A stable radical within a N-Co-N core.
Bhandari, Anirban; Park, Gyeong Min; Lee, Heui Beom; Hong, Sugyeong; Kim, Sun Hee; Byon, Hye Ryung; Lee, Yunho; Chemical communications (Cambridge, England) 60 (2024) 9970–9973; doi:10.1039/d4cc02146k

data_7133507
_publ_section_title
;
 A stable radical within a N-Co-N core.
;
_journal_issue                   73
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9970
_journal_page_last               9973
_journal_paper_doi               10.1039/d4cc02146k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C44 H44 Co N10, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C46 H47 Co F12 N11 P2'
_chemical_formula_weight         1102.81
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-07-01 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   41.229(2)
_cell_length_b                   41.229(2)
_cell_length_c                   20.2204(15)
_cell_measurement_reflns_used    9035
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      22.78
_cell_measurement_theta_min      2.29
_cell_volume                     29766(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0934
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            231144
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.353
_diffrn_reflns_theta_min         1.976
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5486
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1437 before and 0.0884 after correction.
The Ratio of minimum to maximum transmission is 0.7362.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       needle
_exptl_crystal_F_000             10170
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.063(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         12104
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0656P)^2^+81.8744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1282
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9804
_reflns_number_total             12104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02146k2.cif
_cod_data_source_block           ab80_3_0m
_cod_depositor_comments
'Adding full bibliography for 7133505--7133507.cif.'
_cod_original_cell_volume        29766(4)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7133507
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.834
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.937(19)
 0.063(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00L(H00L), C00P(H00P), C00S(H00S), C00T(H00T), C00U(H00U),
 C00W(H00W), C00X(H00X), C00Y(H00Y), C013(H013), C014(H014), C016(H016),
 C01A(H01A), C01B(H01B), C01D(H01D), C01G(H01G), C01N(H01Q), C01O(H01R),
 C01Q(H01V), C01R(H01W)
3.b Idealised Me refined as rotating group:
 C01H(H01C,H01E,H01F), C01J(H01H,H01I,H01J), C01K(H01K,H01L,H01M), C01L(H01N,
 H01O,H01P), C01P(H01S,H01T,H01U), C01S(H01X,H01Y,H), C01U(H01Z,HA,HB),
 C01V(H01,HC,HD), C01Y(H0AA,HE,HF)
;
_shelx_res_checksum              76613
_shelx_hkl_checksum              31801
_shelx_fab_checksum              56007
_olex2_submission_special_instructions 'No special instructions were received'