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_7062878
_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
'2(C18 H36 N2 O6), 2(C6 H4 Cl2), C6 H14, C54 H51 N6 O12 Mn3'
_chemical_formula_sum            'C108 H148 Cl4 K2 Mn3 N10 O24'
_chemical_formula_weight         2355.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 105.726(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5169(7)
_cell_length_b                   30.5496(12)
_cell_length_c                   24.4406(10)
_cell_measurement_reflns_used    9270
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.5590
_cell_measurement_theta_min      2.3780
_cell_volume                     11870.7(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    WinGx
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(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 0.881
_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  0.1177
_diffrn_reflns_av_unetI/netI     0.2193
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            89751
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.398
_diffrn_reflns_theta_min         2.179
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89701
_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            grey
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       plate
_exptl_crystal_F_000             4956
_exptl_crystal_size_max          0.445
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1338
_refine_ls_number_reflns         28876
_refine_ls_number_restraints     528
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.2361
_refine_ls_R_factor_gt           0.0875
_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^)+(0.0886P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11115
_reflns_number_total             28876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04615j2.cif
_cod_data_source_block           HATNA3Mnacac22CryptK
_cod_depositor_comments
'Adding full bibliography for 7062874--7062878.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7062878
_shelx_estimated_absorpt_t_min   0.793
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2013-2
_shelx_res_checksum              79504
_shelx_hkl_checksum              15337