# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CUK-1Co_500mpa
_database_code_depnum_ccdc_archive 'CCDC 2019979'
loop_
_audit_author_name
_audit_author_address
'Paul Iacomi'
;ICGM
France
;
_audit_update_record             
;
2020-10-19 deposited with the CCDC.	2021-03-12 downloaded from the CCDC.
;
_audit_creation_date             2020-07-07
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        'CUK-1(Co) MOF'
_chemical_name_common            CUK-1(Co)
_chemical_formula_moiety         'C14 H8 Co3 N2 O10'
_chemical_formula_sum            'C14 H8 Co3 N2 O10'
_chemical_formula_weight         541.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Co3 C14 N2 O10'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0010 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.2838 0.5277 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0024 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0048 0.0029 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.6026(9)
_cell_length_b                   9.2014(9)
_cell_length_c                   11.0368(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.434(3)
_cell_angle_gamma                90
_cell_volume                     1963.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3583
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.2170
_cell_measurement_theta_min      2.2150
_shelx_estimated_absorpt_T_max   0.819
_shelx_estimated_absorpt_T_min   0.819
_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_absorpt_special_details   ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_ambient_temperature      293(2)
_diffrn_ambient_pressure         500000
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -39.00  38.00   1.00    1.00    --    0.00   0.00   0.00   77
  2  ω    -39.00  38.00   1.00    1.00    --    0.00  30.00   0.00   77
  3  ω    -39.00  38.00   1.00    1.00    --    0.00  60.00   0.00   77
  4  ω    -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_source                   synchrotron
_diffrn_source_type              'SOLEIL CRISTAL beamline'
_diffrn_special_details          'sample under pressure in mDAC'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                797
_reflns_number_total             868
_reflns_odcompleteness_completeness 65.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.21
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_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_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0549
_refine_ls_restrained_S_all      1.115
_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/[σ²(Fo²)+(0.0693P)²+53.9332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1657
_refine_special_details          SQUEEZE
_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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co01 Co 0.57715(6) 0.5464(2) 0.52915(11) 0.0320(7) Uani 1 1 d . . . . .
Co02 Co 1.000000 0.8599(3) 0.250000 0.0316(8) Uani 1 2 d S T P . .
O003 O 0.5208(3) 0.3776(10) 0.4426(6) 0.034(2) Uani 1 1 d . . . . .
H003 H 0.530(2) 0.304(15) 0.474(6) 0.051 Uiso 1 1 calc R U . . .
O004 O 0.6200(3) 0.6315(10) 0.3804(6) 0.039(2) Uani 1 1 d . . . . .
O005 O 0.5675(3) 0.5288(11) 0.2095(6) 0.040(3) Uani 1 1 d . . . . .
O006 O 0.8687(3) 0.7722(12) 0.3895(6) 0.046(3) Uani 1 1 d . . . . .
O007 O 0.9198(4) 0.7076(12) 0.2317(7) 0.048(3) Uani 1 1 d . . . . .
N008 N 0.6736(4) 0.5629(14) 0.0942(7) 0.041(3) Uani 1 1 d . . . . .
C00A C 0.8684(5) 0.7209(17) 0.2868(9) 0.038(4) Uani 1 1 d . . . . .
C00B C 0.7424(4) 0.6619(15) 0.2744(8) 0.032(3) Uani 1 1 d D . . . .
H00B H 0.745738 0.693443 0.355188 0.038 Uiso 1 1 calc R U . . .
C00C C 0.8004(5) 0.6617(16) 0.2174(7) 0.036(3) Uani 1 1 d D . . . .
C00D C 0.7301(5) 0.5673(17) 0.0413(10) 0.044(4) Uani 1 1 d D . . . .
H00D H 0.725876 0.537043 -0.039938 0.052 Uiso 1 1 calc R U . . .
C00E C 0.6797(5) 0.6151(16) 0.2112(8) 0.038(4) Uani 1 1 d D . . . .
C00F C 0.7942(5) 0.6136(18) 0.0987(9) 0.051(4) Uani 1 1 d D . . . .
H00F H 0.832179 0.612080 0.057934 0.062 Uiso 1 1 calc R U . . .
C009 C 0.6180(5) 0.5882(16) 0.2728(9) 0.036(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co01 O003 2.049(8) . ?
Co01 O003 2.114(7) 5_666 ?
Co01 O004 2.114(7) . ?
Co01 O005 2.144(7) 6_566 ?
Co01 O006 2.099(9) 7_666 ?
Co01 N008 2.158(9) 6_566 ?
Co02 O003 2.104(6) 3 ?
Co02 O003 2.104(6) 4_655 ?
