High-pressure induced guest-mediated gate opening behaviour of the Co-based framework ZIF-67
Jones, Isabelle M.; Turner, Gemma F.; Pitts, Kari; Powell, Rees; Riboldi-Tunnicliffe, Alan; Williamson, Rachel; Boer, Stephanie; Allen, Lauren; Moggach, Stephen A.; CrystEngComm 25 (2023) 6533–6538; doi:10.1039/D3CE00979C

data_7247769
_publ_section_title
;
 High-pressure induced guest-mediated gate opening behaviour of the
 Co-based framework ZIF-67
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              6533
_journal_page_last               6538
_journal_paper_doi               10.1039/D3CE00979C
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 H10 Co N4, 2.917[CH3OH]'
_chemical_formula_sum            'C10.92 H21.67 Co N4 O2.92'
_chemical_formula_weight         314.15
_chemical_name_common            ZIF-67
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-04 deposited with the CCDC.	2023-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   17.2086(4)
_cell_length_b                   17.2086(4)
_cell_length_c                   17.2086(4)
_cell_measurement_reflns_used    676
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.1940
_cell_measurement_theta_min      1.6780
_cell_volume                     5096.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_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      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -35.00  35.00   0.10    0.10   0.00   0.00   0.00    --   700
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0304634000
_diffrn_orient_matrix_UB_12      -0.0272955000
_diffrn_orient_matrix_UB_13      -0.0050157000
_diffrn_orient_matrix_UB_21      0.0114707000
_diffrn_orient_matrix_UB_22      -0.0055476000
_diffrn_orient_matrix_UB_23      -0.0392540000
_diffrn_orient_matrix_UB_31      0.0253010000
_diffrn_orient_matrix_UB_32      -0.0304516000
_diffrn_orient_matrix_UB_33      0.0116900000
_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  0.0239
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2148
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        21.176
_diffrn_reflns_theta_max         21.176
_diffrn_reflns_theta_min         1.674
_diffrn_source                   Synchrotron
_diffrn_source_type              'AS beamline MX1'
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0591 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.9342.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'bluish violet'
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             1983
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL zif67_p1_w1_70s_00_a.res in I-43m
CELL   17.2086   17.2086   17.2086     90.00     90.00     90.00
SPGR I-43m
C101 0.202 0.796 0.205 !       1.52 eA-3
C102 1.000 1.000 0.000 !       1.50 eA-3
C103 0.793 0.961 0.222 !       1.05 eA-3
C104 0.491 0.313 0.313 !       0.87 eA-3
C105 0.709 0.657 0.342 !       0.85 eA-3
C106 1.000 1.001 0.234 !       0.78 eA-3
C107 0.837 1.007 0.154 !       0.77 eA-3
C108 0.261 0.730 0.270 !       0.65 eA-3
C109 0.356 0.356 0.356 !       0.62 eA-3
C110 0.221 0.045-0.003 !       0.62 eA-3
C111 0.010 0.016 0.182 !       0.56 eA-3
C112 0.843 0.845 0.155 !       0.54 eA-3
C113 0.139 0.139 0.139 !       0.52 eA-3
;
_refine_diff_density_max         0.129
_refine_diff_density_min         -0.097
_refine_diff_density_rms         0.020
_refine_ls_abs_structure_details
;
 Flack x determined using 203 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.113(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         515
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0185
_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^)+(0.0294P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0516
_reflns_Friedel_coverage         0.711
_reflns_Friedel_fraction_full    0.872
_reflns_Friedel_fraction_max     0.870
_reflns_number_gt                507
_reflns_number_total             515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00979c2.cif
_cod_data_source_block           zif67_p1_w1_70s_00
_cod_depositor_comments
'Adding full bibliography for 7247762--7247779.cif.'
_cod_original_cell_volume        5096.1(4)
_cod_database_code               7247769
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H20 Co N4 O4'
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.862
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_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. Restrained distances
 C3-N1
 1.34 with sigma of 0.01
 C2-C1
 1.48 with sigma of 0.01
 C3-C2
 2.16 with sigma of 0.01
 N1-C2
 1.34 with sigma of 0.01
3. Restrained planarity
 C3, N1, C2, C1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(N1) = Uanis(C3)
5. Rigid body (RIGU) restrains
 C2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
7.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_platon_squeeze_special_details
;
A solvent mask was calculated and 618 electrons were 
found in a volume of 2607\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2.917[CH3OH] per Unit Cell 
which account for 630 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_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 2.272
_oxdiff_exptl_absorpt_empirical_full_min 0.612