Fast Negative Photochromism of 1,1'-Binaphthyl-Bridged Phenoxyl-Imidazolyl Radical Complex.
Yamaguchi, Tetsuo; Kobayashi, Yoichi; Abe, Jiro; Journal of the American Chemical Society 138 (2016) 906–913; doi:10.1021/jacs.5b10924

data_4124872
_publ_section_title
;
 Fast Negative Photochromism of 1,1'-Binaphthyl-Bridged
 Phenoxyl-Imidazolyl Radical Complex.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              906
_journal_page_last               913
_journal_paper_doi               10.1021/jacs.5b10924
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C51 H45 N3 O'
_chemical_formula_weight         715.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                77.068(2)
_cell_angle_beta                 81.666(2)
_cell_angle_gamma                89.163(2)
_cell_formula_units_Z            4
_cell_length_a                   11.619(2)
_cell_length_b                   18.416(3)
_cell_length_c                   19.597(4)
_cell_measurement_reflns_used    750
_cell_measurement_temperature    90.0
_cell_measurement_theta_max      19.4157
_cell_measurement_theta_min      2.4620
_cell_volume                     4043.1(13)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker SMART APEXII'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruker AXS)'
_computing_publication_material  'Generate Report (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      90.0
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18592
_diffrn_reflns_theta_full        24.53
_diffrn_reflns_theta_max         24.53
_diffrn_reflns_theta_min         1.38
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         13266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+1.5277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                9968
_reflns_number_total             13266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10924_si_003.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4124871--4124873.cif.'
_cod_database_code               4124872
_shelx_res_checksum              54188
_shelx_hkl_checksum              90176