Mixed-Valence Tetra- and Hexanuclear Manganese Complexes from the Flexibility of Pyridine-Containing β-Diketone Ligands
Chen-I Yang; Wolfgang Wernsdorfer; Yu-Jhe Tsai; George Chung; Ting-Shen Kuo; Gene-Hsiang Lee; Minghuey Shieh; Hui-Lien Tsai; Inorganic Chemistry 47 (2008) 1925–1939; doi:10.1021/ic7013368

data_4304047
_publ_section_title
;
Mixed-Valence Tetra- and Hexanuclear Manganese Complexes from the
Flexibility of Pyridine-Containing \b-Diketone Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1925
_journal_page_last               1939
_journal_paper_doi               10.1021/ic7013368
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C103 H79 Cl4 Mn6 N3 O24'
_chemical_formula_sum            'C103 H79 Cl4 Mn6 N3 O24'
_chemical_formula_weight         2214.13
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.8750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9030(2)
_cell_length_b                   41.1760(5)
_cell_length_c                   17.3400(3)
_cell_measurement_reflns_used    142532
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      2.037
_cell_volume                     11247.5(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            71842
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.9441
_exptl_absorpt_correction_T_min  0.6682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            brown(dark)
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.820
_refine_diff_density_min         -1.259
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1241
_refine_ls_number_reflns         18653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1569P)^2^+34.1479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2321
_refine_ls_wR_factor_ref         0.2620
_reflns_number_gt                11861
_reflns_number_total             18653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7013368-file002_4.cif
_cod_data_source_block           complex4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4304047