Chemically Reversible Four-Electron Oxidation and Reduction Utilizing Two Inorganic Functional Groups
Michael Nippe; Samuel M. Goodman; Charles G. Fry; John F. Berry; Journal of the American Chemical Society 133 (2011) 2856–2859; doi:10.1021/ja1114248

data_4105715
_publ_contact_author_address
;Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John F. Berry'
_publ_contact_author_phone       809-608-262-7534
_publ_section_title
;
 Chemically Reversible Four-Electron Oxidation and Reduction Utilizing Two
 Inorganic Functional Groups
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2856
_journal_page_last               2859
_journal_paper_doi               10.1021/ja1114248
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
;
C40 H32 N12 W2 O, B C24 H20, O3 S C F3, C4 H10 O, C2 H3 n
;
_chemical_formula_sum            'C71 H65 B F3 N13 O5 S W2'
_chemical_formula_weight         1647.93
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.752(2)
_cell_angle_beta                 69.914(2)
_cell_angle_gamma                77.510(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0857(6)
_cell_length_b                   15.7157(6)
_cell_length_c                   16.9784(7)
_cell_measurement_reflns_used    9596
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.4163
_cell_measurement_theta_min      2.7499
_cell_volume                     3327.3(2)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL, OLEX2 (Dolomanov et al., 2009)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58447
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         6.81
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    3.556
_exptl_absorpt_correction_T_max  0.7713
_exptl_absorpt_correction_T_min  0.4468
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       block
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.614
_refine_diff_density_min         -3.191
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     880
_refine_ls_number_reflns         13355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0708P)^2^+20.5869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                12514
_reflns_number_total             13355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1114248_si_001_2.cif
_cod_data_source_block           2(OTf)(BPh4)
_cod_database_code               4105715