Exploring the Roles of Counterions in Redox-active Viologen on Electrochromic Performance
Parashar, Ranjeev Kumar; Kandpal, Suchita; Kamal, Aditya; Bansal, Love; Gupta, Kirti; Kumar, Rajesh; Mondal, Prakash Chandra; Physical Chemistry Chemical Physics  (2025) –; doi:10.1039/D5CP02803E

data_7251242
_publ_section_title
;
 Exploring the Roles of Counterions in Redox-active Viologen on
 Electrochromic Performance
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D5CP02803E
_journal_year                    2025
_chemical_formula_moiety
'C24 H20 Cl2 N2, Cl O4, Cl1.066 O4.131, 0.73(O)'
_chemical_formula_sum            'C24 H20 Cl4.07 N2 O8.87'
_chemical_formula_weight         622.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-01-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2024-01-31 deposited with the CCDC.	2025-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                76.180(3)
_cell_angle_beta                 86.065(2)
_cell_angle_gamma                60.771(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2172(3)
_cell_length_b                   9.4319(5)
_cell_length_c                   17.5200(6)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.40
_cell_volume                     1288.63(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28661
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         2.398
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1305 before and 0.0630 after correction.
The Ratio of minimum to maximum transmission is 0.9181.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         4549
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0721
_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^)+(0.0970P)^2^+4.4701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1984
_refine_ls_wR_factor_ref         0.2051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3925
_reflns_number_total             4549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cp02803e2.cif
_cod_data_source_block           26deca_b
_cod_database_code               7251242
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl00-O00L \\sim Cl-O00L
 with sigma of 0.02
 Cl00-O1 \\sim Cl-O1A
 with sigma of 0.02
 Cl00-O00Z \\sim Cl-O0
 with sigma of 0.02
 Cl00-O011 \\sim Cl-O2
 with sigma of 0.02
 O00L-O1 \\sim O00L-O1A
 with sigma of 0.04
 O00L-O00Z \\sim O00L-O0
 with sigma of 0.04
 O00L-O011 \\sim O00L-O2
 with sigma of 0.04
 O1-O00Z \\sim O1A-O0
 with sigma of 0.04
 O1-O011 \\sim O1A-O2
 with sigma of 0.04
 O00Z-O011 \\sim O0-O2
 with sigma of 0.04
 O00O-O00P \\sim O010-O012
 with sigma of 0.04
 Cl3-O00O \\sim Cl3-O00P \\sim Cl3-O010 \\sim Cl3-O012
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl, O1A, O2, O0
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O00Z, Cl00, O011, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl4, Cl3, O00O, O00P, O010, O012, O3, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O0)=Sof(O1A)=Sof(O2)=Sof(Cl)=Sof(Cl4)=Sof(O3)=Sof(O6)=1-FVAR(1)
 Sof(Cl00)=Sof(O1)=Sof(O00Z)=Sof(O011)=FVAR(1)
 Sof(Cl3)=Sof(O010)=Sof(O012)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C21(H21), C16(H16), C17(H17), C20(H20), C14(H14), C23(H23),
 C24(H24), C3(H3), C9(H9), C10(H10), C2(H2), C8(H8), C7(H7), C4(H4), C5(H5)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'