Amorphous metal-organic frameworks obtained from a crystalline precursor for the capture of iodine with high capacities
Feng, Ying; Zou, Ming-Yan; Hu, Hao-Chen; Li, Wan-Han; Cai, Songliang; Zhang, Wei-Guang; Zheng, Sheng-Run; Chemical Communications  (2022) –; doi:10.1039/D1CC07229C

data_7129892
_publ_section_title
;
 Amorphous metal-organic frameworks obtained from a crystalline precursor
 for the capture of iodine with high capacities
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC07229C
_journal_year                    2022
_chemical_formula_moiety         'C90 H60 Co2 N27'
_chemical_formula_sum            'C90 H60 Co2 N27'
_chemical_formula_weight         1637.51
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-11 deposited with the CCDC.	2022-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   29.6590(4)
_cell_length_b                   29.6590(4)
_cell_length_c                   20.6874(12)
_cell_measurement_reflns_used    5019
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      64.0990
_cell_measurement_theta_min      4.6760
_cell_volume                     15759.8(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.977
_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    -36.00  34.00   1.00    3.00    --    0.00 -82.00 -60.00   70
  2  \w     19.00 124.00   1.00   10.00    --  101.30 -57.00  30.00  105
  3  \w    129.00 187.00   1.00   10.00    --  101.30  28.00-157.00   58
  4  \w     20.00 127.00   1.00   10.00    --  101.30 -57.00 150.00  107
  5  \w     64.00  89.00   1.00    3.00    --    0.00  57.00  90.00   25
  6  \w     88.00 174.00   1.00   10.00    --  101.30  38.00  60.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0226974000
_diffrn_orient_matrix_UB_12      0.0111191000
_diffrn_orient_matrix_UB_13      0.0689116000
_diffrn_orient_matrix_UB_21      0.0382490000
_diffrn_orient_matrix_UB_22      -0.0184796000
_diffrn_orient_matrix_UB_23      -0.0197381000
_diffrn_orient_matrix_UB_31      0.0402536000
_diffrn_orient_matrix_UB_32      0.0559730000
_diffrn_orient_matrix_UB_33      -0.0200810000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18133
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.213
_diffrn_reflns_theta_min         4.608
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.518
_exptl_crystal_description       block
_exptl_crystal_F_000             2529
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1762 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         6967
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0697
_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^)+(0.1515P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2186
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                4977
_reflns_number_total             6967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc07229c2.cif
_cod_data_source_block           1_sq
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               7129892
_shelx_shelxl_version_number     2018/1
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C14(H14),
 C15(H15)
;
_shelx_res_checksum              29340
_shelx_hkl_checksum              87990
_shelx_fab_checksum              19529
_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 2.059
_oxdiff_exptl_absorpt_empirical_full_min 0.597