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#$Date: 2016-03-23 16:08:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179363 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/60/4326089.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4326089
loop_
_publ_author_name
'Javier Cepeda'
'Rolindes Balda'
'Garikoitz Beobide'
'Oscar Castillo'
'Joaquín Fernández'
'Antonio Luque'
'Sonia Pérez-Yáñez'
'Pascual Román'
'Daniel Vallejo-Sánchez'
_publ_contact_author
;
 Oscar Castillo. Departamento de Quimica Inorganica. 
Facultad de Ciencia y Tecnologia
Universidad del Pais Vasco,  Apdo. 644, 
E-48080 Bilbao, Spain
;
_publ_contact_author_email       oscar.castillo@ehu.es
_publ_contact_author_fax         '+34-946 013 500'
_publ_contact_author_phone       '+34-946 015 991'
_publ_section_title
;
 Lanthanide(III)/Pyrimidine-4,6-dicarboxylate/Oxalate Extended Frameworks:
 A Detailed Study Based on the Lanthanide Contraction and Temperature
 Effects
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8437
_journal_page_last               8451
_journal_paper_doi               10.1021/ic201013v
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C7 H6 N2 O8 Yb, 3(H2 O)'
_chemical_formula_structural     'C7 H6 N2 O8 Yb, 3(H2 O)'
_chemical_formula_sum            'C7 H12 N2 O11 Yb'
_chemical_formula_weight         473.23
_chemical_name_systematic
;
poly-{[(mu-oxalato)bis(mu-pyrimidine-4,6-dicarboxylato)-k2N1,O:k2N3,O')-
tetraacuadiytterbium(III)]hexahydrate}
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 131.74(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.589(3)
_cell_length_b                   13.0259(10)
_cell_length_c                   14.065(2)
_cell_measurement_reflns_used    11324
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.07
_cell_measurement_theta_min      2.92
_cell_volume                     2541.2(10)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11324
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.425
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
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.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.474
_exptl_crystal_density_meas      2.48(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         2.244
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.602
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0383P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                2516
_reflns_number_total             3724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201013v_si_002_02.cif
_cod_data_source_block           1-Yb
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4326089
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Yb1 Yb 0.301413(9) 0.999722(12) 0.230482(12) 0.00614(6) Uani 1 1 d .
N11 N 0.2857(2) 1.1895(2) 0.1847(3) 0.0087(6) Uani 1 1 d .
C12 C 0.2466(3) 1.2604(3) 0.2075(4) 0.0099(7) Uani 1 1 d .
H12 H 0.2081 1.2369 0.2232 0.012 Uiso 1 1 calc R
N13 N 0.2421(2) 0.8613(2) 0.2904(3) 0.0087(6) Uani 1 1 d .
C14 C 0.1872(3) 0.8943(3) 0.3150(3) 0.0092(7) Uani 1 1 d .
C15 C 0.3550(3) 1.3270(3) 0.1587(3) 0.0102(7) Uani 1 1 d .
H15 H 0.3924 1.3505 0.1412 0.012 Uiso 1 1 calc R
C16 C 0.3396(3) 1.2229(3) 0.1596(3) 0.0088(7) Uani 1 1 d .
C17 C 0.3815(3) 1.1396(3) 0.1324(4) 0.0113(7) Uani 1 1 d .
O171 O 0.3674(2) 1.0486(2) 0.1500(3) 0.0125(5) Uani 1 1 d .
O172 O 0.4215(2) 1.1651(2) 0.0929(3) 0.0142(6) Uani 1 1 d .
C18 C 0.1730(3) 1.0099(3) 0.3072(3) 0.0094(7) Uani 1 1 d .
O181 O 0.21268(19) 1.0603(2) 0.2763(2) 0.0101(6) Uani 1 1 d .
O182 O 0.1237(2) 1.0460(2) 0.3294(3) 0.0124(6) Uani 1 1 d .
O21 O 0.40880(19) 1.09065(19) 0.4226(2) 0.0118(5) Uani 1 1 d .
C22 C 0.4903(2) 1.0529(3) 0.5125(3) 0.0090(7) Uani 1 1 d .
O23 O 0.44442(19) 0.90838(19) 0.3807(2) 0.0120(5) Uani 1 1 d .
O1W O 0.29110(19) 0.85477(19) 0.1289(3) 0.0113(5) Uani 1 1 d .
