Isolable Triradical Trication of Hexaaza[16]paracyclophane with Embedded 9,10-Anthrylenes: A Frustrated Three-Spin System.
Kurata, Ryohei; Sakamaki, Daisuke; Uebe, Masashi; Kinoshita, Mariko; Iwanaga, Tetsuo; Matsumoto, Takashi; Ito, Akihiro; Organic letters 19 (2017) 4371–4374; doi:10.1021/acs.orglett.7b02088

data_1547064
_publ_section_title
;
 Isolable Triradical Trication of Hexaaza[16]paracyclophane with Embedded
 9,10-Anthrylenes: A Frustrated Three-Spin System.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              4371
_journal_page_last               4374
_journal_paper_doi               10.1021/acs.orglett.7b02088
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C102.5 H75.5 Cl12.75 N6'
_chemical_formula_sum            'C102.5 H75.5 Cl12.75 N6'
_chemical_formula_weight         1843.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.828(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   24.334(5)
_cell_length_b                   13.557(3)
_cell_length_c                   27.189(5)
_cell_measurement_reflns_used    10849
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.01
_cell_volume                     8969(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, ????)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 5.0rc6'
_computing_publication_material  'CrystalStructure 5.0rc6 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 28.571
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1675
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            70435
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         3.005
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3797.00
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.65
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1195
_refine_ls_number_reflns         20132
_refine_ls_number_restraints     136
_refine_ls_R_factor_all          0.2403
_refine_ls_R_factor_gt           0.1257
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1530P)^2^+9.4927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2926
_refine_ls_wR_factor_ref         0.3692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8559
_reflns_number_total             20132
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol7b02088_si_003.cif
_cod_data_source_block           2b
_cod_database_code               1547064
_shelx_res_checksum              56441
_shelx_hkl_checksum              7724