B-IncStrDB

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: 10222E3ybfL Entry date: 2015-02-19 Last revision: 2022-01-02

3-Eu

Chemical data

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

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

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

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

Formula weight: 440.07 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: (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

a: 9.723(1) Å [ Help ]

b: 15.909(1) Å [ Help ]

c: 7.981(2) Å [ Help ]

α: 90 ° [ Help ]

β: 96.29(5) ° [ Help ]

γ: 90 ° [ Help ]

Volume: 1227.1(5) Å³ [ Help ]

Modulation dimension: 1 [ Help ]

Z: 4 [ Help ]

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

Cell determination reflection Nb.: 24574 [ Help ]

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

θ(max) for cell determination: 30.05 ° [ Help ]

Measured independent wave vectors: (Show/hide table) [ Help ]

Wave vector id	q_x	q_y	q_z
1	0	0	0.33333

μ: 5.088 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: 0.83476 [ Help ]

Maximum transmission factor: 1 [ Help ]

Refinement details

Total nb. of reflections: 10773 [ Help ]

Nb. of observed reflections: 5124 [ 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: 10773 [ Help ]

Nb. of parameters: 316 [ Help ]

R(obs): 0.0363 [ Help ]

wR(obs): 0.0382 [ Help ]

R(all): 0.0795 [ Help ]

wR(all): 0.041 [ Help ]

S(all): 0.98 [ Help ]

S(obs): 1.33 [ Help ]

Δ/σ(max): 0.0253 [ Help ]

Δ/σ(mean): 0.0010 [ Help ]

Δρ(max): 2.52 e_Å^-3 [ Help ]

Δρ(min): -1.23 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
Eu1	Eu	0.865537(16)	0.673228(11)	0.0787(2)	Uani	0.00537(4)	4	1	d	?	?	?
O171	O	0.705(2)	0.57118(15)	-0.0496(3)	Uani	0.0092(7)	4	1	d	?	?	?
O3w	O	0.6278(3)	0.92534(18)	0.0414(3)	Uani	0.0159(9)	4	1	d	?	?	?
O182	O	1.1108(2)	0.68944(14)	0.1484(3)	Uani	0.0088(7)	4	1	d	?	?	?
O21	O	0.9432(2)	0.53575(15)	0.1877(3)	Uani	0.0082(7)	4	1	d	?	?	?
O181	O	0.6867(2)	0.73966(16)	-0.1192(3)	Uani	0.0097(7)	4	1	d	?	?	?
O2w	O	0.8337(2)	0.81853(15)	0.1629(3)	Uani	0.0116(7)	4	1	d	?	?	?
O23	O	0.9764(2)	0.58981(15)	-0.125(3)	Uani	0.0084(7)	4	1	d	?	?	?
O1w	O	0.8987(2)	0.67673(17)	0.3887(3)	Uani	0.0122(7)	4	1	d	?	?	?
N11	N	0.6221(2)	0.67081(19)	0.1882(3)	Uani	0.0065(7)	4	1	d	?	?	?
N13	N	0.9492(3)	0.76774(18)	-0.1642(3)	Uani	0.0067(8)	4	1	d	?	?	?
C16	C	0.5251(3)	0.6317(2)	0.0859(4)	Uani	0.006(9)	4	1	d	?	?	?
C18	C	0.704(3)	0.7844(2)	-0.2438(4)	Uani	0.0065(9)	4	1	d	?	?	?
C15	C	0.3851(3)	0.6408(2)	0.1039(4)	Uani	0.0062(6)	4	1	d	?	?	?
C14	C	0.3518(3)	0.6937(2)	0.2308(4)	Uani	0.0062(6)	4	1	d	?	?	?
O4w	O	0.757(3)	0.5715(2)	0.572(4)	Uani	0.0219(11)	4	1	d	?	?	?
O172	O	0.4872(2)	0.55709(15)	-0.1718(3)	Uani	0.0094(7)	4	1	d	?	?	?
C17	C	0.5757(3)	0.5815(2)	-0.0568(4)	Uani	0.0066(9)	4	1	d	?	?	?
C12	C	1.0805(3)	0.7809(2)	-0.1897(4)	Uani	0.0087(9)	4	1	d	?	?	?
C22	C	0.9903(3)	0.4841(2)	0.0899(4)	Uani	0.0068(9)	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	0.027(2)	2	0.5	d	?	?	?

