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_4330440
_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         Mn4O4C44H43
_chemical_formula_sum            'C44 H43 Mn O4'
_chemical_formula_weight         690.72
_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                97.956(8)
_cell_angle_beta                 91.959(9)
_cell_angle_gamma                111.792(9)
_cell_formula_units_Z            2
_cell_length_a                   9.419(4)
_cell_length_b                   12.287(6)
_cell_length_c                   16.220(7)
_cell_measurement_reflns_used    3024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.84
_cell_measurement_theta_min      2.339
_cell_volume                     1718.7(13)
_computing_cell_refinement       'Saint (Bruker-AXS)'
_computing_data_collection       'COSMO (Bruker-AXS)'
_computing_data_reduction        'TWINABS (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      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8060
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.745619
_exptl_absorpt_correction_T_min  0.614602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Rint = 0.0484  for all   18065  observations and
 Rint = 0.0356  for all    7952  observations with I > 3sigma(I)

 Rint is based on agreement between observed single and composite intensities
 and those calculated from refined unique intensities and twin fractions.

    8197 Corrected reflections written to file
 Reflections merged according to point-group -1    
 Minimum and maximum apparent transmission:  0.614602  0.745619
 Additional spherical absorption correction applied with mu*r =  0.2000

 HKLF 5 dataset constructed from all observations involving domain 1
   12156 Corrected reflections written to file twin5.hkl
 Reflections merged according to point-group -1    
 Single reflections that also occur in composites omitted
 Minimum and maximum apparent transmission:  0.610200  0.745619
 Additional spherical absorption correction applied with mu*r =  0.2000
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       Block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         8060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                5457
_reflns_number_total             8060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202448c_si_002_3.cif
_cod_data_source_block           3a
_cod_database_code               4330440