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_7715013
_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, C50 H39 Cl2 Cu5 N10 O10 P2, 2(O)'
_chemical_formula_sum            'C50 H49 Cl2 Cu5 N10 O52 P3 W12'
_chemical_formula_weight         4309.70
_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             2023-10-10
_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                88.0280(10)
_cell_angle_beta                 84.1660(10)
_cell_angle_gamma                80.5840(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9802(5)
_cell_length_b                   12.7843(5)
_cell_length_c                   15.3506(7)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    299.00
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.42
_cell_volume                     2114.44(16)
_computing_cell_refinement       'Bruker SMART'
_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)'
_diffrn_ambient_temperature      299.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Smart-CCD diffractometer'
_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  0.0599
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19273
_diffrn_reflns_point_group_measured_fraction_full 0.781
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.379
_diffrn_reflns_theta_min         2.416
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    17.696
_exptl_absorpt_correction_T_max  0.155
_exptl_absorpt_correction_T_min  0.107
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.385
_exptl_crystal_description       block
_exptl_crystal_F_000             1947
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.247
_refine_diff_density_min         -3.561
_refine_diff_density_rms         0.423
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(2)
_refine_ls_extinction_coef       0.00050(15)
_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   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1089
_refine_ls_number_reflns         12131
_refine_ls_number_restraints     409
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0628P)^2^+48.0248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1564
_reflns_Friedel_coverage         0.579
_reflns_Friedel_fraction_full    0.575
_reflns_Friedel_fraction_max     0.571
_reflns_number_gt                10916
_reflns_number_total             12131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04052f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7715013--7715017.cif.'
_cod_database_code               7715013
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(2)
 0.51(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid bond restraints
 C48, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43, C44
 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(C43) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C19)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C9) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C34) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C7)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O44) \\sim Ueq, Uanis(O46) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N2) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O37) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O39)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O26) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O40) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O13) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C17)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O33) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O32) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O22) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C33) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N3) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C18) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C47) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O43) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O14)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O36) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O50) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(O42) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O34) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O42) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O47) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),
  C41(H41), C42(H42), C43(H43), C44(H44), C1(H1), C2(H2), C3(H3), C4(H4),
 C17(H17), C18(H18), C19(H19), C20(H20), C31(H31), C32(H32), C33(H33), C34(H34),
  C37(H37), C38(H38), C39(H39), C40(H40), C49(H49), C50(H50), C48(H48)
5.b Fitted hexagon refined as free rotating group:
 N2(C6,C7,C8,C9,C10), N3(C11,C12,C13,C14,C15), N5(C21,C22,C23,C24,C25), N6(C26,
 C27,C28,C29,C30), N9(C41,C42,C43,C44,C45), C5(N1,C1,C2,C3,C4), C17(C18,C19,C20,
 N4,C16), C35(N7,C31,C32,C33,C34), C36(C37,C38,C39,C40,N8), C49(C50,N10,C46,C47,
 C48)
;
_shelx_res_checksum              81296
_olex2_submission_special_instructions 'No special instructions were received'