Cobalt-catalyzed chemoselective dehydrogenation through radical translocation under visible light.
Yu, Wan-Lei; Ren, Zi-Gang; Ma, Ke-Xing; Yang, Hui-Qing; Yang, Jun-Jie; Zheng, Haixue; Wu, Wangsuo; Xu, Peng-Fei; Chemical science 13 (2022) 7947–7954; doi:10.1039/d2sc02291e

data_1567134
_publ_section_title
;
 Cobalt-catalyzed chemoselective dehydrogenation through radical
 translocation under visible light.
;
_journal_issue                   26
_journal_name_full               'Chemical science'
_journal_page_first              7947
_journal_page_last               7954
_journal_paper_doi               10.1039/d2sc02291e
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C31 H34 Co N5 O4 Sn'
_chemical_formula_sum            'C31 H32 Co N5 O4 Sn'
_chemical_formula_weight         716.23
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-14 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0187(7)
_cell_length_b                   14.1539(5)
_cell_length_c                   30.0583(11)
_cell_measurement_reflns_used    9531
_cell_measurement_temperature    275(4)
_cell_measurement_theta_max      30.5710
_cell_measurement_theta_min      2.0960
_cell_volume                     6389.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      275(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -66.00 -24.00   0.50   11.17    --    3.64 -61.00  20.00   84
  2  \w     -8.00  20.00   0.50   11.17    --    3.64 -61.00  20.00   56
  3  \w     -2.00  24.00   0.50   11.17    --   -6.53 -99.00  90.00   52
  4  \w     30.00  64.00   0.50   11.17    --   -6.53  37.00-150.00   68
  5  \w    -17.00  22.00   0.50   11.17    --   -6.53 -99.00  30.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0021542000
_diffrn_orient_matrix_UB_12      0.0500634000
_diffrn_orient_matrix_UB_13      -0.0003063000
_diffrn_orient_matrix_UB_21      -0.0334161000
_diffrn_orient_matrix_UB_22      0.0011583000
_diffrn_orient_matrix_UB_23      -0.0166638000
_diffrn_orient_matrix_UB_31      -0.0332859000
_diffrn_orient_matrix_UB_32      0.0020708000
_diffrn_orient_matrix_UB_33      0.0167148000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.808
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            36488
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.911
_diffrn_reflns_theta_min         2.090
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         8171
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0279P)^2^+0.9128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5195
_reflns_number_total             8171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02291e2.cif
_cod_data_source_block           yuwl_0113_auto
_cod_depositor_comments
'Adding full bibliography for 1567133--1567134.cif.'
_cod_database_code               1567134
_shelx_shelxl_version_number     2018/1
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H79(0.5) H80(0.5) C16(0.5) H38(0.5) C40(0.5) H61(0.5) C17(0.5)
 H41(0.5) C39(0.5) H60(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C18(H42), C19(H44), C43(H62), C45(H64), C63(H81), C13(H32), C11(H28),
 C12(H30), C29(H52), C31(H54), C14(H34), C53(H77), C33(H55), C15(H36), C56(H78),
  C35(H57), C37(H58), C59(H79), C59(H80), C16(H38), C40(H61), C17(H41), C39(H60)
3.b Idealised Me refined as rotating group:
 C49(H71,H72,H73), C51(H74,H75,H76), C48(H68,H69,H70), C47(H65,H66,H67)
;
_shelx_res_checksum              36936
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.620
_oxdiff_exptl_absorpt_empirical_full_min 0.305