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_4330439
_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         '[Mn2 Si4 N2 O2 C48 H62, 0], [C H2 Cl2, 0]'
_chemical_formula_sum            'C49 H64 Cl2 Mn2 N2 O2 Si4'
_chemical_formula_weight         1006.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.6810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.7255(14)
_cell_length_b                   12.6112(9)
_cell_length_c                   20.9188(15)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.9205
_cell_measurement_theta_min      2.624
_cell_volume                     5198.1(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0142
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41561
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

Estimated minimum and maximum transmission:  0.6424  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    1.286
_exptl_crystal_description       Block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         12434
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+3.1209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                10774
_reflns_number_total             12434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202448c_si_002_2.cif
_cod_data_source_block           2
_cod_database_code               4330439