Six polyoxotungstate-based transition metal compounds for electrochemical capacitor application and a comparative analysis of factors affecting capacitances.
Peng, Cai-Hong; Li, Guanghua; Li, Ke-Chang; Cui, Xiao-Bing; Dalton transactions (Cambridge, England : 2003) 53 (2024) 3499–3510; doi:10.1039/d3dt04052f

data_7715014
_publ_section_title
;
 Six polyoxotungstate-based transition metal compounds for electrochemical
 capacitor application and a comparative analysis of factors affecting
 capacitances.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3499
_journal_page_last               3510
_journal_paper_doi               10.1039/d3dt04052f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'2(O40 P W12), 1.5(C54 H32 Cu3 N10 O11), 16.25(O)'
_chemical_formula_sum            'C81 H104.5 Cu4.5 N15 O112.75 P2 W24'
_chemical_formula_weight         7852.56
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-11-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-23 deposited with the CCDC.	2024-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   35.2928(4)
_cell_length_b                   35.2928(4)
_cell_length_c                   22.6516(7)
_cell_measurement_reflns_used    6508
_cell_measurement_temperature    260.0
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.52
_cell_volume                     24434.4(9)
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      260.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_unetI/netI     0.1164
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24355
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.367
_diffrn_reflns_theta_min         2.308
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    17.569
_exptl_absorpt_correction_T_max  0.016
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue-black
_exptl_crystal_density_diffrn    3.202
_exptl_crystal_description       Block
_exptl_crystal_F_000             21204
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         3.631
_refine_diff_density_min         -4.028
_refine_diff_density_rms         0.439
_refine_ls_extinction_coef       0.000023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         9895
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_gt           0.0891
_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^)+(0.1074P)^2^+5057.4058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2216
_refine_ls_wR_factor_ref         0.2724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5913
_reflns_number_total             9895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04052f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7715013--7715017.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C81 H104.50 Cu4.50 N15 O112.75 P2 W24'
_cod_database_code               7715014
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C111-C51
 1.4 with sigma of 0.02
 O2-P1
 1.65 with sigma of 0.02
 C13-C10 = C111-C112
 2.48 with sigma of 0.04
3. Rigid bond restraints
 C20, N19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O23) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O9W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O8W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq, Uanis(N61) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C112)
\\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(N54) \\sim Ueq,
Uanis(C111) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C58)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O19) \\sim Ueq, Uanis(O36) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(P10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O10W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1W) \\sim Ueq, Uanis(O7W) \\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(O20)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: Cu1(0.5) O19(0.5) O27(0.5) N54(0.5) C59(0.5) C58(0.5) C36(0.5)
 C49(0.5) C111(0.5) N61(0.5) C51(0.5) C112(0.5) C113(0.5) C114(0.5) C26(0.5)
 O20(0.5) O23(0.5) O2(0.166667) O34(0.5) O36(0.5) O1W(0.5) O3W(0.5)
 O6W(0.083333) O7W(0.5) O8W(0.5) O9W(0.5) O10W(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C8(H8), C31(H31), C10(H10), C29(H29), C22(H22), C28(H28), C12(H12),
 C18(H18), C15(H15), C23(H23), C25(H25), C20(H20), C21(H21), C16(H16), C7(H7)
6.b Fitted hexagon refined as free rotating group:
 N4(C11,C8,C31,C10,C6), N8(C13,C29,C22,C28,C12), N54(C59,C58,C36,C49,C111),
 N61(C51,C112,C113,C114,C26), C18(C14,C15,C23,N24,C25)
;
_shelx_res_checksum              74264
_olex2_submission_special_instructions 'No special instructions were received'