P-chirogenic Diphosphazanes with Axially Chiral Substituents and their Use in Rh-catalyzed Asymmetric Hydrogenation.
Moritz, Jan-Ole; Chakrabortty, Soumyadeep; Müller, Bernd H; Spannenberg, Anke; Kamer, Paul C. J.; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c01108

data_4038832
_publ_section_title
;
 P-chirogenic Diphosphazanes with Axially Chiral Substituents and their
 Use in Rh-catalyzed Asymmetric Hydrogenation.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01108
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H54 N2 O4 P4 Rh, B F4'
_chemical_formula_sum            'C40 H54 B F4 N2 O4 P4 Rh'
_chemical_formula_weight         940.45
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.2616(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8041(6)
_cell_length_b                   15.3336(8)
_cell_length_c                   13.3346(7)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.62
_cell_measurement_theta_min      4.19
_cell_volume                     2158.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         microfocus
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24957
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        66.687
_diffrn_reflns_theta_max         66.687
_diffrn_reflns_theta_min         3.392
_exptl_absorpt_coefficient_mu    5.100
_exptl_absorpt_correction_T_max  0.41
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.196
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 3495 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7515
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.9520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                7502
_reflns_number_total             7515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01108_si_005.cif
_cod_data_source_block           AX1794
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4038832
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              41680
_shelx_hkl_checksum              56372