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: 10142E2dqqZ Entry date: 2015-02-19 Last revision: 2022-01-02

3-Tb

Chemical data

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

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

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

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

Formula weight: 447.03 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: 9.664(4) Å [ Help ]

b: 15.844(7) Å [ Help ]

c: 7.959(1) Å [ Help ]

α: 90 ° [ Help ]

β: 96.489(4) ° [ Help ]

γ: 90 ° [ Help ]

Volume: 1210.9(4) Å³ [ Help ]

Modulation dimension: 1 [ Help ]

Z: 4 [ Help ]

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

Cell determination reflection Nb.: 34207 [ Help ]

θ(min) for cell determination: 3.09 ° [ Help ]

θ(max) for cell determination: 30.07 ° [ Help ]

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

Wave vector id	q_x	q_y	q_z
1	0	0	0.33333

μ: 5.9 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: 0.1 [ Help ]

Maximum transmission factor: 0.519 [ Help ]

Refinement details

Total nb. of reflections: 10657 [ Help ]

Nb. of observed reflections: 7437 [ 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: 10657 [ Help ]

Nb. of parameters: 322 [ Help ]

Number of constraints: 20 [ Help ]

R(obs): 0.0324 [ Help ]

wR(obs): 0.0389 [ Help ]

R(all): 0.0488 [ Help ]

wR(all): 0.0404 [ Help ]

S(all): 1.6 [ Help ]

S(obs): 1.86 [ Help ]

Δ/σ(max): 0.0417 [ Help ]

Δ/σ(mean): 0.0016 [ Help ]

Δρ(max): 6.47 e_Å^-3 [ Help ]

Δρ(min): -4.91 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
Tb1	Tb	0.866676(12)	0.672929(8)	0.077057(16)	Uani	0.00392(3)	4	1	d	?	?	?
O171	O	0.70713(19)	0.57081(12)	-0.0499(3)	Uani	0.009(5)	4	1	d	?	?	?
O3w	O	0.6293(2)	0.92508(13)	0.0421(3)	Uani	0.0149(6)	4	1	d	?	?	?
O182	O	1.11009(19)	0.68929(12)	0.1482(3)	Uani	0.0083(5)	4	1	d	?	?	?
O21	O	0.9431(2)	0.53632(12)	0.1875(3)	Uani	0.0082(5)	4	1	d	?	?	?
O181	O	0.6874(19)	0.73879(12)	-0.1198(2)	Uani	0.008(5)	4	1	d	?	?	?
O2w	O	0.8374(2)	0.81698(12)	0.1598(3)	Uani	0.0113(6)	4	1	d	?	?	?
O23	O	0.97692(20)	0.59035(11)	-0.1255(2)	Uani	0.0072(5)	4	1	d	?	?	?
O1w	O	0.8989(2)	0.67722(12)	0.385(3)	Uani	0.0104(5)	4	1	d	?	?	?
N11	N	0.6243(2)	0.67181(14)	0.1869(3)	Uani	0.0058(6)	4	1	d	?	?	?
N13	N	0.9509(2)	0.76661(14)	-0.1653(3)	Uani	0.0064(6)	4	1	d	?	?	?
C16	C	0.5264(3)	0.63222(16)	0.085(3)	Uani	0.0054(7)	4	1	d	?	?	?
C18	C	0.7041(3)	0.78378(16)	-0.245(3)	Uani	0.0056(7)	4	1	d	?	?	?
C15	C	0.3856(3)	0.64137(17)	0.1033(3)	Uani	0.0062(7)	4	1	d	?	?	?
C14	C	0.3527(3)	0.69439(16)	0.2296(3)	Uani	0.0052(7)	4	1	d	?	?	?
O4w	O	0.7571(3)	0.57267(15)	0.5723(3)	Uani	0.0222(8)	4	1	d	?	?	?
O172	O	0.4886(20)	0.55682(12)	-0.1727(3)	Uani	0.0091(5)	4	1	d	?	?	?
C17	C	0.5771(3)	0.58143(16)	-0.0584(3)	Uani	0.0056(7)	4	1	d	?	?	?
C12	C	1.0823(3)	0.77944(16)	-0.1916(4)	Uani	0.0073(7)	4	1	d	?	?	?
C22	C	0.9904(2)	0.48474(16)	0.0903(3)	Uani	0.0055(6)	4	1	d	?	?	?
H15	H	0.315038	0.612087	0.0314	Uiso	0.0075	4	1	d	?	?	?
H12	H	1.15293	0.751475	-0.117374	Uiso	0.0088	4	1	d	?	?	?
O5w	O	0.5	0.5	0.5	Uani	0.0221(13)	2	0.5	d	?	?	?

