Mechanistic details of the cobalt-mediated dehydrogenative dimerization of aminoquinoline-directed benzamides.
Xu, Li-Ping; Liu, Elaine E. L.-N.; Bacsa, John; MacBeth, Cora E.; Musaev, Djamaladdin G.; Chemical science 11 (2020) 6085–6096; doi:10.1039/d0sc02066d

data_1558259
_publ_section_title
;
 Mechanistic details of the cobalt-mediated dehydrogenative dimerization
 of aminoquinoline-directed benzamides.
;
_journal_issue                   23
_journal_name_full               'Chemical science'
_journal_page_first              6085
_journal_page_last               6096
_journal_paper_doi               10.1039/d0sc02066d
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C34 H26 Co N4 O2'
_chemical_formula_sum            'C34 H26 Co N4 O2'
_chemical_formula_weight         581.52
_chemical_properties_physical    Air-sensitive
_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             2018-06-07
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-07 deposited with the CCDC.	2020-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.1904(2)
_cell_length_b                   15.2935(3)
_cell_length_c                   23.3304(4)
_cell_measurement_reflns_used    59147
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      45.0870
_cell_measurement_theta_min      1.3190
_cell_volume                     5419.99(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.495
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -88.00 -28.00   0.50   34.95    --  -43.22 120.00-108.00  120
  2  \w    -56.00  32.00   0.50   34.95    --  -43.22  19.00 -60.00  176
  3  \w    -31.00  57.00   0.50   34.95    --   43.53 -17.00   3.00  176
  4  \w     31.00 119.00   0.50   34.95    --   43.53  19.00   0.00  176
  5  \w     30.00 119.00   0.50   34.95    --   43.53  17.00 171.00  178
  6  \w     31.00  70.00   0.50   34.95    --   43.53  38.00  60.00   78
  7  \w   -115.00 -60.00   0.50   34.95    --  -43.22-178.00-150.00  110
  8  \w   -115.00 -28.00   0.50   34.95    --  -43.22 -57.00-180.00  174
  9  \w   -116.00 -58.00   0.50   34.95    --  -43.22 178.00-120.00  116
 10  \w   -116.00 -58.00   0.50   34.95    --  -43.22 178.00-180.00  116
 11  \w   -116.00 -58.00   0.50   34.95    --  -43.22 178.00  60.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0231930000
_diffrn_orient_matrix_UB_12      0.0402384000
_diffrn_orient_matrix_UB_13      0.0000071000
_diffrn_orient_matrix_UB_21      -0.0394418000
_diffrn_orient_matrix_UB_22      0.0224206000
_diffrn_orient_matrix_UB_23      -0.0069380000
_diffrn_orient_matrix_UB_31      -0.0093535000
_diffrn_orient_matrix_UB_32      0.0053679000
_diffrn_orient_matrix_UB_33      0.0295979000
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            218144
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         45.294
_diffrn_reflns_theta_min         1.746
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over 			a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       prism
_exptl_crystal_F_000             2408
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and diethyl ether  by solvent layering'
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.336
_exptl_crystal_size_min          0.286
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         22703
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.8706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18662
_reflns_number_total             22703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02066d2.cif
_cod_data_source_block           el-01-31
_cod_depositor_comments
;Adding full bibliography for 1558259--1558265.cif.

 Adding full bibliography for 1558259--1558265.cif.
;
_cod_original_cell_volume        5420.00(15)
_cod_database_code               1558259
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C272  H208  Co8  N32  O16  '
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.785
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     45.18
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-H17B \\sim C17-H17A \\sim C17-H17C
 with sigma of 0.002
 H17C-H17B \\sim H17C-H17A \\sim H17B-H17A
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uiso(H17A) = Uiso(H17B) = Uiso(H17C)
4.a Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id EL-01-31
_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 1.124
_oxdiff_exptl_absorpt_empirical_full_min 0.900