Photochromic Radical Complexes That Show Heterolytic Bond Dissociation.
Usui, Ryosuke; Yamamoto, Katsuya; Okajima, Hajime; Mutoh, Katsuya; Sakamoto, Akira; Abe, Jiro; Kobayashi, Yoichi; Journal of the American Chemical Society 142 (2020) 10132–10142; doi:10.1021/jacs.0c02739

data_4134968
_publ_section_title
;
 Photochromic Radical Complexes That Show Heterolytic Bond Dissociation.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10132
_journal_page_last               10142
_journal_paper_doi               10.1021/jacs.0c02739
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C33 H21 N3 S'
_chemical_formula_sum            'C33 H21 N3 S'
_chemical_formula_weight         491.59
_chemical_name_systematic        PTZ
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-28
_audit_creation_method
;
Olex2 1.2-ac4
(compiled 2018.05.17 svn.r3504 for Rigaku Oxford Diffraction, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.211(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7383(3)
_cell_length_b                   11.5764(3)
_cell_length_c                   22.1767(5)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.4610
_cell_measurement_theta_min      2.0760
_cell_volume                     4803.06(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.945
_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    -30.00  -4.00   0.50   12.49    --   20.00  54.00 -30.00   52
  2  \w     59.00  85.00   0.50   12.49    --   20.00  54.00 -30.00   52
  3  \w    -73.00  45.00   0.50   12.49    --   20.00  54.00-180.00  236
  4  \w     49.00 103.00   0.50   12.49    --   20.00  54.00-180.00  108
  5  \w    -74.00 -37.00   0.50   12.49    --   20.00  54.00  30.00   74
  6  \w    -16.00  11.00   0.50   12.49    --   20.00  54.00  30.00   54
  7  \w     33.00  59.00   0.50   12.49    --   20.00  54.00  30.00   52
  8  \w    -73.00 -48.00   0.50   12.49    --   20.00  54.00 120.00   50
  9  \w      0.00 103.00   0.50   12.49    --   20.00  54.00 120.00  206
 10  \w    -73.00 -37.00   0.50   12.49    --   20.00  54.00 -60.00   72
 11  \w    -66.00  27.00   0.50   12.49    --   20.00  54.00-120.00  186
 12  \w    -69.00 -44.00   0.50   12.49    --   20.00  54.00 -30.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II (JP)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0316194000
_diffrn_orient_matrix_UB_12      0.0337667000
_diffrn_orient_matrix_UB_13      0.0003652000
_diffrn_orient_matrix_UB_21      0.0208272000
_diffrn_orient_matrix_UB_22      -0.0511375000
_diffrn_orient_matrix_UB_23      0.0000271000
_diffrn_orient_matrix_UB_31      -0.0017722000
_diffrn_orient_matrix_UB_32      0.0002908000
_diffrn_orient_matrix_UB_33      -0.0320360000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24678
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.599
_diffrn_reflns_theta_min         1.839
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0835P)^2^+5.7801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5647
_reflns_number_total             6980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02739_si_002.cif
_cod_data_source_block           181227_ptz_usui
_cod_depositor_comments
;Adding full bibliography for 4134968--4134969.cif.

 Adding full bibliography for 4134968--4134969.cif.
;
_cod_database_code               4134968
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.923
_reflns_odcompleteness_completeness 98.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C27(H27), C37(H37), C21(H21), C31(H31), C36(H36), C33(H33), C9(H9),
 C12(H12), C35(H35), C28(H28), C19(H19), C2(H2), C10(H10), C5(H5), C30(H30),
 C20(H20), C11(H11), C34(H34), C29(H29), C4(H4)
;
_shelx_res_checksum              9775
_shelx_hkl_checksum              6983
_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 1.057
_oxdiff_exptl_absorpt_empirical_full_min 0.967