Anion-Controlled Assembly of Four Manganese Ions: Structural, Magnetic, and Electrochemical Properties of Tetramanganese Complexes Stabilized by Xanthene-Bridged Schiff Base Ligands
Masakazu Hirotsu; Yuu Shimizu; Naoto Kuwamura; Rika Tanaka; Isamu Kinoshita; Ryoichi Takada; Yoshio Teki; Hideki Hashimoto; Inorganic Chemistry 51 (2012) 766–768; doi:10.1021/ic202287k

data_4328041
_publ_section_title
;
 Anion-Controlled Assembly of Four Manganese Ions: Structural, Magnetic,
 and Electrochemical Properties of Tetramanganese Complexes Stabilized by
 Xanthene-Bridged Schiff Base Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              766
_journal_page_last               768
_journal_paper_doi               10.1021/ic202287k
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C74 H70 Mn4 N4 O14, 4(C H2 Cl2), 2(C3 H8 O)'
_chemical_formula_sum            'C84 H94 Cl8 Mn4 N4 O16'
_chemical_formula_weight         1918.99
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_author_name               'Tanaka, R.'
_audit_creation_date             2011-04-22
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.483(11)
_cell_angle_beta                 70.914(12)
_cell_angle_gamma                83.701(15)
_cell_formula_units_Z            1
_cell_length_a                   12.384(2)
_cell_length_b                   13.3307(19)
_cell_length_c                   15.2393(14)
_cell_measurement_reflns_used    7233
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0112
_cell_volume                     2162.2(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -80.0000 - 100.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 35.0574
              2theta: 9.9748
scan:
    Number of images: 100
               Slice: -30.0000 - 20.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 35.0574
              2theta: 9.9748
scan:
    Number of images: 100
               Slice: -30.0000 - 20.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 35.0574
              2theta: 9.9748
scan:
    Number of images: 100
               Slice: -30.0000 - 20.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 35.0574
              2theta: 9.9748

;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w or \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21110
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.01
_diffrn_source_current           150.0000
_diffrn_source_power             7.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  0.9407
_exptl_absorpt_correction_T_min  0.7355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       Prism
_exptl_crystal_F_000             990
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.496
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         9306
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+5.4777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1728
_reflns_number_gt                7100
_reflns_number_total             9306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202287k_si_002_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        2162.2(5)
_cod_database_code               4328041