A highly stable cerium–organic framework: an efficient catalyst for the cycloaddition of CO2 and aziridines under mild-pressure
Liu, Tong-Ji; Xu, Hang; Shi, Ying; Zhao, Bin; CrystEngComm 26 (2024) 3687–3693; doi:10.1039/D4CE00167B

data_7248785
_publ_section_title
;
 A highly stable cerium--organic framework: an efficient catalyst for the
 cycloaddition of CO2 and aziridines under mild-pressure
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              3687
_journal_page_last               3693
_journal_paper_doi               10.1039/D4CE00167B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C29 H25 Ce N4 O7'
_chemical_formula_sum            'C29 H25 Ce N4 O7'
_chemical_formula_weight         681.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-02-17 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.488(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.0632(7)
_cell_length_b                   9.1635(3)
_cell_length_c                   32.5260(10)
_cell_measurement_reflns_used    13073
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.7930
_cell_measurement_theta_min      3.3350
_cell_volume                     5703.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.894
_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      4.00  87.00   1.00   10.00    --   18.47  57.00  60.00   83
  2  \w    -26.00  89.00   1.00   10.00    --   18.47  19.00   0.00  115
  3  \w     -1.00  89.00   1.00   10.00    --   18.47  77.00-180.00   90
  4  \w    -19.00   7.00   1.00   10.00    --   18.47 -99.00 -60.00   26
  5  \w     22.00  60.00   1.00   10.00    --   18.47 -99.00 -60.00   38
  6  \w     70.00  95.00   1.00   10.00    --   18.47-178.00 -90.00   25
  7  \w     42.00  80.00   1.00   10.00    --   18.47 178.00-150.00   38
  8  \w    -76.00 -42.00   1.00   10.00    --  -19.64 124.00  -3.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0146354000
_diffrn_orient_matrix_UB_12      0.0175878000
_diffrn_orient_matrix_UB_13      0.0166990000
_diffrn_orient_matrix_UB_21      -0.0304338000
_diffrn_orient_matrix_UB_22      0.0270023000
_diffrn_orient_matrix_UB_23      -0.0155178000
_diffrn_orient_matrix_UB_31      -0.0153138000
_diffrn_orient_matrix_UB_32      -0.0703412000
_diffrn_orient_matrix_UB_33      -0.0017566000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            25129
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.071
_diffrn_reflns_theta_min         2.841
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       blcok
_exptl_crystal_F_000             2728
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0133P)^2^+6.0447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6054
_reflns_number_total             6826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00167b2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7248785.cif.'
_cod_database_code               7248785
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C13(H13), C3(H3), C5(H5), C20(H20), C10(H10), C7(H7), C18(H18),
 C22(H22), C17(H17), C16(H16), C14(H14), C23(H23)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C)
;
_shelx_res_checksum              13033
_shelx_hkl_checksum              83720
_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 2.008
_oxdiff_exptl_absorpt_empirical_full_min 0.664