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_1567579
_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         'C48 H52 Co2 N4 O6, C6 H6'
_chemical_formula_sum            'C54 H58 Co2 N4 O6'
_chemical_formula_weight         976.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 105.0699(10)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   13.5589(3)
_cell_length_b                   35.2233(10)
_cell_length_c                   16.1183(5)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.31
_cell_measurement_theta_min      2.33
_cell_volume                     7433.2(4)
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            477535
_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         34.370
_diffrn_reflns_theta_min         2.313
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.8827
_exptl_absorpt_correction_T_min  0.7889
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Stalke et al., 2015)

 Equivalent reflections defined by point group 2/m 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) =  0.1137 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0575 (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  0.1361  0.215 - 0.307  1.002 - 1.019  1.186  0.0172  58.0    8365    3397
   2  15.7  0.0572  0.189 - 0.324  1.002 - 1.027  0.910  0.0172  58.0   38260   24558
   3  15.7  0.0476  0.136 - 0.242  0.998 - 1.021  0.875  0.0172  58.0   69405   48212
   4  15.7  0.0478  0.161 - 0.203  1.000 - 1.027  0.872  0.0172  58.0   78302   53460
   5  15.7  0.0431  0.128 - 0.216  1.000 - 1.027  0.842  0.0172  58.0   38276   26812
   6  15.7  0.0543  0.208 - 0.256  1.002 - 1.027  0.896  0.0172  58.0   38059   25684
   7  15.7  0.0447  0.143 - 0.183  0.999 - 1.027  0.859  0.0172  58.0   38243   26348
   8  15.7  0.0464  0.154 - 0.199  1.002 - 1.026  0.853  0.0172  58.0   32938   22571
   9  15.7  0.0499  0.139 - 0.328  1.004 - 1.027  0.877  0.0172  58.0   38278   25322
  10  15.7  0.0432  0.129 - 0.191  0.998 - 1.027  0.843  0.0172  58.0   38153   26560
  11  15.7  0.0476  0.167 - 0.193  0.998 - 1.027  0.871  0.0172  58.0   32943   22351
  12  15.7  0.0477  0.160 - 0.185  1.002 - 1.027  0.864  0.0172  58.0   38290   26553
  13f  0.0  0.0699  0.139 - 0.180  1.002 - 1.019  0.860  0.0172  58.0    8151    5394

 Estimated minimum and maximum transmission:  0.7889  0.8827
 Additional spherical absorption correction applied with mu*r =  0.0800
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       prism
_exptl_crystal_F_000             3072
_exptl_crystal_recrystallization_method 'from a hot benzene solution'
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         31156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+2.7883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25404
_reflns_number_total             31156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03028d4.cif
_cod_data_source_block           st0011
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1567579
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.913
_shelx_res_checksum              96876
_shelx_hkl_checksum              42660