Co02 O005 2.136(9) 4_655 ?
Co02 O005 2.136(9) 3 ?
Co02 O007 2.090(9) 2_755 ?
Co02 O007 2.090(9) . ?
O003 H003 0.77(15) . ?
O004 C009 1.247(12) . ?
O005 C009 1.241(13) . ?
O006 C00A 1.226(13) . ?
O007 C00A 1.266(12) . ?
N008 C00D 1.333(13) . ?
N008 C00E 1.365(14) . ?
C00A C00C 1.525(15) . ?
C00B H00B 0.9300 . ?
C00B C00C 1.387(11) . ?
C00B C00E 1.378(11) . ?
C00C C00F 1.370(11) . ?
C00D H00D 0.9300 . ?
C00D C00F 1.380(12) . ?
C00E C009 1.501(14) . ?
C00F H00F 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O003 Co01 O003 83.5(4) . 5_666 ?
O003 Co01 O004 99.9(3) . . ?
O003 Co01 O005 75.5(3) 5_666 6_566 ?
O003 Co01 O005 93.8(3) . 6_566 ?
O003 Co01 O006 176.6(3) . 7_666 ?
O003 Co01 N008 150.8(3) 5_666 6_566 ?
O003 Co01 N008 100.3(4) . 6_566 ?
O004 Co01 O003 118.6(3) . 5_666 ?
O004 Co01 O005 161.3(3) . 6_566 ?
O004 Co01 N008 89.6(3) . 6_566 ?
O005 Co01 N008 75.3(3) 6_566 6_566 ?
O006 Co01 O003 94.7(3) 7_666 5_666 ?
O006 Co01 O004 78.5(3) 7_666 . ?
O006 Co01 O005 88.5(3) 7_666 6_566 ?
O006 Co01 N008 82.8(4) 7_666 6_566 ?
O003 Co02 O003 171.1(5) 3 4_655 ?
O003 Co02 O005 97.5(3) 4_655 4_655 ?
O003 Co02 O005 75.9(3) 3 4_655 ?
O003 Co02 O005 97.5(3) 3 3 ?
O003 Co02 O005 75.9(3) 4_655 3 ?
O005 Co02 O005 86.6(5) 3 4_655 ?
O007 Co02 O003 99.6(3) . 3 ?
O007 Co02 O003 99.6(3) 2_755 4_655 ?
O007 Co02 O003 86.4(3) . 4_655 ?
O007 Co02 O003 86.4(3) 2_755 3 ?
O007 Co02 O005 91.5(4) . 4_655 ?
O007 Co02 O005 161.7(3) . 3 ?
O007 Co02 O005 91.5(4) 2_755 3 ?
O007 Co02 O005 161.7(3) 2_755 4_655 ?
O007 Co02 O007 95.8(6) . 2_755 ?
Co01 O003 Co01 96.5(4) . 5_666 ?
Co01 O003 Co02 122.0(4) . 3_445 ?
Co01 O003 H003 112.5 5_666 . ?
Co01 O003 H003 112.5 . . ?
Co02 O003 Co01 98.3(3) 3_445 5_666 ?
Co02 O003 H003 112.5 3_445 . ?
C009 O004 Co01 131.8(8) . . ?
Co02 O005 Co01 96.4(4) 3_445 6_565 ?
C009 O005 Co01 118.8(6) . 6_565 ?
C009 O005 Co02 131.8(7) . 3_445 ?
C00A O006 Co01 128.9(8) . 7_666 ?
C00A O007 Co02 122.3(8) . . ?
C00D N008 Co01 127.8(8) . 6_565 ?
C00D N008 C00E 116.9(9) . . ?
C00E N008 Co01 114.5(6) . 6_565 ?
O006 C00A O007 126.6(10) . . ?
O006 C00A C00C 118.3(8) . . ?
O007 C00A C00C 115.1(9) . . ?
C00C C00B H00B 120.0 . . ?
C00E C00B H00B 120.0 . . ?
C00E C00B C00C 120.0(9) . . ?
C00B C00C C00A 119.1(8) . . ?
C00F C00C C00A 121.9(8) . . ?
C00F C00C C00B 118.9(9) . . ?
N008 C00D H00D 117.7 . . ?
N008 C00D C00F 124.7(10) . . ?
C00F C00D H00D 117.7 . . ?
N008 C00E C00B 121.4(9) . . ?
N008 C00E C009 114.7(8) . . ?
C00B C00E C009 122.6(9) . . ?
C00C C00F C00D 118.0(9) . . ?
C00C C00F H00F 121.0 . . ?
C00D C00F H00F 121.0 . . ?
O004 C009 C00E 118.5(9) . . ?
