Polarity-Reversal Strategy for Functionalization of Electrophilic Strained Molecules via Light-Driven Cobalt Catalysis.
Ociepa, Micha; Wierzba, Aleksandra J.; Turkowska, Joanna; Gryko, Dorota; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00245

data_4134371
_publ_section_title
;
 Polarity-Reversal Strategy for Functionalization of Electrophilic
 Strained Molecules via Light-Driven Cobalt Catalysis.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00245
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_sum            'C62 H84 Cl Co N4 O20 S'
_chemical_formula_weight         1331.77
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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
_cell_angle_alpha                95.530(2)
_cell_angle_beta                 105.779(2)
_cell_angle_gamma                100.114(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5732(2)
_cell_length_b                   12.8414(3)
_cell_length_c                   13.5828(2)
_cell_measurement_reflns_used    23080
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0830
_cell_measurement_theta_min      2.7090
_cell_volume                     1563.48(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38508
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.156
_diffrn_reflns_theta_min         2.261
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 6888 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         16142
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.3413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.833
_reflns_number_gt                15377
_reflns_number_total             16142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00245_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1563.47(6)
_cod_database_code               4134371
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              19519
_shelx_hkl_checksum              35555