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: 10202Eh7wvj Entry date: 2015-02-19 Last revision: 2022-01-02

3-Sm

Chemical data

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

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

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

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

Formula weight: 438.47 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: 9.7465(3) Å [ Help ]

b: 15.9265(5) Å [ Help ]

c: 7.9809(7) Å [ Help ]

α: 90 ° [ Help ]

β: 96.2159(3) ° [ Help ]

γ: 90 ° [ Help ]

Volume: 1231.6(2) Å³ [ Help ]

Modulation dimension: 1 [ Help ]

Z: 4 [ Help ]

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

Cell determination reflection Nb.: 25423 [ Help ]

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

θ(max) for cell determination: 30.09 ° [ Help ]

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

Wave vector id	q_x	q_y	q_z
1	0	0	0.33333

μ: 4.768 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: 0.607 [ Help ]

Maximum transmission factor: 0.788 [ Help ]

Refinement details

Total nb. of reflections: 10840 [ Help ]

Nb. of observed reflections: 6160 [ 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: 10840 [ Help ]

Nb. of parameters: 322 [ Help ]

R(obs): 0.0458 [ Help ]

wR(obs): 0.0576 [ Help ]

R(all): 0.0728 [ Help ]

wR(all): 0.059 [ Help ]

S(all): 1.71 [ Help ]

S(obs): 2.24 [ Help ]

Δ/σ(max): 0.0343 [ Help ]

Δ/σ(mean): 0.0027 [ Help ]

Δρ(max): 5.62 e_Å^-3 [ Help ]

Δρ(min): -2.91 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
Sm1	Sm	0.8649(2)	0.67327(14)	0.08019(3)	Uani	0.00546(6)	4	1	d	?	?	?
O171	O	0.7036(3)	0.57145(19)	-0.0491(4)	Uani	0.0107(9)	4	1	d	?	?	?
O3w	O	0.6274(3)	0.9257(2)	0.0419(4)	Uani	0.0188(11)	4	1	d	?	?	?
O182	O	1.1111(3)	0.68864(18)	0.15(4)	Uani	0.0093(9)	4	1	d	?	?	?
O21	O	0.9435(3)	0.53553(18)	0.1878(4)	Uani	0.0089(9)	4	1	d	?	?	?
O181	O	0.6866(3)	0.74057(19)	-0.1176(4)	Uani	0.0098(9)	4	1	d	?	?	?
O2w	O	0.8322(3)	0.81896(18)	0.1662(4)	Uani	0.0124(9)	4	1	d	?	?	?
O23	O	0.9753(3)	0.59008(18)	-0.1248(4)	Uani	0.0079(8)	4	1	d	?	?	?
O1w	O	0.8979(3)	0.6761(2)	0.3914(4)	Uani	0.0137(9)	4	1	d	?	?	?
N11	N	0.621(3)	0.6706(2)	0.1895(4)	Uani	0.0069(9)	4	1	d	?	?	?
N13	N	0.9485(3)	0.7684(2)	-0.1625(4)	Uani	0.0064(9)	4	1	d	?	?	?
C16	C	0.5237(4)	0.6317(3)	0.0865(5)	Uani	0.0055(11)	4	1	d	?	?	?
C18	C	0.7037(4)	0.7851(3)	-0.2427(5)	Uani	0.0058(11)	4	1	d	?	?	?
C15	C	0.3844(4)	0.6409(3)	0.1049(5)	Uani	0.0072(11)	4	1	d	?	?	?
C14	C	0.3512(4)	0.6932(2)	0.2317(5)	Uani	0.0058(11)	4	1	d	?	?	?
O4w	O	0.7571(4)	0.5706(2)	0.5741(5)	Uani	0.0256(13)	4	1	d	?	?	?
O172	O	0.4872(3)	0.55754(18)	-0.1711(4)	Uani	0.0096(8)	4	1	d	?	?	?
C17	C	0.5747(4)	0.5817(3)	-0.0567(5)	Uani	0.0061(11)	4	1	d	?	?	?
C12	C	1.0795(4)	0.7812(3)	-0.1889(5)	Uani	0.0077(11)	4	1	d	?	?	?
C22	C	0.9908(4)	0.4841(3)	0.0894(5)	Uani	0.0069(11)	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	0.033(3)	2	0.5	d	?	?	?

