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_4105714
_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         'W2 O1 (C10 H8 N3)4, 2 I3, 2 CH2Cl2'
_chemical_formula_sum            'C41 H34 Cl2 I6.02 N12 O0.98 W2'
_chemical_formula_weight         1912.70
_chemical_name_systematic
; 
 ? 
;
_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                101.2720(10)
_cell_angle_beta                 92.9690(10)
_cell_angle_gamma                94.350(2)
_cell_formula_units_Z            4
_cell_length_a                   16.3610(5)
_cell_length_b                   16.8722(6)
_cell_length_c                   19.1403(6)
_cell_measurement_reflns_used    9314
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.6985
_cell_measurement_theta_min      2.8871
_cell_volume                     5154.8(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            227729
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    8.212
_exptl_absorpt_correction_T_max  0.4793
_exptl_absorpt_correction_T_min  0.3308
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            borwn
_exptl_crystal_density_diffrn    2.465
_exptl_crystal_description       block
_exptl_crystal_F_000             3491
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.214
_refine_diff_density_min         -1.998
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1209
_refine_ls_number_reflns         30005
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+16.3183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0565
_reflns_number_gt                27849
_reflns_number_total             30005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1114248_si_001_1.cif
_cod_data_source_block           2(I3)2
_cod_database_code               4105714