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#$Date: 2017-03-04 15:11:25 +0200 (Sat, 04 Mar 2017) $
#$Revision: 193426 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/51/4345159.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_4345159
loop_
_publ_author_name
'Marinho, Maria Vanda'
'Reis, Daniella O.'
'Oliveira, Willian X. C.'
'Marques, Lippy F.'
'Stumpf, Humberto O.'
'Déniz, Mariadel'
'Pasán, Jorge'
'Ruiz-Pérez, Catalina'
'Cano, Joan'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 Photoluminescent and Slow Magnetic Relaxation Studies on
 Lanthanide(III)-2,5-pyrazinedicarboxylate Frameworks.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2108
_journal_page_last               2123
_journal_paper_doi               10.1021/acs.inorgchem.6b02774
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C9 H13 Ce N3 O11'
_chemical_formula_weight         479.26
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                72.607(5)
_cell_angle_beta                 88.789(5)
_cell_angle_gamma                88.980(5)
_cell_formula_units_Z            2
_cell_length_a                   6.099(5)
_cell_length_b                   10.501(5)
_cell_length_c                   13.688(5)
_cell_measurement_reflns_used    5004
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.461
_cell_measurement_theta_min      3.284
_cell_volume                     836.3(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31f (release 05-03-2014 CrysAlis171 .NET)
(compiled Mar  5 2014,18:34:03)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31f (release 05-03-2014 CrysAlis171 .NET)
(compiled Mar  5 2014,18:34:03)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31f (release 05-03-2014 CrysAlis171 .NET)
(compiled Mar  5 2014,18:34:03)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5004
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         73.461
_diffrn_reflns_theta_min         3.384
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    21.612
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.115
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_description       needle
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.405
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0590P)²+0.7524P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3118
_reflns_number_total             3200
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02774_si_002.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
'Adding full bibliography for 4345159--4345161.cif.'
_cod_original_cell_volume        836.3(8)
_cod_database_code               4345159
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.046
_shelx_estimated_absorpt_t_max   0.563
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ce1 Ce 0.74860(3) 0.33898(2) 0.29069(2) 0.01959(10) Uani 1 1 d . . .
C1 C 0.6007(7) 0.1313(4) 0.5269(3) 0.0259(8) Uani 1 1 d . . .
C3 C 1.1089(7) 0.0517(4) 0.4116(3) 0.0302(9) Uani 1 1 d . . .
H6 H 1.1894 0.0853 0.3511 0.036 Uiso 1 1 calc R U .
O1 O 0.5458(5) 0.2284(3) 0.4529(2) 0.0325(6) Uani 1 1 d . . .
O2 O 0.4974(6) 0.0894(4) 0.6097(3) 0.0428(8) Uani 1 1 d . . .
O3 O 0.9376(5) 0.3024(4) 0.1416(2) 0.0359(7) Uani 1 1 d . . .
O4 O 1.0015(7) 0.3211(5) -0.0222(3) 0.0507(10) Uani 1 1 d . . .
N2 N 0.5656(6) 0.4437(4) 0.1005(3) 0.0278(7) Uani 1 1 d . . .
N1 N 0.9214(5) 0.1119(4) 0.4249(3) 0.0274(7) Uani 1 1 d . . .
C2 C 0.8133(6) 0.0603(4) 0.5136(3) 0.0253(8) Uani 1 1 d . . .
C5 C 0.6826(7) 0.4262(4) 0.0223(3) 0.0265(8) Uani 1 1 d . . .
C4 C 0.8908(7) 0.3430(4) 0.0481(3) 0.0290(8) Uani 1 1 d . . .
C6 C 0.3826(7) 0.5177(4) 0.0783(3) 0.0298(8) Uani 1 1 d . . .
H3 H 0.2971 0.5319 0.1312 0.036 Uiso 1 1 calc R U .
O2W O 0.8471(6) 0.5829(3) 0.2184(2) 0.0366(7) Uani 1 1 d . . .
O1W O 0.5648(6) 0.1504(3) 0.2521(3) 0.0428(8) Uani 1 1 d . . .
O6 O 1.4390(4) 0.4774(3) 0.3251(2) 0.0269(6) Uani 1 1 d . . .
O5 O 1.1554(5) 0.3589(3) 0.3011(2) 0.0287(6) Uani 1 1 d . . .
C7 C 1.2475(6) 0.4326(4) 0.3433(3) 0.0229(7) Uani 1 1 d . . .
C8 C 1.1166(6) 0.4710(4) 0.4257(3) 0.0233(7) Uani 1 1 d . . .
N3 N 0.9102(5) 0.4273(4) 0.4413(3) 0.0254(7) Uani 1 1 d . . .
C9 C 0.7946(6) 0.4558(4) 0.5156(3) 0.0257(8) Uani 1 1 d . . .
H9 H 0.6510 0.4262 0.5286 0.031 Uiso 1 1 calc R U .
O3W O 0.3709(13) 0.1599(8) 0.0727(7) 0.115(3) Uani 1 1 d . . .
