Bis(perfluoroalkyl) Phosphino-Oxazoline: A Modular, Stable, Strongly π-Accepting Ligand for Asymmetric Catalysis
Zongjian Hu; Yuguang Li; Kai Liu; Qilong Shen; Journal of Organic Chemistry 77 (2012) 7957–7967; doi:10.1021/jo3011717

data_4027504
_publ_section_title
;
 Bis(perfluoroalkyl) Phosphino-Oxazoline: A Modular, Stable, Strongly
 \p-Accepting Ligand for Asymmetric Catalysis
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7957
_journal_page_last               7967
_journal_paper_doi               10.1021/jo3011717
_journal_volume                  77
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_sum            'C24 H25 F12 N O P Pd Sb'
_chemical_formula_weight         830.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.9980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6342(6)
_cell_length_b                   31.0416(18)
_cell_length_c                   10.4692(6)
_cell_measurement_reflns_used    8880
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.790
_cell_measurement_theta_min      4.445
_cell_volume                     2977.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16108
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68263
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.211
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         8160
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.7810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                7833
_reflns_number_total             8160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo3011717_si_004.cif
_cod_data_source_block           cd211223
_cod_database_code               4027504