Evidence for “cocktail”-type catalysis in Buchwald–Hartwig reaction. A mechanistic study
Prima, Darya O.; Madiyeva, Malena; Burykina, Julia V.; Minyaev, Mikhail E.; Boiko, Daniil A.; Ananikov, Valentine P.; Catalysis Science & Technology 11 (2021) 7171–7188; doi:10.1039/D1CY01601F

data_1564766
_publ_section_title
;
 Evidence for &#x201C;cocktail&#x201D;-type catalysis in Buchwald--Hartwig
 reaction. A mechanistic study
;
_journal_issue                   21
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              7171
_journal_page_last               7188
_journal_paper_doi               10.1039/D1CY01601F
_journal_volume                  11
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C54 H74 Br2 N4 O2 Pd2'
_chemical_formula_sum            'C54 H74 Br2 N4 O2 Pd2'
_chemical_formula_weight         1183.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-04-25 deposited with the CCDC.	2021-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.5667(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4263(3)
_cell_length_b                   14.7841(4)
_cell_length_c                   16.2288(4)
_cell_measurement_reflns_used    9239
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.92
_cell_measurement_theta_min      2.58
_cell_volume                     2898.23(13)
_computing_cell_refinement       'SAINT (Bruker, 2019)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2019)'
_computing_data_reduction        'SAINT (Bruker, 2019)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)'
_computing_publication_material
'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)'
_computing_structure_refinement
'SHELXL-2018 (Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_structure_solution
'SHELXT, SHELXS-2013 (Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS D8 QUEST, Photon III detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            170408
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.998
_diffrn_reflns_theta_min         2.321
_diffrn_source                   'sealed X-Ray tube'
_diffrn_source_current           30
_diffrn_source_power             50
_diffrn_source_size              '0.6 mm, fine-focus'
_exptl_absorpt_coefficient_mu    2.038
_exptl_absorpt_correction_T_max  0.2720
_exptl_absorpt_correction_T_min  0.1529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS 2016/2 (Krause et al., J. Appl. Cryst. 2015, 48, 3-10)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.952
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         23690
_refine_ls_number_restraints     465
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+2.3365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1079
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                19373
_reflns_number_total             23690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy01601f2.cif
_cod_data_source_block           3B
_cod_depositor_comments
'Adding full bibliography for 1564765--1564770.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1564766
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.390
_shelx_estimated_absorpt_t_max   0.454
_shelx_res_checksum              53784
_shelx_fab_checksum              77312