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_1569728
_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_formula_moiety         'C32 H22 P, F6 P'
_chemical_formula_sum            'C32 H22 F6 P2'
_chemical_formula_weight         582.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-09-21
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-09 deposited with the CCDC.	2023-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8054(4)
_cell_length_b                   11.5114(4)
_cell_length_c                   19.2346(7)
_cell_measurement_reflns_used    6305
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.47
_cell_volume                     2609.35(16)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24633
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         1.973
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6996
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1329 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.9383.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1192
_exptl_crystal_preparation       Luminescent
_refine_diff_density_max         1.399
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5982
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0774
_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^)+(0.1180P)^2^+4.5118P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2140
_refine_ls_wR_factor_ref         0.2335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4502
_reflns_number_total             5982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03201a2.cif
_cod_data_source_block           y1_a
_cod_depositor_comments
'Adding full bibliography for 1569716--1569732.cif.'
_cod_database_code               1569728
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F1-F5 \\sim F1-F3 \\sim F1-F6 \\sim F1-F2 \\sim F5-F3 \\sim F5-F6 \\sim F5-F4
\\sim F3-F4 \\sim F3-F2 \\sim F6-F4
 \\sim F6-F2 \\sim F4-F2
 with sigma of 0.02
 P2-F1 \\sim P2-F5 \\sim P2-F3 \\sim P2-F6 \\sim P2-F4 \\sim P2-F2
 with sigma of 0.02
 C31-H30 \\sim C29-H30
 with sigma of 0.04
 C30-C31 \\sim C30-C29 \\sim C30-H30
 with sigma of 0.02
 C29-C30 \\sim C30-C31
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C19(H19), C8(H8), C14(H14), C2(H2), C3(H3), C7(H7), C22(H22),
 C16(H16), C6(H6), C5(H5), C18(H18), C17(H17), C26(H26), C23(H23), C24(H24),
 C28(H28), C25(H25), C32(H32), C31(H31), C29(H29), C30(H30)
;
_olex2_submission_special_instructions 'No special instructions were received'