Synthesis, crystallographic and spectroscopic characterization, and theoretical elucidation of an elusive aminyl radical containing a Cu<sup>II</sup>-aminyl-iminosemiquinone complex.
Sarkar, Prasenjit; Sarmah, Amrit; Mukherjee, Chandan; Chemical communications (Cambridge, England) 57 (2021) 1352–1355; doi:10.1039/d0cc07378d

data_7127641
_publ_section_title
;
 Synthesis, crystallographic and spectroscopic characterization, and
 theoretical elucidation of an elusive aminyl radical containing a
 Cu<sup>II</sup>-aminyl-iminosemiquinone complex.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1352
_journal_page_last               1355
_journal_paper_doi               10.1039/d0cc07378d
_journal_volume                  57
_journal_year                    2021
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C48 H57 Cu N4 O2, Cl O4'
_chemical_formula_sum            'C48 H57 Cl Cu N4 O6'
_chemical_formula_weight         884.97
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2020-07-11 deposited with the CCDC.	2020-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                63.174(6)
_cell_angle_beta                 76.983(5)
_cell_angle_gamma                82.077(4)
_cell_formula_units_Z            2
_cell_length_a                   11.1397(5)
_cell_length_b                   15.3727(9)
_cell_length_c                   15.8265(10)
_cell_measurement_reflns_used    15828
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.35
_cell_volume                     2354.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15964
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             934
_exptl_crystal_recrystallization_method 'dicholoromethane and methanol'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.117
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         8283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+3.0779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1512
_reflns_number_gt                7054
_reflns_number_total             8283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0cc07378d2.cif
_cod_data_source_block           platon_sqd
_cod_depositor_comments          'Adding full bibliography for 7127641.cif.'
_cod_original_cell_volume        2354.4(2)
_cod_database_code               7127641