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_1567578
_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 H80 Co2 N8 O6'
_chemical_formula_sum            'C60 H80 Co2 N8 O6'
_chemical_formula_weight         1127.18
_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                77.6834(4)
_cell_angle_beta                 76.0242(5)
_cell_angle_gamma                66.2040(4)
_cell_formula_units_Z            2
_cell_length_a                   13.2692(3)
_cell_length_b                   15.2605(4)
_cell_length_c                   16.5352(4)
_cell_measurement_reflns_used    99224
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.85
_cell_measurement_theta_min      2.30
_cell_volume                     2947.53(12)
_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 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            383090
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.035
_diffrn_reflns_theta_min         1.945
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.8890
_exptl_absorpt_correction_T_min  0.7584
_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) =  0.1194 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0518 (selected reflections only, after parameter refinement)

 Run 2theta R(int) Incid. factors Diffr. factors    K      g   I/s(lim) Total I>2sig(I)
   1  11.7  0.0396  0.269 - 0.518  0.988 - 1.023  0.793  0.0218  45.9   49422   40324
   2  27.7  0.0522  0.355 - 0.478  0.988 - 1.018  0.828  0.0218  45.9   12018    8508
   3  27.7  0.0528  0.329 - 0.402  0.988 - 1.024  0.814  0.0218  45.9   12092    8316
   4  27.7  0.0523  0.339 - 0.454  0.988 - 1.018  0.843  0.0218  45.9   12017    8590
   5  11.7  0.0397  0.356 - 0.475  0.989 - 1.018  0.808  0.0218  45.9   15333   12327
   6  11.7  0.0418  0.302 - 0.559  0.989 - 1.024  0.828  0.0218  45.9   54719   43903
   7  11.7  0.0382  0.251 - 0.408  0.988 - 1.024  0.830  0.0218  45.9   15281   12443
   8  27.7  0.0537  0.352 - 0.511  0.988 - 1.022  0.792  0.0218  45.9   12006    8157
   9  27.7  0.0575  0.525 - 0.567  0.988 - 1.021  0.843  0.0218  45.9   12166    8152
  10  11.8  0.0395  0.303 - 0.499  0.988 - 1.016  0.814  0.0218  45.9   15451   12399
  11  11.8  0.0383  0.407 - 0.495  0.988 - 1.024  0.787  0.0218  45.9   13682   11054
  12  11.7  0.0412  0.439 - 0.554  0.988 - 1.012  0.785  0.0218  45.9   15347   12227
  13  11.8  0.0408  0.489 - 0.551  0.988 - 1.019  0.787  0.0218  45.9   12189    9690
  14  11.8  0.0377  0.291 - 0.417  0.989 - 1.024  0.822  0.0218  45.9   14303   11667
  15  11.7  0.0393  0.366 - 0.489  0.988 - 1.024  0.801  0.0218  45.9   15283   12211
  16  11.8  0.0411  0.346 - 0.498  0.988 - 1.018  0.795  0.0218  45.9   14026   11254
  17  11.7  0.0416  0.296 - 0.553  0.989 - 1.024  0.780  0.0218  45.9   55784   44899
  18  11.7  0.0406  0.265 - 0.525  0.988 - 1.016  0.812  0.0218  45.9   15340   12433
  19   0.0  0.0772  0.341 - 0.503  0.990 - 1.021  0.863  0.0218  45.9   26264   18427
  20f  0.0  0.1330  0.356 - 0.515  0.992 - 1.019  0.885  0.0218  45.9   20649   10521

 361 Overloads replaced by fast scan measurements
 393084 Corrected reflections written to file sad.hkl
 Estimated minimum and maximum transmission:  0.7584  0.8890
 Additional spherical absorption correction applied with mu*r =  0.0790
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       prism
_exptl_crystal_F_000             1196
_exptl_crystal_recrystallization_method
'diffusion of pentane to a benzene solution'
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         29806
_refine_ls_number_restraints     747
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0521P)^2^+1.5005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25212
_reflns_number_total             29806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03028d4.cif
_cod_data_source_block           st0117
_cod_database_code               1567578
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.822
_shelx_estimated_absorpt_t_max   0.925
_shelx_res_checksum              58980
_shelx_hkl_checksum              1281