Electron Storage System Based on a Two-Way Inversion of Redox Potentials.
Gosset, Alexis; Wilbraham, Liam; Lachmanova, Stepanka Novakova; Sokolova, Romana; Dupeyre, Grégory; Tuyèras, Fabien; Ochsenbein, Philippe; Perruchot, Christian; Jacquot de Rouville, Henri-Pierre; Randriamahazaka, Hyacinthe; Pospisil, Lubomir; Ciofini, Ilaria; Hromadová, Magdaléna; Lainé, Philippe P; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b12762

data_4134368
_publ_section_title
;
 Electron Storage System Based on a Two-Way Inversion of Redox Potentials.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12762
_journal_year                    2020
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C22 H20 N2, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C24 H23 F12 N3 P2'
_chemical_formula_weight         646.4
_chemical_name_common
'1,8-di(N-methylpyrid-4-ylium)naphthalene hexafluorophosphate'
_chemical_name_systematic
'1,8-di(N-methylpyrid-4-ylium)naphthalene hexafluorophosphate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             'Aug 16 17:10:25 2016'
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.9293(13)
_cell_length_b                   10.4396(5)
_cell_length_c                   18.2519(8)
_cell_measurement_reflns_used    973
_cell_measurement_temperature    113(1)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4.5
_cell_volume                     5321.7(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'SHELXP-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      113(1)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Instrument Service v2011.8.1.0'
_diffrn_measurement_method       '\p and \w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            82493
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.178
_diffrn_reflns_theta_min         1.458
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       Block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.643
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 8600 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.074(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.672
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         20221
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.672
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0700P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1538
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                18587
_reflns_number_total             20221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12762_si_003.cif
_cod_data_source_block           xea
_cod_depositor_comments
;

2020-03-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C22 H20 N2), 4(F6 P), 2(C2 H3 N)'
_cod_original_formula_sum        'C48 H46 F24 N6 P4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1292.8
_cod_database_code               4134368
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.974
_shelxl_version_number           2013-2
_shelx_res_checksum              1790
_shelx_hkl_checksum              27044