Crystal Structure of a Mixed-valent Hexanuclear Manganese Complex Made-up from Two Oxido-centered Triangular Mn<sup>II</sup>Mn<sup>III</sup><sub>2</sub> Cores
MIKURIYA, Masahiro; ONO, Sayuri; KOYAMA, Yoshiki; MITSUHASHI, Ryoji; TSUBOI, Motohiro; X-ray Structure Analysis Online 37 (2021) 41–43; doi:10.2116/xraystruct.37.41

data_1564541
_publ_section_title
;
 Crystal Structure of a Mixed-valent Hexanuclear Manganese Complex Made-up
 from Two Oxido-centered Triangular
 Mn&lt;sup&gt;II&lt;/sup&gt;Mn&lt;sup&gt;III&lt;/sup&gt;&lt;sub&gt;2&lt;/sub&gt;
 Cores
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              41
_journal_page_last               43
_journal_paper_doi               10.2116/xraystruct.37.41
_journal_volume                  37
_journal_year                    2021
_chemical_formula_moiety         'C82 H80 Mn6 N20 O34, 2.5(C4 H8 O), C H4 O'
_chemical_formula_sum            'C93 H104 Mn6 N20 O37.5'
_chemical_formula_weight         2431.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 93.147(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.253(3)
_cell_length_b                   16.630(2)
_cell_length_c                   29.508(4)
_cell_measurement_reflns_used    32541
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      1.681
_cell_volume                     10414(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1037
_diffrn_reflns_av_unetI/netI     0.1424
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            32541
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.681
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       needle
_exptl_crystal_F_000             5008
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         11924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1742
_refine_ls_R_factor_gt           0.0836
_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^)+(0.1101P)^2^+26.6592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2008
_refine_ls_wR_factor_ref         0.2500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6034
_reflns_number_total             11924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            37_41_1.txt
_cod_data_source_block           MnSO181_0m
_cod_original_cell_volume        10413(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C93 H104 Mn6 N20 O37.50'
_cod_database_code               1564541
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.730
_shelx_estimated_absorpt_t_max   0.896
_shelx_res_checksum              71069
_shelx_hkl_checksum              19509