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_7247779
_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, 18.667(N0.5)'
_chemical_formula_sum            'C8 H10 Co N13.33'
_chemical_formula_weight         351.89
_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             2023-10-04
_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                   16.5684(3)
_cell_length_b                   16.5684(3)
_cell_length_c                   16.5684(3)
_cell_measurement_reflns_used    7907
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.7480
_cell_measurement_theta_min      3.4610
_cell_volume                     4548.22(14)
_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 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -84.00 -30.00   0.50   33.13    --   13.12 -29.00 -95.00  108
  2  \w     62.00  96.00   0.50   33.13    --   13.12  29.00  65.00   68
  3  \w    -99.00 -30.00   0.50   33.13    --  -13.27 -29.00 -95.00  138
  4  \w    -16.00  43.00   0.50   33.13    --   13.12 -38.00-180.00  118
  5  \w    -41.00  22.00   0.50   33.13    --   13.12  53.00 162.00  126
  6  \w    -41.00  22.00   0.50   33.13    --   13.12  53.00 -17.00  126
  7  \w    -22.00  57.00   0.50   33.13    --   13.12 -53.00  17.00  158
  8  \w      5.00  84.00   0.50   33.13    --   13.12-114.00  45.00  158
  9  \w    -59.00  -5.00   0.50   33.13    --   13.12 114.00 135.00  108
 10  \w    -10.00  68.00   0.50   33.13    --   13.12 -82.00-151.00  156
 11  \w    -94.00 -68.00   0.50   33.13    --   13.12 178.00 -90.00   52
 12  \w    -26.00  53.00   0.50   33.13    --  -13.27 -40.00-167.00  158
 13  \w    -53.00  26.00   0.50   33.13    --  -13.27  40.00 -12.00  158
 14  \w    -63.00   4.00   0.50   33.13    --  -13.27  57.00-180.00  134
 15  \w     -3.00  50.00   0.50   33.13    --  -13.27 -97.00  35.00  106
 16  \w     54.00  96.00   0.50   33.13    --   13.12-178.00 -90.00   84
 17  \w    -36.00 -16.00   0.50   33.13    --   13.12  38.00   0.00   40
 18  \w     68.00  96.00   0.50   33.13    --   13.12-178.00  90.00   56
 19  \w    -27.00  -3.00   0.50   33.13    --  -13.27  19.00-150.00   48
 20  \w    -43.00 -18.00   0.50   33.13    --  -13.27  38.00-180.00   50
 21  \w    -68.00  10.00   0.50   33.13    --  -13.27  82.00 -29.00  156
 22  \w    -32.00  47.00   0.50   33.13    --  -13.27 -26.00   8.00  158
 23  \w    -38.00  -9.00   0.50   33.13    --  -13.27  77.00 150.00   58
;
_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      -0.0392875000
_diffrn_orient_matrix_UB_12      -0.0074377000
_diffrn_orient_matrix_UB_13      -0.0152804000
_diffrn_orient_matrix_UB_21      0.0063490000
_diffrn_orient_matrix_UB_22      -0.0421331000
_diffrn_orient_matrix_UB_23      0.0041757000
_diffrn_orient_matrix_UB_31      -0.0157705000
_diffrn_orient_matrix_UB_32      0.0015640000
_diffrn_orient_matrix_UB_33      0.0397717000
_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  0.0666
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16850
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        18.983
_diffrn_reflns_theta_max         18.983
_diffrn_reflns_theta_min         3.478
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  0.7309
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0861 before and 0.0728 after correction.
The Ratio of minimum to maximum transmission is 0.9243.
The \l/2 correction factor is Not present.
;
_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    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Flack x determined using 143 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.088(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         373
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0796
_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^)+(0.1708P)^2^+9.6005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2069
_refine_ls_wR_factor_ref         0.2121
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                346
_reflns_number_total             373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00979c2.cif
_cod_data_source_block           zif67_ln2_2900
_cod_depositor_comments
'Adding full bibliography for 7247762--7247779.cif.'
_cod_original_cell_volume        4548.2(2)
_cod_database_code               7247779
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co C8 H10 N4'
_chemical_oxdiff_usercomment     'ZIF67 @ 2.9 GPa in LN2'
_shelx_estimated_absorpt_t_max   0.903
_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-C2
 1.55 with sigma of 0.01
 N1-C2
 1.337 with sigma of 0.01
 C1-N1
 1.387 with sigma of 0.01
 C1-C2
 2.175 with sigma of 0.01
 N9-N8
 1.08 with sigma of 0.02
 N4-N5
 1.08 with sigma of 0.02
 N8-N9
 1.09 with sigma of 0.02
3. Restrained planarity
 C1, C2, N1, C3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2) = Uanis(N1)
Uiso(N15) = Uiso(N13)
Uiso(N4) = Uiso(N5)
Uiso(N3) = Uiso(N2)
Uiso(N6) = Uiso(N7)
Uiso(N9) = Uiso(N8)
5. Rigid body (RIGU) restrains
 C3, C2
 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) N3(0.166667) N6(0.05555)
 N4(0.25) N11(0.083333) N12(0.083333) N7(0.11112) N13(0.083333) N10(0.083333)
 N15(0.08335)
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 15.828
_oxdiff_exptl_absorpt_empirical_full_min 0.726