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_1567574
_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         'C44 H44 Co2 N4 O6, 4(C6 H6)'
_chemical_formula_sum            'C68 H68 Co2 N4 O6'
_chemical_formula_weight         1155.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9817(4)
_cell_length_b                   17.1391(6)
_cell_length_c                   31.4588(11)
_cell_measurement_reflns_used    25503
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.82
_cell_measurement_theta_min      2.30
_cell_volume                     5921.1(4)
_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 0.999
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            89048
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.262
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.9434
_exptl_absorpt_correction_T_min  0.7757
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Stalke et al., 2015)

 Equivalent reflections defined by point group mmm 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) =  0.0719 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0571 (selected reflections only, after parameter refinement)

 Run 2theta R(int) Incid. factors Diffr. factors    K      g   I/s(lim) Total I>2sig(I)
   1  10.1  0.0589  0.343 - 0.368  0.993 - 1.078  0.799  0.0371  27.0   19284   12094
   2  10.1  0.0615  0.314 - 0.350  0.971 - 1.036  0.820  0.0371  27.0   19427   11926
   3  10.1  0.0634  0.325 - 0.359  0.970 - 1.087  0.830  0.0371  27.0   18777   11426
   4  10.1  0.0599  0.303 - 0.378  0.969 - 1.071  0.793  0.0371  27.0   20568   12743
   5  10.1  0.0611  0.312 - 0.387  0.969 - 1.078  0.806  0.0371  27.0   27745   16860
   6f  0.0  0.2738  0.427 - 0.561  0.969 - 1.038  0.963  0.0371  27.0   25820    8877
   7f  0.0  0.3902  0.372 - 0.428  0.969 - 1.037  1.346  0.0371  27.0   16123    3549

 79 Overloads replaced by fast scan measurements
 Estimated minimum and maximum transmission:  0.7757  0.9434
 Additional spherical absorption correction applied with mu*r =  0.0394
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       prism
_exptl_crystal_F_000             2424
_exptl_crystal_recrystallization_method
'diffusion of pentane to a benzene solution'
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6516
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0374P)^2^+9.8228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5371
_reflns_number_total             6516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03028d4.cif
_cod_data_source_block           st0069
_cod_database_code               1567574
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              6836
_shelx_hkl_checksum              44925