A Series of Peroxomanganese(III) Complexes Supported by Tetradentate Aminopyridyl Ligands: Detailed Spectroscopic and Computational Studies
Robert A. Geiger; Swarup Chattopadhyay; Victor W. Day; Timothy A. Jackson; Journal of the American Chemical Society 132 (2010) 2821–2831; doi:10.1021/ja910235g

data_4101975
_publ_section_title
;
 A Series of Peroxomanganese(III) Complexes Supported by Tetradentate
 Aminopyridyl Ligands: Detailed Spectroscopic and Computational Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2821
_journal_page_last               2831
_journal_paper_doi               10.1021/ja910235g
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C20 H26 Br2 Cl2 Mn N4 O9'
_chemical_formula_weight         752.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.5110(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8008(5)
_cell_length_b                   17.9804(10)
_cell_length_c                   15.1570(8)
_cell_measurement_reflns_used    6351
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.38
_cell_volume                     2653.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30806
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    3.767
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow-brown
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular parallelepiped'
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         7991
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0437P)^2^+0.9585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                6166
_reflns_number_total             7991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910235g_si_003.cif
_cod_data_source_block           Cmpd_1-Br_(k46g)
_cod_database_code               4101975