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_1568294
_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         'C18 H9 Cl6 P'
_chemical_formula_sum            'C18 H9 Cl6 P'
_chemical_formula_weight         468.92
_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.cc2d9w7v
_audit_creation_date             2022-08-08
_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                98.197(2)
_cell_angle_beta                 91.021(3)
_cell_angle_gamma                94.611(4)
_cell_formula_units_Z            2
_cell_length_a                   4.8136(3)
_cell_length_b                   12.6603(4)
_cell_length_c                   15.5459(3)
_cell_measurement_reflns_used    6430
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.3410
_cell_measurement_theta_min      2.8710
_cell_volume                     934.27(7)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.948
_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     26.00  95.00   0.50    0.05    --   46.87  73.00   8.00  138
  2  \w    136.00 162.00   0.50    0.05    --  107.00  73.00   8.00   52
  3  \w    146.00 177.00   0.50    0.05    --  107.00  30.00  30.00   62
  4  \w    103.00 173.00   0.50    0.05    --  107.00  45.00 -60.00  140
  5  \w     92.00 142.00   0.50    0.05    --  107.00  30.00  30.00  100
  6  \w     81.00 106.00   0.50    0.05    --  107.00 -73.00-121.00   50
  7  \w     57.00 106.00   0.50    0.05    --  107.00 -94.00 -60.00   98
  8  \w     80.00 105.00   0.50    0.05    --  107.00-125.00 -30.00   50
  9  \w     36.00  63.00   0.50    0.05    --   46.87 -73.00-121.00   54
 10  \w     20.00  92.00   0.50    0.05    --   46.87-125.00-120.00  144
 11  \w     35.00  61.00   0.50    0.05    --  107.00 -73.00-121.00   52
 12  \w     34.00  68.00   0.50    0.05    --  107.00 -94.00-120.00   68
 13  \w     36.00  73.00   0.50    0.05    --  107.00-125.00 -30.00   74
 14  \w     22.00  47.00   0.50    0.05    --   46.87-125.00  30.00   50
 15  \w     60.00  95.00   0.50    0.05    --   46.87-125.00  30.00   70
 16  \w     41.00  67.00   0.50    0.05    --  107.00 -94.00  90.00   52
 17  \w     37.00 106.00   0.50    0.05    --  107.00 -94.00 120.00  138
 18  \w     45.00 111.00   0.50    0.05    --  107.00-125.00  90.00  132
 19  \w     -1.00  31.00   0.50    0.05    --   46.87 -73.00-121.00   64
 20  \w    -31.00  12.00   0.50    0.05    --  -46.87  73.00   8.00   86
 21  \w    -55.00 -29.00   0.50    0.05    -- -102.00 125.00 150.00   52
 22  \w    -59.00 -30.00   0.50    0.05    -- -102.00 125.00  30.00   58
 23  \w    -86.00 -61.00   0.50    0.05    -- -102.00  73.00   8.00   50
 24  \w   -108.00 -72.00   0.50    0.05    -- -102.00 125.00  30.00   72
 25  \w   -113.00 -30.00   0.50    0.05    -- -102.00  45.00  30.00  166
 26  \w   -105.00 -60.00   0.50    0.05    -- -102.00 125.00 150.00   90
 27  \w   -115.00 -53.00   0.50    0.05    --  -46.87 -73.00-121.00  124
 28  \w    -58.00 -27.00   0.50    0.05    -- -102.00  30.00-150.00   62
 29  \w    -88.00 -40.00   0.50    0.05    -- -102.00  61.00-180.00   96
 30  \w   -117.00 -67.00   0.50    0.05    -- -102.00  30.00-150.00  100
 31  \w   -174.00-121.00   0.50    0.05    -- -102.00 -73.00-121.00  106
 32  \w   -101.00 -76.00   0.50    0.05    --  -46.87-125.00-150.00   50
 33  \w   -114.00 -74.00   0.50    0.05    --  -46.87-125.00   0.00   80
 34  \w   -174.00 -87.00   0.50    0.05    -- -102.00 -77.00 -90.00  174
;
_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      0.1047772000
_diffrn_orient_matrix_UB_12      -0.0911769000
_diffrn_orient_matrix_UB_13      0.0444623000
_diffrn_orient_matrix_UB_21      -0.1658707000
_diffrn_orient_matrix_UB_22      -0.0830385000
_diffrn_orient_matrix_UB_23      -0.0678213000
_diffrn_orient_matrix_UB_31      0.2543484000
_diffrn_orient_matrix_UB_32      -0.0035364000
_diffrn_orient_matrix_UB_33      -0.0587909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9201
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.594
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.193
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29531
_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    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          2
_exptl_crystal_size_mid          1
_exptl_crystal_size_min          1
_refine_diff_density_max         1.202
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0691
_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^)+(0.1948P)^2^+0.3435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3338
_reflns_number_total             3709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05753k3.cif
_cod_data_source_block           DCP
_cod_depositor_comments
'Adding full bibliography for 1568291--1568295.cif.'
_cod_database_code               1568294
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H P Cl'
_shelx_estimated_absorpt_t_max   0.039
_shelx_estimated_absorpt_t_min   0.020
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C8(H8), C10(H10), C12(H12), C14(H14), C16(H16),
 C18(H18)
;
_shelx_res_checksum              57417
_shelx_hkl_checksum              39566
_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 3.921
_oxdiff_exptl_absorpt_empirical_full_min 0.297