Manganese(ii) complexes of hexaazatrinaphthylene and hexaazatrianthracene: synthesis, structure and properties
Mikhailenko, Maxim V.; Ivanov, Vladislav V.; Faraonov, Maxim A.; Kuzmin, Aleksey V.; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Konarev, Dmitri V.; New Journal of Chemistry 47 (2023) 22339–22349; doi:10.1039/D3NJ04615J

data_7062877
_publ_section_title
;
 Manganese(ii) complexes of hexaazatrinaphthylene and
 hexaazatrianthracene: synthesis, structure and properties
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              22339
_journal_page_last               22349
_journal_paper_doi               10.1039/D3NJ04615J
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety
'C24 H48 Mn3 N6 I6, 3(C18 H36 N2 K O6), 5(C6 H4 Cl2)'
_chemical_formula_sum            'C108 H140 Cl10 I6 K3 Mn3 N12 O18'
_chemical_formula_weight         3292.33
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2023-09-26 deposited with the CCDC.	2023-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                78.617(1)
_cell_angle_beta                 89.964(1)
_cell_angle_gamma                70.368(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8553(2)
_cell_length_b                   19.0211(3)
_cell_length_c                   27.1938(5)
_cell_measurement_reflns_used    41401
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      29.8030
_cell_measurement_theta_min      2.5000
_cell_volume                     6600.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      103(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            99123
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.022
_diffrn_reflns_theta_min         2.108
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.046
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       bulk
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.729
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.122
_refine_diff_density_max         3.847
_refine_diff_density_min         -3.373
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1612
_refine_ls_number_reflns         33961
_refine_ls_number_restraints     3001
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+38.8573P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25649
_reflns_number_total             33961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04615j2.cif
_cod_data_source_block           HATNA3MnI23CryptK
_cod_depositor_comments
'Adding full bibliography for 7062874--7062878.cif.'
_cod_database_code               7062877
_shelx_estimated_absorpt_t_min   0.317
_shelx_estimated_absorpt_t_max   0.788
_shelxl_version_number           2013-2
_shelx_res_checksum              67338
_shelx_hkl_checksum              90921