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_7247776
_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, 5.417[CH3OH]'
_chemical_formula_sum            'C13.42 H31.67 Co N4 O5.42'
_chemical_formula_weight         394.79
_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                   17.1651(3)
_cell_length_b                   17.1651(3)
_cell_length_c                   17.1651(3)
_cell_measurement_reflns_used    1616
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.2000
_cell_measurement_theta_min      2.3570
_cell_volume                     5057.54(15)
_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 0.952
_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    -31.60  35.00   0.10    0.10   0.00   0.00   0.00    --   666
;
_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      -0.0263789000
_diffrn_orient_matrix_UB_12      -0.0048160000
_diffrn_orient_matrix_UB_13      -0.0313199000
_diffrn_orient_matrix_UB_21      -0.0057060000
_diffrn_orient_matrix_UB_22      -0.0394790000
_diffrn_orient_matrix_UB_23      0.0109308000
_diffrn_orient_matrix_UB_31      -0.0313134000
_diffrn_orient_matrix_UB_32      0.0113287000
_diffrn_orient_matrix_UB_33      0.0245592000
_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  0.0516
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2236
_diffrn_reflns_point_group_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        23.197
_diffrn_reflns_theta_max         23.197
_diffrn_reflns_theta_min         1.678
_diffrn_source                   Synchrotron
_diffrn_source_type              'AS beamline MX1'
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.5642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1055 before and 0.0819 after correction.
The Ratio of minimum to maximum transmission is 0.7582.
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    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             2527
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL zif67_p4_w1_70s_0057_a.res in I-43m
CELL   17.1651   17.1651   17.1651     90.00     90.00     90.00
SPGR I-43m
C101 1.000 1.003 0.469 !       3.29 eA-3
C102 0.219 0.219 0.219 !       2.85 eA-3
C103 0.724 0.725 0.459 !       2.79 eA-3
C104 0.029 0.220 0.220 !       2.63 eA-3
C105 0.501 0.491 0.266 !       1.88 eA-3
C106 0.378 0.378 0.378 !       1.84 eA-3
C107 0.278 1.000 0.000 !       1.72 eA-3
C108 0.921 0.078 0.079 !       1.71 eA-3
C109 0.032 0.080 0.080 !       1.54 eA-3
C110 0.094 0.094 0.094 !       1.47 eA-3
C111 0.329 0.673 0.327 !       1.37 eA-3
C112 0.274 0.951 0.048 !       1.23 eA-3
C113 0.259 0.064 0.039 !       1.19 eA-3
C114 0.537 0.548 0.406 !       1.14 eA-3
Q115 0.408 0.408 0.204 !       1.08 eA-3
C116 0.878 0.871 0.128 !       1.06 eA-3
C117 0.206 0.199 0.144 !       1.06 eA-3
Q118 0.060 0.705 0.120 !       1.04 eA-3
Q119 0.560 0.205 0.620 !       1.04 eA-3
Q120 0.127 0.299 0.942 !       1.02 eA-3
C121 0.538 0.541 0.467 !       1.00 eA-3
C122 0.030 0.030 0.030 !       0.99 eA-3
Q123 0.171 0.301 0.941 !       0.97 eA-3
Q124 0.736 0.735 0.002 !       0.94 eA-3
C125 0.278 0.545 0.455 !       0.93 eA-3
C126 0.579 0.582 0.360 !       0.93 eA-3
Q127 0.562 0.172 0.435 !       0.91 eA-3
C128 0.683 0.692 0.308 !       0.91 eA-3
C129 0.333 0.364 0.380 !       0.91 eA-3
C130 0.364 0.380 0.333 !       0.91 eA-3
C131 0.094 0.091 0.156 !       0.90 eA-3
C132 0.184 0.740 0.249 !       0.89 eA-3
C133 0.846 0.843 0.003 !       0.88 eA-3
Q134 0.247 0.084 0.185 !       0.87 eA-3
Q135 0.651 0.032 0.032 !       0.87 eA-3
C136 0.152 0.862 0.054 !       0.85 eA-3
Q137 0.031 0.455 0.455 !       0.84 eA-3
C138 0.294 0.452 0.453 !       0.81 eA-3
Q139 0.783 0.658 0.373 !       0.81 eA-3
Q140 0.195 0.451 0.280 !       0.80 eA-3
C141 0.862 0.095 0.190 !       0.78 eA-3
Q142 0.188 0.704 0.188 !       0.78 eA-3
Q143 0.860 0.730 0.270 !       0.75 eA-3
Q144 0.360 0.230 0.770 !       0.75 eA-3
C145 0.465 0.366 0.417 !       0.74 eA-3
C146 0.754 0.079 0.079 !       0.74 eA-3
Q147 0.756 0.375 0.482 !       0.73 eA-3
C148 0.656 0.346 0.437 !       0.72 eA-3
Q149 0.222 0.703 0.108 !       0.72 eA-3
Q150 0.296 0.704 0.048 !       0.67 eA-3
Q151 0.341 0.211 0.789 !       0.62 eA-3
C152 1.000 0.875 0.008 !       0.56 eA-3
Q153 0.307 0.689 0.193 !       0.56 eA-3
Q154 0.252 0.096 0.139 !       0.54 eA-3
Q155 0.223 0.637 0.301 !       0.53 eA-3
Q156 0.338 0.078 0.024 !       0.52 eA-3
C157 0.473 0.494 0.307 !       0.51 eA-3
C158 0.499 0.671 0.509 !       0.50 eA-3
;
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 220 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.22(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         627
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0634
_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^)+(0.1067P)^2^+8.5343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1801
_reflns_Friedel_coverage         0.650
_reflns_Friedel_fraction_full    0.785
_reflns_Friedel_fraction_max     0.782
_reflns_number_gt                581
_reflns_number_total             627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00979c2.cif
_cod_data_source_block           zif67_p4_w1_70s_0057
_cod_depositor_comments
'Adding full bibliography for 7247762--7247779.cif.'
_cod_original_cell_volume        5057.5(3)
_cod_database_code               7247776
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H25 Co N4 O4'
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.858
_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
 1.35 with sigma of 0.01
 C2-C1
 1.48 with sigma of 0.01
 C3-C2
 2.169 with sigma of 0.01
 N1-C2
 1.35 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 1168 electrons were 
found in a volume of 2626\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
65[CH3OH] per Unit Cell 
which account for 1080 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 1.575
_oxdiff_exptl_absorpt_empirical_full_min 0.616