Further Insight into the Manganese(II) 2,2′-Bipyridine-1,1′-dioxide Homoleptic Complex: Single-Crystal X-ray Structure Determination of the Perchlorate Salt and DFT Calculations
Castro, Jesús; Ferraro, Valentina; Bortoluzzi, Marco; Crystals 14 (2024) 422–; doi:10.3390/cryst14050422

data_1571551
_publ_section_title
;
 Further Insight into the Manganese(II)
 2,2&#x2032;-Bipyridine-1,1&#x2032;-dioxide Homoleptic Complex:
 Single-Crystal X-ray Structure Determination of the Perchlorate Salt and
 DFT Calculations
;
_journal_issue                   5
_journal_name_full               Crystals
_journal_page_first              422
_journal_paper_doi               10.3390/cryst14050422
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C30 H24 Mn N6 O6, 2(Cl O4), 1.3333(H2 O)'
_chemical_formula_sum            'C30 H26.66667 Cl2 Mn N6 O15.33333'
_chemical_formula_weight         842.41
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 90.517(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   21.266(2)
_cell_length_b                   19.1361(16)
_cell_length_c                   25.447(2)
_cell_measurement_reflns_used    9653
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.33
_cell_volume                     10355.2(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HeliosTM multilayer optics'
_diffrn_radiation_source         'Incoatec high brillance I\muS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            591875
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.407
_diffrn_reflns_theta_min         1.915
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.7144
_exptl_absorpt_correction_T_min  0.6299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       prism
_exptl_crystal_F_000             5164
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.095
_refine_diff_density_max         1.685
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1483
_refine_ls_number_reflns         25850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0574P)^2^+24.3352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22753
_reflns_number_total             25850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MnBipyO2_ClO4.cif
_cod_data_source_block           '_CCDC_2260009'
_cod_depositor_comments
;

2025-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C90 H80 Cl6 Mn3 N18 O46'
_cod_original_formula_weight         2527.24
_cod_original_formula_moiety         '3(C30 H24 Mn N6 O6), 6(Cl O4), 4(H2 O)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        10355.0(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1571551
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.879
_shelx_estimated_absorpt_t_max   0.943
_shelx_res_checksum              26807
_shelx_hkl_checksum              38597