A series of POM-based compounds by tuning coordination groups and spacers of ligands: electrocatalytic, capacitive and photoelectrocatalytic properties
Sun, Chenxi; Ying, Jun; Zhang, Yanping; Jin, Liang; Tian, Aixiang; Wang, Xiuli; CrystEngComm 24 (2022) 587–600; doi:10.1039/D1CE01419F

data_7244020
_publ_section_title
;
 A series of POM-based compounds by tuning coordination groups and spacers
 of ligands: electrocatalytic, capacitive and photoelectrocatalytic
 properties
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              587
_journal_page_last               600
_journal_paper_doi               10.1039/D1CE01419F
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety
'2(O40 Si W12), C52 H82 Cu N24 O40 Si W12, 8(H2 O)'
_chemical_formula_sum            'C52 H98 Cu N24 O128 Si3 W36'
_chemical_formula_weight         9873.95
_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   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc27sxml
_audit_creation_date             2021-11-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-11-30 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                71.143(4)
_cell_angle_beta                 87.189(4)
_cell_angle_gamma                84.839(4)
_cell_formula_units_Z            1
_cell_length_a                   14.767(3)
_cell_length_b                   16.296(3)
_cell_length_c                   18.365(3)
_cell_measurement_reflns_used    2069
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.361
_cell_measurement_theta_min      2.530
_cell_volume                     4164.3(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.1500
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23558
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.373
_diffrn_reflns_theta_min         1.795
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    24.997
_exptl_absorpt_correction_T_max  0.0289
_exptl_absorpt_correction_T_min  0.0069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1312 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.2388.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.937
_exptl_crystal_description       block
_exptl_crystal_F_000             4337
_refine_diff_density_max         3.424
_refine_diff_density_min         -2.894
_refine_diff_density_rms         0.539
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1246
_refine_ls_number_reflns         17696
_refine_ls_number_restraints     519
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1609
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1060P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.2351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9153
_reflns_number_total             17696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01419f2.cif
_cod_data_source_block           11221_0m
_cod_depositor_comments
'Adding full bibliography for 7244020--7244026.cif.'
_cod_original_cell_volume        4164.5(13)
_cod_database_code               7244020
_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, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O63) \\sim Ueq, Uanis(O68) \\sim Ueq, Uanis(O31)
\\sim Ueq, Uanis(O65) \\sim Ueq, Uanis(O33) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O59) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O29)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C20) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O11) \\sim Ueq, Uanis(O55) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O25) \\sim Ueq, Uanis(O25A) \\sim Ueq, Uanis(O51) \\sim Ueq, Uanis(O51A)
\\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(O67) \\sim Ueq,
Uanis(O67A) \\sim Ueq, Uanis(O13A) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O19A) \\sim Ueq, Uanis(O19) \\sim Ueq,
Uanis(O11A) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O43) \\sim Ueq, Uanis(O43A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O55A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O49) \\sim Ueq, Uanis(O49A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O45) \\sim Ueq, Uanis(O45A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, N1, N2, N3, N4, N5, N6, N7, N8,
 N9, N10, N11, N12, Cu1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O3(0.5) O3A(0.5) O5(0.5) O5A(0.5) O11(0.5) O11A(0.5) O13(0.5)
 O13A(0.5) O15(0.5) O19(0.5) O19A(0.5) O25(0.5) O25A(0.5) O27(0.5) O29(0.5)
 O43(0.5) O43A(0.5) O45(0.5) O45A(0.5) O49(0.5) O49A(0.5) O51(0.5) O51A(0.5)
 O55(0.5) O55A(0.5) O59(0.5) O67(0.5) O67A(0.5) O2(0.5) H2B(0.5) H2C(0.5)
 O33(0.5) H33A(0.5) H33B(0.5) O65(0.5) H65A(0.5) H65B(0.5) O68(0.5) H68A(0.5)
 H68B(0.5)
5.a Riding coordinates:
 O2(H2B,H2C), O31(H31A,H31B), O33(H33A,H33B), O63(H63A,H63B), O65(H65A,H65B),
 O68(H68A,H68B)
5.b Ternary CH refined with riding coordinates:
 N3(H3)
5.c Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), N9(H9A,H9B), C3(H3A,H3B), C4(H4A,H4B), C5(H5C,H5D), C7(H7A,H7B),
 C11(H11A,H11B), C13(H13A,H13B), C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B)
5.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N11(H11), C1(H1), C2(H2A), C6(H6), C9(H9), C10(H10), C12(H12),
 C15(H15), C18(H18), C20(H20), C25(H25)
;
_olex2_submission_special_instructions 'No special instructions were received'