Dynamic Kinetic Asymmetric Heck Reaction for the Simultaneous Generation of Central and Axial Chirality.
Carmona, José A; Hornillos, Valentín; Ramírez-López, Pedro; Ros, Abel; Iglesias-Sigüenza, Javier; Gómez-Bengoa, Enrique; Fernández, Rosario; Lassaletta, José M; Journal of the American Chemical Society 140 (2018) 11067–11075; doi:10.1021/jacs.8b05819

data_4132729
_publ_section_title
;
 Dynamic Kinetic Asymmetric Heck Reaction for the Simultaneous Generation
 of Central and Axial Chirality.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11067
_journal_page_last               11075
_journal_paper_doi               10.1021/jacs.8b05819
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C65 H49 F0 N O0.5 P2 Pd S0'
_chemical_formula_weight         1020.39
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.715(3)
_cell_angle_beta                 81.105(3)
_cell_angle_gamma                80.949(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7654(11)
_cell_length_b                   15.5021(14)
_cell_length_c                   15.5871(12)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      22.10
_cell_measurement_theta_min      2.22
_cell_volume                     2840.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36629
_diffrn_reflns_theta_full        22.21
_diffrn_reflns_theta_max         22.21
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
 X-ray Solutions, Madison, Wisconsin, USA. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.272
_refine_diff_density_min         -1.504
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.811
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1252
_refine_ls_number_reflns         23352
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.811
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.4953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                20536
_reflns_number_total             23352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b05819_si_006.cif
_cod_data_source_block           igl6617a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P1
_cod_original_formula_sum        'C65 H49 F0 N O0.50 P2 Pd S0'
_cod_database_code               4132729
_platon_squeeze_void_probe_radius 1.20