Planar-Chiral Phosphine-Olefin Ligands Exploiting a (Cyclopentadienyl)manganese(I) Scaffold To Achieve High Robustness and High Enantioselectivity.
Kamikawa, Ken; Tseng, Ya-Yi; Jian, Jia-Hong; Takahashi, Tamotsu; Ogasawara, Masamichi; Journal of the American Chemical Society 139 (2017) 1545–1553; doi:10.1021/jacs.6b11243

data_4125727
_publ_section_title
;
 Planar-Chiral Phosphine-Olefin Ligands Exploiting a
 (Cyclopentadienyl)manganese(I) Scaffold To Achieve High Robustness and
 High Enantioselectivity.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1545
_journal_page_last               1553
_journal_paper_doi               10.1021/jacs.6b11243
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C39 H37 Mn O2 P2'
_chemical_formula_weight         654.56
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                106.575(3)
_cell_angle_beta                 108.044(3)
_cell_angle_gamma                95.5983(12)
_cell_formula_units_Z            2
_cell_length_a                   10.322(2)
_cell_length_b                   13.409(3)
_cell_length_c                   13.848(3)
_cell_measurement_reflns_used    6140
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      27.4391
_cell_measurement_theta_min      3.2385
_cell_volume                     1709.9(6)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      253(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'RIGAKU Saturn'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13889
_diffrn_reflns_point_group_measured_fraction_full 0.705
_diffrn_reflns_point_group_measured_fraction_max 0.676
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.440
_diffrn_reflns_theta_min         3.239
_exptl_absorpt_coefficient_mu    0.512
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       prism
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 2530 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.022(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     828
_refine_ls_number_reflns         10570
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.413
_reflns_Friedel_fraction_full    0.435
_reflns_Friedel_fraction_max     0.395
_reflns_number_gt                9512
_reflns_number_total             10570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11243_si_003.cif
_cod_data_source_block           ydkr
_cod_original_cell_volume        1709.8(7)
_cod_database_code               4125727
_shelx_estimated_absorpt_t_min   0.905
_shelx_estimated_absorpt_t_max   0.905
_shelxl_version_number           2014-3
_shelx_res_checksum              1596
_shelx_hkl_checksum              60926