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_7247762
_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, 0.646(N8), 0.167[CH2CH3OH]'
_chemical_formula_sum            'C8.34 H11 Co N9.17 O0.17'
_chemical_formula_weight         301.33
_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     direct
_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                   17.1155(7)
_cell_length_b                   17.1155(7)
_cell_length_c                   17.1155(7)
_cell_measurement_reflns_used    1646
_cell_measurement_temperature    293
_cell_measurement_theta_max      18.3250
_cell_measurement_theta_min      3.3460
_cell_volume                     5013.8(4)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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    -30.00   4.00   0.50   75.00    --   24.20  52.00-177.00   68
  2  \w    -21.00  42.00   0.50   75.00    --  -24.44  58.00 -58.00  126
  3  \w     30.00  63.00   0.50   75.00    --   24.20 -99.00-120.00   66
  4  \w    -23.00  16.00   0.50   75.00    --   24.20  67.00 157.00   78
  5  \w     -4.00  18.00   0.50   75.00    --  -24.44 -57.00  30.00   44
  6  \w    -18.00   4.00   0.50   75.00    --   24.20  57.00   0.00   44
  7  \w    -30.00  10.00   0.50   75.00    --   24.20  82.00 -29.00   80
  8  \w     30.00  55.00   0.50   75.00    --   24.20 -99.00  30.00   50
  9  \w    -36.00 -16.00   0.50   75.00    --  -24.44  38.00 150.00   40
;
_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      -0.0146957000
_diffrn_orient_matrix_UB_12      0.0072747000
_diffrn_orient_matrix_UB_13      -0.0380227000
_diffrn_orient_matrix_UB_21      0.0041925000
_diffrn_orient_matrix_UB_22      0.0407949000
_diffrn_orient_matrix_UB_23      0.0061865000
_diffrn_orient_matrix_UB_31      0.0385062000
_diffrn_orient_matrix_UB_32      -0.0016488000
_diffrn_orient_matrix_UB_33      -0.0152380000
_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  0.0768
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3887
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        18.354
_diffrn_reflns_theta_max         18.354
_diffrn_reflns_theta_min         3.367
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_correction_T_min  0.4804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1072 before and 0.0718 after correction.
The Ratio of minimum to maximum transmission is 0.6455.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       block
_exptl_crystal_F_000             1843
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 138 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         367
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      147.691
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0660
_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^)+(0.1359P)^2^+7.6237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.1875
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                343
_reflns_number_total             367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00979c2.cif
_cod_data_source_block           zif67_500mpa
_cod_depositor_comments
'Adding full bibliography for 7247762--7247779.cif.'
_cod_original_cell_volume        5013.8(6)
_cod_database_code               7247762
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co C8 H8 N4'
_chemical_oxdiff_usercomment     'ZIF67 @ 0.5 GPa in LN2 scs'
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.869
_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
 N1-C1
 1.387 with sigma of 0.01
 C2-N1_$1
 1.337 with sigma of 0.01
 C1-C2
 2.175 with sigma of 0.02
 C2-C3
 1.55 with sigma of 0.02
3. Restrained planarity
 C1, N1, C2, C3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2) = Uanis(N1) = Uanis(C1)
Uiso(N2) = Uiso(N3)
5. Rigid body (RIGU) restrains
 C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H3A(0.5) H3B(0.5) H3C(0.5) N5(0.125) N8(0.25) N3(0.125) N9(0.25)
 N6(0.083333) N4(0.25) N7(0.083333)
7.a Me refined with riding coordinates:
 C3(H3A,H3B,H3C)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 48 electrons were 
found in a volume of 436\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[CH2CH3OH] per Unit Cell 
which account for 52 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 8.420
_oxdiff_exptl_absorpt_empirical_full_min 0.654