O005 C009 O004 125.0(9) . . ?
O005 C009 C00E 116.4(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co01 O004 C009 O005 36.5(19) . . . . ?
Co01 O004 C009 C00E -146.7(9) . . . . ?
Co01 O005 C009 O004 -177.1(10) 6_565 . . . ?
Co01 O005 C009 C00E 5.9(15) 6_565 . . . ?
Co01 O006 C00A O007 40(2) 7_666 . . . ?
Co01 O006 C00A C00C -142.0(9) 7_666 . . . ?
Co01 N008 C00D C00F -166.2(12) 6_565 . . . ?
Co01 N008 C00E C00B 167.2(10) 6_565 . . . ?
Co01 N008 C00E C009 -0.5(14) 6_565 . . . ?
Co02 O005 C009 O004 -45.7(19) 3_445 . . . ?
Co02 O005 C009 C00E 137.4(10) 3_445 . . . ?
Co02 O007 C00A O006 -34.9(18) . . . . ?
Co02 O007 C00A C00C 147.1(9) . . . . ?
O006 C00A C00C C00B -3(2) . . . . ?
O006 C00A C00C C00F 174.6(14) . . . . ?
O007 C00A C00C C00B 175.3(12) . . . . ?
O007 C00A C00C C00F -7(2) . . . . ?
N008 C00D C00F C00C -2(2) . . . . ?
N008 C00E C009 O004 179.3(12) . . . . ?
N008 C00E C009 O005 -3.5(18) . . . . ?
C00A C00C C00F C00D -177.4(14) . . . . ?
C00B C00C C00F C00D 0(2) . . . . ?
C00B C00E C009 O004 12(2) . . . . ?
C00B C00E C009 O005 -171.0(13) . . . . ?
C00C C00B C00E N008 3(2) . . . . ?
C00C C00B C00E C009 169.2(13) . . . . ?
C00D N008 C00E C00B -3.9(19) . . . . ?
C00D N008 C00E C009 -171.6(12) . . . . ?
C00E N008 C00D C00F 3(2) . . . . ?
C00E C00B C00C C00A 177.0(13) . . . . ?
C00E C00B C00C C00F -1(2) . . . . ?



loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 -0.994 222.0 57.7 '9 N'
2 0.500 0.000 -0.861 222.0 57.7 '9 N'

_smtbx_masks_special_details     ?
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CUK-1Co_300mpa
_database_code_depnum_ccdc_archive 'CCDC 2019981'
loop_
_audit_author_name
_audit_author_address
'Paul Iacomi'
;ICGM
France
;
_audit_update_record             
;
2020-10-19 deposited with the CCDC.	2021-03-12 downloaded from the CCDC.
;
_audit_creation_date             2020-09-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        'CUK-1(Co) MOF'
_chemical_name_common            CUK-1(Co)
_chemical_formula_moiety         'C14 H8 Co3 N2 O10'
_chemical_formula_sum            'C14 H8 Co3 N2 O10'
_chemical_formula_weight         541.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Co3 C14 N2 O10'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0010 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.2838 0.5277 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0024 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0048 0.0029 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.974(3)
_cell_length_b                   11.0427(15)
_cell_length_c                   10.9677(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.796(9)
_cell_angle_gamma                90
_cell_volume                     2257.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    922
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.0250
_cell_measurement_theta_min      2.1510
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33966
_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_absorpt_special_details   ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.523
_diffrn_reflns_Laue_measured_fraction_max 0.523
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1396
_diffrn_reflns_point_group_measured_fraction_full 0.523
_diffrn_reflns_point_group_measured_fraction_max 0.523
_diffrn_reflns_theta_full        16.031
_diffrn_reflns_theta_max         16.031
_diffrn_reflns_theta_min         2.161
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         300000
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'RayoniX SX-165'
_diffrn_measured_fraction_theta_full 0.523
_diffrn_measured_fraction_theta_max 0.523
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -39.00  38.00   1.00    1.00    --    0.00  30.00   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      0.0202544000
_diffrn_orient_matrix_UB_12      -0.0278473000
_diffrn_orient_matrix_UB_13      -0.0084832000
_diffrn_orient_matrix_UB_21      0.0058454000
_diffrn_orient_matrix_UB_22      -0.0114330000
_diffrn_orient_matrix_UB_23      0.0461602000
_diffrn_orient_matrix_UB_31      -0.0178016000
_diffrn_orient_matrix_UB_32      -0.0354217000
_diffrn_orient_matrix_UB_33      -0.0082719000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.5137
_diffrn_source                   synchrotron
_diffrn_source_type              'SOLEIL CRISTAL beamline'
_diffrn_special_details          'sample under pressure in mDAC'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                666
_reflns_number_total             771
_reflns_odcompleteness_completeness 51.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.03
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         771
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0522
_refine_ls_restrained_S_all      1.055
_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/[σ²(Fo²)+(0.0926P)²+22.8540P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1490
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 H004-O004
 0.96 with sigma of 0.02
3. Rigid bond restraints
 N007, C00B, C00C, C00A, C00D, C00E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O006, C00F, O008, O003, C009, O005
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00E(H00E)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co01 Co 0.500000 0.11579(18) 0.750000 0.0253(7) Uani 1 2 d S T P . .
