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_4304045
_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         'C44 H30 Cl22 Mn4 N2 O18'
_chemical_formula_sum            'C44 H30 Cl22 Mn4 N2 O18'
_chemical_formula_weight         1874.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.8210(10)
_cell_angle_gamma                90.0000(10)
_cell_formula_units_Z            4
_cell_length_a                   14.2480(2)
_cell_length_b                   23.4740(3)
_cell_length_c                   21.1190(4)
_cell_measurement_reflns_used    171978
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     7062.68(19)
_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      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1169
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            94600
_diffrn_reflns_theta_full        25.22
_diffrn_reflns_theta_max         25.22
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.594
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         12709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1492
_refine_ls_R_factor_gt           0.0965
_refine_ls_shift/su_max          0.102
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1331P)^2^+24.7174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2472
_refine_ls_wR_factor_ref         0.2878
_reflns_number_gt                8104
_reflns_number_total             12709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7013368-file002_2.cif
_cod_data_source_block           complex2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4304045