Coulombic Aggregations of MnIIIsalen-Type Complexes and Keggin-Type Polyoxometalates: Isolation of Mn2 Single-Molecule Magnets
Yuki Sawada; Wataru Kosaka; Yoshihito Hayashi; Hitoshi Miyasaka; Inorganic Chemistry 51 (2012) 4824–4832; doi:10.1021/ic300215q

data_4328984
_publ_section_title
;
 Coulombic Aggregations of MnIIIsalen-Type Complexes and Keggin-Type
 Polyoxometalates: Isolation of Mn2 Single-Molecule Magnets
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4824
_journal_page_last               4832
_journal_paper_doi               10.1021/ic300215q
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C64 H64 Mn4 N8 O52 Si W12'
_chemical_formula_sum            'C64 H64 Mn4 N8 O52 Si W12'
_chemical_formula_weight         4231.27
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                73.882(4)
_cell_angle_beta                 81.157(6)
_cell_angle_gamma                89.561(6)
_cell_formula_units_Z            1
_cell_length_a                   13.1100(11)
_cell_length_b                   15.9661(12)
_cell_length_c                   16.1721(10)
_cell_measurement_reflns_used    15295
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.14
_cell_volume                     3211.2(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35158
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.168
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_description       block
_exptl_crystal_F_000             1922.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         2.570
_refine_diff_density_min         -2.680
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  8295 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.230(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         22572
_refine_ls_number_restraints     487
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0333P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                20237
_reflns_number_total             22572
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic300215q_si_003.cif
_cod_data_source_block           SiKeggin_MnSalen
_cod_original_cell_volume        3211.2(5)
_cod_database_code               4328984