Co02 Co 0.91831(7) 0.46281(13) 0.46397(9) 0.0261(6) Uani 1 1 d . . . . .
O003 O 0.9303(4) 0.4801(7) 0.7857(5) 0.032(2) Uani 1 1 d . U . . .
O004 O 0.9803(4) 0.6041(6) 0.5556(5) 0.0289(15) Uiso 1 1 d D . . . .
O005 O 0.8751(4) 0.3923(7) 0.6098(5) 0.034(2) Uani 1 1 d . U . . .
O006 O 0.5806(5) 0.2473(7) 0.7723(6) 0.044(2) Uani 1 1 d . U . . .
N007 N 0.8217(6) 0.4339(8) 0.8997(6) 0.039(3) Uani 1 1 d . U . . .
O008 O 0.6393(5) 0.1899(8) 0.6221(5) 0.049(3) Uani 1 1 d . U . . .
C009 C 0.8767(6) 0.4210(10) 0.7214(7) 0.029(3) Uani 1 1 d . U . . .
C00A C 0.6974(6) 0.3117(11) 0.7815(7) 0.031(3) Uani 1 1 d . U . . .
C00B C 0.8174(7) 0.3886(11) 0.7814(8) 0.035(3) Uani 1 1 d . U . . .
C00C C 0.7577(6) 0.3277(10) 0.7205(8) 0.035(3) Uani 1 1 d . U . . .
H00C H 0.756295 0.297259 0.641000 0.042 Uiso 1 1 calc R U . . .
C00D C 0.7025(7) 0.3600(10) 0.8980(9) 0.038(3) Uani 1 1 d . U . . .
H00D H 0.664637 0.352930 0.940440 0.046 Uiso 1 1 calc R U . . .
C00E C 0.7665(8) 0.4210(13) 0.9531(9) 0.054(4) Uani 1 1 d . U . . .
H00E H 0.768993 0.453632 1.031999 0.065 Uiso 1 1 calc R U . . .
C00F C 0.6332(8) 0.2457(10) 0.7182(8) 0.037(3) Uani 1 1 d . U . . .
H004 H 0.961(7) 0.671(6) 0.504(8) 0.05(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co01 O003 2.084(8) 3_445 ?
Co01 O003 2.084(8) 4_646 ?
Co01 O004 2.099(6) 4_646 ?
Co01 O004 2.099(6) 3_445 ?
Co01 O006 2.090(9) 2_656 ?
Co01 O006 2.090(9) . ?
Co02 O003 2.107(7) 6_565 ?
Co02 O004 2.109(8) 5_766 ?
Co02 O004 2.093(6) . ?
Co02 O005 2.080(7) . ?
Co02 N007 2.162(10) 6_565 ?
Co02 O008 2.132(7) 7_656 ?
O003 C009 1.298(13) . ?
O004 H004 0.96(2) . ?
O005 C009 1.259(11) . ?
O006 C00F 1.252(16) . ?
N007 C00B 1.379(13) . ?
N007 C00E 1.300(18) . ?
O008 C00F 1.245(14) . ?
C009 C00B 1.452(18) . ?
C00A C00C 1.440(17) . ?
C00A C00D 1.371(16) . ?
C00A C00F 1.477(17) . ?
C00B C00C 1.378(16) . ?
C00C H00C 0.9300 . ?
C00D H00D 0.9300 . ?
C00D C00E 1.419(18) . ?
C00E H00E 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O003 Co01 O003 88.0(4) 3_445 4_646 ?
O003 Co01 O004 98.5(3) 4_646 4_646 ?
O003 Co01 O004 98.5(3) 3_445 3_445 ?
O003 Co01 O004 76.3(2) 4_646 3_445 ?
O003 Co01 O004 76.3(3) 3_445 4_646 ?
O003 Co01 O006 162.6(2) 3_445 . ?
O003 Co01 O006 92.6(3) 4_646 . ?
O003 Co01 O006 92.6(3) 3_445 2_656 ?
