Suzuki–Miyaura catalyst-transfer polymerization: new mechanistic insights
Howell, Mitchell T.; Kei, Peter; Anokhin, Maksim V.; Losovyj, Yaroslav; Fronczek, Frank R.; Nesterov, Evgueni E.; Polymer Chemistry 14 (2023) 4319–4337; doi:10.1039/D3PY00580A

data_1569745
_publ_section_title
;
 Suzuki--Miyaura catalyst-transfer polymerization: new mechanistic
 insights
;
_journal_issue                   37
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4319
_journal_page_last               4337
_journal_paper_doi               10.1039/D3PY00580A
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C37 H50 I O2 P Pd, C12 H9 N'
_chemical_formula_sum            'C49 H59 I N O2 P Pd'
_chemical_formula_weight         958.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2022-06-04 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.613(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.435(2)
_cell_length_b                   15.715(4)
_cell_length_c                   29.428(6)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.55
_cell_volume                     4314.1(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEX-II DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            127212
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.883
_diffrn_reflns_theta_min         1.400
_exptl_absorpt_coefficient_mu    1.223
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause <i>et al.</i>, 2015)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       needle
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.385
_refine_diff_density_min         -1.716
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         17342
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+15.6455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11838
_reflns_number_total             17342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py00580a2.cif
_cod_data_source_block           Nesterov2
_cod_depositor_comments
'Adding full bibliography for 1569745--1569747.cif.'
_cod_original_cell_volume        4314.0(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1569745
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.919
_shelx_res_checksum              82758
_shelx_hkl_checksum              89160