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_1564768
_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 H72 I4 N4 Pd2, C H2 Cl2'
_chemical_formula_sum            'C55 H74 Cl2 I4 N4 Pd2'
_chemical_formula_weight         1582.48
_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                 100.0640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5373(3)
_cell_length_b                   15.0465(3)
_cell_length_c                   16.1547(3)
_cell_measurement_reflns_used    9653
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.33
_cell_measurement_theta_min      2.79
_cell_volume                     3000.57(11)
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            220125
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.347
_diffrn_reflns_theta_min         2.258
_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    2.783
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6088
_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            red
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       block
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 13267 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack, Wagner, Acta Cryst., 2013, B69, 249-259).
;
_refine_ls_abs_structure_Flack   0.010(3)
_refine_ls_extinction_coef       0.00128(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         29074
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0185
_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^)+(0.0159P)^2^+1.0134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0417
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                28350
_reflns_number_total             29074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy01601f2.cif
_cod_data_source_block           2C
_cod_depositor_comments
'Adding full bibliography for 1564765--1564770.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1564768
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.310
_shelx_estimated_absorpt_t_max   0.388
_shelx_res_checksum              7615