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: 10402EmPcj8 Entry date: 2015-02-19 Last revision: 2022-01-02

3-Er

Chemical data

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

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

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

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

Formula weight: 455.37 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: 9.5926(3) Å [ Help ]

b: 15.7938(4) Å [ Help ]

c: 7.923(3) Å [ Help ]

α: 90 ° [ Help ]

β: 96.759(3) ° [ Help ]

γ: 90 ° [ Help ]

Volume: 1192.02(7) Å³ [ Help ]

Modulation dimension: 1 [ Help ]

Z: 4 [ Help ]

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

Cell determination reflection Nb.: 38236 [ Help ]

θ(min) for cell determination: 2.72 ° [ Help ]

θ(max) for cell determination: 30.08 ° [ Help ]

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

Wave vector id	q_x	q_y	q_z
1	0	0	0.33333

μ: 7.102 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: 0.233 [ Help ]

Maximum transmission factor: 0.647 [ Help ]

Refinement details

Total nb. of reflections: 10510 [ Help ]

Nb. of observed reflections: 7495 [ 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: 10510 [ Help ]

Nb. of parameters: 310 [ Help ]

R(obs): 0.069 [ Help ]

wR(obs): 0.0772 [ Help ]

R(all): 0.0879 [ Help ]

wR(all): 0.079 [ Help ]

S(all): 3.33 [ Help ]

S(obs): 3.88 [ Help ]

Δ/σ(max): 0.0468 [ Help ]

Δ/σ(mean): 0.0041 [ Help ]

Δρ(max): 17.13 e_Å^-3 [ Help ]

Δρ(min): -12.18 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
Er1	Er	0.86722(2)	0.672596(13)	0.07183(3)	Uani	0.00484(7)	4	1	d	?	?	?
O171	O	0.7099(4)	0.5705(2)	-0.0527(5)	Uani	0.0094(10)	4	1	d	?	?	?
O3w	O	0.6297(5)	0.9249(3)	0.0412(5)	Uani	0.0213(13)	4	1	d	?	?	?
O182	O	1.1088(4)	0.6896(2)	0.1449(5)	Uani	0.0084(10)	4	1	d	?	?	?
O21	O	0.9435(4)	0.5377(2)	0.1867(5)	Uani	0.0097(10)	4	1	d	?	?	?
O181	O	0.6872(4)	0.7367(2)	-0.1242(4)	Uani	0.0081(10)	4	1	d	?	?	?
O2w	O	0.8413(4)	0.8159(2)	0.1498(5)	Uani	0.0114(11)	4	1	d	?	?	?
O23	O	0.9776(4)	0.5901(2)	-0.1278(4)	Uani	0.007(9)	4	1	d	?	?	?
O1w	O	0.8987(4)	0.6787(2)	0.3774(5)	Uani	0.013(11)	4	1	d	?	?	?
N11	N	0.6264(5)	0.6733(2)	0.1827(5)	Uani	0.0054(11)	4	1	d	?	?	?
N13	N	0.9521(4)	0.7645(3)	-0.1696(5)	Uani	0.0064(11)	4	1	d	?	?	?
C16	C	0.5274(5)	0.6322(3)	0.0813(6)	Uani	0.005(12)	4	1	d	?	?	?
C18	C	0.7037(5)	0.7826(3)	-0.2494(6)	Uani	0.0064(12)	4	1	d	?	?	?
C15	C	0.3858(5)	0.6409(3)	0.1001(6)	Uani	0.0061(12)	4	1	d	?	?	?
C14	C	0.3531(5)	0.6951(3)	0.2256(6)	Uani	0.0048(12)	4	1	d	?	?	?
O4w	O	0.7547(6)	0.5744(3)	0.5664(6)	Uani	0.0329(17)	4	1	d	?	?	?
O172	O	0.4892(4)	0.5555(2)	-0.1753(4)	Uani	0.0081(9)	4	1	d	?	?	?
C17	C	0.578(5)	0.5807(3)	-0.0601(6)	Uani	0.0065(13)	4	1	d	?	?	?
C12	C	1.085(5)	0.7774(3)	-0.197(6)	Uani	0.007(12)	4	1	d	?	?	?
C22	C	0.9901(5)	0.4851(3)	0.0912(6)	Uani	0.006(12)	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	0.025(3)	2	0.5	d	?	?	?

