Design and synthesis of new chiral phosphorus-olefin bidentate ligands and their use in the rhodium-catalyzed asymmetric addition of organoboroxines to N-sulfonyl imines
Ryo Shintani; Rintaro Narui; Yosuke Tsutsumi; Sayuri Hayashi; Tamio Hayashi; Chem.Commun. 47 (2011) 6123–; doi:10.1039/c1cc11823d

data_7106419
_publ_section_title
;
 Design and synthesis of new chiral phosphorus-olefin bidentate ligands
 and their use in the rhodium-catalyzed asymmetric addition of
 organoboroxines to N-sulfonyl imines
;
_journal_name_full               Chem.Commun.
_journal_page_first              6123
_journal_paper_doi               10.1039/c1cc11823d
_journal_volume                  47
_journal_year                    2011
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C29 H31 N O2 P Rh '
_chemical_formula_sum            'C29 H31 N O2 P Rh'
_chemical_formula_weight         559.45
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.270(3)
_cell_length_b                   11.652(5)
_cell_length_c                   26.490(8)
_cell_measurement_reflns_used    19130
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2552.6(16)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      123(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.102
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            22742
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.06
_refine_diff_density_min         -3.34
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2473 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     339
_refine_ls_number_reflns         18345
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.0059
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
63.9849 68.2451 17.9686
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                18233
_reflns_number_total             5782
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c1cc11823d.txt
_cod_data_source_block           '_100602yuki'
_cod_original_cell_volume        2552.7(15)
_cod_original_formula_sum        'C29 H31 N O2 P Rh '
_cod_database_code               7106419