Functional Phosphine Derivatives Having Stationary and Flexible Chiralities: Their Preparation and Chirality Controlling.
Zhang, Yu; Nie, Shao-Zhen; Ye, Jing-Jing; Wang, Ji-Ping; Zhou, Meng-Meng; Zhao, Chang-Qiu; Li, Qiang; The Journal of organic chemistry 84 (2019) 8423–8439; doi:10.1021/acs.joc.9b00346

data_4034128
_publ_section_title
;
 Functional Phosphine Derivatives Having Stationary and Flexible
 Chiralities: Their Preparation and Chirality Controlling.
;
_journal_issue                   13
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8423
_journal_page_last               8439
_journal_paper_doi               10.1021/acs.joc.9b00346
_journal_volume                  84
_journal_year                    2019
_chemical_absolute_configuration S
_chemical_formula_sum            'C48 H66 Cl2 O2 P2 Pd'
_chemical_formula_weight         914.24
_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-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90.917(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7166(13)
_cell_length_b                   25.022(2)
_cell_length_c                   15.1067(15)
_cell_measurement_reflns_used    4945
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.930
_cell_measurement_theta_min      2.640
_cell_volume                     4806.3(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1091
_diffrn_reflns_av_unetI/netI     0.1983
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23747
_diffrn_reflns_point_group_measured_fraction_full 0.862
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.639
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.330
_exptl_transmission_factor_max   0.821
_exptl_transmission_factor_min   0.766
_refine_diff_density_max         3.415
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details
;
 Flack x determined using 2487 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         14991
_refine_ls_number_restraints     3086
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1902
_refine_ls_R_factor_gt           0.1030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1048P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2287
_refine_ls_wR_factor_ref         0.2675
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_full    0.750
_reflns_Friedel_fraction_max     0.770
_reflns_number_gt                7855
_reflns_number_total             14991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b00346_si_012.cif
_cod_data_source_block           180702g
_cod_original_cell_volume        4806.2(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4034128
_shelx_estimated_absorpt_t_min   0.766
_shelx_estimated_absorpt_t_max   0.827
_shelxl_version_number           2014/6
_shelx_res_checksum              66035
_shelx_hkl_checksum              39804