Crystals springing into action: metal‒organic framework CUK-1 as a pressure-driven molecular spring
Iacomi, Paul; Lee, Ji Sun; Vanduyfhuys, Louis; Cho, Kyung Ho; Fertey, Pierre; Wieme, Jelle; Granier, Dominique; Maurin, Guillaume; Van Speybroeck, Veronique; Chang, Jong-San; Yot, Pascal G.; Chemical Science 12 (2021) 5682–5687; doi:10.1039/D1SC00205H

data_1561006
_publ_section_title
;
 Crystals springing into action: metal--organic framework CUK-1 as a
 pressure-driven molecular spring
;
_journal_issue                   15
_journal_name_full               'Chemical Science'
_journal_page_first              5682
_journal_page_last               5687
_journal_paper_doi               10.1039/D1SC00205H
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C14 H8 Co3 N2 O10'
_chemical_formula_sum            'C14 H8 Co3 N2 O10'
_chemical_formula_weight         541.01
_chemical_name_common            CUK-1(Co)
_chemical_name_systematic        'CUK-1(Co) MOF'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-10-19 deposited with the CCDC.	2021-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.434(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6026(9)
_cell_length_b                   9.2014(9)
_cell_length_c                   11.0368(3)
_cell_measurement_reflns_used    3583
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.2170
_cell_measurement_theta_min      2.2150
_cell_volume                     1963.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_pressure         500000
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'RayoniX SX-165'
_diffrn_measured_fraction_theta_full 0.660
_diffrn_measured_fraction_theta_max 0.660
_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    -39.00  38.00   1.00    1.00    --    0.00   0.00   0.00   77
  2  \w    -39.00  38.00   1.00    1.00    --    0.00  30.00   0.00   77
  3  \w    -39.00  38.00   1.00    1.00    --    0.00  60.00   0.00   77
  4  \w    -39.00  38.00   1.00    1.00    --    0.00  90.00   0.00   77
;
_diffrn_measurement_device       '2 circle'
_diffrn_measurement_device_type  'RayoniX SX-165'
_diffrn_measurement_method       'omega rotation'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0134440000
_diffrn_orient_matrix_UB_12      -0.0468814000
_diffrn_orient_matrix_UB_13      0.0051677000
_diffrn_orient_matrix_UB_21      -0.0002874000
_diffrn_orient_matrix_UB_22      -0.0122216000
_diffrn_orient_matrix_UB_23      -0.0455060000
_diffrn_orient_matrix_UB_31      0.0229122000
_diffrn_orient_matrix_UB_32      -0.0276873000
_diffrn_orient_matrix_UB_33      0.0114126000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.5137
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.660
_diffrn_reflns_Laue_measured_fraction_max 0.660
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4552
_diffrn_reflns_point_group_measured_fraction_full 0.660
_diffrn_reflns_point_group_measured_fraction_max 0.660
_diffrn_reflns_theta_full        16.209
_diffrn_reflns_theta_max         16.209
_diffrn_reflns_theta_min         2.704
_diffrn_source                   synchrotron
_diffrn_source_type              'SOLEIL CRISTAL beamline'
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83266
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1068
_exptl_crystal_preparation       'outgassed at 250C in secondary vacuum'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         868
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0693P)^2^+53.9332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                797
_reflns_number_total             868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00205h2.cif
_cod_data_source_block           CUK-1Co_500mpa
_cod_depositor_comments
'Adding full bibliography for 1561006--1561008.cif.'
_cod_original_sg_symbol_Hall     '-C 2yn'
_cod_database_code               1561006
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co3 C14 N2 O10'
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.819
_reflns_odcompleteness_completeness 65.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C00F-C00C \\sim C00C-C00B \\sim C00E-C00B \\sim C00F-C00D
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates and stretchable bonds:
 O003(H003)
3.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00D(H00D), C00F(H00F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2