Five POM-based compounds modified by mono- and bis-triazole derivatives: photocatalytic, electrochemical and supercapacitor properties
Xu, Xi; Zhang, Yanping; Ying, Jun; Jin, Liang; Tian, Aixiang; Wang, Xiuli; CrystEngComm  (2022) –; doi:10.1039/D1CE01596F

data_7244135
_publ_section_title
;
 Five POM-based compounds modified by mono- and bis-triazole derivatives:
 photocatalytic, electrochemical and supercapacitor properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01596F
_journal_year                    2022
_chemical_formula_moiety         'O40 P W12, C60 H74 Cu6 N30 O48 P W12'
_chemical_formula_sum            'C60 H74 Cu6 N30 O88 P2 W24'
_chemical_formula_weight         7479.07
_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.cc28zkzt
_audit_creation_date             2021-08-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-09 deposited with the CCDC.	2022-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                78.479(2)
_cell_angle_beta                 89.827(2)
_cell_angle_gamma                76.701(2)
_cell_formula_units_Z            1
_cell_length_a                   12.4291(9)
_cell_length_b                   12.7620(10)
_cell_length_c                   25.4693(19)
_cell_measurement_reflns_used    3461
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      2.33
_cell_volume                     3848.5(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0933
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22269
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.067
_diffrn_reflns_theta_max         25.067
_diffrn_reflns_theta_min         0.817
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.773
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1164 before and 0.0367 after correction.
The Ratio of minimum to maximum transmission is 0.6617.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.227
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.257
_refine_diff_density_min         -2.749
_refine_diff_density_rms         0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         13648
_refine_ls_number_restraints     780
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0704P)^2^+23.4274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8498
_reflns_number_total             13648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01596f2.cif
_cod_data_source_block           2_CCDC3
_cod_database_code               7244135
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.6079
_shelx_estimated_absorpt_t_min   0.5568
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
C5: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
Uanis(O30) \\sim Ueq, Uanis(P2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(P2) \\sim Ueq, Uanis(O32) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C24) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O17) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(W10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: W1(0.5) O30(0.5) O32(0.5) O27(0.5) O31(0.5) O17(0.5) O16(0.5)
 O19(0.5) O20(0.5) W13(0.5)
4.a Riding coordinates:
 O46(H46A), O46(H46B), C11(H11)
4.b Rotating group:
 O48(H48A,H48B)
4.c Ternary CH refined with riding coordinates:
 O47(H47)
4.d Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C24(H24A,H24B), C6(H6A,H6B), C13(H13A,H13B), C3(H3A,H3B)
4.e Aromatic/amide H refined with riding coordinates:
 C23(H23), C4(H4), C14(H14), C16(H16), C21(H21), C15(H15), C5(H5), C8(H8),
 C26(H26), C20(H20), C17(H17), C10(H10), C27(H27), C30(H30), C2(H2), C9(H9),
 C1(H1), C29(H29), C22(H22)
4.f X=CH2 refined with riding coordinates:
 O45(H45A,H45B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              79496
_shelx_hkl_checksum              4159
_shelx_fab_checksum              29121
_olex2_submission_special_instructions 'No special instructions were received'