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_4134969
_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 O'
_chemical_formula_sum            'C33 H21 N3 O'
_chemical_formula_weight         475.53
_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_creation_date             2019-03-06
_audit_creation_method
;
Olex2 1.2-ac4
(compiled 2018.05.17 svn.r3504 for Rigaku Oxford Diffraction, GUI svn.r5492)
;
_cell_angle_alpha                92.607(5)
_cell_angle_beta                 93.237(5)
_cell_angle_gamma                105.501(5)
_cell_formula_units_Z            2
_cell_length_a                   6.8256(4)
_cell_length_b                   12.4886(8)
_cell_length_c                   14.5776(9)
_cell_measurement_reflns_used    4761
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.3970
_cell_measurement_theta_min      2.1710
_cell_volume                     1193.14(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.937
_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      5.00 109.00   0.50    1.31    --   20.00  54.00  30.00  208
  2  \w    -61.00 -18.00   0.50    1.31    --   20.00  54.00 150.00   86
  3  \w     66.00  92.00   0.50    1.31    --   20.00  54.00 150.00   52
  4  \w    -71.00 -28.00   0.50    1.31    --   20.00  54.00-180.00   86
  5  \w    -12.00 107.00   0.50    1.31    --   20.00  54.00-180.00  238
  6  \w    -74.00 -39.00   0.50    1.31    --   20.00  54.00  90.00   70
  7  \w    -11.00  60.00   0.50    1.31    --   20.00  54.00  90.00  142
  8  \w     69.00 103.00   0.50    1.31    --   20.00  54.00  90.00   68
  9  \w    -71.00 110.00   0.50    1.31    --   20.00  54.00 -30.00  362
 10  \w    -73.00 -46.00   0.50    1.31    --   20.00  54.00  60.00   54
 11  \w      4.00  32.00   0.50    1.31    --   20.00  54.00  60.00   56
 12  \w    -35.00 -10.00   0.50    1.31    --   20.00  54.00   0.00   50
 13  \w    -66.00  24.00   0.50    1.31    --   20.00  54.00 120.00  180
 14  \w    -64.00 -38.00   0.50    1.31    --   20.00  54.00-150.00   52
 15  \w    -67.00 -41.00   0.50    1.31    --   20.00  54.00 -90.00   52
 16  \w     71.00  97.00   0.50    1.31    --   20.00  54.00 -90.00   52
 17  \w    -29.00  -2.00   0.50    1.31    --   20.00  54.00  30.00   54
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0842199000
_diffrn_orient_matrix_UB_12      -0.0288313000
_diffrn_orient_matrix_UB_13      0.0237469000
_diffrn_orient_matrix_UB_21      0.0081274000
_diffrn_orient_matrix_UB_22      0.0488903000
_diffrn_orient_matrix_UB_23      0.0283574000
_diffrn_orient_matrix_UB_31      -0.0673057000
_diffrn_orient_matrix_UB_32      0.0163158000
_diffrn_orient_matrix_UB_33      -0.0318821000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19675
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.593
_diffrn_reflns_theta_min         1.696
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.40a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0995P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4818
_reflns_number_total             6879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02739_si_003.cif
_cod_data_source_block           190306_poz-pic
_cod_depositor_comments
;Adding full bibliography for 4134968--4134969.cif.

 Adding full bibliography for 4134968--4134969.cif.
;
_cod_database_code               4134969
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.14
_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:
 C6(H6), C20(H20), C4(H4), C3(H3), C23(H23), C33(H33), C21(H21), C37(H37),
 C22(H22), C27(H27), C13(H13), C36(H36), C29(H29), C31(H31), C35(H35), C10(H10),
  C34(H34), C30(H30), C12(H12), C28(H28), C11(H11)
;
_shelx_res_checksum              41497
_shelx_hkl_checksum              21508
_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 1.208
_oxdiff_exptl_absorpt_empirical_full_min 0.827