Dynamic Kinetic Resolution in Rhodium-Catalyzed Asymmetric Arylation of Phospholene Oxides.
Lim, Kelvin Meng-Hui; Hayashi, Tamio; Journal of the American Chemical Society 139 (2017) 8122–8125; doi:10.1021/jacs.7b04570

data_4126201
_publ_section_title
;
 Dynamic Kinetic Resolution in Rhodium-Catalyzed Asymmetric Arylation of
 Phospholene Oxides.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8122
_journal_page_last               8125
_journal_paper_doi               10.1021/jacs.7b04570
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C31 H35 Cl N O P Pd'
_chemical_formula_sum            'C31 H35 Cl N O P Pd'
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_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
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_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS D8 Venture '
_diffrn_measurement_method       'profile data from \q/2\q scans'
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_diffrn_reflns_av_R_equivalents  0.0675
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_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
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_diffrn_reflns_point_group_measured_fraction_max 0.912
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_diffrn_reflns_theta_max         25.675
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_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.699
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_refine_ls_abs_structure_details
;
 Flack x determined using 1191 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.605
_reflns_Friedel_fraction_full    0.804
_reflns_Friedel_fraction_max     0.797
_reflns_number_gt                3719
_reflns_number_total             4667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04570_si_001.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 4126201.cif.'
_cod_original_cell_volume        2693(3)
_cod_database_code               4126201
_shelx_estimated_absorpt_t_min   0.815
_shelx_estimated_absorpt_t_max   0.951
_shelxl_version_number           2014/6
_shelx_res_checksum              71286
_shelx_hkl_checksum              38391