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_4314934
_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 H83 Fe Li N4 O4'
_chemical_formula_weight         1011.11
_chemical_name_common            '[(tpe)Fe(py)][Li(thf)2(Et2O)2]'
_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                 102.561(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.4776(12)
_cell_length_b                   15.5448(10)
_cell_length_c                   38.314(2)
_cell_measurement_reflns_used    5033
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.4740
_cell_measurement_theta_min      2.5091
_cell_volume                     11322.9(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            49291
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.69
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  0.9752
_exptl_absorpt_correction_T_min  0.9425
_exptl_crystal_colour            'translucent orange'
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4352
_exptl_crystal_recrystallization_method 'diethyl ether and tetrahydrofuran'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         12980
_refine_ls_number_restraints     559
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+3.1103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1691
_reflns_number_gt                7084
_reflns_number_total             12980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100028y_si_002_1.cif
_cod_data_source_block           gts002
_cod_original_cell_volume        11322.8(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4314934