Ligand-Centered Redox Activity: Redox Properties of 3d Transition Metal Ions Ligated by the Weak-Field Tris(pyrrolyl)ethane Trianion
Graham T. Sazama; Theodore A. Betley; Inorganic Chemistry 49 (2010) 2512–2524; doi:10.1021/ic100028y

data_4314937
_publ_contact_author_address
;Department of Chemistry and Chemical Biology
Harvard University
Mallinckrodt 306E
12 Oxford Street
Cambridge, MA 02139
;
_publ_contact_author_email       betley@chemistry.harvard.edu
_publ_contact_author_name        'Theodore A. Betley'
_publ_contact_author_phone       617-496-9944
_publ_section_title
;
 Ligand-Centered Redox Activity: Redox Properties of 3d Transition Metal
 Ions Ligated by the Weak-Field Tris(pyrrolyl)ethane Trianion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2512
_journal_page_last               2524
_journal_paper_doi               10.1021/ic100028y
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'chemical synthesis'
_chemical_formula_sum            'C62 H79 Li Mn N4 O4'
_chemical_formula_weight         1006.17
_chemical_name_common            '[(tpe)Mn(py)][Li(thf)4]'
_chemical_properties_physical
'air-sensitive, moisture-sensitive, oxygen-sensitive, paramagnetic'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.5460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.6178(9)
_cell_length_b                   16.7236(8)
_cell_length_c                   38.7477(18)
_cell_measurement_reflns_used    15424
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.24
_cell_volume                     11776.3(10)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'SMART V5.625 (Bruker AXS, 2001a)'
_computing_data_reduction
; 
SAINT V7.34A (Bruker AXS, 2006), SADABS (Bruker AXS, 2004) 
;
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001b)'
_computing_publication_material  'SHELXTL v6.12 (Bruker AXS, 2001b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex I CCD'
_diffrn_measurement_method       'omega scans 0.3%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            53543
_diffrn_reflns_theta_full        26.66
_diffrn_reflns_theta_max         26.66
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_correction_T_min  0.9016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            'translucent yellow'
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4312
_exptl_crystal_recrystallization_method 'diethyl ether and tetrahydrofuran'
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_platon_squeeze_details          ' '
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.050
_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     722
_refine_ls_number_reflns         12398
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+5.3310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1597
_reflns_number_gt                9762
_reflns_number_total             12398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100028y_si_002_4.cif
_cod_data_source_block           gts006
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4314937