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: 10362EyGhBk Entry date: 2015-02-19 Last revision: 2022-01-02

3-Dy

Chemical data

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

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

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

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

Formula weight: 450.61 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: 9.65(4) Å [ Help ]

b: 15.845(5) Å [ Help ]

c: 7.955(3) Å [ Help ]

α: 90 ° [ Help ]

β: 96.555(4) ° [ Help ]

γ: 90 ° [ Help ]

Volume: 1208.4(1) Å³ [ Help ]

Modulation dimension: 1 [ Help ]

Z: 4 [ Help ]

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

Cell determination reflection Nb.: 23630 [ Help ]

θ(min) for cell determination: 2.71 ° [ Help ]

θ(max) for cell determination: 28.95 ° [ Help ]

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

Wave vector id	q_x	q_y	q_z
1	0	0	0.33333

μ: 6.267 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: 0.159 [ Help ]

Maximum transmission factor: 0.545 [ Help ]

Refinement details

Total nb. of reflections: 8283 [ Help ]

Nb. of observed reflections: 5454 [ 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: 8283 [ Help ]

Nb. of parameters: 310 [ Help ]

R(obs): 0.0524 [ Help ]

wR(obs): 0.0606 [ Help ]

R(all): 0.0737 [ Help ]

wR(all): 0.0623 [ Help ]

S(all): 2.29 [ Help ]

S(obs): 2.76 [ Help ]

Δ/σ(max): 0.0463 [ Help ]

Δ/σ(mean): 0.0023 [ Help ]

Δρ(max): 8.56 e_Å^-3 [ Help ]

