Stereoselective preparation of P,axial-stereogenic allenyl bisphosphine oxides via chirality-transfer.
Qiu, Mao-Ran; Zheng, Hong-Xing; Ye, Jing-Jing; Yan, Bing-Xia; Zhao, Chang-Qiu; Li, Qiang; Organic & biomolecular chemistry 18 (2020) 3017–3021; doi:10.1039/d0ob00390e

data_7157422
_publ_section_title
;
 Stereoselective preparation of P,axial-stereogenic allenyl bisphosphine
 oxides via chirality-transfer.
;
_journal_issue                   16
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3017
_journal_page_last               3021
_journal_paper_doi               10.1039/d0ob00390e
_journal_volume                  18
_journal_year                    2020
_chemical_absolute_configuration R
_chemical_formula_sum            'C26 H33 O3 P'
_chemical_formula_weight         424.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2019-06-05 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8154(7)
_cell_length_b                   11.3911(9)
_cell_length_c                   24.121(2)
_cell_measurement_reflns_used    3164
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.927
_cell_measurement_theta_min      2.455
_cell_volume                     2422.2(3)
_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 0.976
_diffrn_measured_fraction_theta_max 0.999
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11725
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.014
_diffrn_reflns_theta_min         2.459
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_exptl_transmission_factor_max   0.966
_exptl_transmission_factor_min   0.955
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 1080 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.12(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0513P)^2^+0.1562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1113
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3059
_reflns_number_total             4272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob00390e2.cif
_cod_data_source_block           180113g
_cod_depositor_comments
'Adding full bibliography for 7157420--7157422.cif.'
_cod_database_code               7157422
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.967
_shelxl_version_number           2014/6
_shelx_res_checksum              52967