Incorporation of Axial Chirality into Phosphino-Imidazoline Ligands for Enantioselective Catalysis
Paioti, Paulo H. S.; Abboud, Khalil A.; Aponick, Aaron; ACS Catalysis 7 (2017) 2133–; doi:10.1021/acscatal.7b00133

data_4514051
_publ_section_title
;
 Incorporation of Axial Chirality into Phosphino-Imidazoline Ligands for
 Enantioselective Catalysis
;
_journal_issue                   3
_journal_name_full               'ACS Catalysis'
_journal_page_first              2133
_journal_paper_doi               10.1021/acscatal.7b00133
_journal_volume                  7
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C44 H30 F5 N2 P'
_chemical_formula_weight         712.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-07-02 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 97.6938(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3700(4)
_cell_length_b                   45.6483(14)
_cell_length_c                   12.6634(4)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     7086.3(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            125872
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         0.892
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.9926
_exptl_absorpt_correction_T_min  0.9687
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL v6.14 (Bruker 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 10882 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1873
_refine_ls_number_reflns         32537
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0462P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0873
_reflns_Friedel_coverage         0.972
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                26176
_reflns_number_total             32537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b00133_si_002.cif
_cod_data_source_block           paulo3
_cod_depositor_comments
;

2020-09-22
Z value changed to bi consistent with given formula
                 miguel
;
_cod_original_formula_units_Z            8
_cod_database_code               4514051
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.959
_shelx_res_checksum              59000
_shelx_hkl_checksum              28785