Δρ(min): -5.42 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
Dy1	Dy	0.8669(2)	0.672903(14)	0.07562(3)	Uani	0.00401(7)	4	1	d	?	?	?
O171	O	0.7082(3)	0.5706(2)	-0.0505(5)	Uani	0.0087(11)	4	1	d	?	?	?
O3w	O	0.6297(4)	0.9254(3)	0.042(5)	Uani	0.0185(13)	4	1	d	?	?	?
O182	O	1.1096(4)	0.6895(2)	0.1473(5)	Uani	0.0081(10)	4	1	d	?	?	?
O21	O	0.9433(4)	0.5369(2)	0.1874(4)	Uani	0.0082(10)	4	1	d	?	?	?
O181	O	0.6876(3)	0.7383(2)	-0.1207(4)	Uani	0.0074(10)	4	1	d	?	?	?
O2w	O	0.8391(4)	0.8168(2)	0.1575(5)	Uani	0.0122(12)	4	1	d	?	?	?
O23	O	0.9771(3)	0.5904(2)	-0.1261(4)	Uani	0.0063(10)	4	1	d	?	?	?
O1w	O	0.8987(4)	0.6773(2)	0.383(5)	Uani	0.0111(11)	4	1	d	?	?	?
N11	N	0.625(4)	0.6722(2)	0.1862(5)	Uani	0.005(11)	4	1	d	?	?	?
N13	N	0.9517(4)	0.7659(3)	-0.1665(5)	Uani	0.005(12)	4	1	d	?	?	?
C16	C	0.5267(5)	0.6319(3)	0.0839(6)	Uani	0.0048(14)	4	1	d	?	?	?
C18	C	0.7048(5)	0.7834(3)	-0.2461(6)	Uani	0.0042(13)	4	1	d	?	?	?
C15	C	0.3858(5)	0.6411(3)	0.1023(6)	Uani	0.0049(13)	4	1	d	?	?	?
C14	C	0.353(5)	0.6946(3)	0.2282(6)	Uani	0.0046(13)	4	1	d	?	?	?
O4w	O	0.7559(5)	0.5729(3)	0.5707(6)	Uani	0.0269(16)	4	1	d	?	?	?
O172	O	0.4892(4)	0.5565(2)	-0.1734(4)	Uani	0.0083(10)	4	1	d	?	?	?
C17	C	0.5769(5)	0.5812(3)	-0.0584(6)	Uani	0.0047(14)	4	1	d	?	?	?
C12	C	1.0832(5)	0.779(3)	-0.1926(6)	Uani	0.0059(14)	4	1	d	?	?	?
C22	C	0.9904(5)	0.4849(3)	0.0898(6)	Uani	0.0049(13)	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
Dy1	Dy	0.00142(12)	0.00591(13)	0.00444(13)	0.00081(10)	-0.00075(8)	-0.00059(10)
O171	O	0.0032(16)	0.0089(18)	0.014(2)	0.0008(15)	0.0012(15)	-0.0004(15)
O3w	O	0.011(2)	0.028(2)	0.015(2)	0.0066(19)	-0.0037(18)	-0.0101(19)
O182	O	0.0035(16)	0.0112(19)	0.0091(19)	0.0004(14)	-0.0009(14)	-0.003(14)
O21	O	0.0108(18)	0.0072(18)	0.0064(18)	0.0032(15)	-0.0003(15)	0.0001(14)
O181	O	0.004(16)	0.0103(18)	0.0073(19)	-0.002(15)	-0.0019(14)	0.0036(15)
O2w	O	0.0122(19)	0.0105(19)	0.014(2)	0.001(16)	0.0009(16)	-0.0034(15)
O23	O	0.006(16)	0.0068(17)	0.0057(18)	0.0014(14)	-0.0015(14)	0.0013(14)
O1w	O	0.0104(18)	0.019(2)	0.0031(18)	0.0049(17)	-0.0015(14)	-0.0054(16)
N11	N	0.0025(18)	0.006(19)	0.006(2)	0.0004(17)	-0.0017(16)	0.0028(17)
N13	N	0.0047(19)	0.006(2)	0.005(2)	0.0007(17)	0.0001(16)	-0.0018(16)
C16	C	0.007(2)	0.003(2)	0.005(2)	0(2)	0.0004(19)	0.0029(19)
C18	C	0.004(2)	0.003(2)	0.006(2)	0.0008(19)	0(19)	-0.0029(19)
C15	C	0.004(2)	0.006(2)	0.004(2)	-0.001(2)	-0.0022(19)	0.0015(19)
C14	C	0.005(2)	0.005(2)	0.004(2)	0.0009(5)	0.0016(8)	0.0025(9)
O4w	O	0.032(3)	0.032(3)	0.017(3)	-0.007(2)	0.002(2)	-0.002(2)
O172	O	0.0074(16)	0.0093(18)	0.0078(18)	0.0003(15)	-0.0012(14)	-0.0038(14)
C17	C	0.005(2)	0.003(2)	0.007(3)	0.001(2)	0.002(19)	0.0022(19)
C12	C	0.004(2)	0.008(2)	0.005(2)	0.001(2)	-0.0003(19)	0.0004(19)
C22	C	0.0021(10)	0.0081(2)	0.005(2)	-0.0008(9)	-0.0021(18)	0.0005(2)
O5w	O	0.027(5)	0.032(4)	0.016(4)	0.001(4)	0.01(4)	-0.005(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
Dy1x1	Dy1	x	1
Dy1y1	Dy1	y	1
Dy1z1	Dy1	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
Dy1x1	0.00194(4)	0.00059(5)
Dy1y1	0.00394(2)	-0.01015(19)
Dy1z1	-0.00765(5)	-0.00568(5)
O171x1	0.0043(6)	-0.0011(6)
O171y1	0.0003(3)	-0.0109(3)
O171z1	-0.006(8)	-0.0009(8)
O3wx1	0.0016(7)	-0.0142(6)
O3wy1	0.006(4)	-0.0277(4)
O3wz1	-0.007(8)	0.0278(8)
O182x1	0.0029(6)	0.0015(6)
O182y1	0.0057(3)	-0.0065(3)
O182z1	-0.0107(7)	-0.0057(7)
O21x1	0.0067(6)	0.006(6)
O21y1	0.008(3)	-0.0074(3)
O21z1	0.002(7)	-0.0045(7)
O181x1	-0.0002(6)	0.0004(6)
O181y1	-0.0033(3)	-0.012(3)
O181z1	-0.0082(7)	-0.0009(7)
O2wx1	-0.0022(7)	0.0058(7)
O2wy1	0.0057(3)	-0.0098(3)
O2wz1	-0.0093(8)	-0.005(8)
O23x1	0.0065(6)	0(6)
O23y1	-0.0046(3)	-0.0097(3)
O23z1	-0.0049(7)	-0.0034(7)
O1wx1	0.0024(7)	0.0053(7)
O1wy1	0.0141(3)	-0.0031(3)
O1wz1	-0.0054(7)	-0.0086(7)
N11x1	0.0031(8)	0.0026(8)
N11y1	0.001(3)	-0.0081(3)
N11z1	0.0005(9)	-0.0033(9)
N13x1	-0.0009(7)	-0.0033(7)
N13y1	-0.0002(4)	-0.0087(4)
N13z1	-0.0072(9)	0.0021(8)
C16x1	0.003(9)	0.0021(9)
C16y1	0.0011(4)	-0.0065(4)
C16z1	-0.0037(10)	-0.0047(10)
C18x1	-0.0018(8)	-0.0026(8)
C18y1	0.0004(4)	-0.0076(4)
C18z1	-0.0007(10)	0.0063(10)
C15x1	0.0035(9)	0.0018(9)
C15y1	0.0016(5)	-0.006(4)
C15z1	-0.0037(10)	-0.0072(10)
C14x1	0.0016(9)	0.0017(8)
C14y1	0.0007(4)	-0.0065(4)
C14z1	0.0006(10)	-0.0052(10)
O4wx1	0.0076(7)	0.0601(7)
O4wy1	0.0082(4)	-0.0193(4)
O4wz1	-0.0259(9)	-0.0119(8)
O172x1	0.0019(6)	-0.0025(6)
O172y1	-0.0013(3)	-0.0078(3)
O172z1	-0.0058(7)	-0.0016(7)
C17x1	0.004(9)	-0.0007(9)
C17y1	-0.001(4)	-0.009(4)
C17z1	-0.0051(11)	-0.0048(10)
C12x1	-0.0007(9)	-0.0029(9)
C12y1	0.0007(4)	-0.0088(4)
C12z1	-0.0062(10)	0.0018(10)
C22x1	0.0001(9)	0.0038(9)
C22y1	0.0038(4)	-0.0098(4)
C22z1	0.0007(10)	-0.0044(11)
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	0.0617(13)
O5wy1	0	0.0547(7)
O5wz1	0	-0.0219(15)