Five Keggin-based compounds modified by bis- and mono-[1,3,4]triazole ligands: characterization, and selective photocatalytic and electrochemical properties
Zhang, Baoyue; Ying, Jun; Zhang, Xinyue; Wang, Chen; Tian, Aixiang; New Journal of Chemistry 44 (2020) 18074–18083; doi:10.1039/D0NJ03485A

data_7060006
_publ_section_title
;
 Five Keggin-based compounds modified by bis- and mono-[1,3,4]triazole
 ligands: characterization, and selective photocatalytic and
 electrochemical properties
;
_journal_issue                   41
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18074
_journal_page_last               18083
_journal_paper_doi               10.1039/D0NJ03485A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'O40 Si W12, 2.5(H2 O), C36 H40 Cu4 N12 O4'
_chemical_formula_sum            'C36 H45 Cu4 N12 O46.5 Si W12'
_chemical_formula_weight         3878.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-09-06 deposited with the CCDC.	2020-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.026(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.310(5)
_cell_length_b                   21.462(5)
_cell_length_c                   22.041(5)
_cell_measurement_reflns_used    4016
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      27.604
_cell_measurement_theta_min      2.545
_cell_volume                     7573(3)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_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      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0625
_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       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24223
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         1.587
_exptl_absorpt_coefficient_mu    19.354
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1351 before and 0.0385 after correction.
The Ratio of minimum to maximum transmission is 0.5009.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.402
_exptl_crystal_description       block
_exptl_crystal_F_000             6940
_refine_diff_density_max         2.250
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7826
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0516P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5618
_reflns_number_total             7826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03485a2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7060005--7060009.cif.'
_cod_original_formula_sum        'C36 H45 Cu4 N12 O46.50 Si W12'
_cod_database_code               7060006
_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 C(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C5-C1A = C1A-C2A
 1.4 with sigma of 0.02
 C5-C1 = C1-C2
 1.4 with sigma of 0.02
 H3-O3 = O2-H2
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C18A)
\\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(C15A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C2A)
\\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C12, C13, C13A, C14, C14A, C15, C15A, C16, C16A,
 C17, C17A, C18, C18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C1A, C2, C2A, C3, C3A, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H12C)=Sof(H12D)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=
 Sof(H18A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(C15A)=Sof(H15A)=1-FVAR(1)
 Sof(H12A)=Sof(H12B)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=
 Sof(C18)=Sof(H18)=Sof(C13)=Sof(C14)=Sof(H14)=FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(H5B)=1-FVAR(2)
 Sof(H5A)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2B)=Sof(C3)=Sof(H3B)=FVAR(2)
 Fixed Sof: O24(0.5) H24A(0.5) H24B(0.5) O1(0.75) H1B(0.75) H1C(0.75)
6.a Riding coordinates:
 O24(H24A,H24B), O2(H2), O3(H3), O1(H1B,H1C)
6.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C12(H12A,H12B), C12(H12C,H12D)
6.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C5(H5A), C5(H5B), C1(H1), C2(H2B), C3(H3B),
 C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16), C17(H17),
 C18(H18), C14(H14), C16A(H16A), C17A(H17A), C18A(H18A), C13A(H13A), C15A(H15A)
6.d Fitted hexagon refined as free rotating group:
 C5(C1,C2,C3,C6,C4), C15(C16,C17,C18,C13,C14), C16A(C17A,C18A,C13A,C14A,C15A)
;
_shelx_res_checksum              70046
_olex2_submission_special_instructions 'No special instructions were received'