Metal-organic frameworks with two different-sized aromatic ring-confined nanotraps for benchmark natural gas upgrade.
Li, Shu-Yi; Xue, Ying-Ying; Wang, Jia-Wen; Li, Hai-Peng; Lei, Jiao; Lv, Hong-Juan; Bu, Xianhui; Zhang, Peng; Wang, Ying; Yuan, Wen-Yu; Zhai, Quan-Guo; Chemical science 15 (2024) 17547–17555; doi:10.1039/d4sc04387a

data_1572795
_publ_section_title
;
 Metal-organic frameworks with two different-sized aromatic ring-confined
 nanotraps for benchmark natural gas upgrade.
;
_journal_issue                   42
_journal_name_full               'Chemical science'
_journal_page_first              17547
_journal_page_last               17555
_journal_paper_doi               10.1039/d4sc04387a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'C17.5 Co N2.5 O4.167, [+ solvents]0.167[C3H7NO]'
_chemical_formula_sum            'C105 H63 Co6 N15 O25'
_chemical_formula_weight         2288.28
_space_group_crystal_system      hexagonal
_space_group_IT_number           188
_space_group_name_Hall           'P -6c 2'
_space_group_name_H-M_alt        'P -6 c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-06-09
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2023-06-09 deposited with the CCDC.	2024-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   19.7252(10)
_cell_length_b                   19.7252(10)
_cell_length_c                   23.5747(11)
_cell_measurement_reflns_used    7820
_cell_measurement_temperature    218(13)
_cell_measurement_theta_max      23.3530
_cell_measurement_theta_min      1.7860
_cell_volume                     7943.6(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (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  'olex2.refine 1.3-ac4 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3-ac4 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      218(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     26.00  71.50   0.50   55.00    --   20.00  54.00   0.00   91
  2  \w     78.00 108.00   0.50   55.00    --   20.00  54.00   0.00   60
  3  \w    -73.00  45.00   0.50   55.00    --   20.00  54.00 150.00  236
  4  \w    -73.00  -5.50   0.50   55.00    --   20.00  54.00  60.00  135
  5  \w     62.00  90.00   0.50   55.00    --   20.00  54.00  60.00   56
  6  \w    -73.00 -35.50   0.50   55.00    --   20.00  54.00   0.00   75
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0221805000
_diffrn_orient_matrix_UB_12      0.0192676000
_diffrn_orient_matrix_UB_13      0.0006174000
_diffrn_orient_matrix_UB_21      -0.0319200000
_diffrn_orient_matrix_UB_22      -0.0330707000
_diffrn_orient_matrix_UB_23      -0.0128936000
_diffrn_orient_matrix_UB_31      -0.0146148000
_diffrn_orient_matrix_UB_32      -0.0161906000
_diffrn_orient_matrix_UB_33      0.0271700000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30486
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.065
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    0.957
_exptl_crystal_description       sphere
_exptl_crystal_F_000             2320
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.643
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.29(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4979
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1738P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2238
_refine_ls_wR_factor_ref         0.2389
_reflns_Friedel_coverage         0.899
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4062
_reflns_number_total             4979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04387a2.cif
_cod_data_source_block           SNNU-185
_cod_depositor_comments
'Adding full bibliography for 1572795--1572796.cif.'
_cod_original_cell_volume        7943.6(9)
_cod_database_code               1572795
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'Co C N O H'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.71(5)
 0.29(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C5(H5), C1(H1), C2(H2), C10(H10), C9(H9), C11(H11), C12(H12),
 C15(H15), C7(H7), C17(H17)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 96 electrons were 
found in a volume of 3902\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
0.45[C2H6O], 1[C3H7NO] per Unit Cell 
which account for 103 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.757
_oxdiff_exptl_absorpt_empirical_full_min 0.811