Mechanistic Studies on a Cooperative NHC Organocatalysis/Palladium Catalysis System: Uncovering Significant Lessons for Mixed Chiral Pd(NHC)(PR<sub>3</sub>) Catalyst Design.
Guo, Chang; Janssen-Müller, Daniel; Fleige, Mirco; Lerchen, Andreas; Daniliuc, Constantin G.; Glorius, Frank; Journal of the American Chemical Society 139 (2017) 4443–4451; doi:10.1021/jacs.7b00462

data_4131225
_publ_section_title
;
 Mechanistic Studies on a Cooperative NHC Organocatalysis/Palladium
 Catalysis System: Uncovering Significant Lessons for Mixed Chiral
 Pd(NHC)(PR<sub>3</sub>) Catalyst Design.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4443
_journal_page_last               4451
_journal_paper_doi               10.1021/jacs.7b00462
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C42 H41 B F4 N3 O P Pd'
_chemical_formula_weight         827.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9380(3)
_cell_length_b                   13.7755(4)
_cell_length_c                   24.4883(7)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      68.3840
_cell_measurement_theta_min      3.6099
_cell_volume                     3689.81(18)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'APEX2 v.2014.1.1 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_type           ' Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            18570
_diffrn_reflns_theta_full        68.45
_diffrn_reflns_theta_max         68.45
_diffrn_reflns_theta_min         3.61
_diffrn_source                   'Cu ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    4.958
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.493
_refine_ls_abs_structure_details
;

Flack x determined using 2159 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.063(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         6261
_refine_ls_number_restraints     476
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0339P)^2^+3.0935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                5747
_reflns_number_total             6261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00462_si_002.cif
_cod_data_source_block           glo8599
_cod_database_code               4131225
_shelx_res_checksum              896
_shelx_hkl_checksum              85963