Electron transitions in a Ce(iii)-catecholate metal–organic framework
Knapp, Julia G.; Ray, Debmalya; Calio, Paul B.; Wasson, Megan C.; Scott, Thais R.; Gagliardi, Laura; Farha, Omar K.; Chemical Communications  (2022) –; doi:10.1039/D1CC06440A

data_7129389
_publ_section_title
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 Electron transitions in a Ce(iii)-catecholate metal--organic framework
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06440A
_journal_year                    2022
_chemical_formula_moiety
'C28.364 H8.727 Ce4.364 N0.727 O20.727, 0.727[C5H10N2O]'
_chemical_formula_sum            'C28.36 H8.73 Ce4.36 N0.73 O20.73'
_chemical_formula_weight         1302.70
_chemical_name_common            NU-1701
_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_Hall           '-F 4vw 2vw 3'
_space_group_name_H-M_alt        'F d -3 m :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-11-05
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2021-11-15 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            22
_cell_length_a                   34.9097(6)
_cell_length_b                   34.9097(6)
_cell_length_c                   34.9097(6)
_cell_measurement_reflns_used    11531
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.6790
_cell_measurement_theta_min      3.0160
_cell_volume                     42544.0(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.925
_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    -11.00  25.00   0.25  135.00    --   -0.38 -83.00 157.00  144
  2  \w    -32.00  -3.00   0.25  135.00    --   -0.38 -75.00  42.00  116
  3  \w    -17.00  32.00   0.25  135.00    --   -0.38 -99.00 -60.00  196
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            41838
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.326
_diffrn_reflns_theta_min         1.935
_exptl_absorpt_coefficient_mu    2.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             13264
_exptl_crystal_recrystallization_method 'Solvothermal Synthesis'
_refine_diff_density_max         1.480
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         2559
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0583P)^2^+616.4481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2109
_reflns_number_total             2559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06440a2.cif
_cod_data_source_block           02022021ce-hhtp120c_auto
_cod_original_cell_volume        42544(2)
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_database_code               7129389
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-O003
 1.2 with sigma of 0.02
 C1-C2
 1.46 with sigma of 0.02
3. Others
 Fixed Sof: O008(0.25) O00A(0.25) O2(0.25) O0AA(0.125) C1(0.125) C2(0.125)
4.a Aromatic/amide H refined with riding coordinates:
 C007(H007)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1009 electrons were 
found in a volume of 23754\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.727[C5H10N2O] per Unit Cell 
which account for 992 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48207
_shelx_hkl_checksum              98350
_shelx_fab_checksum              16031
_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
;