Direct observation of reversible bond homolysis by 2D EXSY NMR
Takebayashi, Satoshi; Fayzullin, Robert R.; Bansal, Richa; Chemical Science 13 (2022) 9202–9209; doi:10.1039/D2SC03028D

data_1567576
_publ_section_title
;
 Direct observation of reversible bond homolysis by 2D EXSY NMR
;
_journal_issue                   32
_journal_name_full               'Chemical Science'
_journal_page_first              9202
_journal_page_last               9209
_journal_paper_doi               10.1039/D2SC03028D
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C52 H60 Co2 N4 O6'
_chemical_formula_sum            'C52 H60 Co2 N4 O6'
_chemical_formula_weight         954.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-04-10 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                81.6740(9)
_cell_angle_beta                 71.6133(9)
_cell_angle_gamma                84.1723(9)
_cell_formula_units_Z            2
_cell_length_a                   11.1341(4)
_cell_length_b                   13.1609(4)
_cell_length_c                   17.4589(6)
_cell_measurement_reflns_used    51096
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.07
_cell_measurement_theta_min      2.33
_cell_volume                     2397.89(14)
_computing_cell_refinement       'APEX3 v2021.4-0 (Bruker AXS)'
_computing_data_collection       'APEX3 v2021.4-0 (Bruker AXS)'
_computing_data_reduction        'APEX3 v2021.4-0 (Bruker AXS)'
_computing_molecular_graphics
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012);
PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012);
PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            157918
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         1.567
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.9315
_exptl_absorpt_correction_T_min  0.8357
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Stalke et al., 2015)

 Equivalent reflections defined by point group -1 for scaling and error model
 Restraint esd for equal adjacent scale factors =  0.0050
 Maximum odd and even orders for spherical harmonics =   3   6
 wR2(int) =  0.0839 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0613 (selected reflections only, after parameter refinement)

 Run 2theta R(int) Incid. factors Diffr. factors    K      g   I/s(lim) Total I>2sig(I)
   1   9.9  0.0585  0.223 - 0.306  0.996 - 1.039  1.112  0.0211  47.5   29043   17485
   2  10.0  0.0579  0.296 - 0.336  0.996 - 1.035  1.030  0.0211  47.5    3233    2054
   3  10.0  0.0467  0.247 - 0.320  1.003 - 1.059  0.998  0.0211  47.5    3119    1891
   4  10.0  0.0648  0.346 - 0.375  1.000 - 1.034  1.106  0.0211  47.5    4509    2494
   5   9.9  0.0622  0.290 - 0.349  0.996 - 1.059  1.058  0.0211  47.5    8267    4634
   6  10.0  0.0512  0.324 - 0.361  1.004 - 1.028  1.045  0.0211  47.5    3021    1925
   7  10.0  0.0582  0.333 - 0.355  0.996 - 1.055  1.052  0.0211  47.5    3718    2260
   8  10.0  0.0533  0.282 - 0.350  0.996 - 1.032  1.042  0.0211  47.5    4771    2996
   9   9.9  0.0602  0.237 - 0.299  0.996 - 1.057  1.078  0.0211  47.5   31132   18592
  10  10.0  0.0590  0.249 - 0.320  1.001 - 1.059  1.066  0.0211  47.5    3731    2023
  11   9.9  0.0585  0.257 - 0.365  0.996 - 1.051  1.056  0.0211  47.5    8490    4952
  12  10.0  0.0621  0.309 - 0.339  1.004 - 1.040  1.093  0.0211  47.5    5185    2820
  13  10.0  0.0575  0.306 - 0.350  0.996 - 1.038  1.033  0.0211  47.5    3733    2411
  14  10.0  0.0634  0.311 - 0.358  0.996 - 1.058  1.030  0.0211  47.5    4247    2543
  15  10.0  0.0560  0.303 - 0.358  1.000 - 1.034  1.090  0.0211  47.5    4577    2643
  16  10.0  0.0552  0.251 - 0.319  1.002 - 1.059  1.019  0.0211  47.5    4216    2242
  17   9.9  0.0589  0.265 - 0.301  1.000 - 1.032  1.040  0.0211  47.5    7917    5186
  18   9.9  0.0646  0.260 - 0.320  0.996 - 1.057  1.128  0.0211  47.5   35325   20699
  19   9.9  0.0568  0.266 - 0.297  0.996 - 1.032  1.074  0.0211  47.5    7584    4614
  20  10.0  0.0565  0.284 - 0.330  0.996 - 1.028  1.047  0.0211  47.5    4619    3032
  21  10.0  0.0590  0.309 - 0.363  0.996 - 1.034  1.069  0.0211  47.5    6527    3746
  22  10.0  0.0626  0.309 - 0.333  1.003 - 1.040  1.056  0.0211  47.5    5966    3360
  23f  0.0  0.0968  0.261 - 0.340  0.996 - 1.049  1.100  0.0211  47.5   13346    6897
  24f  0.0  0.2060  0.287 - 0.351  0.999 - 1.037  1.541  0.0211  47.5    5758    1950

 6 Overloads replaced by fast scan measurements
 Estimated minimum and maximum transmission:  0.8357  0.9315
 Additional spherical absorption correction applied with mu*r =  0.0430
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       prism
_exptl_crystal_F_000             1004
_exptl_crystal_recrystallization_method
'diffusion of pentane to a benzene solution'
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         11897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+2.0281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9098
_reflns_number_total             11897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03028d4.cif
_cod_data_source_block           st0066
_cod_database_code               1567576
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.898
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              72942
_shelx_hkl_checksum              20828