Mn(iii)-mediated C-P bond activation of diphosphines: toward a highly emissive phosphahelicene cation scaffold and modulated circularly polarized luminescence.
Yang, Bo; Yan, Suqiong; Li, Chengbo; Ma, Hui; Feng, Fanda; Zhang, Yuan; Huang, Wei; Chemical science 14 (2023) 10446–10457; doi:10.1039/d3sc03201a

data_1569727
_publ_section_title
;
 Mn(iii)-mediated C-P bond activation of diphosphines: toward a highly
 emissive phosphahelicene cation scaffold and modulated circularly
 polarized luminescence.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              10446
_journal_page_last               10457
_journal_paper_doi               10.1039/d3sc03201a
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration S
_chemical_formula_sum            'C58 H44 O2 P2'
_chemical_formula_weight         834.87
_chemical_name_systematic
(6,6'-bis(4-methoxyphenyl)-[1,1'-binaphthalene]-2,2'-diyl)bis(diphenylphosphane)
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-12-09 deposited with the CCDC.	2023-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                95.700(3)
_cell_angle_beta                 99.414(3)
_cell_angle_gamma                101.148(4)
_cell_formula_units_Z            2
_cell_length_a                   9.2214(9)
_cell_length_b                   13.2109(12)
_cell_length_c                   18.8909(16)
_cell_measurement_reflns_used    9648
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      55.047
_cell_measurement_theta_min      4.583
_cell_volume                     2207.0(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.983
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20889
_diffrn_reflns_point_group_measured_fraction_full 0.701
_diffrn_reflns_point_group_measured_fraction_max 0.686
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_min         2.050
_exptl_absorpt_coefficient_mu    0.143
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 3179 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1121
_refine_ls_number_reflns         13951
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0670P)^2^+0.2138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1313
_reflns_Friedel_coverage         0.394
_reflns_Friedel_fraction_full    0.416
_reflns_Friedel_fraction_max     0.388
_reflns_number_gt                12229
_reflns_number_total             13951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03201a2.cif
_cod_data_source_block           20220320YB12B3_0m
_cod_depositor_comments
'Adding full bibliography for 1569716--1569732.cif.'
_cod_database_code               1569727
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              58267