Structural and Spectroscopic Characterization of Metastable Thiolate-Ligated Manganese(III)-Alkylperoxo Species
Michael K. Coggins; Julie A. Kovacs; Journal of the American Chemical Society 133 (2011) 12470–12473; doi:10.1021/ja205520u

data_4106586
_publ_contact_author_address
;
Department of Chemistry
University of Washington
Seattle
Washington, 98195, USA
;
_publ_contact_author_email       kaminsky@chem.washington.edu
_publ_contact_author_fax         00(206)6858665
_publ_contact_author_name        'Werner Kaminsky'
_publ_contact_author_phone       00(206)5437585
_publ_section_title
;
 Structural and Spectroscopic Characterization of Metastable
 Thiolate-Ligated Manganese(III)-Alkylperoxo Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12470
_journal_page_last               12473
_journal_paper_doi               10.1021/ja205520u
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
'C36 H40 Mn N4 O2 S, C24 H20 B, C4 H10 O, C2 H3 N'
_chemical_formula_sum            'C66 H73 B Mn N5 O3 S'
_chemical_formula_weight         1082.1
_chemical_name_common            michael039
_chemical_name_systematic
;
 michael039
;
_space_group_IT_number           2
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_symmetry_Int_Tables_number      2
_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
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_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-05-17T13:42:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                69.84(2)
_cell_angle_beta                 83.47(2)
_cell_angle_gamma                78.29(2)
_cell_formula_units_Z            4
_cell_length_a                   15.098(5)
_cell_length_b                   20.289(7)
_cell_length_c                   20.645(7)
_cell_measurement_reflns_used    421
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     5806(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.4497
_diffrn_reflns_av_unetI/netI     0.7641
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52214
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         1.9
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.9906
_exptl_absorpt_correction_T_min  0.9845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       needle
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.59
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1404
_refine_ls_number_reflns         19485
_refine_ls_number_restraints     550
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.4381
_refine_ls_R_factor_gt           0.162
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3001
_refine_ls_wR_factor_ref         0.4441
_reflns_number_gt                4473
_reflns_number_total             19485
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja205520u_si_003.cif
_cod_data_source_block           michael039_0m
_cod_original_cell_volume        5806(3)
_cod_database_code               4106586