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

Atom site label	Atom site symbol	U11	U22	U33	U12	U13	U23
Tb1	Tb	0.00242(6)	0.00495(6)	0.00431(6)	0.00062(5)	0.00003(4)	-0.00065(5)
O171	O	0.005(8)	0.0097(9)	0.0126(10)	-0.0001(7)	0.0017(8)	-0.0021(8)
O3w	O	0.0124(10)	0.0184(10)	0.0134(12)	0.0042(8)	-0.001(9)	-0.0046(9)
O182	O	0.0048(8)	0.0117(9)	0.008(10)	-0.0006(7)	-0.0012(7)	-0.0031(7)
O21	O	0.0114(9)	0.0072(9)	0.006(9)	0.003(7)	0.0017(8)	-0.0004(7)
O181	O	0.0054(8)	0.0129(9)	0.0053(9)	-0.0009(7)	-0.0008(7)	0.0026(8)
O2w	O	0.0132(10)	0.0085(9)	0.0122(11)	0.0017(7)	0.0019(9)	-0.0033(8)
O23	O	0.0091(9)	0.0056(8)	0.0069(9)	0.0019(7)	0.0012(8)	0.0013(7)
O1w	O	0.0108(9)	0.015(9)	0.0049(9)	0.0045(8)	-0.0011(8)	-0.0028(8)
N11	N	0.0052(9)	0.0062(9)	0.006(10)	-0.0007(8)	-0.0001(8)	0.0002(9)
N13	N	0.0047(9)	0.006(10)	0.0084(11)	0.0002(8)	0.0009(9)	-0.0006(9)
C16	C	0.0071(11)	0.0041(11)	0.0051(12)	0.0002(9)	0.001(9)	0.0012(9)
C18	C	0.0049(10)	0.0052(11)	0.0067(12)	0.0003(9)	0.0012(9)	-0.0032(10)
C15	C	0.0056(11)	0.0062(11)	0.0067(13)	-0.0001(9)	-0.0001(10)	-0.0001(10)
C14	C	0.0053(11)	0.0049(11)	0.0057(12)	0.0008(8)	0.0018(9)	0.002(9)
O4w	O	0.025(14)	0.026(12)	0.0153(13)	-0.0021(10)	0.0008(11)	-0.001(10)
O172	O	0.0089(9)	0.0093(9)	0.0087(9)	0.0002(7)	-0.0012(8)	-0.0032(8)
C17	C	0.0084(11)	0.0029(11)	0.0058(12)	0.0005(9)	0.0016(10)	0.0013(9)
C12	C	0.0058(11)	0.0075(12)	0.0086(13)	0.0019(9)	0.0001(10)	0.001(10)
C22	C	0.0023(10)	0.0078(11)	0.0059(12)	-0.0005(9)	-0.0017(9)	0.0003(10)
O5w	O	0.025(2)	0.024(2)	0.018(2)	-0.0032(17)	0.006(2)	-0.007(18)