O003 Co01 O006 162.6(2) 4_646 2_656 ?
O004 Co01 O004 172.9(4) 3_445 4_646 ?
O006 Co01 O004 98.6(3) . 3_445 ?
O006 Co01 O004 86.4(3) 2_656 3_445 ?
O006 Co01 O004 86.4(3) . 4_646 ?
O006 Co01 O004 98.6(3) 2_656 4_646 ?
O006 Co01 O006 92.0(5) . 2_656 ?
O003 Co02 O004 75.6(3) 6_565 5_766 ?
O003 Co02 N007 76.8(3) 6_565 6_565 ?
O003 Co02 O008 87.8(3) 6_565 7_656 ?
O004 Co02 O003 94.2(3) . 6_565 ?
O004 Co02 O004 82.4(3) . 5_766 ?
O004 Co02 N007 152.3(3) 5_766 6_565 ?
O004 Co02 N007 97.4(3) . 6_565 ?
O004 Co02 O008 175.9(3) . 7_656 ?
O004 Co02 O008 94.6(3) 5_766 7_656 ?
O005 Co02 O003 162.2(3) . 6_565 ?
O005 Co02 O004 116.4(3) . 5_766 ?
O005 Co02 O004 100.2(3) . . ?
O005 Co02 N007 90.9(3) . 6_565 ?
O005 Co02 O008 78.5(3) . 7_656 ?
O008 Co02 N007 86.6(4) 7_656 6_565 ?
Co01 O003 Co02 98.1(3) 3 6_566 ?
C009 O003 Co01 135.9(6) . 3 ?
C009 O003 Co02 116.4(7) . 6_566 ?
Co01 O004 Co02 97.6(2) 3 5_766 ?
Co01 O004 H004 122(6) 3 . ?
Co02 O004 Co01 120.7(4) . 3 ?
Co02 O004 Co02 97.6(3) . 5_766 ?
Co02 O004 H004 118(8) 5_766 . ?
Co02 O004 H004 100(6) . . ?
C009 O005 Co02 135.3(7) . . ?
C00F O006 Co01 124.4(7) . . ?
C00B N007 Co02 113.3(8) . 6_566 ?
C00E N007 Co02 128.1(6) . 6_566 ?
C00E N007 C00B 118.3(9) . . ?
C00F O008 Co02 130.1(8) . 7_656 ?
O003 C009 C00B 118.2(8) . . ?
O005 C009 O003 121.9(11) . . ?
O005 C009 C00B 119.9(9) . . ?
C00C C00A C00F 119.9(8) . . ?
C00D C00A C00C 117.5(9) . . ?
C00D C00A C00F 122.6(11) . . ?
N007 C00B C009 115.0(9) . . ?
C00C C00B N007 122.1(11) . . ?
C00C C00B C009 122.5(8) . . ?
C00A C00C H00C 120.4 . . ?
C00B C00C C00A 119.1(8) . . ?
C00B C00C H00C 120.4 . . ?
C00A C00D H00D 120.4 . . ?
C00A C00D C00E 119.2(13) . . ?
C00E C00D H00D 120.4 . . ?
N007 C00E C00D 123.8(10) . . ?
N007 C00E H00E 118.1 . . ?
C00D C00E H00E 118.1 . . ?
O006 C00F C00A 115.5(9) . . ?
O008 C00F O006 128.1(11) . . ?
O008 C00F C00A 116.3(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co01 O003 C009 O005 35.6(16) 3 . . . ?
Co01 O003 C009 C00B -144.1(9) 3 . . . ?
Co01 O006 C00F O008 20.2(15) . . . . ?
Co01 O006 C00F C00A -155.2(7) . . . . ?
Co02 O003 C009 O005 173.3(8) 6_566 . . . ?
Co02 O003 C009 C00B -6.4(12) 6_566 . . . ?
Co02 O005 C009 O003 -27.9(17) . . . . ?
Co02 O005 C009 C00B 151.8(8) . . . . ?
Co02 N007 C00B C009 -1.6(12) 6_566 . . . ?
Co02 N007 C00B C00C -175.3(9) 6_566 . . . ?
Co02 N007 C00E C00D 174.0(9) 6_566 . . . ?
Co02 O008 C00F O006 -20.1(17) 7_656 . . . ?
Co02 O008 C00F C00A 155.3(8) 7_656 . . . ?
O003 C009 C00B N007 5.3(15) . . . . ?
O003 C009 C00B C00C 179.0(11) . . . . ?
O005 C009 C00B N007 -174.4(10) . . . . ?
O005 C009 C00B C00C -0.7(17) . . . . ?
N007 C00B C00C C00A 0.7(17) . . . . ?
