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_4304046
_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         'C207 H170 Cl6 Mn12 N6 O52'
_chemical_formula_sum            'C207 H170 Cl6 Mn12 N6 O52'
_chemical_formula_weight         4445.47
_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                 98.11
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.20160(10)
_cell_length_b                   34.6578(3)
_cell_length_c                   17.6014(2)
_cell_measurement_reflns_used    73319
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     9784.55(15)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            69181
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.8874
_exptl_absorpt_correction_T_min  0.7869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            brown(dark)
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4544
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.012
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1282
_refine_ls_number_reflns         17548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          1.296
_refine_ls_shift/su_mean         0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+19.7377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1979
_refine_ls_wR_factor_ref         0.2401
_reflns_number_gt                11146
_reflns_number_total             17548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7013368-file002_3.cif
_cod_data_source_block           complex3
_cod_original_cell_volume        9784.53(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4304046