O2W O 0.14743(19) 1.00282(18) 0.0372(2) 0.0121(5) Uani 1 1 d .
O3W O 0.03133(19) 1.20599(19) 0.1637(3) 0.0142(6) Uani 1 1 d .
O4W O 0.5250(2) 0.3430(2) 0.4636(3) 0.0169(6) Uani 1 1 d .
O5W O 0.14811(19) 0.7209(2) 0.9849(3) 0.0127(5) Uani 1 1 d .
H11W H 0.3110 0.8364 0.0919 0.019 Uiso 1 1 d .
H12W H 0.2496 0.8030 0.1097 0.019 Uiso 1 1 d .
H21W H 0.1348 0.9875 -0.0315 0.019 Uiso 1 1 d .
H22W H 0.1043 1.0483 0.0114 0.019 Uiso 1 1 d .
H31W H 0.0613 1.1557 0.2154 0.019 Uiso 1 1 d .
H32W H 0.0382 1.2691 0.1536 0.019 Uiso 1 1 d .
H41W H 0.5297 0.3250 0.5269 0.019 Uiso 1 1 d .
H42W H 0.5422 0.2885 0.4492 0.019 Uiso 1 1 d .
H51W H 0.0917 0.7488 0.9395 0.019 Uiso 1 1 d .
H52W H 0.1338 0.6808 1.0183 0.019 Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O171 Yb1 O181 141.93(10) . .
O171 Yb1 O2W 93.85(10) . .
O181 Yb1 O2W 76.15(9) . .
O171 Yb1 O1W 76.52(9) . .
O181 Yb1 O1W 133.24(9) . .
O2W Yb1 O1W 75.82(9) . .
O171 Yb1 O23 85.76(10) . .
O181 Yb1 O23 121.53(9) . .
O2W Yb1 O23 148.64(9) . .
O1W Yb1 O23 73.60(9) . .
O171 Yb1 O21 96.09(10) . .
O181 Yb1 O21 73.75(9) . .
O2W Yb1 O21 142.40(9) . .
O1W Yb1 O21 141.78(9) . .
O23 Yb1 O21 68.44(9) . .
O171 Yb1 N11 66.61(9) . .
O181 Yb1 N11 75.50(9) . .
O2W Yb1 N11 80.71(9) . .
O1W Yb1 N11 134.40(9) . .
O23 Yb1 N11 126.75(9) . .
O21 Yb1 N11 70.38(9) . .
O171 Yb1 N13 151.01(10) . .
O181 Yb1 N13 66.05(9) . .
O2W Yb1 N13 86.01(9) . .
O1W Yb1 N13 75.36(9) . .
O23 Yb1 N13 79.74(10) . .
O21 Yb1 N13 101.60(10) . .
N11 Yb1 N13 141.30(10) . .
O171 Yb1 C22 88.49(10) . 5_676
O181 Yb1 C22 108.67(9) . 5_676
O2W Yb1 C22 168.37(9) . 5_676
O1W Yb1 C22 93.71(9) . 5_676
O23 Yb1 C22 20.20(9) . 5_676
O21 Yb1 C22 48.25(9) . 5_676
N11 Yb1 C22 110.59(10) . 5_676
N13 Yb1 C22 86.44(10) . 5_676
O171 Yb1 C22 92.73(10) . .
O181 Yb1 C22 88.71(9) . .
O2W Yb1 C22 162.48(9) . .
O1W Yb1 C22 121.56(9) . .
O23 Yb1 C22 48.16(9) . .
O21 Yb1 C22 20.29(9) . .
N11 Yb1 C22 87.05(10) . .
N13 Yb1 C22 95.98(10) . .
C22 Yb1 C22 27.97(13) 5_676 .
O171 Yb1 C17 18.36(9) . .
O181 Yb1 C17 124.06(9) . .
O2W Yb1 C17 92.94(9) . .
O1W Yb1 C17 94.03(9) . .
O23 Yb1 C17 95.98(9) . .
O21 Yb1 C17 85.73(9) . .
N11 Yb1 C17 48.56(9) . .
N13 Yb1 C17 169.28(10) . .
C22 Yb1 C17 92.83(10) 5_676 .
C22 Yb1 C17 88.24(9) . .
O171 Yb1 C18 159.36(9) . .
