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_7247775
_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, 4.5[CH3OH]'
_chemical_formula_sum            'C12.5 H28 Co N4 O4.5'
_chemical_formula_weight         365.32
_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                   16.9823(4)
_cell_length_b                   16.9823(4)
_cell_length_c                   16.9823(4)
_cell_measurement_reflns_used    1106
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.1970
_cell_measurement_theta_min      2.3830
_cell_volume                     4897.7(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 0.958
_diffrn_measured_fraction_theta_max 0.951
_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      -0.0049956000
_diffrn_orient_matrix_UB_12      -0.0311397000
_diffrn_orient_matrix_UB_13      -0.0272343000
_diffrn_orient_matrix_UB_21      -0.0398394000
_diffrn_orient_matrix_UB_22      0.0113736000
_diffrn_orient_matrix_UB_23      -0.0056573000
_diffrn_orient_matrix_UB_31      0.0116657000
_diffrn_orient_matrix_UB_32      0.0253913000
_diffrn_orient_matrix_UB_33      -0.0311095000
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2317
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        23.186
_diffrn_reflns_theta_max         23.186
_diffrn_reflns_theta_min         1.696
_diffrn_source                   Synchrotron
_diffrn_source_type              'AS beamline MX1'
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0917 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.7041.
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    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL zif67_p5_w1_70s_0058_a.res in I-43m
CELL   16.9823   16.9823   16.9823     90.00     90.00     90.00
SPGR I-43m
C101 0.500 0.500 0.000 !       6.08 eA-3
C102 0.724 0.542 0.283 !       4.19 eA-3
C103 1.000 0.438 0.000 !       3.96 eA-3
C104 0.733 0.267 0.267 !       3.50 eA-3
C105 0.527 0.286 0.286 !       3.12 eA-3
C106 0.500 0.509 0.219 !       2.98 eA-3
C107 0.580 0.420 0.420 !       2.37 eA-3
C108 0.127 0.865 0.170 !       1.98 eA-3
Q109 0.328 0.784 0.216 !       1.04 eA-3
C110 0.427 0.427 0.427 !       0.99 eA-3
C111 0.190 0.815 0.185 !       0.73 eA-3
C112 0.038 0.038 0.038 !       0.71 eA-3
Q113 0.910 0.201 0.299 !       0.68 eA-3
C114 0.020 0.992 0.059 !       0.65 eA-3
Q115 0.644 0.363-0.004 !       0.60 eA-3
Q116 0.750 0.998 0.475 !       0.56 eA-3
Q117 0.250 0.498 0.975 !       0.56 eA-3
Q118 0.250 0.970 0.537 !       0.56 eA-3
C119 0.120 0.134 0.198 !       0.52 eA-3
;
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 258 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         631
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0701P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.724
_reflns_Friedel_fraction_full    0.871
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                623
_reflns_number_total             631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00979c2.cif
_cod_data_source_block           zif67_p5_w1_70s_0058
_cod_depositor_comments
'Adding full bibliography for 7247762--7247779.cif.'
_cod_original_cell_volume        4897.7(4)
_cod_original_formula_sum        'C12.50 H28 Co N4 O4.50'
_cod_database_code               7247775
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H20 Co N4 O4'
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.855
_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
 C1, C2
 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 974 electrons were 
found in a volume of 2489\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
54[CH3OH] per Unit Cell 
which account for 900 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 1.829
_oxdiff_exptl_absorpt_empirical_full_min 0.721