TADDOL-based <i>P</i>,<i>S</i>-bidentate phosphoramidite ligands in palladium-catalyzed asymmetric allylic substitution.
Gavrilov, Konstantin N.; Chuchelkin, Ilya V.; Firsin, Ilya D.; Trunina, Valeria M.; Gavrilov, Vladislav K.; Zheglov, Sergey V.; Fedorov, Denis A.; Tafeenko, Victor A.; Zamilatskov, Ilya A.; Zimarev, Vladislav S.; Goulioukina, Nataliya S.; Organic & biomolecular chemistry 22 (2024) 538–549; doi:10.1039/d3ob01891a

data_7159711
_publ_section_title
;
 TADDOL-based <i>P</i>,<i>S</i>-bidentate phosphoramidite ligands in
 palladium-catalyzed asymmetric allylic substitution.
;
_journal_issue                   3
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              538
_journal_page_last               549
_journal_paper_doi               10.1039/d3ob01891a
_journal_volume                  22
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C39 H45 B F4 N O4 P Pd S'
_chemical_formula_sum            'C39 H45 B F4 N O4 P Pd S'
_chemical_formula_weight         848.00
_space_group_crystal_system      hexagonal
_space_group_IT_number           172
_space_group_name_Hall           'P 64'
_space_group_name_H-M_alt        'P 64'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-11-17 deposited with the CCDC.	2023-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   29.2000(10)
_cell_length_b                   29.2000(10)
_cell_length_c                   10.1029(4)
_cell_measurement_reflns_used    567
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      4.83
_cell_volume                     7460.1(5)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      295
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  STOE
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  none
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.2007
_diffrn_reflns_av_unetI/netI     0.5361
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            32191
_diffrn_reflns_point_group_measured_fraction_full 0.826
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        55.802
_diffrn_reflns_theta_max         55.802
_diffrn_reflns_theta_min         3.027
_diffrn_source                   'Cu GeniX 3D'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.102
_exptl_absorpt_correction_T_max  0.611
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          .28
_exptl_crystal_size_mid          .21
_exptl_crystal_size_min          .14
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 248 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(2)
_refine_ls_extinction_coef       0.00139(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.618
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         5314
_refine_ls_number_restraints     346
_refine_ls_restrained_S_all      0.610
_refine_ls_R_factor_all          0.2115
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0614P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1613
_reflns_Friedel_coverage         0.554
_reflns_Friedel_fraction_full    0.632
_reflns_Friedel_fraction_max     0.632
_reflns_number_gt                1259
_reflns_number_total             5314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob01891a2.cif
_cod_data_source_block           gavr88sr
_cod_depositor_comments
'Adding full bibliography for 7159710--7159711.cif.'
_cod_original_cell_volume        7460.1(6)
_cod_database_code               7159711
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              15808