ADP components: (Show/hide table) [ Help ]

Atom site label	Atom site symbol	U11	U22	U33	U12	U13	U23
Eu1	Eu	0.00351(6)	0.00699(8)	0.00556(7)	0.00052(8)	0.00025(5)	-0.00053(8)
O171	O	0.0056(10)	0.0107(13)	0.0113(11)	-0.0004(10)	0.0012(9)	-0.0028(10)
O3w	O	0.0111(13)	0.0206(16)	0.0152(15)	0.0069(13)	-0.0024(11)	-0.0079(12)
O182	O	0.0052(9)	0.0113(14)	0.0093(11)	-0.0005(9)	-0.001(8)	-0.002(9)
O21	O	0.0116(11)	0.0063(12)	0.0069(11)	0.0041(10)	0.0017(9)	0.0013(9)
O181	O	0.0049(10)	0.0164(14)	0.0071(11)	-0.0019(10)	-0.0014(8)	0.0028(10)
O2w	O	0.0139(11)	0.0088(13)	0.0122(12)	0.0002(11)	0.0014(10)	-0.003(10)
O23	O	0.0097(11)	0.0069(13)	0.0085(11)	0.0008(10)	0.0004(9)	0.0021(9)
O1w	O	0.0142(11)	0.0157(13)	0.0064(10)	0.0032(13)	-0.0002(9)	-0.0021(11)
N11	N	0.0062(11)	0.0069(13)	0.0066(11)	-0.0003(12)	0.0015(9)	0.0021(12)
N13	N	0.0054(11)	0.0078(15)	0.0068(13)	0.0004(11)	0.0007(10)	-0.0014(11)
C16	C	0.009(14)	0.0035(16)	0.0057(14)	-0.0008(13)	0.0011(11)	0.0031(12)
C18	C	0.0067(13)	0.0069(17)	0.006(14)	-0.0008(13)	0.0016(11)	-0.0046(12)
C15	C	0.0067(10)	0.0058(11)	0.006(10)	-0.0025(9)	0.0001(8)	0.0035(8)
C14	C	0.0067(10)	0.0058(11)	0.006(10)	-0.0025(9)	0.0001(8)	0.0035(8)
O4w	O	0.0214(19)	0.0293(19)	0.0147(16)	-0.0037(15)	0.0006(14)	-0.0015(13)
O172	O	0.0102(10)	0.01(13)	0.0075(11)	0(10)	-0.0007(9)	-0.0017(9)
C17	C	0.0098(14)	0.0031(16)	0.0074(15)	0.0004(13)	0.0033(12)	0.0019(12)
C12	C	0.0079(14)	0.0103(18)	0.0075(15)	0.0013(14)	-0.0003(11)	-0.0008(13)
C22	C	0.0036(12)	0.0099(18)	0.0065(14)	-0.0014(14)	-0.0009(11)	0.0009(13)
O5w	O	0.035(4)	0.024(3)	0.024(3)	0.006(3)	0.014(3)	-0.007(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	0.33333

Occupation crenel coefficients: (Show/hide table) [ Help ]

Atom site label	Center (x0)	Width
O5w	0	0.5

Definition of the displacive (translational) Fourier series: (Show/hide table) [ Help ]