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

Atom site label	Atom site symbol	U11	U22	U33	U12	U13	U23
Er1	Er	0.00347(12)	0.00666(11)	0.00466(11)	0.00085(8)	0.00163(8)	-0.0008(8)
O171	O	0.0062(17)	0.0094(16)	0.0131(17)	0.0006(13)	0.0035(14)	-0.0024(14)
O3w	O	0.018(2)	0.029(2)	0.016(2)	0.009(19)	-0.0003(17)	-0.0108(19)
O182	O	0.0038(17)	0.014(17)	0.0076(16)	0.0003(13)	0.0013(13)	-0.0022(14)
O21	O	0.0135(19)	0.0077(16)	0.0085(17)	0.0041(14)	0.0039(14)	0.0007(14)
O181	O	0.0074(17)	0.0126(17)	0.0048(16)	-0.0009(14)	0.0029(13)	0.004(14)
O2w	O	0.014(2)	0.0094(17)	0.0109(18)	0.0018(14)	0.0004(15)	-0.0031(14)
O23	O	0.0071(17)	0.0084(15)	0.0059(15)	0.0024(13)	0.0029(13)	0.0009(13)
O1w	O	0.0115(19)	0.022(2)	0.0056(16)	0.0051(16)	0.002(14)	-0.0063(15)
N11	N	0.007(2)	0.0072(17)	0.0021(17)	-0.0007(15)	0.0009(14)	0.0023(15)
N13	N	0.0052(19)	0.0058(18)	0.0088(19)	0.0012(15)	0.003(15)	-0.0013(16)
C16	C	0.007(2)	0.004(2)	0.004(2)	0.0006(17)	0.0015(16)	0.0002(17)
C18	C	0.005(2)	0.006(2)	0.008(2)	0.0007(17)	0.0024(17)	-0.0018(18)
C15	C	0.006(2)	0.007(2)	0.006(2)	0.0009(17)	0.0007(17)	0.0003(18)
C14	C	0.008(2)	0.004(19)	0.0028(19)	0.0014(17)	0.0014(17)	0.0027(16)
O4w	O	0.043(4)	0.033(3)	0.024(3)	-0.011(2)	0.006(2)	-0.003(2)
O172	O	0.0082(17)	0.0102(16)	0.0059(15)	0(14)	0.0009(13)	-0.0023(14)
C17	C	0.009(2)	0.005(2)	0.007(2)	0.0003(17)	0.0042(17)	0.0018(17)
C12	C	0.006(2)	0.009(2)	0.006(2)	-0.0006(18)	0.0023(17)	0.0035(18)
C22	C	0.002(2)	0.011(2)	0.005(2)	0(18)	0.0007(16)	0.0022(18)
O5w	O	0.027(5)	0.031(4)	0.019(4)	-0.001(4)	0.009(4)	-0.006(3)

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
Er1x1	Er1	x	1
Er1y1	Er1	y	1
Er1z1	Er1	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
Er1x1	0.0024(4)	0.00067(4)
Er1y1	0.003506(19)	-0.008179(18)
Er1z1	-0.00675(4)	-0.00537(4)
O171x1	0.0035(6)	-0.0016(6)
O171y1	0.0002(3)	-0.0093(3)
O171z1	-0.0047(7)	-0.0011(7)
O3wx1	0.0018(7)	-0.0147(7)
O3wy1	0.0053(4)	-0.0262(4)
O3wz1	-0.0061(7)	0.0259(7)
O182x1	0.0036(6)	0.0017(6)
O182y1	0.0051(3)	-0.0051(3)
O182z1	-0.0098(6)	-0.0064(6)
O21x1	0.0064(6)	0.007(6)
O21y1	0.0077(3)	-0.0052(3)
O21z1	0.0025(7)	-0.0033(7)
O181x1	0.0001(6)	0.0004(6)
O181y1	-0.0028(3)	-0.0104(3)
O181z1	-0.0078(6)	-0.0016(6)
O2wx1	-0.0023(6)	0.0061(6)
O2wy1	0.005(3)	-0.0076(3)
O2wz1	-0.0087(6)	-0.0067(7)
O23x1	0.0058(6)	-0.0011(6)
O23y1	-0.0035(3)	-0.0076(3)
O23z1	-0.0051(6)	-0.0023(6)
O1wx1	0.0039(6)	0.0056(6)
O1wy1	0.0125(3)	-0.0012(3)
O1wz1	-0.0043(6)	-0.0078(6)
N11x1	0.0033(7)	0.0022(7)
N11y1	0.0012(3)	-0.0075(3)
N11z1	0.0017(7)	-0.0029(7)
N13x1	-0.0007(7)	-0.0027(7)
N13y1	-0.0006(3)	-0.0065(3)
N13z1	-0.0071(8)	-0.0003(8)
C16x1	0.0026(8)	0.0017(8)
C16y1	0.0008(4)	-0.006(4)
C16z1	-0.0025(9)	-0.005(9)
C18x1	-0.0019(8)	-0.0018(8)
C18y1	0.0009(4)	-0.0064(4)
C18z1	0(9)	0.0061(9)
C15x1	0.003(8)	0.0021(8)
C15y1	0.0009(4)	-0.0044(4)
C15z1	-0.0033(9)	-0.0058(9)
C14x1	0.0016(8)	0.002(8)
C14y1	0.0007(4)	-0.0049(4)
C14z1	0.0013(8)	-0.004(8)
O4wx1	0.0096(8)	0.0609(8)
O4wy1	0.0077(4)	-0.0189(4)
O4wz1	-0.0232(8)	-0.0109(8)
O172x1	0.0019(6)	-0.0014(6)
O172y1	-0.0016(3)	-0.0069(3)
O172z1	-0.0032(6)	-0.001(6)
C17x1	0.0028(8)	-0.0009(9)
C17y1	-0.0004(4)	-0.0071(4)
C17z1	-0.0044(9)	-0.0037(9)
C12x1	-0.0015(8)	-0.0021(8)
C12y1	0.0004(4)	-0.0075(4)
C12z1	-0.0053(9)	0.0005(9)
C22x1	0.0008(8)	0.0025(8)
C22y1	0.0036(4)	-0.0077(4)
C22z1	0.0018(9)	-0.0042(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	0.0634(14)
O5wy1	0	0.0589(7)
O5wz1	0	-0.0257(14)