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_1567572
_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 H40 Br4 Co2 N4 O6'
_chemical_formula_sum            'C44 H40 Br4 Co2 N4 O6'
_chemical_formula_weight         1158.30
_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                66.4289(10)
_cell_angle_beta                 77.1738(11)
_cell_angle_gamma                84.9305(11)
_cell_formula_units_Z            1
_cell_length_a                   9.4017(4)
_cell_length_b                   10.5681(5)
_cell_length_c                   12.6960(6)
_cell_measurement_reflns_used    44331
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.63
_cell_measurement_theta_min      2.55
_cell_volume                     1127.35(9)
_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 0.980
_diffrn_measured_fraction_theta_max 0.911
_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  0.0283
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73279
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.751
_diffrn_reflns_theta_min         2.551
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.331
_exptl_absorpt_correction_T_max  0.2168
_exptl_absorpt_correction_T_min  0.1074
_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 =  0.0060
 Maximum odd and even orders for spherical harmonics =   5   8
 wR2(int) =  0.1017 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0422 (selected reflections only, after parameter refinement)

 Run 2theta R(int) Incid. factors Diffr. factors    K      g   I/s(lim) Total I>2sig(I)
   1  11.0  0.0266  0.593 - 0.890  0.895 - 1.067  0.771  0.0314  31.8   19356   16879
   2  11.0  0.0338  0.840 - 1.044  0.892 - 1.067  0.901  0.0314  31.8    2813    2347
   3  11.0  0.0342  0.736 - 0.788  0.898 - 1.034  0.822  0.0314  31.8    2853    2507
   4  11.0  0.0333  0.995 - 1.108  0.904 - 1.066  0.862  0.0314  31.8    3053    2557
   5  11.0  0.0327  0.945 - 1.031  0.892 - 1.056  0.880  0.0314  31.8    3148    2647
   6  11.0  0.0258  0.698 - 0.986  0.903 - 1.067  0.800  0.0314  31.8    5876    4937
   7  11.0  0.0399  0.674 - 0.812  0.904 - 1.067  0.924  0.0314  31.8    2794    2314
   8  11.0  0.0300  0.857 - 0.982  0.898 - 1.035  0.804  0.0314  31.8    3191    2820
   9  11.0  0.0264  0.562 - 0.922  0.892 - 1.067  0.791  0.0314  31.8   21271   18403
  10  11.0  0.0241  0.757 - 0.953  0.899 - 1.067  0.776  0.0314  31.8    5904    5122
  11  11.0  0.0355  0.999 - 1.086  0.892 - 1.056  0.858  0.0314  31.8    3020    2539
  12f  0.0  0.0957  0.686 - 0.901  0.892 - 1.055  1.844  0.0314  31.8    7015    5031

 0 Overloads replaced by fast scan measurements
 Estimated minimum and maximum transmission:  0.1074  0.2168
 Additional spherical absorption correction applied with mu*r =  0.7360
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       prism
_exptl_crystal_F_000             574
_exptl_crystal_recrystallization_method
'diffusion of pentane to a benzene/THF solution'
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.746
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         10272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0318P)^2^+0.8755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9006
_reflns_number_total             10272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03028d4.cif
_cod_data_source_block           st0102
_cod_database_code               1567572
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.305
_shelx_estimated_absorpt_t_max   0.526
_shelx_res_checksum              28493
_shelx_hkl_checksum              1980