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_7715015
_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         'C48 H36 N8 O42 Si W12 Zn2, 2(O)'
_chemical_formula_sum            'C48 H40 N8 O44 Si W12 Zn2'
_chemical_formula_weight         3797.91
_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             2023-10-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-07 deposited with the CCDC.	2024-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                83.241(2)
_cell_angle_beta                 84.184(2)
_cell_angle_gamma                65.508(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2370(9)
_cell_length_b                   14.0325(10)
_cell_length_c                   22.9061(15)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.49
_cell_volume                     3548.5(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      298.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_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  0.0563
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33027
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.429
_diffrn_reflns_theta_min         2.302
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    20.143
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.2479
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1434 before and 0.0803 after correction.
The Ratio of minimum to maximum transmission is 0.3327.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.554
_exptl_crystal_description       block
_exptl_crystal_F_000             3396
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.029
_refine_diff_density_min         -6.109
_refine_diff_density_rms         0.544
_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     1036
_refine_ls_number_reflns         12921
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0863P)^2^+48.4563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11640
_reflns_number_total             12921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04052f2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7715013--7715017.cif.'
_cod_database_code               7715015
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O12) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(Si28) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O61) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C68) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C49) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C66) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15), C17(H17),
 C21(H21), C22(H22), C24(H24), C25(H25), C28(H28), C30(H30), C31(H31), C32(H32),
  C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C49(H49), C52(H52),
 C54(H54), C58(H58), C66(H66), C68(H68), C69(H69), C71(H71), C72(H72), C74(H74),
  C79(H79)
3.b X=CH2 refined with riding coordinates:
 O42(H42A,H42B), O57(H57A,H57B)
;
_shelx_res_checksum              92142
_olex2_submission_special_instructions 'No special instructions were received'