Investigation of the preparation and reactivity of metal-organic frameworks of cerium and pyridine-2,4,6-tricarboxylate.
Fonseca de Lima, Juliana; Moreno, Fernanda V. S.; Menezes, Bruno A. T.; da Silva Barbosa, Jader; Waddington, Matthew C.; Franklin, Siân A; Clarkson, Guy J.; Walker, Marc; Serra, Osvaldo A.; Walton, Richard I.; Dalton transactions (Cambridge, England : 2003) 51 (2021) 145–155; doi:10.1039/d1dt03514b

data_7709039
_publ_section_title
;
 Investigation of the preparation and reactivity of metal-organic
 frameworks of cerium and pyridine-2,4,6-tricarboxylate.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              145
_journal_page_last               155
_journal_paper_doi               10.1039/d1dt03514b
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety         'C8 H2 N Na3 O6'
_chemical_formula_sum            'C8 H2 N Na3 O6'
_chemical_formula_weight         277.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-20
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2021-09-20 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.590(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.42187(8)
_cell_length_b                   16.9689(4)
_cell_length_c                   15.1988(4)
_cell_measurement_reflns_used    9232
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.4890
_cell_measurement_theta_min      4.6660
_cell_volume                     882.18(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  25.00   1.00   60.00    --  -16.15 -99.00  30.00   45
  2  \w     -7.00  92.00   1.00   60.00    --   17.24  37.00 -60.00   99
  3  \w     34.00 104.00   1.00   60.00    --   17.24-178.00-120.00   70
  4  \w    -11.00  90.00   1.00   60.00    --   17.24  57.00   0.00  101
  5  \w    -59.00  50.00   1.00   60.00    --   17.24 -77.00-120.00  109
  6  \w    -40.00  58.00   1.00   60.00    --  -16.15  37.00   0.00   98
  7  \w   -103.00 -55.00   1.00   60.00    --  -16.15 178.00 -60.00   48
  8  \w    -20.00  25.00   1.00   60.00    --  -16.15 -99.00   0.00   45
  9  \w    -20.00  58.00   1.00   60.00    --   17.24 -99.00 -60.00   78
 10  \w    -11.00  90.00   1.00   60.00    --   17.24  57.00-180.00  101
 11  \w    -59.00  47.00   1.00   60.00    --   17.24 -77.00 -60.00  106
 12  \w    -20.00  58.00   1.00   60.00    --   17.24 -99.00  90.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0181264000
_diffrn_orient_matrix_UB_12      0.0060074000
_diffrn_orient_matrix_UB_13      -0.0458919000
_diffrn_orient_matrix_UB_21      0.2041658000
_diffrn_orient_matrix_UB_22      0.0057283000
_diffrn_orient_matrix_UB_23      0.0062907000
_diffrn_orient_matrix_UB_31      0.0312086000
_diffrn_orient_matrix_UB_32      -0.0409724000
_diffrn_orient_matrix_UB_33      -0.0058398000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12566
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.770
_diffrn_reflns_theta_min         3.600
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1278 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
Flack x: -0.07(7) Shelx 2018
Hooft y: -0.08(7) Olex2
Not really important as interested in the structure and not the handedness of the crystal
;
_refine_ls_abs_structure_Flack   -0.08(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2773
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.3737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.896
_reflns_number_gt                2735
_reflns_number_total             2773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03514b2.cif
_cod_data_source_block           rwj14
_cod_depositor_comments
'Adding full bibliography for 7709038--7709041.cif.'
_cod_original_cell_volume        882.19(3)
_cod_database_code               7709039
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N2 O8 Ce'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7)
;
_shelx_res_checksum              44385
_shelx_hkl_checksum              31538
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.510
_oxdiff_exptl_absorpt_empirical_full_min 0.703