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_7247778
_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_formula_moiety         'C8 H10 Co N4, 1.833[C2H5OH]'
_chemical_formula_sum            'C11.67 H21 Co N4 O1.83'
_chemical_formula_weight         305.57
_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             2023-10-03
_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                   16.9230(5)
_cell_length_b                   16.9230(5)
_cell_length_c                   16.9230(5)
_cell_measurement_reflns_used    1379
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.4330
_cell_measurement_theta_min      3.6440
_cell_volume                     4846.5(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 2018/2 (Sheldrick, 2018)'
_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_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.978
_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    -28.00  22.00   0.50    1.81    --   45.98 -13.00 -62.00  100
  2  \w     79.00 175.00   0.50   26.93    --  102.69  87.00 106.00  192
  3  \w     74.00 119.00   0.50    1.81    --   45.98 125.00-180.00   90
  4  \w     30.00  69.00   0.50   26.93    --  102.69 -61.00  30.00   78
  5  \w     25.00  60.00   0.50    1.81    --   45.98  74.00   2.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0541423000
_diffrn_orient_matrix_UB_12      0.0643617000
_diffrn_orient_matrix_UB_13      0.0344414000
_diffrn_orient_matrix_UB_21      0.0610527000
_diffrn_orient_matrix_UB_22      -0.0159498000
_diffrn_orient_matrix_UB_23      -0.0657676000
_diffrn_orient_matrix_UB_31      -0.0405417000
_diffrn_orient_matrix_UB_32      0.0622410000
_diffrn_orient_matrix_UB_33      -0.0526951000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4186
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.582
_diffrn_reflns_theta_min         3.694
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.347
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 243 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         880
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0584
_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^)+(0.1285P)^2^+0.6552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.1899
_reflns_Friedel_coverage         0.673
_reflns_Friedel_fraction_full    0.879
_reflns_Friedel_fraction_max     0.812
_reflns_number_gt                741
_reflns_number_total             880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00979c2.cif
_cod_data_source_block           zif_67_2
_cod_depositor_comments
'Adding full bibliography for 7247762--7247779.cif.'
_cod_original_cell_volume        4846.5(4)
_cod_database_code               7247778
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co C8 H10 N4'
_chemical_oxdiff_usercomment     'ZIF-67 test 2'
_shelx_estimated_absorpt_t_max   0.520
_shelx_estimated_absorpt_t_min   0.388
_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 planarity
 C1, N1, C2, C3
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(N1) = Uanis(C2)
4. Rigid body (RIGU) restrains
 C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H3A(0.5) H3B(0.5) H3C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
6.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 577 electrons were 
found in a volume of 2453\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 22[C2H5OH] per Unit Cell 
which account for 572 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.328
_oxdiff_exptl_absorpt_empirical_full_min 0.745