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_7060008
_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 P W12, C30 H31 Cu N15, 3(H2 O)'
_chemical_formula_sum            'C30 H37 Cu N15 O43 P W12'
_chemical_formula_weight         3596.45
_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_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                98.765(2)
_cell_angle_beta                 95.235(2)
_cell_angle_gamma                110.197(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6599(10)
_cell_length_b                   14.1240(12)
_cell_length_c                   20.5224(18)
_cell_measurement_reflns_used    2369
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.81
_cell_volume                     3096.9(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17771
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.016
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.658
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1215 before and 0.0395 after correction.
The Ratio of minimum to maximum transmission is 0.6572.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.857
_exptl_crystal_description       block
_exptl_crystal_F_000             3196
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.089
_refine_diff_density_min         -1.707
_refine_diff_density_rms         0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         10862
_refine_ls_number_restraints     369
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7124
_reflns_number_total             10862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03485a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7060005--7060009.cif.'
_cod_database_code               7060008
_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
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O20) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O35) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(O43) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
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, C27, C28, C028, C29, N1, N2, N3,
 N4, N5, N6, N7, N8, N9, N10, N11, N12, N13, N14, N15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Riding coordinates:
 O41(H41A,H41B), O42(H42A,H42B), O43(H43A,H43B)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C10(H10A,H10B), C15(H15A,H15B), C20(H20A,H20B), C26(H26A,H26B)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1A), C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24),
  C25(H25), C28(H28), C028(H028), C29(H29)
;
_shelx_res_checksum              23351
_olex2_submission_special_instructions 'No special instructions were received'