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_1551032
_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_sum            'C66.5 H72 Cl5 N6 Ni'
_chemical_formula_weight         1191.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-03-23 deposited with the CCDC.    2019-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                76.353(4)
_cell_angle_beta                 82.030(3)
_cell_angle_gamma                78.350(3)
_cell_formula_units_Z            4
_cell_length_a                   14.2135(4)
_cell_length_b                   17.6443(8)
_cell_length_c                   26.4127(11)
_cell_measurement_temperature    93(2)
_cell_volume                     6275.5(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.950
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0900
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            85166
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.145
_diffrn_reflns_theta_min         1.729
_exptl_absorpt_coefficient_mu    2.742
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_refine_diff_density_max         4.197
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.420
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1506
_refine_ls_number_reflns         23864
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.421
_refine_ls_R_factor_all          0.1945
_refine_ls_R_factor_gt           0.1495
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3772
_refine_ls_wR_factor_ref         0.4111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14273
_reflns_number_total             23864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01631g2.cif
_cod_data_source_block           18032adi
_cod_depositor_comments
;

2019-08-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C133 H144 Cl10 N12 Ni2'
_cod_original_formula_weight         2382.51
_cod_original_formula_units_Z            2
_cod_database_code               1551032
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.684
_shelx_estimated_absorpt_t_max   0.947
_shelx_res_checksum              326