Oxygen Atom Transfer and Oxidative Water Incorporation in Cuboidal Mn3MOn Complexes Based on Synthetic, Isotopic Labeling, and Computational Studies
Jacob S. Kanady; Jose L. Mendoza-Cortes; Emily Y. Tsui; Robert J. Nielsen; William A. Goddard; Theodor Agapie; Journal of the American Chemical Society 135 (2013) 1073–1082; doi:10.1021/ja310022p

data_4119205
_publ_section_title
;
 Oxygen Atom Transfer and Oxidative Water Incorporation in Cuboidal Mn3MOn
 Complexes Based on Synthetic, Isotopic Labeling, and Computational
 Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1073
_journal_page_last               1082
_journal_paper_doi               10.1021/ja310022p
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C70 H61 F3 Mn3 N7 O17 S Sc'
_chemical_formula_weight         1571.10
_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                73.250(2)
_cell_angle_beta                 84.410(3)
_cell_angle_gamma                72.393(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7160(7)
_cell_length_b                   15.8986(7)
_cell_length_c                   16.3736(8)
_cell_measurement_reflns_used    9817
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.28
_cell_measurement_theta_min      2.42
_cell_volume                     3258.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            364399
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         43.86
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  0.8843
_exptl_absorpt_correction_T_min  0.7866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       trapezoidal
_exptl_crystal_F_000             1610
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.479
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         47053
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.270
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1220
_reflns_number_gt                32649
_reflns_number_total             47053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja310022p_si_002.cif
_cod_data_source_block           eyt115
_cod_database_code               4119205