Modulation code	Atom site label	Displacement axis	Wave vector code
Eu1x1	Eu1	x	1
Eu1y1	Eu1	y	1
Eu1z1	Eu1	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
Eu1x1	0.00174(4)	0.00078(4)
Eu1y1	0.004361(18)	-0.011746(17)
Eu1z1	-0.00834(4)	-0.00593(5)
O171x1	0.0036(5)	-0.0016(5)
O171y1	-0.0009(3)	-0.012(3)
O171z1	-0.0061(6)	-0.0011(6)
O3wx1	0.0028(5)	-0.0149(5)
O3wy1	0.0059(3)	-0.0306(3)
O3wz1	-0.0072(6)	0.0295(5)
O182x1	0.0028(5)	0.0008(5)
O182y1	0.0062(3)	-0.0068(3)
O182z1	-0.0113(5)	-0.008(5)
O21x1	0.0074(5)	0.0065(5)
O21y1	0.0097(2)	-0.0079(2)
O21z1	0.0037(5)	-0.0044(5)
O181x1	0.0006(5)	-0.0001(5)
O181y1	-0.0039(3)	-0.0134(3)
O181z1	-0.0109(6)	-0.001(5)
O2wx1	-0.0037(5)	0.0078(5)
O2wy1	0.0061(3)	-0.0109(2)
O2wz1	-0.0117(5)	-0.0043(6)
O23x1	0.0054(5)	-0.0002(5)
O23y1	-0.0046(2)	-0.0102(2)
O23z1	-0.0054(6)	-0.0045(5)
O1wx1	0.0008(5)	0.0078(6)
O1wy1	0.0158(2)	-0.0025(3)
O1wz1	-0.0068(5)	-0.0081(6)
N11x1	0.0036(6)	0.0021(6)
N11y1	0.0019(3)	-0.0098(3)
N11z1	0.0012(7)	-0.0033(7)
N13x1	-0.0006(6)	-0.0023(6)
N13y1	0.0003(3)	-0.009(3)
N13z1	-0.0065(7)	0.0006(7)
C16x1	0.002(7)	0.0014(7)
C16y1	0.0014(3)	-0.0082(3)
C16z1	-0.0034(8)	-0.0053(7)
C18x1	-0.0014(7)	-0.0011(7)
C18y1	0.0004(4)	-0.0084(3)
C18z1	-0.0012(8)	0.0079(8)
C15x1	0.0036(7)	0.0011(7)
C15y1	0.0019(4)	-0.0067(3)
C15z1	-0.0044(8)	-0.0078(7)
C14x1	0.0009(7)	0.0015(7)
C14y1	0.0009(4)	-0.0072(4)
C14z1	0.0008(8)	-0.0061(7)
O4wx1	0.0046(5)	0.063(5)
O4wy1	0.009(3)	-0.0204(3)
O4wz1	-0.0266(6)	-0.0118(5)
O172x1	0.0024(5)	-0.002(5)
O172y1	-0.0011(3)	-0.0088(2)
O172z1	-0.0067(6)	-0.0021(5)
C17x1	0.0029(7)	0.0002(7)
C17y1	-0.0006(3)	-0.0102(3)
C17z1	-0.0059(8)	-0.0047(8)
C12x1	0.0001(7)	-0.0034(7)
C12y1	0.0014(4)	-0.0099(4)
C12z1	-0.0049(8)	0.001(8)
C22x1	0.0002(7)	0.0032(7)
C22y1	0.0042(4)	-0.0113(4)
C22z1	0.0005(8)	-0.0053(8)
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	0.0481(7)
O5wy1	0	0.0403(4)
O5wz1	0	-0.0158(8)

Definition of the ADP Fourier series: (Show/hide table) [ Help ]

Modulation code	Atom site label	Tensor element	Wave vector code
Eu1U111	Eu1	U11	1
Eu1U221	Eu1	U22	1
Eu1U331	Eu1	U33	1
Eu1U121	Eu1	U12	1
Eu1U131	Eu1	U13	1
Eu1U231	Eu1	U23	1

ADP Fourier coefficients: (Show/hide table) [ Help ]

Modulation code	Cosine coefficient	Sine coefficient
Eu1U111	-0.0004(2)	0.00032(17)
Eu1U221	-0.00244(14)	0.00008(15)
Eu1U331	-0.00088(16)	0.00041(14)
Eu1U121	0.00003(10)	-0.00025(12)
Eu1U131	0.00004(14)	-0.00034(13)
Eu1U231	0.00008(10)	-0.00211(11)