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_7247763
_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, 12.889(N0.5)'
_chemical_formula_sum            'C8 H10 Co N10.44'
_chemical_formula_weight         311.41
_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                   16.9979(6)
_cell_length_b                   16.9979(6)
_cell_length_c                   16.9979(6)
_cell_measurement_reflns_used    1983
_cell_measurement_temperature    293
_cell_measurement_theta_max      20.7810
_cell_measurement_theta_min      3.3720
_cell_volume                     4911.2(3)
_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
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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    -36.00  29.00   0.50   75.00    --  -24.44 -53.00  38.00  130
  2  \w    -27.00  -3.00   0.50   75.00    --   24.20  19.00-150.00   48
  3  \w    -23.00  16.00   0.50   75.00    --   24.20  67.00 -23.00   78
  4  \w    -36.00 -16.00   0.50   75.00    --  -24.44  38.00 150.00   40
  5  \w     -4.00  18.00   0.50   75.00    --  -24.44 -57.00  30.00   44
  6  \w    -36.00 -16.00   0.50   75.00    --  -24.44  38.00 -30.00   40
  7  \w    -36.00 -16.00   0.50   75.00    --   24.20  38.00  30.00   40
  8  \w     30.00  55.00   0.50   75.00    --   24.20 -99.00  30.00   50
  9  \w     30.00  71.00   0.50   75.00    --   24.20 -99.00-150.00   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      -0.0147531000
_diffrn_orient_matrix_UB_12      0.0070913000
_diffrn_orient_matrix_UB_13      -0.0383535000
_diffrn_orient_matrix_UB_21      0.0040678000
_diffrn_orient_matrix_UB_22      0.0411162000
_diffrn_orient_matrix_UB_23      0.0059826000
_diffrn_orient_matrix_UB_31      0.0388200000
_diffrn_orient_matrix_UB_32      -0.0016011000
_diffrn_orient_matrix_UB_33      -0.0152482000
_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  0.0906
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5119
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        20.781
_diffrn_reflns_theta_max         20.781
_diffrn_reflns_theta_min         3.390
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.4799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1078 before and 0.0816 after correction.
The Ratio of minimum to maximum transmission is 0.6446.
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    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             1897
_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         0.830
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details
;
 Flack x determined using 182 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         505
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0801
_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^)+(0.1966P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2325
_refine_ls_wR_factor_ref         0.2398
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                463
_reflns_number_total             505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00979c2.cif
_cod_data_source_block           zif67_ln2_1300
_cod_depositor_comments
'Adding full bibliography for 7247762--7247779.cif.'
_cod_original_cell_volume        4911.2(5)
_cod_database_code               7247763
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co C8 H10 N4'
_chemical_oxdiff_usercomment     'ZIF67 @ 1.3 GPa'
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.866
_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
 C2-C3
 1.55 with sigma of 0.02
 N1-C2
 1.337 with sigma of 0.01
 N1-C1
 1.387 with sigma of 0.01
 C1-C2
 2.175 with sigma of 0.01
3. Restrained planarity
 C1, N1, C2, C3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C1) = Uanis(C2)
Uiso(N11) = Uiso(N10)
Uiso(N4) = Uiso(N5)
Uiso(N3) = Uiso(N2)
Uiso(N9) = Uiso(N8)
Uiso(N6) = Uiso(N7)
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) N2(0.083333) N8(0.25) N3(0.166667)
 N9(0.25) N6(0.11111) N4(0.166667) N7(0.05556) N10(0.11112) N11(0.083333)
 N12(0.083333)
7.a Me refined with riding coordinates:
 C3(H3A,H3B,H3C)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_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 3.598
_oxdiff_exptl_absorpt_empirical_full_min 0.614