C009 C00B C00C C00A -172.6(11) . . . . ?
C00A C00D C00E N007 -0.3(19) . . . . ?
C00B N007 C00E C00D 1.8(19) . . . . ?
C00C C00A C00D C00E -1.0(16) . . . . ?
C00C C00A C00F O006 -172.7(9) . . . . ?
C00C C00A C00F O008 11.3(15) . . . . ?
C00D C00A C00C C00B 0.8(16) . . . . ?
C00D C00A C00F O006 7.1(15) . . . . ?
C00D C00A C00F O008 -168.9(10) . . . . ?
C00E N007 C00B C009 171.8(11) . . . . ?
C00E N007 C00B C00C -2.0(17) . . . . ?
C00F C00A C00C C00B -179.5(11) . . . . ?
C00F C00A C00D C00E 179.3(12) . . . . ?




loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.006 388.8 121.4 ?
2 0.500 0.500 -0.557 388.8 121.4 ?

_smtbx_masks_special_details     ?
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CUK-1Co_680mpa
_database_code_depnum_ccdc_archive 'CCDC 2019980'
loop_
_audit_author_name
_audit_author_address
'Paul Iacomi'
;ICGM
France
;
_audit_update_record             
;
2020-10-19 deposited with the CCDC.	2021-03-12 downloaded from the CCDC.
;
_audit_creation_date             2020-07-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        'CUK-1(Co) MOF'
_chemical_name_common            CUK-1(Co)
_chemical_formula_moiety         'C14 H8 Co3 N2 O10'
_chemical_formula_sum            'C14 H8 Co3 N2 O10'
_chemical_formula_weight         541.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Co3 C14 N2 O10'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0010 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.2838 0.5277 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0024 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0048 0.0029 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.6011(9)
_cell_length_b                   9.2018(9)
_cell_length_c                   11.0360(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.435(3)
_cell_angle_gamma                90
_cell_volume                     1963.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3651
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.2310
_cell_measurement_theta_min      2.2150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67803
_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_absorpt_special_details   ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1060
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.691
_diffrn_reflns_Laue_measured_fraction_max 0.691
_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            4729
_diffrn_reflns_point_group_measured_fraction_full 0.691
_diffrn_reflns_point_group_measured_fraction_max 0.691
_diffrn_reflns_theta_full        16.246
_diffrn_reflns_theta_max         16.246
_diffrn_reflns_theta_min         2.705
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         680000
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'RayoniX SX-165'
_diffrn_measured_fraction_theta_full 0.691
_diffrn_measured_fraction_theta_max 0.691
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -39.00  38.00   1.00    1.00    --    0.00   0.00   0.00   77
  2  ω    -39.00  38.00   1.00    1.00    --    0.00  30.00   0.00   77
  3  ω    -39.00  38.00   1.00    1.00    --    0.00  60.00   0.00   77
  4  ω    -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      -0.0134493000
_diffrn_orient_matrix_UB_12      -0.0468810000
_diffrn_orient_matrix_UB_13      0.0051688000
_diffrn_orient_matrix_UB_21      -0.0002892000
_diffrn_orient_matrix_UB_22      -0.0122262000
_diffrn_orient_matrix_UB_23      -0.0455057000
_diffrn_orient_matrix_UB_31      0.0229111000
_diffrn_orient_matrix_UB_32      -0.0276918000
_diffrn_orient_matrix_UB_33      0.0114121000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.5137
_diffrn_source                   synchrotron
_diffrn_source_type              'SOLEIL CRISTAL beamline'
_diffrn_special_details          'sample under pressure in mDAC'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                835
_reflns_number_total             916
_reflns_odcompleteness_completeness 69.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     16.03
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         916
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0610
_refine_ls_restrained_S_all      1.193
_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/[σ²(Fo²)+(0.1041P)²+50.4518P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1971
_refine_ls_wR_factor_ref         0.2079
_refine_special_details          Twin,SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C00F-C00E \\sim C00F-C00C \\sim C00D-C00C \\sim C00D-C00A
 with sigma of 0.02
3. Rigid bond restraints
 C00F, C00E, N008, C00A, C00D, C00C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00E(H00E), C00F(H00F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co01 Co 1.000000 0.3601(3) 0.250000 0.0300(8) Uani 1 2 d S T P . .
Co02 Co 0.92284(6) 0.4535(2) 0.47092(11) 0.0301(7) Uani 1 1 d . . . . .
O003 O 0.9795(3) 0.6219(10) 0.5577(6) 0.030(2) Uani 1 1 d . . . . .
H003 H 0.972(2) 0.680(16) 0.533(7) 0.045 Uiso 1 1 calc R U . . .
