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_7715017
_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         'O40 P W12, 2(C36 H24 N6 Zn), 5(O)'
_chemical_formula_sum            'C72 H58 N12 O45 P W12 Zn2'
_chemical_formula_weight         4179.21
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-11-07
_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                105.088(3)
_cell_angle_beta                 90.564(3)
_cell_angle_gamma                97.682(3)
_cell_formula_units_Z            1
_cell_length_a                   12.0386(11)
_cell_length_b                   13.6743(12)
_cell_length_c                   14.7316(13)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.39
_cell_volume                     2318.0(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      200.00
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.987
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21389
_diffrn_reflns_point_group_measured_fraction_full 0.789
_diffrn_reflns_point_group_measured_fraction_max 0.784
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.417
_diffrn_reflns_theta_min         2.388
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    15.440
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.2892
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1323 before and 0.0734 after correction.
The Ratio of minimum to maximum transmission is 0.3881.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.994
_exptl_crystal_description       block
_exptl_crystal_F_000             1897
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.393
_refine_diff_density_min         -5.486
_refine_diff_density_rms         0.365
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(4)
_refine_ls_extinction_coef       0.00049(12)
_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   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1210
_refine_ls_number_reflns         13403
_refine_ls_number_restraints     552
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0664
_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^)+(0.0860P)^2^+88.6654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.1940
_reflns_Friedel_coverage         0.587
_reflns_Friedel_fraction_full    0.587
_reflns_Friedel_fraction_max     0.580
_reflns_number_gt                11173
_reflns_number_total             13403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04052f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7715013--7715017.cif.'
_cod_database_code               7715017
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(4)
 0.50(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C1-C39
 1.32 with sigma of 0.02
 C39-C24
 1.32 with sigma of 0.02
 C24-C103
 1.32 with sigma of 0.02
 C90-C93
 1.32 with sigma of 0.02
 C90-C27
 1.32 with sigma of 0.02
 C93-C22
 1.32 with sigma of 0.02
 C78-C31
 1.32 with sigma of 0.02
 C78-C80
 1.32 with sigma of 0.02
 C31-C14
 1.32 with sigma of 0.02
 C58-C4
 1.32 with sigma of 0.02
 C58-C37
 1.32 with sigma of 0.02
 C4-C36
 1.32 with sigma of 0.02
 O5-P12
 1.56 with sigma of 0.02
 P12-O12
 1.56 with sigma of 0.02
 O7-P12
 1.56 with sigma of 0.02
 C103-C39
 2.33 with sigma of 0.04
 C1-C24
 2.33 with sigma of 0.04
 C90-C22
 2.33 with sigma of 0.04
 C27-C93
 2.33 with sigma of 0.04
 C78-C14
 2.33 with sigma of 0.04
 C80-C31
 2.33 with sigma of 0.04
 C37-C4
 2.33 with sigma of 0.04
 C58-C36
 2.33 with sigma of 0.04
4. Rigid bond restraints
 P12, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, C58
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C37, C58
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C48, C59
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O5 \\sim P12: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O5 \\sim O17: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O5 \\sim O6: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O5 \\sim O7: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O5 \\sim O3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(O4W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O54) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O68) \\sim Ueq, Uanis(O36)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O28) \\sim Ueq, Uanis(O33) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O2) \\sim Ueq, Uanis(O64) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O26) \\sim Ueq, Uanis(O41) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O13) \\sim Ueq, Uanis(O69) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C1) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C66)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C82) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C65) \\sim Ueq,
Uanis(C90) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C82) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C45) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(N7) \\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C100) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C109)
\\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C78) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C19) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C101)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C17) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N17) \\sim Ueq, Uanis(C111) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C75) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C87) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C86) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C42) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C97) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C72) \\sim Ueq, Uanis(C76) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C93) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C58) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N23) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O35) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O20) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O17) \\sim Ueq: with
sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O32) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O31) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C16) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C57) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of
11 and sigma for terminal atoms of 22
Uanis(O52) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O30) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C13)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C57) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
6. Others
 Fixed Sof: O6(0.5) O1(0.5) O3(0.5) O4(0.5) O12(0.5) O17(0.5) O7(0.5) O5(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C42(H42), C2(H2), C18(H18), C15(H15), C116(H116), C100(H100), C89(H89),
 C111(H111), C75(H75), C66(H66), C136(H136), C117(H117), C132(H132), C120(H120),
  C97(H97), C57(H57), C82(H82), C128(H128), C35(H35), C65(H65), C74(H74),
 C78(H78), C86(H86), C90(H90), C93(H93), C101(H101), C45(H45), C3(H3), C16(H16),
  C17(H17), C24(H24), C26(H26), C31(H31), C39(H39), C58(H58), C4(H4), C5(H5),
 C59(H59), C48(H48), C19(H19), C7(H7), C6(H6), C10(H10), C9(H9), C109(H109),
 C126(H126), C41(H41), C47(H47)
7.b Fitted hexagon refined as free rotating group:
 N8(C44,C36,C42,C2,C18), N13(C61,C14,C15,C116,C100), N17(C89,C111,C75,C37,C43),
  N20(C66,C136,C117,C103,C87), N21(C72,C127,C132,C120,C97), N62(C82,C128,C35,
 C79,C76), C101(C45,C3,C22,C50,N12), N16(C5,C59,C48,C12,C11), N19(C33,C8,C19,C7,
 C6), N34(C109,C126,C41,C80,C13)
;
_shelx_res_checksum              62748
_olex2_submission_special_instructions 'No special instructions were received'