A Redox-Active Heterocyclic Capsule: Radical Generation, Oxygenation, and Guest Uptake/Release.
Satoh, Yoshiyuki; Catti, Lorenzo; Akita, Munetaka; Yoshizawa, Michito; Journal of the American Chemical Society 141 (2019) 12268–12273; doi:10.1021/jacs.9b03419

data_4128654
_publ_contact_author             'Michito Yoshizawa'
_publ_section_title
;
 A Redox-Active Heterocyclic Capsule: Radical Generation, Oxygenation, and
 Guest Uptake/Release.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12268
_journal_page_last               12273
_journal_paper_doi               10.1021/jacs.9b03419
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C42 H47 Cl2 N5 O3 S2'
_chemical_formula_weight         804.86
_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
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                70.6230(10)
_cell_angle_beta                 88.7730(10)
_cell_angle_gamma                86.7690(10)
_cell_formula_units_Z            2
_cell_length_a                   11.3638(12)
_cell_length_b                   12.3409(13)
_cell_length_c                   15.7074(17)
_cell_measurement_reflns_used    8831
_cell_measurement_temperature    90
_cell_measurement_theta_max      29.06
_cell_measurement_theta_min      2.50
_cell_volume                     2074.7(4)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHELXle (Bruker AXS)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2016 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0096
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12549
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.065
_diffrn_reflns_theta_min         1.374
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         9624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+1.5820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8663
_reflns_number_total             9624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03419_si_002.cif
_cod_data_source_block           YST082
_cod_database_code               4128654
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              17289
_shelx_hkl_checksum              9126