O4W O 0.380(5) -0.179(4) 0.142(4) 0.34(3) Uani 0.5 1 d . . P
O5W O 0.833(2) 0.7717(9) 0.3170(10) 0.196(6) Uani 1 1 d . . .
O6W O 0.998(4) 0.983(2) 0.1690(19) 0.171(10) Uani 0.5 1 d . . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -1.8482 9.6596 '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
O3 Ce1 O6 137.72(10) . 1_455
O3 Ce1 O1W 72.63(12) . .
O6 Ce1 O1W 103.76(12) 1_455 .
O3 Ce1 O1 144.50(12) . .
O6 Ce1 O1 67.18(10) 1_455 .
O1W Ce1 O1 76.82(12) . .
O3 Ce1 O5 68.70(10) . .
O6 Ce1 O5 131.77(10) 1_455 .
O1W Ce1 O5 124.33(12) . .
O1 Ce1 O5 117.19(10) . .
O3 Ce1 O2W 87.46(12) . .
O6 Ce1 O2W 71.19(11) 1_455 .
O1W Ce1 O2W 144.01(11) . .
O1 Ce1 O2W 128.03(11) . .
O5 Ce1 O2W 71.63(11) . .
O3 Ce1 N3 129.39(11) . .
O6 Ce1 N3 77.95(10) 1_455 .
O1W Ce1 N3 144.85(11) . .
O1 Ce1 N3 71.59(11) . .
O5 Ce1 N3 61.30(10) . .
O2W Ce1 N3 70.48(11) . .
O3 Ce1 N1 93.67(11) . .
O6 Ce1 N1 126.75(10) 1_455 .
O1W Ce1 N1 74.61(12) . .
O1 Ce1 N1 60.62(11) . .
O5 Ce1 N1 69.68(10) . .
O2W Ce1 N1 137.84(11) . .
N3 Ce1 N1 76.69(11) . .
O3 Ce1 N2 61.25(11) . .
O6 Ce1 N2 77.09(10) 1_455 .
O1W Ce1 N2 73.83(11) . .
O1 Ce1 N2 125.92(11) . .
O5 Ce1 N2 116.89(10) . .
O2W Ce1 N2 70.30(11) . .
N3 Ce1 N2 138.48(11) . .
N1 Ce1 N2 144.36(11) . .
O2 C1 O1 125.8(4) . .
O2 C1 C2 118.1(4) . .
O1 C1 C2 116.2(4) . .
N1 C3 C2 121.3(4) . 2_756
C1 O1 Ce1 129.9(3) . .
C4 O3 Ce1 130.4(3) . .
C5 N2 C6 117.2(4) . .
C5 N2 Ce1 115.6(3) . .
C6 N2 Ce1 127.0(3) . .
C3 N1 C2 116.8(4) . .
C3 N1 Ce1 125.8(3) . .
C2 N1 Ce1 117.3(3) . .
N1 C2 C3 121.8(4) . 2_756
N1 C2 C1 115.7(4) . .
C3 C2 C1 122.5(4) 2_756 .
N2 C5 C6 121.5(4) . 2_665
N2 C5 C4 116.9(4) . .
C6 C5 C4 121.6(4) 2_665 .
O4 C4 O3 125.2(4) . .
O4 C4 C5 119.0(4) . .
O3 C4 C5 115.8(4) . .
N2 C6 C5 121.3(4) . 2_665
C7 O6 Ce1 121.8(3) . 1_655
C7 O5 Ce1 124.8(2) . .
O5 C7 O6 126.5(3) . .
O5 C7 C8 116.5(3) . .
O6 C7 C8 116.9(3) . .
N3 C8 C9 121.2(4) . 2_766
N3 C8 C7 116.3(3) . .
C9 C8 C7 122.5(3) 2_766 .
C9 N3 C8 117.4(4) . .
C9 N3 Ce1 126.3(3) . .
C8 N3 Ce1 114.9(2) . .
N3 C9 C8 121.5(4) . 2_766
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce1 O3 2.448(3) .
Ce1 O6 2.485(3) 1_455
Ce1 O1W 2.487(3) .
Ce1 O1 2.490(3) .
Ce1 O5 2.504(3) .
Ce1 O2W 2.533(3) .
Ce1 N3 2.710(4) .
Ce1 N1 2.746(4) .
Ce1 N2 2.757(4) .
C1 O2 1.247(5) .
C1 O1 1.250(5) .
C1 C2 1.519(6) .
C3 N1 1.332(6) .
C3 C2 1.393(6) 2_756
O3 C4 1.260(5) .
O4 C4 1.239(6) .
N2 C5 1.330(5) .
N2 C6 1.336(6) .
N1 C2 1.338(5) .
C2 C3 1.393(6) 2_756
C5 C6 1.390(6) 2_665
C5 C4 1.515(6) .
C6 C5 1.390(6) 2_665
O6 C7 1.259(5) .
O6 Ce1 2.485(3) 1_655
O5 C7 1.242(5) .
C7 C8 1.514(5) .
C8 N3 1.338(5) .
C8 C9 1.390(6) 2_766
N3 C9 1.329(5) .
C9 C8 1.390(6) 2_766
