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_4314936
_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 N4 Ni O4'
_chemical_formula_weight         1009.94
_chemical_name_common            '[(tpe)Ni(py)][Li(thf)4]'
_chemical_properties_physical
'air-sensitive, moisture-sensitive, , oxygen-sensitive, paramagnetic'
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.16(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0737(17)
_cell_length_b                   22.273(3)
_cell_length_c                   19.323(5)
_cell_measurement_reflns_used    11608
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.99
_cell_measurement_theta_min      2.31
_cell_volume                     5618.1(18)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            78916
_diffrn_reflns_theta_full        27.31
_diffrn_reflns_theta_max         27.31
_diffrn_reflns_theta_min         1.40
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.395
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_correction_T_min  0.8181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            'translucent green'
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2168
_exptl_crystal_recrystallization_method 'hexanes and tetrahydrofuran'
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         12606
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0686P)^2^+1.8500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1429
_reflns_number_gt                8609
_reflns_number_total             12606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100028y_si_002_3.cif
_cod_data_source_block           gts004
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4314936