O004 O 0.5672(3) 0.0280(11) 0.2094(6) 0.037(2) Uani 1 1 d . . . . .
O005 O 0.6200(4) 0.1312(11) 0.3804(6) 0.037(2) Uani 1 1 d . . . . .
O006 O 0.8684(3) 0.2732(11) 0.3895(6) 0.042(3) Uani 1 1 d . . . . .
O007 O 0.9200(4) 0.2067(12) 0.2316(7) 0.046(3) Uani 1 1 d . . . . .
N008 N 0.6733(4) 0.0629(13) 0.0949(8) 0.035(3) Uani 1 1 d . U . . .
C009 C 0.6175(5) 0.0897(16) 0.2714(9) 0.034(3) Uani 1 1 d . . . . .
C00A C 0.6794(5) 0.1151(16) 0.2114(8) 0.038(4) Uani 1 1 d D U . . .
C00B C 0.8682(5) 0.2223(17) 0.2862(10) 0.036(4) Uani 1 1 d . . . . .
C00C C 0.8003(5) 0.1614(15) 0.2175(8) 0.033(3) Uani 1 1 d D U . . .
C00D C 0.7423(4) 0.1621(15) 0.2742(9) 0.031(3) Uani 1 1 d D U . . .
H00D H 0.745737 0.194281 0.354891 0.037 Uiso 1 1 calc R U . . .
C00E C 0.7293(5) 0.0658(18) 0.0418(10) 0.042(4) Uani 1 1 d D U . . .
H00E H 0.724809 0.034119 -0.039156 0.050 Uiso 1 1 calc R U . . .
C00F C 0.7942(5) 0.1127(18) 0.0985(9) 0.049(4) Uani 1 1 d D U . . .
H00F H 0.832005 0.111063 0.057395 0.059 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co01 O007 2.095(9) . ?
Co01 O007 2.095(9) 2_755 ?
Co01 O003 2.101(6) 5_766 ?
Co01 O003 2.101(6) 6_565 ?
Co01 O004 2.126(9) 3 ?
Co01 O004 2.126(9) 4_655 ?
Co02 O003 2.050(8) . ?
Co02 O006 2.093(9) . ?
Co02 O003 2.109(7) 5_766 ?
Co02 O005 2.110(7) 7_656 ?
Co02 O004 2.143(8) 4_655 ?
Co02 N008 2.155(9) 4_655 ?
O003 H003 0.61(16) . ?
O004 C009 1.241(13) . ?
O005 C009 1.256(13) . ?
O006 C00B 1.232(13) . ?
O007 C00B 1.271(13) . ?
N008 C00E 1.326(14) . ?
N008 C00A 1.359(15) . ?
C009 C00A 1.494(14) . ?
C00A C00D 1.381(12) . ?
C00B C00C 1.526(14) . ?
C00C C00F 1.375(12) . ?
C00C C00D 1.385(11) . ?
C00D H00D 0.9300 . ?
C00E C00F 1.391(12) . ?
C00E H00E 0.9300 . ?
C00F H00F 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O007 Co01 O007 95.3(6) . 2_755 ?
O007 Co01 O003 99.7(3) . 5_766 ?
O007 Co01 O003 86.5(3) 2_755 5_766 ?
O007 Co01 O003 86.5(3) . 6_565 ?
O007 Co01 O003 99.7(3) 2_755 6_565 ?
O003 Co01 O003 170.9(5) 5_766 6_565 ?
O007 Co01 O004 161.7(3) . 3 ?
O007 Co01 O004 91.7(4) 2_755 3 ?
O003 Co01 O004 97.6(3) 5_766 3 ?
O003 Co01 O004 75.7(3) 6_565 3 ?
O007 Co01 O004 91.7(4) . 4_655 ?
O007 Co01 O004 161.7(3) 2_755 4_655 ?
O003 Co01 O004 75.7(3) 5_766 4_655 ?
O003 Co01 O004 97.6(3) 6_565 4_655 ?
O004 Co01 O004 86.8(5) 3 4_655 ?
O003 Co02 O006 176.7(3) . . ?
O003 Co02 O003 83.3(3) . 5_766 ?
O006 Co02 O003 95.0(3) . 5_766 ?
O003 Co02 O005 99.8(3) . 7_656 ?
O006 Co02 O005 78.5(3) . 7_656 ?
O003 Co02 O005 118.8(3) 5_766 7_656 ?
O003 Co02 O004 93.9(3) . 4_655 ?
O006 Co02 O004 88.4(3) . 4_655 ?
O003 Co02 O004 75.1(3) 5_766 4_655 ?
