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_7709041
_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_absolute_configuration ad
_chemical_formula_moiety         'C16 H16 Ce2 N2 O18'
_chemical_formula_sum            'C16 H16 Ce2 N2 O18'
_chemical_formula_weight         804.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-20 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.4339(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.70661(9)
_cell_length_b                   9.44049(14)
_cell_length_c                   17.0698(2)
_cell_measurement_reflns_used    29097
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.5340
_cell_measurement_theta_min      3.0450
_cell_volume                     1079.78(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_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     35.00 102.00   1.00   13.50    --   13.26 178.00  60.00   67
  2  \w    -75.00 101.00   1.00   13.50    --   13.26   0.00-180.00  176
  3  \w    -25.00  27.00   1.00   13.50    --  -14.04 -99.00 -60.00   52
  4  \w    -25.00  27.00   1.00   13.50    --  -14.04 -99.00  30.00   52
  5  \w    -42.00  59.00   1.00   13.50    --  -14.04  57.00  60.00  101
  6  \w    -25.00  27.00   1.00   13.50    --  -14.04 -99.00   0.00   52
  7  \w    -61.00  38.00   1.00   13.50    --   13.26 -38.00  90.00   99
  8  \w    -15.00  86.00   1.00   13.50    --   13.26  57.00-120.00  101
  9  \w   -101.00 -53.00   1.00   13.50    --  -14.04 178.00 120.00   48
 10  \w    -75.00 -24.00   1.00   13.50    --  -14.04 134.00-131.00   51
 11  \w    -47.00  62.00   1.00   13.50    --  -14.04  77.00 120.00  109
 12  \w    -25.00  54.00   1.00   13.50    --   13.26 -99.00-120.00   79
 13  \w    -25.00  54.00   1.00   13.50    --   13.26 -99.00  30.00   79
 14  \w    -25.00  27.00   1.00   13.50    --  -14.04 -99.00  60.00   52
 15  \w    -76.00 -26.00   1.00   13.50    --  -14.04 136.00  47.00   50
 16  \w    -25.00  27.00   1.00   13.50    --  -14.04 -99.00 -90.00   52
 17  \w    -47.00  62.00   1.00   13.50    --  -14.04  77.00-180.00  109
 18  \w    -47.00 -22.00   1.00   13.50    --  -14.04  77.00  30.00   25
 19  \w    -25.00  27.00   1.00   13.50    --  -14.04 -99.00-120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0191532000
_diffrn_orient_matrix_UB_12      -0.0725066000
_diffrn_orient_matrix_UB_13      0.0075293000
_diffrn_orient_matrix_UB_21      0.0682555000
_diffrn_orient_matrix_UB_22      -0.0196522000
_diffrn_orient_matrix_UB_23      -0.0287049000
_diffrn_orient_matrix_UB_31      0.0786199000
_diffrn_orient_matrix_UB_32      -0.0006155000
_diffrn_orient_matrix_UB_33      0.0291439000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43697
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.676
_diffrn_reflns_theta_min         2.466
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.264
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
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    2.475
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 2850 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
Flack x: -0.021(7) Shelx 2018
Hooft y: -0.003(6) Olex2
Not really important as interested in the connectivity and not in defining the handedness 
of the crystal chosen. 
;
_refine_ls_abs_structure_Flack   -0.021(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6306
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0211
_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/[\s^2^(Fo^2^)+(0.0210P)^2^+0.3271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0437
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.904
_reflns_number_gt                6122
_reflns_number_total             6306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03514b2.cif
_cod_data_source_block           mcw1
_cod_depositor_comments
'Adding full bibliography for 7709038--7709041.cif.'
_cod_original_cell_volume        1079.77(3)
_cod_database_code               7709041
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N2 O6 Ce'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.02
_olex2_refinement_description
;
Most of the hydrogens on the chelated oxygens were located in a difference map but refined with distance
restraints.

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H11B-O210_$1
 2.1 with sigma of 0.01
 O108_$6-H21B
 2.35 with sigma of 0.02
 O102-H23A
 2.3 with sigma of 0.02
 H23B_$2-O111_$4
 2.4 with sigma of 0.02
 H12A-O202_$2
 2.5 with sigma of 0.02
 O11-H11A = O11-H11B = O21-H21A = O21-H21B = O22-H22A = O22-H22B
 0.85 with sigma of 0.02
 O12-H12A = O12-H12B = O13-H13A = O13-H13B = O23-H23A = O23-H23B
 0.85 with sigma of 0.015
 H12B-O208_$4
 2.4 with sigma of 0.02
 H11B-H11A = H12A-H12B = H13A-H13B = H21A-H21B = H22A-H22B = H23A-H23B
 1.4 with sigma of 0.03
3.a Aromatic/amide H refined with riding coordinates:
 C104(H104), C106(H106), C204(H204), C206(H206)
;
_shelx_res_checksum              71986
_shelx_hkl_checksum              26394
_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 1.454
_oxdiff_exptl_absorpt_empirical_full_min 0.787