Stable radical versus reversible σ-bond formation of (porphyrinyl)dicyanomethyl radicals
Osuka, Atsuhiro; Shimizu, Daiki; Furukawa, Ko; Adinarayana, Bellamkonda; Chemical Science  (2019) –; doi:10.1039/C9SC01631G

data_1551031
_publ_section_title
;
 Stable radical versus reversible \s-bond formation of
 (porphyrinyl)dicyanomethyl radicals
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01631G
_journal_year                    2019
_chemical_formula_moiety         'C65 C71 Br N6 Ni, C H2 Cl2'
_chemical_formula_sum            'C66 H73 Br Cl2 N6 Ni'
_chemical_formula_weight         1159.82
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-03-04 deposited with the CCDC.    2019-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.698(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3078(7)
_cell_length_b                   21.1896(11)
_cell_length_c                   25.4949(17)
_cell_measurement_reflns_used    5101
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      73.1
_cell_measurement_theta_min      30.8
_cell_volume                     6002.6(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41753
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         73.333
_diffrn_reflns_theta_min         4.042
_exptl_absorpt_coefficient_mu    2.403
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2432
_refine_diff_density_max         1.751
_refine_diff_density_min         -2.455
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         11695
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0819
_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^)+(0.1874P)^2^+11.9820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2541
_refine_ls_wR_factor_ref         0.2591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10452
_reflns_number_total             11695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01631g2.cif
_cod_data_source_block           0306ad2
_cod_database_code               1551031
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              18992