O181 Yb1 C18 17.99(9) . .
O2W Yb1 C18 77.09(9) . .
O1W Yb1 C18 118.02(9) . .
O23 Yb1 C18 111.67(9) . .
O21 Yb1 C18 81.08(9) . .
N11 Yb1 C18 93.41(9) . .
N13 Yb1 C18 48.06(9) . .
C22 Yb1 C18 104.15(9) 5_676 .
C22 Yb1 C18 91.27(9) . .
C17 Yb1 C18 141.95(9) . .
C12 N11 C16 117.4(3) . .
C12 N11 Yb1 127.2(2) . .
C16 N11 Yb1 114.0(2) . .
N13 C12 N11 125.8(4) 4 .
C12 N13 C14 116.4(3) 4_545 .
C12 N13 Yb1 127.9(3) 4_545 .
C14 N13 Yb1 115.5(2) . .
N13 C14 C15 121.9(3) . 4_545
N13 C14 C18 115.0(3) . .
C15 C14 C18 123.1(3) 4_545 .
C14 C15 C16 117.4(3) 4 .
N11 C16 C15 121.0(3) . .
N11 C16 C17 115.6(3) . .
C15 C16 C17 123.4(3) . .
O172 C17 O171 127.0(4) . .
O172 C17 C16 118.8(3) . .
O171 C17 C16 114.1(3) . .
O172 C17 Yb1 160.7(3) . .
C16 C17 Yb1 80.5(2) . .
C17 O171 Yb1 127.9(2) . .
O182 C18 O181 126.0(3) . .
O182 C18 C14 118.7(3) . .
O181 C18 C14 115.3(3) . .
O182 C18 Yb1 159.9(3) . .
C14 C18 Yb1 81.4(2) . .
C18 O181 Yb1 128.2(2) . .
C22 O21 Yb1 119.5(2) . .
O23 C22 O21 127.4(3) 5_676 .
O23 C22 C22 117.0(4) 5_676 5_676
O21 C22 C22 115.6(4) . 5_676
O21 C22 Yb1 167.7(3) . 5_676
C22 C22 Yb1 76.6(3) 5_676 5_676
C22 C22 Yb1 75.4(3) 5_676 .
Yb1 C22 Yb1 152.03(13) 5_676 .
C22 O23 Yb1 119.5(2) 5_676 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Yb1 O171 2.245(3) .
Yb1 O181 2.275(2) .
Yb1 O2W 2.285(3) .
Yb1 O1W 2.297(2) .
Yb1 O23 2.338(3) .
Yb1 O21 2.347(3) .
Yb1 N11 2.522(3) .
Yb1 N13 2.533(3) .
Yb1 C22 3.145(4) 5_676
Yb1 C22 3.162(4) .
Yb1 C17 3.190(4) .
Yb1 C18 3.211(4) .
N11 C12 1.339(4) .
N11 C16 1.340(5) .
C12 N13 1.328(4) 4
N13 C12 1.328(4) 4_545
N13 C14 1.347(5) .
C14 C15 1.382(5) 4_545
C14 C18 1.520(5) .
C15 C14 1.382(5) 4
C15 C16 1.386(5) .
C16 C17 1.526(5) .
C17 O172 1.233(4) .
C17 O171 1.273(4) .
C18 O182 1.242(4) .
C18 O181 1.261(4) .
O21 C22 1.259(4) .
C22 O23 1.247(4) 5_676
C22 C22 1.524(7) 5_676
C22 Yb1 3.145(4) 5_676
O23 C22 1.247(4) 5_676
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O5W 0.85 1.84 2.688(4) 172.5 7_566
O1W H12W O5W 0.92 1.84 2.653(4) 146.6 1_554
O2W H21W O182 0.85 1.88 2.725(4) 172.8 6_575
O2W H22W O4W 0.86 1.82 2.673(4) 172.6 8_465
O3W H31W O182 0.85 1.87 2.719(4) 177.9 .
O3W H32W O23 0.86 1.96 2.814(4) 174.3 4
O4W H41W O3W 0.87 1.95 2.811(4) 174.7 8_566
O4W H42W O172 0.86 1.98 2.836(4) 177.1 2_645
O5W H51W O3W 0.86 1.81 2.668(4) 174.0 5_576
O5W H52W O21 0.86 1.89 2.743(3) 174.9 4_546
