Synthesis and Structural Characterization of a Series of MnIIIOR Complexes, Including a Water-Soluble MnIIIOH That Promotes Aerobic Hydrogen-Atom Transfer
Michael K. Coggins; Lisa M. Brines; Julie A. Kovacs; Inorganic Chemistry 52 (2013) 12383–12393; doi:10.1021/ic401234t

data_4336525
_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
;
 Synthesis and Structural Characterization of a Series of MnIIIOR
 Complexes, Including a Water-Soluble MnIIIOH That Promotes Aerobic
 Hydrogen-Atom Transfer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12383
_journal_page_last               12393
_journal_paper_doi               10.1021/ic401234t
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C17 H30 Mn N4 O S, C4 H10 O, F6 P, C2 H3 N'
_chemical_formula_sum            'C23 H43 F6 Mn N5 O2 P S'
_chemical_formula_weight         653.59
_chemical_name_common            michael043
_chemical_name_systematic
;
 michael043
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-05-24T11:57:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.872(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4834(3)
_cell_length_b                   16.4970(7)
_cell_length_c                   22.0354(9)
_cell_measurement_reflns_used    1191
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     3054.8(2)
_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 1
_diffrn_measured_fraction_theta_max 0.997
_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  0.0313
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            106880
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.55
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.9697
_exptl_absorpt_correction_T_min  0.8607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7668
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+1.5184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                6727
_reflns_number_total             7668
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic401234t_si_004.cif
_cod_data_source_block           michael043_0ma
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4336525