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_1567575
_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         'C60 H76 Co2 N4 O6, 4(C6 H6)'
_chemical_formula_sum            'C84 H100 Co2 N4 O6'
_chemical_formula_weight         1379.53
_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                72.164(2)
_cell_angle_beta                 70.4512(18)
_cell_angle_gamma                89.2308(19)
_cell_formula_units_Z            1
_cell_length_a                   11.1838(5)
_cell_length_b                   12.1674(6)
_cell_length_c                   15.6011(8)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.48
_cell_measurement_theta_min      2.63
_cell_volume                     1895.03(16)
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_collection       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'APEX3 v2019.1-0 (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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0626
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            144988
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.521
_diffrn_reflns_theta_min         2.467
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.9000
_exptl_absorpt_correction_T_min  0.7307
_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 =  0.0150
 Maximum odd and even orders for spherical harmonics =   3   6
 wR2(int) =  0.1440 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0719 (selected reflections only, after parameter refinement)

 Run 2theta R(int) Incid. factors Diffr. factors    K      g   I/s(lim) Total I>2sig(I)
   1f  0.0  0.1121  0.099 - 0.426  0.974 - 1.066  1.664  0.0385  26.0    1747    1215
   2  15.7  0.0488  0.064 - 0.135  0.974 - 1.133  0.860  0.0385  26.0   27086   21331
   3  15.7  0.0572  0.119 - 0.151  0.979 - 1.111  0.848  0.0385  26.0    3939    2988
   4  36.7  0.0652  0.135 - 0.179  0.974 - 1.111  0.880  0.0385  26.0    5670    4020
   5  15.7  0.1065  0.060 - 0.104  0.976 - 1.135  1.680  0.0385  26.0    5742    3755
   6  15.7  0.0613  0.127 - 0.172  0.974 - 1.134  0.880  0.0385  26.0    7975    5986
   7  15.7  0.0582  0.129 - 0.137  0.974 - 1.111  0.837  0.0385  26.0    5541    4130
   8  15.7  0.0493  0.060 - 0.129  0.974 - 1.110  0.810  0.0385  26.0    7931    6169
   9  15.7  0.0683  0.105 - 0.177  0.980 - 1.135  0.944  0.0385  26.0    5627    4099
  10  15.7  0.0613  0.123 - 0.143  0.975 - 1.102  0.948  0.0385  26.0    4315    3231
  11  15.7  0.0555  0.069 - 0.147  0.974 - 1.135  0.969  0.0385  26.0   30079   23009
  12  15.7  0.0601  0.130 - 0.181  0.992 - 1.127  0.854  0.0385  26.0    5948    4397
  13  15.7  0.0530  0.094 - 0.124  0.974 - 1.111  0.865  0.0385  26.0    7896    6058
  14  15.7  0.0624  0.156 - 0.182  0.974 - 1.105  0.885  0.0385  26.0    4055    2905
  15  15.7  0.1103  0.060 - 0.108  0.976 - 1.111  1.903  0.0385  26.0    6671    3881
  16   0.0  0.0957  0.086 - 0.141  0.974 - 1.133  0.973  0.0385  26.0   16495   11064

 22 Overloads replaced by fast scan measurements
 Estimated minimum and maximum transmission:  0.7307  0.9000
 Additional spherical absorption correction applied with mu*r =  0.0700
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       prism
_exptl_crystal_F_000             734
_exptl_crystal_recrystallization_method 'from a hot benzene solution'
_exptl_crystal_size_max          0.534
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         12609
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.7939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10784
_reflns_number_total             12609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03028d4.cif
_cod_data_source_block           st0003
_cod_database_code               1567575
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.930
_shelx_res_checksum              43933
_shelx_hkl_checksum              37581