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_7709040
_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 H6 Ce N O8, 1.5(O)'
_chemical_formula_sum            'C8 H6 Ce N O9.5'
_chemical_formula_weight         408.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2021-09-20 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.334(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.79808(15)
_cell_length_b                   12.0497(3)
_cell_length_c                   13.5329(3)
_cell_measurement_reflns_used    13456
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.3170
_cell_measurement_theta_min      3.0320
_cell_volume                     1090.56(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.936
_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     35.00 104.00   1.00   11.50    --   15.10 178.00 -90.00   69
  2  \w    -25.00  25.00   1.00   11.50    --  -16.04 -99.00-150.00   50
  3  \w   -104.00  66.00   1.00   11.50    --  -16.04   0.00 -90.00  170
  4  \w    -99.00  72.00   1.00   11.50    --  -16.04   0.00 120.00  171
  5  \w    -25.00  25.00   1.00   11.50    --  -16.04 -99.00  90.00   50
  6  \w   -103.00 -53.00   1.00   11.50    --  -16.04 178.00 -30.00   50
  7  \w    -25.00  20.00   1.00   11.50    --  -16.04 -99.00 -30.00   45
  8  \w    -98.00 -53.00   1.00   11.50    --  -16.04 178.00 -90.00   45
  9  \w    -25.00  25.00   1.00   11.50    --  -16.04 -99.00 150.00   50
 10  \w    -44.00  54.00   1.00   11.50    --  -16.04  57.00 -60.00   98
 11  \w    -22.00  56.00   1.00   11.50    --   15.10 -99.00-150.00   78
 12  \w    -25.00  13.00   1.00   11.50    --  -16.04 -99.00 -90.00   38
;
_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      -0.0687312000
_diffrn_orient_matrix_UB_12      -0.0253234000
_diffrn_orient_matrix_UB_13      0.0267485000
_diffrn_orient_matrix_UB_21      0.0805955000
_diffrn_orient_matrix_UB_22      -0.0189301000
_diffrn_orient_matrix_UB_23      0.0368259000
_diffrn_orient_matrix_UB_31      -0.0042770000
_diffrn_orient_matrix_UB_32      0.0497232000
_diffrn_orient_matrix_UB_33      0.0276330000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17555
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.408
_diffrn_reflns_theta_min         3.046
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.227
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.487
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.074
_refine_diff_density_max         2.037
_refine_diff_density_min         -2.323
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.335
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3369
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.334
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0467
_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^)+10.9530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3061
_reflns_number_total             3369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03514b2.cif
_cod_data_source_block           rwj13
_cod_depositor_comments
'Adding full bibliography for 7709038--7709041.cif.'
_cod_original_cell_volume        1090.56(5)
_cod_original_formula_sum        'C8 H6 Ce N O9.50'
_cod_database_code               7709040
_chemical_oxdiff_formula         'C8 H6 N O9.5 Ce'
_reflns_odcompleteness_completeness 99.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_olex2_refinement_description
;

There are three molecules of water in a void in the structure that were modeled at 
50% occupancy each.
The hydrogens were only located on the fully occupied waters O1 and O2. They were 
refined with DFIX and DANG restraints to give them idealized geometries.

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
 O1-H1A = O1-H1B = O2-H2A = O2-H2B
 0.82 with sigma of 0.02
 H1A-H1B = H2A-H2B
 1.35 with sigma of 0.04
3. Others
 Fixed Sof: O4(0.5) O3(0.5) O5(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7)
;
_shelx_res_checksum              17765
_shelx_hkl_checksum              61409
_shelx_shelxl_version_number     2014/7
_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 1.072
_oxdiff_exptl_absorpt_empirical_full_min 0.938