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

Atom site label	Atom site symbol	U11	U22	U33	U12	U13	U23
Sm1	Sm	0.00196(9)	0.00773(11)	0.00636(9)	0.0008(9)	-0.00104(6)	-0.00052(10)
O171	O	0.0052(13)	0.012(16)	0.0147(15)	0.001(12)	0(11)	-0.001(12)
O3w	O	0.012(17)	0.028(2)	0.0146(19)	0.0084(16)	-0.0053(14)	-0.0103(15)
O182	O	0.003(12)	0.0144(17)	0.0101(15)	-0.001(11)	-0.0016(11)	-0.0024(12)
O21	O	0.0102(14)	0.009(16)	0.0075(14)	0.0037(12)	0.0006(11)	0.0012(11)
O181	O	0.0044(12)	0.0144(17)	0.0104(15)	-0.0014(12)	-0.0002(11)	0.0037(12)
O2w	O	0.0134(15)	0.0102(16)	0.0128(15)	0.001(13)	-0.0012(12)	-0.003(12)
O23	O	0.0069(13)	0.009(15)	0.0077(14)	0.0009(11)	0.0002(11)	0.0014(11)
O1w	O	0.0125(15)	0.0191(17)	0.0085(14)	0.005(15)	-0.003(11)	-0.0053(14)
N11	N	0.0042(14)	0.0091(17)	0.0071(15)	0.0009(14)	-0.0014(11)	0.0033(14)
N13	N	0.0037(14)	0.0076(18)	0.0079(16)	0.0002(13)	0.0008(12)	-0.0018(13)
C16	C	0.0075(17)	0.0029(19)	0.0056(18)	0.0001(15)	-0.0009(14)	0.0027(15)
C18	C	0.0043(16)	0.005(2)	0.0078(18)	-0.0004(15)	-0.0014(14)	-0.0043(15)
C15	C	0.0074(18)	0.0073(19)	0.0065(19)	-0.0023(15)	-0.0013(14)	0.0012(15)
C14	C	0.005(16)	0.005(2)	0.0072(18)	-0.0005(14)	0.0005(14)	0.0038(14)
O4w	O	0.025(2)	0.036(2)	0.015(2)	-0.0069(18)	-0.0005(18)	-0.0013(17)
O172	O	0.0078(13)	0.0108(16)	0.0097(14)	-0.0001(12)	-0.0017(11)	-0.0023(11)
C17	C	0.0049(17)	0.005(2)	0.0086(19)	0.0014(15)	0.002(14)	0.0011(15)
C12	C	0.0059(17)	0.009(2)	0.008(18)	0.0031(16)	-0.0009(14)	-0.0003(16)
C22	C	0.0027(16)	0.01(2)	0.0074(18)	-0.0002(15)	-0.0022(13)	0.0001(16)
O5w	O	0.041(5)	0.036(4)	0.024(4)	0.008(4)	0.013(4)	-0.007(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
Sm1x1	Sm1	x	1
Sm1y1	Sm1	y	1
Sm1z1	Sm1	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
Sm1x1	0.00154(4)	0.00087(5)
Sm1y1	0.00422(2)	-0.011375(19)
Sm1z1	-0.00803(5)	-0.00576(5)
O171x1	0.0033(6)	-0.0008(6)
O171y1	-0.0002(3)	-0.0111(3)
O171z1	-0.0047(7)	-0.0008(7)
O3wx1	0.0025(6)	-0.0141(6)
O3wy1	0.0062(3)	-0.0292(3)
O3wz1	-0.007(7)	0.0292(7)
O182x1	0.0032(5)	0.0015(5)
O182y1	0.0057(3)	-0.0065(3)
O182z1	-0.0112(6)	-0.0079(6)
O21x1	0.0081(6)	0.006(6)
O21y1	0.0088(3)	-0.0078(3)
O21z1	0.0025(6)	-0.0048(6)
O181x1	0.0012(6)	-0.0002(5)
O181y1	-0.0038(3)	-0.0125(3)
O181z1	-0.0099(7)	-0.0004(7)
O2wx1	-0.0036(6)	0.0064(6)
O2wy1	0.0058(3)	-0.0103(3)
O2wz1	-0.0104(7)	-0.004(7)
O23x1	0.006(6)	-0.0007(5)
O23y1	-0.0041(3)	-0.0104(3)
O23z1	-0.0059(6)	-0.0034(6)
O1wx1	-0.0002(6)	0.0076(6)
O1wy1	0.0148(3)	-0.0027(3)
O1wz1	-0.0057(7)	-0.0089(7)
N11x1	0.0031(7)	0.0021(7)
N11y1	0.0019(3)	-0.0093(3)
N11z1	-0.0001(8)	-0.003(8)
N13x1	0(7)	-0.0032(6)
N13y1	0.0007(3)	-0.0088(3)
N13z1	-0.006(8)	0.0011(8)
C16x1	0.0021(8)	0.0009(8)
C16y1	0.0018(4)	-0.008(4)
C16z1	-0.0037(9)	-0.0054(9)
C18x1	-0.0006(8)	0.0005(8)
C18y1	0.0006(4)	-0.0078(4)
C18z1	-0.001(9)	0.0072(9)
C15x1	0.0029(8)	0.0003(8)
C15y1	0.0012(4)	-0.0066(4)
C15z1	-0.0041(9)	-0.0074(9)
C14x1	-0.0009(8)	0.001(7)
C14y1	0.0008(4)	-0.0073(4)
C14z1	0.0007(9)	-0.0062(9)
O4wx1	0.0049(6)	0.0609(6)
O4wy1	0.0088(4)	-0.0196(3)
O4wz1	-0.0267(7)	-0.0137(7)
O172x1	0.0024(6)	-0.0023(6)
O172y1	-0.0011(3)	-0.0083(3)
O172z1	-0.0068(7)	-0.0016(7)
C17x1	0.0044(8)	-0.0011(8)
C17y1	-0.0007(4)	-0.01(4)
C17z1	-0.006(9)	-0.0033(9)
C12x1	-0.001(8)	-0.0015(8)
C12y1	0.0019(4)	-0.0098(4)
C12z1	-0.0036(9)	0.0017(9)
C22x1	0.0008(8)	0.0026(8)
C22y1	0.004(4)	-0.0104(4)
C22z1	0.0014(9)	-0.0048(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	0.0497(10)
O5wy1	0	0.0399(5)
O5wz1	0	-0.0154(11)

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

Modulation code	Atom site label	Tensor element	Wave vector code
Sm1U111	Sm1	U11	1
Sm1U221	Sm1	U22	1
Sm1U331	Sm1	U33	1
Sm1U121	Sm1	U12	1
Sm1U131	Sm1	U13	1
Sm1U231	Sm1	U23	1

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

Modulation code	Cosine coefficient	Sine coefficient
Sm1U111	-0.0006(2)	0.00011(19)
Sm1U221	-0.00217(18)	0.00022(17)
Sm1U331	-0.00003(19)	0.00074(17)
Sm1U121	-0.00011(12)	0.00022(13)
Sm1U131	-0.00001(16)	-0.00024(14)
Sm1U231	-0.00059(12)	-0.00143(13)