O005 Co02 O004 161.4(3) 7_656 4_655 ?
O003 Co02 N008 100.4(4) . 4_655 ?
O006 Co02 N008 82.5(4) . 4_655 ?
O003 Co02 N008 150.3(3) 5_766 4_655 ?
O005 Co02 N008 89.9(3) 7_656 4_655 ?
O004 Co02 N008 75.2(3) 4_655 4_655 ?
Co02 O003 Co01 122.1(4) . 5_766 ?
Co02 O003 Co02 96.7(3) . 5_766 ?
Co01 O003 Co02 98.6(3) 5_766 5_766 ?
Co02 O003 H003 112.3 . . ?
Co01 O003 H003 112.3 5_766 . ?
Co02 O003 H003 112.3 5_766 . ?
C009 O004 Co01 132.8(7) . 3_445 ?
C009 O004 Co02 118.3(6) . 4_645 ?
Co01 O004 Co02 96.7(4) 3_445 4_645 ?
C009 O005 Co02 132.4(8) . 7_656 ?
C00B O006 Co02 128.5(8) . . ?
C00B O007 Co01 121.4(8) . . ?
C00E N008 C00A 117.4(9) . . ?
C00E N008 Co02 127.0(8) . 4_645 ?
C00A N008 Co02 114.9(6) . 4_645 ?
O004 C009 O005 124.8(9) . . ?
O004 C009 C00A 117.1(9) . . ?
O005 C009 C00A 118.1(9) . . ?
N008 C00A C00D 121.3(9) . . ?
N008 C00A C009 114.3(9) . . ?
C00D C00A C009 123.4(9) . . ?
O006 C00B O007 126.9(10) . . ?
O006 C00B C00C 118.0(9) . . ?
O007 C00B C00C 115.0(9) . . ?
C00F C00C C00D 119.0(9) . . ?
C00F C00C C00B 121.8(8) . . ?
C00D C00C C00B 119.2(8) . . ?
C00A C00D C00C 120.2(9) . . ?
C00A C00D H00D 119.9 . . ?
C00C C00D H00D 119.9 . . ?
N008 C00E C00F 124.7(10) . . ?
N008 C00E H00E 117.6 . . ?
C00F C00E H00E 117.6 . . ?
C00C C00F C00E 117.4(10) . . ?
C00C C00F H00F 121.3 . . ?
C00E C00F H00F 121.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co01 O004 C009 O005 -43(2) 3_445 . . . ?
Co02 O004 C009 O005 -175.8(10) 4_645 . . . ?
Co01 O004 C009 C00A 136.6(10) 3_445 . . . ?
Co02 O004 C009 C00A 3.8(16) 4_645 . . . ?
Co02 O005 C009 O004 33.5(19) 7_656 . . . ?
Co02 O005 C009 C00A -146.1(10) 7_656 . . . ?
C00E N008 C00A C00D -3(2) . . . . ?
Co02 N008 C00A C00D 167.3(11) 4_645 . . . ?
C00E N008 C00A C009 -171.9(12) . . . . ?
Co02 N008 C00A C009 -1.3(15) 4_645 . . . ?
O004 C009 C00A N008 -1.6(18) . . . . ?
O005 C009 C00A N008 178.1(12) . . . . ?
O004 C009 C00A C00D -169.9(13) . . . . ?
O005 C009 C00A C00D 10(2) . . . . ?
Co02 O006 C00B O007 41(2) . . . . ?
Co02 O006 C00B C00C -143.2(9) . . . . ?
Co01 O007 C00B O006 -36.6(19) . . . . ?
Co01 O007 C00B C00C 147.7(9) . . . . ?
O006 C00B C00C C00F 175.0(14) . . . . ?
O007 C00B C00C C00F -9(2) . . . . ?
O006 C00B C00C C00D -2(2) . . . . ?
O007 C00B C00C C00D 174.5(12) . . . . ?
N008 C00A C00D C00C 2(2) . . . . ?
C009 C00A C00D C00C 169.8(13) . . . . ?
C00F C00C C00D C00A 0(2) . . . . ?
C00B C00C C00D C00A 176.4(13) . . . . ?
C00A N008 C00E C00F 3(2) . . . . ?
Co02 N008 C00E C00F -166.6(12) 4_645 . . . ?
C00D C00C C00F C00E 0(2) . . . . ?
C00B C00C C00F C00E -176.9(14) . . . . ?
N008 C00E C00F C00C -1(2) . . . . ?




loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.248 125.0 49.5 '6 N'
2 0.500 0.500 -0.616 125.0 49.5 '6 N'

_smtbx_masks_special_details     ?
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2



