Synthesis, Structure, and Magnetic Studies of Manganese-Oxygen Clusters of Reduced Coordination Number, Featuring an Unchelated, 5-Coordinate Octanuclear Manganese Cluster with Water-Derived Oxo Ligands
Sandeep K. Kondaveeti; Shivaiah Vaddypally; Carol Lam; Daigorou Hirai; Ni Ni; Robert J. Cava; Michael J. Zdilla; Inorganic Chemistry 51 (2012) 10095–10104; doi:10.1021/ic202448c

data_4330443
_publ_section_title
;
 Synthesis, Structure, and Magnetic Studies of Manganese-Oxygen Clusters
 of Reduced Coordination Number, Featuring an Unchelated, 5-Coordinate
 Octanuclear Manganese Cluster with Water-Derived Oxo Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10095
_journal_page_last               10104
_journal_paper_doi               10.1021/ic202448c
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C96 H108 Mn8 O20'
_chemical_formula_sum            'C96 H108 Mn8 O20'
_chemical_formula_weight         2021.34
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 129.425(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.479(3)
_cell_length_b                   45.599(6)
_cell_length_c                   20.072(3)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.509
_cell_measurement_theta_min      2.1825
_cell_volume                     18721(4)
_computing_cell_refinement       'Saint (Bruker-AXS)'
_computing_data_collection       'COSMO (Bruker-AXS)'
_computing_data_reduction        'SADABS (Bruker-AXS)'
_computing_molecular_graphics    XP
_computing_publication_material  'APEX II report generator (Bruker-AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Kappa APEX II DUO'
_diffrn_measurement_method       'Omega scans'
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59022
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    1.110
_exptl_absorpt_correction_T_max  0.5630
_exptl_absorpt_correction_T_min  0.4340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Documents\X-Ray\Shiva\246\work\mo_246_0m.hkl
 Estimated minimum and maximum transmission:  0.4340  0.5630
 The ratio of these values is more reliable than their absolute values!
 Additional spherical absorption correction applied with mu*r =  0.4000
 Lambda/2 correction factor = 0.0015
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       Block
_exptl_crystal_F_000             8352
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2348
_refine_ls_number_reflns         32503
_refine_ls_number_restraints     616
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.141
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+81.9822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                22258
_reflns_number_total             32503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202448c_si_002_6.cif
_cod_data_source_block           5
_cod_database_code               4330443