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_1569724
_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 P
_chemical_formula_moiety         'Br, C34 H26 P, C H2 Cl2'
_chemical_formula_sum            'C35 H28 Br Cl2 P'
_chemical_formula_weight         630.35
_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_date             2022-08-28
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.280(4)
_cell_length_b                   12.550(4)
_cell_length_c                   19.659(6)
_cell_measurement_reflns_used    9281
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      53.748
_cell_measurement_theta_min      3.692
_cell_volume                     3029.7(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18500
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.295
_diffrn_reflns_theta_min         1.955
_exptl_absorpt_coefficient_mu    1.609
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.2791
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1630 before and 0.1126 after correction.
The Ratio of minimum to maximum transmission is 0.3718.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.395(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0719P)^2^+1.0679P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5175
_reflns_number_total             5454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03201a2.cif
_cod_data_source_block           (p)-bianp(phch3)2br
_cod_depositor_comments
'Adding full bibliography for 1569716--1569732.cif.'
_cod_original_cell_volume        3029.7(16)
_cod_database_code               1569724
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.856
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.605(12)
 0.395(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C35(H,HA)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26),
  C29(H29), C30(H30), C32(H32), C33(H33)
3.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C34(H34A,H34B,H34C)
;
_olex2_submission_special_instructions 'No special instructions were received'