Ground-State Copper(III) Stabilized by N-Confused/N-Linked Corroles: Synthesis, Characterization, and Redox Reactivity.
Maurya, Yogesh Kumar; Noda, Katsuya; Yamasumi, Kazuhisa; Mori, Shigeki; Uchiyama, Tomoki; Kamitani, Kazutaka; Hirai, Tomoyasu; Ninomiya, Kakeru; Nishibori, Maiko; Hori, Yuta; Shiota, Yoshihito; Yoshizawa, Kazunari; Ishida, Masatoshi; Furuta, Hiroyuki; Journal of the American Chemical Society 140 (2018) 6883–6892; doi:10.1021/jacs.8b01876

data_4132149
_publ_section_title
;
 Ground-State Copper(III) Stabilized by N-Confused/N-Linked Corroles:
 Synthesis, Characterization, and Redox Reactivity.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6883
_journal_page_last               6892
_journal_paper_doi               10.1021/jacs.8b01876
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C82 H36 Cu2 F30 N8 O2'
_chemical_formula_weight         1862.27
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                66.502(3)
_cell_angle_beta                 77.999(3)
_cell_angle_gamma                76.171(3)
_cell_formula_units_Z            2
_cell_length_a                   15.3803(4)
_cell_length_b                   16.8229(5)
_cell_length_c                   16.9418(5)
_cell_measurement_reflns_used    22789
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.36
_cell_measurement_theta_min      1.76
_cell_volume                     3872.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65703
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.741
_diffrn_source                   'Varimax 50 kV 24 mA Rotating anode'
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.966
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1181
_refine_ls_number_reflns         18654
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1100P)^2^+16.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12860
_reflns_number_total             18654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01876_si_004.cif
_cod_data_source_block           shelxl
_cod_database_code               4132149
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.980
_shelx_res_checksum              42468
_shelx_hkl_checksum              13443