Tuning the Formal Potential of Ferrocyanide over a 2.1 V Range
McNicholas, Brendon James; Grubbs, Robert H.; Winkler, Jay; Gray, Harry B.; Despagnet-Ayoub, Emmanuelle; Chemical Science  (2019) –; doi:10.1039/C8SC04972F

data_1550629
_publ_section_title
;
 Tuning the Formal Potential of Ferrocyanide over a 2.1 V Range
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04972F
_journal_year                    2019
_chemical_formula_sum            'C148.57 H175.16 B6 Cl5.16 Fe N10'
_chemical_formula_weight         2404.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-11-07 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5522(6)
_cell_length_b                   21.2914(7)
_cell_length_c                   35.9929(11)
_cell_measurement_reflns_used    9801
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.43
_cell_measurement_theta_min      2.46
_cell_volume                     13450.9(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX3 v2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1619
_diffrn_reflns_av_unetI/netI     0.0919
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            155470
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.493
_diffrn_reflns_theta_min         2.411
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.250
_exptl_absorpt_correction_T_max  0.5953
_exptl_absorpt_correction_T_min  0.4527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             5121
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
; 
 Flack x determined using 5356 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.392(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2341
_refine_ls_number_reflns         27477
_refine_ls_number_restraints     8929
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.1006
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1512P)^2^+15.9617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2528
_refine_ls_wR_factor_ref         0.2890
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                18248
_reflns_number_total             27477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04972f2.cif
_cod_data_source_block           P17026
_cod_database_code               1550629
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.662
_shelx_estimated_absorpt_t_max   0.896
_shelx_res_checksum              76901