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_1567577
_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         'C52 H60 Co2 N4 O10, C5 H12'
_chemical_formula_sum            'C57 H72 Co2 N4 O10'
_chemical_formula_weight         1091.04
_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                 97.5070(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3182(3)
_cell_length_b                   12.0109(3)
_cell_length_c                   15.9104(4)
_cell_measurement_reflns_used    57243
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.95
_cell_measurement_theta_min      2.22
_cell_volume                     2712.73(11)
_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 0.998
_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  0.0455
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            134219
_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         34.337
_diffrn_reflns_theta_min         2.131
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  0.7922
_exptl_absorpt_correction_T_min  0.6658
_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 =  0.0080
 Maximum odd and even orders for spherical harmonics =   3   6
 wR2(int) =  0.1342 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0535 (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  0.0417  0.252 - 0.461  0.983 - 1.032  0.892  0.0232  43.1   31871   24515
   2  11.7  0.0420  0.293 - 0.472  0.983 - 1.037  0.858  0.0232  43.1   12895    9849
   3  27.7  0.0649  0.285 - 0.334  0.983 - 1.031  1.039  0.0232  43.1   10923    6910
   4  11.7  0.0426  0.257 - 0.479  0.983 - 1.031  0.913  0.0232  43.1   19894   15245
   5  11.7  0.0422  0.256 - 0.446  0.983 - 1.030  0.889  0.0232  43.1   28189   21402
   6  11.7  0.0449  0.254 - 0.440  0.983 - 1.031  0.946  0.0232  43.1   13829   10326
   7   0.0  0.0647  0.272 - 0.473  0.980 - 1.033  0.886  0.0232  43.1   24112   17605
   8f  0.0  0.1272  0.275 - 0.471  0.981 - 1.034  1.038  0.0232  43.1   21285   10374
   9f  0.0  0.3774  2.722 - 4.372  0.980 - 1.037  0.805  0.0232  43.1   14436    4265

 535 Overloads replaced by fast scan measurements
 142248 Corrected reflections written to file sad.hkl
 Estimated minimum and maximum transmission:  0.6658  0.7922
 Additional spherical absorption correction applied with mu*r =  0.1520
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_recrystallization_method
'diffusion of pentane to a benzene solution'
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.228
_refine_diff_density_max         2.175
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         11333
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0788P)^2^+2.2688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9676
_reflns_number_total             11333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03028d4.cif
_cod_data_source_block           st0116
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1567577
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.829
_shelx_estimated_absorpt_t_max   0.862
_shelx_res_checksum              75276
_shelx_hkl_checksum              8721