Photochromic Carbazolyl-Imidazolyl Radical Complex
Kawanishi, Yasuki; Segawa, Yasutomo; Mutoh, Katsuya; Abe, Jiro; Kobayashi, Yoichi; Chemical Communications  (2022) –; doi:10.1039/D2CC01196D

data_7129889
_publ_section_title
;
 Photochromic Carbazolyl-Imidazolyl Radical Complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01196D
_journal_year                    2022
_chemical_formula_moiety         'C43 H33 N3, C H4 O'
_chemical_formula_sum            'C44 H37 N3 O'
_chemical_formula_weight         623.76
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-09 deposited with the CCDC.	2022-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                89.445(4)
_cell_angle_beta                 77.255(5)
_cell_angle_gamma                70.765(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8537(6)
_cell_length_b                   11.6155(3)
_cell_length_c                   15.5263(8)
_cell_measurement_reflns_used    8479
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      29.7770
_cell_measurement_theta_min      2.8980
_cell_volume                     1632.70(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.828
_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      2.00  35.00   0.50   25.14    --   12.51  37.00   0.00   66
  2  \w    -33.00  41.00   0.50   25.14    --  -11.26  32.00 -54.00  148
  3  \w    -67.00  12.00   0.50   25.14    --  -11.26 -57.00  90.00  158
  4  \w    -11.00  51.00   0.50   25.14    --   12.51 -99.00 120.00  124
  5  \w    -78.00   3.00   0.50   25.14    --  -11.26 -32.00 146.00  162
  6  \w    -83.00  18.00   0.50   25.14    --  -11.26 -77.00 -60.00  202
  7  \w      6.00  32.00   0.50   25.14    --   12.51 -99.00-180.00   52
  8  \w    -70.00 -45.00   0.50   25.14    --  -11.26-179.00 150.00   50
  9  \w    -89.00 -52.00   0.50   25.14    --  -11.26 179.00 -60.00   74
 10  \w     46.00  83.00   0.50   25.14    --   12.51 179.00 -30.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0114880000
_diffrn_orient_matrix_UB_12      -0.0551578000
_diffrn_orient_matrix_UB_13      0.0137085000
_diffrn_orient_matrix_UB_21      0.0673417000
_diffrn_orient_matrix_UB_22      -0.0183904000
_diffrn_orient_matrix_UB_23      0.0140501000
_diffrn_orient_matrix_UB_31      -0.0383542000
_diffrn_orient_matrix_UB_32      0.0286703000
_diffrn_orient_matrix_UB_33      0.0426471000
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26911
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         31.405
_diffrn_reflns_theta_min         2.696
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
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    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         8933
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0866P)^2^+0.3727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6192
_reflns_number_total             8933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01196d2.cif
_cod_data_source_block           CICtBuPh
_cod_database_code               7129889
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.989
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_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. Restrained distances
 H1-O1
 0.83 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C11(H11), C27(H27), C18(H18), C12(H12), C15(H15), C29(H29),
 C23(H23), C16(H16), C26(H26), C33(H33), C6(H6), C3(H3), C25(H25), C30(H30),
 C24(H24), C38(H38), C39(H39), C31(H31), C35(H35), C5(H5), C32(H32), C36(H36),
 C4(H4)
3.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C)
;
_shelx_res_checksum              93893
_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 1.345
_oxdiff_exptl_absorpt_empirical_full_min 0.734