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_7133505
_publ_section_title
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 A stable radical within a N-Co-N core.
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_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
'2(C44 H44 Co N10), 2(F6 P), C H2 Cl2, 1[CH2Cl2], 0.5[H2O]'
_chemical_formula_sum            'C90 H93 Cl4 Co2 F12 N20 O0.5 P2'
_chemical_formula_weight         2012.44
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-20
_audit_creation_method
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Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
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2024-04-30 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                70.146(3)
_cell_angle_beta                 79.514(3)
_cell_angle_gamma                85.984(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0852(9)
_cell_length_b                   17.3585(14)
_cell_length_c                   22.5821(18)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      24.25
_cell_measurement_theta_min      2.29
_cell_volume                     4381.1(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            200742
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.280
_diffrn_reflns_theta_min         1.822
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6359
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1185 before and 0.0783 after correction.
The Ratio of minimum to maximum transmission is 0.8533.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       plate
_exptl_crystal_F_000             2074
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1206
_refine_ls_number_reflns         15776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.0800
_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^)+(0.0857P)^2^+23.7193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1947
_refine_ls_wR_factor_ref         0.2447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10580
_reflns_number_total             15776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02146k2.cif
_cod_data_source_block           ab453_0m
_cod_depositor_comments
'Adding full bibliography for 7133505--7133507.cif.'
_cod_original_formula_sum        'C90 H93 Cl4 Co2 F12 N20 O0.50 P2'
_cod_database_code               7133505
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.835
_olex2_refinement_description
;
1. Others
 Sof(Cl2)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(Cl1)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(C89)=Sof(H89A)=Sof(H89B)=FVAR(1)
 Fixed Sof: F14(0.75) F11(0.75) F7(0.75) F10(0.75) F12A(0.75) F8A(0.75)
 F9(0.75) F8(0.75)
2.a Secondary CH2 refined with riding coordinates:
 C89(H89A,H89B), C90(H90A,H90B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C39(H39), C38(H38), C19(H19), C3(H3), C74(H74), C34(H34), C11(H11),
 C61(H61), C33(H33), C31(H31), C20(H20), C77(H77), C5(H5), C9(H9), C27(H27),
 C24(H24), C17(H17), C60(H60), C42(H42), C75(H75), C25(H25), C16(H16), C69(H69),
  C8(H8), C50(H50), C52(H52), C71(H71), C82(H82), C72(H72), C41(H41), C47(H47),
 C49(H49), C63(H63), C86(H86), C64(H64), C55(H55), C83(H83), C53(H53), C85(H85)
2.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C22(H22A,H22B,H22C), C14(H14A,H14B,H14C), C66(H66A,H66B,
 H66C), C21(H21A,H21B,H21C), C43(H43A,H43B,H43C), C13(H13A,H13B,H13C), C65(H65A,
 H65B,H65C), C36(H36A,H36B,H36C), C87(H87A,H87B,H87C), C80(H80A,H80B,H80C),
 C35(H35A,H35B,H35C), C79(H79A,H79B,H79C), C57(H57A,H57B,H57C), C88(H88A,H88B,
 H88C), C58(H58A,H58B,H58C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 59 electrons were 
found in a volume of 157\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[CH2Cl2], 0.5[H2O] per Formula Unit 
which account for 94 electrons 
per unit cell.
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_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80332
_shelx_hkl_checksum              40742
_shelx_fab_checksum              84022
_olex2_submission_special_instructions 'No special instructions were received'