Supramolecular Mn(II) and Mn(II)/Mn(III) Grid Complexes with [Mn9(μ2-O)12] Core Structures. Structural, Magnetic, and Redox Properties and Surface Studies
Liang Zhao; Zhiqiang Xu; Hilde Grove; Victoria A. Milway; Louise N. Dawe; Tareque S. M. Abedin; Laurence K. Thompson; Timothy L. Kelly; Rosemary G. Harvey; David O. Miller; Laura Weeks; Joseph G. Shapter; Kenneth J. Pope; Inorganic Chemistry 43 (2004) 3812–3824; doi:10.1021/ic030319v

data_4311141
_publ_section_title
;
 Supramolecular Mn(II) and Mn(II)/Mn(III) Grid Complexes with
 [Mn9(\m2-O)12] Core Structures. Structural, Magnetic, and Redox
 Properties and Surface Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3812
_journal_page_last               3824
_journal_paper_doi               10.1021/ic030319v
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C105 H127 Mn9 N71 O43'
_chemical_formula_weight         3566.24
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.7880(10)
_cell_angle_beta                 101.547(2)
_cell_angle_gamma                91.1250(10)
_cell_formula_units_Z            2
_cell_length_a                   18.1578(12)
_cell_length_b                   18.2887(12)
_cell_length_c                   26.7641(15)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.7
_cell_volume                     8353.6(9)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.1242
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            42722
_diffrn_reflns_theta_full        25.74
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  0.78658
_exptl_absorpt_correction_T_min  0.67553
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            'red / brown'
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3646
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.45
_refine_diff_density_max         1.668
_refine_diff_density_min         -1.317
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.301
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1856
_refine_ls_number_reflns         31487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.301
_refine_ls_R_factor_all          0.2259
_refine_ls_R_factor_gt           0.1342
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3757
_refine_ls_wR_factor_ref         0.4293
_reflns_number_gt                14527
_reflns_number_total             31487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030319v_3.cif
_cod_data_source_block           shelxl(3)
_cod_database_code               4311141