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_1550631
_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_moiety
'B6 C114 F90 Fe N6, 4(C36 H30 N P2), 5.25(C H2 Cl2)'
_chemical_formula_sum            'C263.25 H130.49 B6 Cl10.49 F90 Fe N10 P8'
_chemical_formula_weight         5883.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506),
 SHELXL-2017/1, and manual edit
;
_audit_update_record
;
2018-11-07 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                65.073(6)
_cell_angle_beta                 68.449(19)
_cell_angle_gamma                80.849(6)
_cell_formula_units_Z            1
_cell_length_a                   19.290(4)
_cell_length_b                   19.912(4)
_cell_length_c                   20.432(4)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.35
_cell_measurement_theta_min      2.5
_cell_volume                     6619(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker-AXS, 2016)'
_computing_data_collection
'BIS V6.2.6/2017-03-27 & APEX3_2017.3-0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker-AXS, 2016)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.69
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            158484
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.7
_diffrn_reflns_theta_max         70.4
_diffrn_reflns_theta_min         2.4
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.947
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1136 before and 0.0629 after correction. 
The Ratio of minimum to maximum transmission is 0.7413. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.628
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1839
_refine_ls_number_reflns         24649
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0743
_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^)+(0.1256P)^2^+8.9964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19024
_reflns_number_total             24649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04972f2.cif
_cod_data_source_block           v18101
_cod_database_code               1550631
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.577
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl3A-C57A \\sim Cl4A-C57A \\sim Cl3B-C57B \\sim Cl4B-C57B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl5, Cl6, C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, Cl2A, Cl2B, C56, Cl3A, Cl4A, C57A, Cl3B, Cl4B, C57B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H53A)=Sof(C51C)=Sof(H51C)=Sof(C52C)=Sof(H52C)=Sof(C54C)=Sof(H54C)=
 Sof(C55C)=Sof(H55C)=1-FVAR(1)
 Sof(H53B)=Sof(C51B)=Sof(H51B)=Sof(C52B)=Sof(H52B)=Sof(C54B)=Sof(H54B)=
 Sof(C55B)=Sof(H55B)=FVAR(1)
 Sof(Cl2B)=Sof(H56C)=Sof(H56D)=1-FVAR(2)
 Sof(Cl2A)=Sof(H56A)=Sof(H56B)=FVAR(2)
 Sof(Cl3A)=Sof(Cl4A)=Sof(C57A)=Sof(H57A)=Sof(H57B)=FVAR(3)
 Sof(Cl3B)=Sof(Cl4B)=Sof(C57B)=Sof(H57C)=Sof(H57D)=FVAR(4)
 Sof(Cl5)=Sof(Cl6)=Sof(C58)=Sof(H58A)=Sof(H58B)=FVAR(5)
5.a Secondary CH2 refined with riding coordinates:
 C56(H56C,H56D), C56(H56A,H56B), C57A(H57A,H57B), C58(H58A,H58B), C57B(H57C,
 H57D)
5.b Aromatic/amide H refined with riding coordinates:
 C21B(H21B), C22B(H22B), C23B(H23B), C24B(H24B), C25B(H25B), C27B(H27B),
 C28B(H28B), C29B(H29B), C30B(H30B), C31B(H31B), C33B(H33B), C34B(H34B),
 C35B(H35B), C36B(H36B), C37B(H37B), C39B(H39B), C40B(H40B), C41B(H41B),
 C42B(H42B), C43B(H43B), C45B(H45B), C46B(H46B), C47B(H47B), C48B(H48B),
 C49B(H49B), C53B(H53B), C53B(H53A), C51B(H51B), C52B(H52B), C54B(H54B),
 C55B(H55B), C51C(H51C), C52C(H52C), C54C(H54C), C55C(H55C), C21A(H21A),
 C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A), C27A(H27A), C28A(H28A),
 C29A(H29A), C30A(H30A), C31A(H31A), C33A(H33A), C34A(H34A), C35A(H35A),
 C36A(H36A), C37A(H37A), C39A(H39A), C40A(H40A), C41A(H41A), C42A(H42A),
 C43A(H43A), C45A(H45A), C46A(H46A), C47A(H47A), C48A(H48A), C49A(H49A),
 C51A(H51A), C52A(H52A), C53A(H53C), C54A(H54A), C55A(H55A)
;
_shelx_res_checksum              23938
_shelx_fab_checksum              54952
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'