Manipulating D-A interaction to achieve stable photoinduced organic radicals in triphenylphosphine crystals.
Tang, Chunlin; Song, Lijuan; Zhou, Kang; Ren, Peng; Zhao, Engui; He, Zikai; Chemical science 14 (2023) 1871–1877; doi:10.1039/d2sc05753k

data_1568293
_publ_section_title
;
 Manipulating D-A interaction to achieve stable photoinduced organic
 radicals in triphenylphosphine crystals.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              1871
_journal_page_last               1877
_journal_paper_doi               10.1039/d2sc05753k
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C20 H14 Cl6 N P'
_chemical_formula_sum            'C20 H14 Cl6 N P'
_chemical_formula_weight         511.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2d9w5s
_audit_creation_date             2022-06-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-19 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                84.150(2)
_cell_angle_beta                 67.715(3)
_cell_angle_gamma                79.756(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8206(3)
_cell_length_b                   10.8079(3)
_cell_length_c                   11.4388(3)
_cell_measurement_reflns_used    7172
_cell_measurement_temperature    236(4)
_cell_measurement_theta_max      27.3400
_cell_measurement_theta_min      1.9450
_cell_volume                     1104.73(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      236(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00  21.00   0.50    0.21    --    6.16 -57.00 -90.00   96
  2  \w     -7.00  80.00   0.50    0.21    --    6.16  38.00-149.00  174
  3  \w     39.00  78.00   0.50    0.21    --    6.16  57.00-120.00   78
  4  \w     -1.00  25.00   0.50    0.21    --    6.16  57.00-120.00   52
  5  \w    -67.00  19.00   0.50    0.21    --    6.16 -38.00  55.00  172
  6  \w    -16.00  26.00   0.50    0.21    --   -5.85 -99.00  30.00   84
  7  \w     13.00  39.00   0.50    0.21    --    6.16 -99.00  30.00   52
  8  \w    -18.00  29.00   0.50    0.21    --    6.16 -99.00 150.00   94
  9  \w    -77.00 -17.00   0.50    0.21    --   -5.85 -37.00 -60.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0571100000
_diffrn_orient_matrix_UB_12      -0.0222711000
_diffrn_orient_matrix_UB_13      0.0239958000
_diffrn_orient_matrix_UB_21      -0.0472422000
_diffrn_orient_matrix_UB_22      0.0235751000
_diffrn_orient_matrix_UB_23      0.0599827000
_diffrn_orient_matrix_UB_31      -0.0272374000
_diffrn_orient_matrix_UB_32      -0.0583294000
_diffrn_orient_matrix_UB_33      0.0179876000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17478
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.825
_diffrn_reflns_theta_min         1.916
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       plate
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         5591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0590P)^2^+0.2418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3785
_reflns_number_total             5591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05753k3.cif
_cod_data_source_block           TCP-DMA
_cod_depositor_comments
'Adding full bibliography for 1568291--1568295.cif.'
_cod_database_code               1568293
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H P N Cl'
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.834
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C8(H8), C12(H12), C14(H14), C15(H15), C17(H17), C18(H18)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              54349
_shelx_hkl_checksum              78645
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.377
_oxdiff_exptl_absorpt_empirical_full_min 0.745