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_4330438
_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         'C32 H62 Mn2 N2 O4 Si4'
_chemical_formula_sum            'C32 H62 Mn2 N2 O4 Si4'
_chemical_formula_weight         761.08
_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                97.530(2)
_cell_angle_beta                 106.0430(10)
_cell_angle_gamma                107.005(2)
_cell_formula_units_Z            1
_cell_length_a                   8.8769(7)
_cell_length_b                   10.9042(8)
_cell_length_c                   12.3175(9)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0585
_cell_measurement_theta_min      2.6415
_cell_volume                     1066.23(14)
_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      293(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14471
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.9434
_exptl_absorpt_correction_T_min  0.7984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Estimated minimum and maximum transmission:  0.6204  0.7456
 The ratio of these values is more reliable than their absolute values!
 Additional spherical absorption correction applied with mu*r =  0.2000
 Lambda/2 correction factor = 0.0015 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       needle
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         5028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.5566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1089
_reflns_number_gt                3999
_reflns_number_total             5028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202448c_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4330438