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_7157420
_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/S
_chemical_formula_sum            'C37 H40 O2 P2'
_chemical_formula_weight         578.63
_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                   12.9764(11)
_cell_length_b                   14.3781(12)
_cell_length_c                   17.5765(15)
_cell_measurement_reflns_used    3285
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.236
_cell_measurement_theta_min      2.318
_cell_volume                     3279.4(5)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.972
_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  0.0609
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16603
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.015
_diffrn_reflns_theta_min         2.317
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.310
_exptl_transmission_factor_max   0.951
_exptl_transmission_factor_min   0.932
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 1199 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.08(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0480P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3586
_reflns_number_total             5766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob00390e2.cif
_cod_data_source_block           170915c_sq_d
_cod_depositor_comments
'Adding full bibliography for 7157420--7157422.cif.'
_cod_database_code               7157420
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.951
_shelxl_version_number           2014/6
_shelx_res_checksum              59619