) 0(2) 0.009(2) -0.009(2)

Fourier Wave Vectors (explicit: q_x,q_y,q_z or coefficients: q_1,q_2,...): [ Help ]

Wave vector code q_x q_y q_z
1 0 0 0.33333

Occupation crenel coefficients: [ Help ]

Atom site label Center (x0) Width
O5w 0 0.5

Definition of the displacive (translational) Fourier series: [ Help ]

Modulation code Atom site label Displacement axis Wave vector code
Gd1x1 Gd1 x 1
Gd1y1 Gd1 y 1
Gd1z1 Gd1 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: [ Help ]

Modulation code Cosine coefficient Sine coefficient
Gd1x1 0.00169(3) 0.00058(3)
Gd1y1 0.004213(13) -0.011524(13)
Gd1z1 -0.00837(3) -0.00577(3)
O171x1 0.0033(4) -0.0015(4)
O171y1 -0.0003(2) -0.0119(2)
O171z1 -0.0069(4) -0.0009(4)
O3wx1 0.0027(4) -0.0144(4)
O3wy1 0.0058(2) -0.0298(2)
O3wz1 -0.0066(4) 0.0284(4)
O182x1 0.0034(4) 0.0018(4)
O182y1 0.0065(2) -0.0069(2)
O182z1 -0.0115(4) -0.0072(4)
O21x1 0.0068(4) 0.0067(4)
O21y1 0.00922(20) -0.00752(20)
O21z1 0.0026(4) -0.0044(4)
O181x1 0.0011(4) 0.0009(4)
O181y1 -0.004(2) -0.0132(2)
O181z1 -0.0099(4) -0.0005(4)
O2wx1 -0.0033(4) 0.007(4)
O2wy1 0.0061(2) -0.01099(19)
O2wz1 -0.0109(4) -0.0052(4)
O23x1 0.0063(4) -0.001(4)
O23y1 -0.0043(2) -0.01053(19)
O23z1 -0.0056(4) -0.0039(4)
O1wx1 0.0025(4) 0.0067(4)
O1wy1 0.0162(2) -0.003(2)
O1wz1 -0.0063(4) -0.008(4)
N11x1 0.003(5) 0.0023(5)
N11y1 0.0019(2) -0.0098(2)
N11z1 0.0007(5) -0.0036(5)
N13x1 -0.0002(4) -0.0021(4)
N13y1 0.0001(2) -0.0095(2)
N13z1 -0.0066(5) 0.0011(5)
C16x1 0.0028(5) 0.0012(5)
C16y1 0.0011(3) -0.0082(3)
C16z1 -0.003(5) -0.0056(6)
C18x1 -0.0017(5) -0.0012(5)
C18y1 0.0008(3) -0.0081(3)
C18z1 -0.0005(6) 0.0072(6)
C15x1 0.0028(5) 0.0006(5)
C15y1 0.0014(3) -0.0069(3)
C15z1 -0.0048(6) -0.0081(6)
C14x1 0.0011(5) 0.0015(5)
C14y1 0.0006(3) -0.007(3)
C14z1 0.0007(5) -0.0058(5)
O4wx1 0.0057(4) 0.0623(4)
O4wy1 0.0097(2) -0.0204(2)
O4wz1 -0.0278(5) -0.0123(5)
O172x1 0.0018(4) -0.0024(4)
O172y1 -0.0016(2) -0.0087(2)
O172z1 -0.0061(4) -0.0012(4)
C17x1 0.0032(5) -0.001(5)
C17y1 -0.0004(3) -0.0102(3)
C17z1 -0.0061(6) -0.0027(6)
C12x1 -0.0011(5) -0.0022(5)
C12y1 0.0013(3) -0.0101(3)
C12z1 -0.0052(6) 0.0012(6)
C22x1 0.0003(5) 0.003(5)
C22y1 0.0042(3) -0.011(3)
C22z1 0.0018(6) -0.0055(6)
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 0.0508(6)
O5wy1 0 0.0414(4)
O5wz1 0 -0.0155(7)

Definition of the ADP Fourier series: [ Help ]

Modulation code Atom site label Tensor element Wave vector code
Gd1U111 Gd1 U11 1
Gd1U221 Gd1 U22 1
Gd1U331 Gd1 U33 1
Gd1U121 Gd1 U12 1
Gd1U131 Gd1 U13 1
Gd1U231 Gd1 U23 1

ADP Fourier coefficients: [ Help ]

Modulation code Cosine coefficient Sine coefficient
Gd1U111 -0.00045(14) 0.00026(12)
Gd1U221 -0.00227(10) 0.0004(11)
Gd1U331 -0.00056(10) 0.00034(9)
Gd1U121 -0.00003(7) 0.00005(8)
Gd1U131 -0.00022(11) -0.00028(9)
Gd1U231 -0.00011(8) -0.00203(9)