Rh(I)/Bisoxazolinephosphine-Catalyzed Regio- and Enantioselective Allylic Substitutions
Xu, Wen-Bin; Ghorai, Samir; Huang, Wenyu; Li, Changkun; ACS Catalysis  (2020) 4491–4496; doi:10.1021/acscatal.0c00712

data_4517523
_publ_section_title
;
 Rh(I)/Bisoxazolinephosphine-Catalyzed Regio- and Enantioselective Allylic
 Substitutions
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              4491
_journal_page_last               4496
_journal_paper_doi               10.1021/acscatal.0c00712
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H40 Cl N2 O2 P Rh, C F3 O3 S'
_chemical_formula_sum            'C35 H40 Cl F3 N2 O5 P Rh S'
_chemical_formula_weight         827.08
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.9434(6)
_cell_length_b                   10.9434(6)
_cell_length_c                   60.442(4)
_cell_measurement_reflns_used    9456
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      68.35
_cell_measurement_theta_min      4.11
_cell_volume                     7238.4(7)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            87504
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.521
_diffrn_reflns_theta_min         2.924
_exptl_absorpt_coefficient_mu    5.960
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.190
_exptl_transmission_factor_max   0.1665
_exptl_transmission_factor_min   0.0350
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.034(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0415P)^2^+1.9477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.673
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6460
_reflns_number_total             6650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c00712_si_003.cif
_cod_data_source_block           a_a
_cod_depositor_comments
'Adding full bibliography for 4517522--4517523.cif.'
_cod_original_cell_volume        7238.4(9)
_cod_database_code               4517523
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.329
_shelx_estimated_absorpt_t_max   0.397
_shelx_res_checksum              68715
_shelx_hkl_checksum              55605