An electrically conductive metallocycle: densely packed molecular hexagons with π-stacked radicals
Cui, Mengxing; Murase, Ryuichi; Shen, Yongbing; Sato, Tetsu; Koyama, Shohei; Uchida, Kaiji; Tanabe, Tappei; Takaishi, Shinya; Yamashita, Masahiro; Iguchi, Hiroaki; Chemical Science  (2022) –; doi:10.1039/D2SC00447J

data_1566782
_publ_section_title
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 An electrically conductive metallocycle: densely packed molecular
 hexagons with \p-stacked radicals
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00447J
_journal_year                    2022
_chemical_formula_moiety         'C168 H168 N54 Ni6 O54, 5.046(C4 H9 N O)'
_chemical_formula_sum            'C188.19 H213.43 N59.05 Ni6 O59.05'
_chemical_formula_weight         4599.64
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-09 deposited with the CCDC.	2022-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   45.980(2)
_cell_length_b                   45.980(2)
_cell_length_c                   9.5196(7)
_cell_measurement_reflns_used    3252
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.5940
_cell_measurement_theta_min      2.3230
_cell_volume                     17429.6(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    Sir2019
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.829
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0896
_diffrn_reflns_av_unetI/netI     0.2050
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.829
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21975
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.614
_diffrn_reflns_theta_min         2.344
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       needle
_exptl_crystal_F_000             7189
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         9025
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.2263
_refine_ls_R_factor_gt           0.0992
_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^)+(0.1022P)^2^+199.1361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2428
_refine_ls_wR_factor_ref         0.2908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3964
_reflns_number_total             9025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00447j2.cif
_cod_data_source_block           PMC-hexagon
_cod_original_cell_volume        17430(2)
_cod_database_code               1566782
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.989
_oxdiff_exptl_absorpt_empirical_full_min 0.849
_oxdiff_exptl_absorpt_empirical_full_max 1.238
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              38007
_shelx_hkl_checksum              82046
_shelx_fab_checksum              31022