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_7247764
_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, 1[CH2CH3OH]'
_chemical_formula_sum            'C10 H16 Co N4 O'
_chemical_formula_weight         267.20
_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                   17.0426(4)
_cell_length_b                   17.0426(4)
_cell_length_c                   17.0426(4)
_cell_measurement_reflns_used    2137
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.2840
_cell_measurement_theta_min      2.9140
_cell_volume                     4950.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 41.115a 64-bit (release 06-08-2021))'
_computing_data_reduction        'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023)'
_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 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.932
_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    -29.00  67.00   0.50  132.95    --  -15.69  23.00 112.00  192
  2  \w    -87.00 -41.00   0.50  132.95    --   15.53-178.00-180.00   92
  3  \w    -81.00 -40.00   0.50  132.95    --   15.53 -19.00 -90.00   82
;
_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      -0.0173725000
_diffrn_orient_matrix_UB_12      -0.0377825000
_diffrn_orient_matrix_UB_13      -0.0015767000
_diffrn_orient_matrix_UB_21      -0.0186261000
_diffrn_orient_matrix_UB_22      0.0070334000
_diffrn_orient_matrix_UB_23      0.0365611000
_diffrn_orient_matrix_UB_31      -0.0329014000
_diffrn_orient_matrix_UB_32      0.0159724000
_diffrn_orient_matrix_UB_33      -0.0198453000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6643
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.440
_diffrn_reflns_theta_min         2.390
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.70a (Rigaku Oxford Diffraction, 2023)
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            'clear bluish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.074
_platon_squeeze_details
;
TITL zif67_ambient_a.res in I-43m
CELL   17.0426   17.0426   17.0426     90.00     90.00     90.00
SPGR I-43m
C101 0.316 0.316 0.316 !       1.36 eA-3
C102 0.672 0.656 0.675 !       1.09 eA-3
C103 0.172 0.156 0.175 !       1.09 eA-3
C104 0.356 0.306 0.693 !       1.03 eA-3
C105 0.215 0.218 0.168 !       0.99 eA-3
C106 0.070 0.174 0.174 !       0.98 eA-3
C107 0.861 0.801 0.114 !       0.87 eA-3
C108 0.036 0.036 0.036 !       0.84 eA-3
C109 0.116 0.866 0.133 !       0.82 eA-3
C110 0.410 0.410 0.410 !       0.82 eA-3
C111 0.716 0.650 0.353 !       0.79 eA-3
C112 0.090 0.015 0.207 !       0.78 eA-3
C113 0.297 0.376 0.292 !       0.75 eA-3
C114 0.295 0.708 0.470 !       0.73 eA-3
C115 0.702 0.482 0.482 !       0.73 eA-3
C116 0.957 0.168 0.168 !       0.69 eA-3
C117 0.084 0.209 0.077 !       0.68 eA-3
C118 0.584 0.709 0.577 !       0.68 eA-3
C119 0.584 0.577 0.709 !       0.68 eA-3
C120 0.279 0.463 0.327 !       0.67 eA-3
C121 0.916 0.197 0.921 !       0.67 eA-3
C122 0.916 0.921 0.197 !       0.67 eA-3
C123 0.360 0.687 0.453 !       0.67 eA-3
C124 0.359 0.635 0.407 !       0.67 eA-3
C125 0.859 0.135 0.907 !       0.67 eA-3
C126 0.919 0.221 0.156 !       0.67 eA-3
C127 0.711 0.699 0.302 !       0.66 eA-3
C128 0.359 0.407 0.635 !       0.66 eA-3
C129 0.172 0.890 0.162 !       0.65 eA-3
C130 0.179 0.827-0.007 !       0.64 eA-3
C131 0.402 0.294 0.397 !       0.63 eA-3
C132 0.347 0.347 0.347 !       0.62 eA-3
C133 0.783 1.002 0.780 !       0.60 eA-3
C134 0.283 0.502 0.280 !       0.60 eA-3
C135 0.217 0.784 1.002 !       0.60 eA-3
C136 0.063 0.126 0.219 !       0.57 eA-3
C137 0.562 0.685 0.466 !       0.57 eA-3
C138 0.913 0.128 0.172 !       0.57 eA-3
C139 0.565 0.737 0.426 !       0.57 eA-3
C140 0.378 0.456 0.377 !       0.56 eA-3
C141 0.514 0.625 0.341 !       0.55 eA-3
C142 0.452 0.460 0.374 !       0.54 eA-3
C143 0.242 0.045 0.045 !       0.54 eA-3
C144 0.548 0.509 0.290 !       0.53 eA-3
;
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 240 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.035(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         893
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0575P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                679
_reflns_number_total             893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00979c2.cif
_cod_data_source_block           zif67_ambient
_cod_depositor_comments
'Adding full bibliography for 7247762--7247779.cif.'
_cod_original_cell_volume        4950.0(3)
_cod_database_code               7247764
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co C11 H20 N4 O3'
_chemical_oxdiff_usercomment     'zif67 G NO CONFIDENCE'
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.859
_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
 C005, C003, N002, C004
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(C004) = Uanis(N002) = Uanis(C003)
4. Rigid body (RIGU) restrains
 C005, C003
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H00C(0.5) H00A(0.5) H00B(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C004(H004)
6.b Idealised Me refined as rotating group:
 C005(H00C,H00A,H00B)
;
_platon_squeeze_special_details
;
A solvent mask was calculated and 304 electrons were 
found in a volume of 2464\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
12[C2H5OH] per Unit Cell 
which account for 312 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 1.129
_oxdiff_exptl_absorpt_empirical_full_min 0.895