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
Tb1x1	Tb1	x	1
Tb1y1	Tb1	y	1
Tb1z1	Tb1	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
Tb1x1	0.0018(2)	0.00067(2)
Tb1y1	0.004259(11)	-0.011624(10)
Tb1z1	-0.00854(3)	-0.00594(3)
O171x1	0.0038(3)	-0.0018(3)
O171y1	-0.00043(17)	-0.01251(17)
O171z1	-0.0064(4)	-0.0012(4)
O3wx1	0.0024(3)	-0.0149(3)
O3wy1	0.0063(18)	-0.03028(19)
O3wz1	-0.0069(4)	0.0297(4)
O182x1	0.0032(3)	0.0019(3)
O182y1	0.00613(17)	-0.0072(17)
O182z1	-0.0121(4)	-0.0078(4)
O21x1	0.0073(3)	0.0067(3)
O21y1	0.00947(16)	-0.00761(16)
O21z1	0.0028(4)	-0.0052(4)
O181x1	0.0006(3)	0.0005(3)
O181y1	-0.00407(17)	-0.01354(17)
O181z1	-0.0102(4)	-0.0005(4)
O2wx1	-0.0037(3)	0.0065(3)
O2wy1	0.00632(17)	-0.01134(17)
O2wz1	-0.0112(4)	-0.0048(4)
O23x1	0.0061(3)	-0.0011(3)
O23y1	-0.00443(16)	-0.01067(16)
O23z1	-0.0057(4)	-0.0045(4)
O1wx1	0.0019(3)	0.0066(3)
O1wy1	0.01617(17)	-0.00302(17)
O1wz1	-0.0067(4)	-0.0086(4)
N11x1	0.0029(4)	0.002(4)
N11y1	0.00191(18)	-0.00993(18)
N11z1	0.0004(5)	-0.003(5)
N13x1	-0.0001(4)	-0.0026(4)
N13y1	-0.00006(19)	-0.00967(19)
N13z1	-0.0062(5)	0.0016(5)
C16x1	0.0033(4)	0.001(4)
C16y1	0.0015(2)	-0.0081(2)
C16z1	-0.0038(5)	-0.0051(5)
C18x1	-0.0019(4)	-0.0018(4)
C18y1	0.0005(2)	-0.0083(2)
C18z1	-0.0007(5)	0.0066(5)
C15x1	0.002(4)	0.0003(4)
C15y1	0.0016(2)	-0.0069(2)
C15z1	-0.0057(5)	-0.0077(5)
C14x1	0.0017(4)	0.0013(4)
C14y1	0.0009(2)	-0.0073(2)
C14z1	0.0009(5)	-0.0064(5)
O4wx1	0.0054(4)	0.0626(4)
O4wy1	0.0096(2)	-0.021(2)
O4wz1	-0.0279(5)	-0.0129(5)
O172x1	0.0023(3)	-0.002(3)
O172y1	-0.00154(16)	-0.00897(17)
O172z1	-0.0066(4)	-0.0011(4)
C17x1	0.004(4)	-0.0005(4)
C17y1	-0.0003(2)	-0.0103(2)
C17z1	-0.0061(5)	-0.0029(5)
C12x1	-0.0004(4)	-0.0017(4)
C12y1	0.0011(2)	-0.0103(2)
C12z1	-0.0054(6)	0.0016(5)
C22x1	0.0006(4)	0.0033(4)
C22y1	0.0044(2)	-0.0106(2)
C22z1	0.0017(5)	-0.0051(5)
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	0.0517(5)
O5wy1	0	0.0424(3)
O5wz1	0	-0.0172(6)

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

Modulation code	Atom site label	Tensor element	Wave vector code
Tb1U111	Tb1	U11	1
Tb1U221	Tb1	U22	1
Tb1U331	Tb1	U33	1
Tb1U121	Tb1	U12	1
Tb1U131	Tb1	U13	1
Tb1U231	Tb1	U23	1

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

Modulation code	Cosine coefficient	Sine coefficient
Tb1U111	-0.00023(11)	0.00037(9)
Tb1U221	-0.00218(8)	0.00049(8)
Tb1U331	-0.00105(10)	0.00027(9)
Tb1U121	0.00007(6)	-0.00018(6)
Tb1U131	-0.00016(9)	-0.00044(8)
Tb1U231	0.0004(6)	-0.00237(7)