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_1547066
_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         'C213.35 H122.46 B3 Cl0.88 F60 N6 O7'
_chemical_formula_sum            'C213.35 H122.46 B3 Cl0.88 F60 N6 O7'
_chemical_formula_weight         4085.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.5040
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.3119
_cell_length_b                   24.2584
_cell_length_c                   46.9151
_cell_measurement_reflns_used    35864
_cell_measurement_temperature    93
_cell_measurement_theta_max      72.03
_cell_measurement_theta_min      2.91
_cell_volume                     18529.628
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.3'
_computing_publication_material  'CrystalStructure 4.2.3 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            99863
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         2.928
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            nONE
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8282.08
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.13
_refine_diff_density_min         -0.83
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     2673
_refine_ls_number_reflns         33817
_refine_ls_number_restraints     4878
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.1125
_refine_ls_shift/su_max          0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1572P)^2^+71.1287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3116
_refine_ls_wR_factor_ref         0.3219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28177
_reflns_number_total             33817
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol7b02088_si_002.cif
_cod_data_source_block           2atrication
_cod_original_cell_volume        18529.5821
_cod_database_code               1547066
_shelx_res_checksum              15872
_shelx_hkl_checksum              4711