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_7060009
_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         'Mo12 O40 P, C20 H25 Cu N8, H2 O'
_chemical_formula_sum            'C20 H27 Cu Mo12 N8 O41 P'
_chemical_formula_weight         2281.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/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                 109.3380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9377(9)
_cell_length_b                   15.5396(8)
_cell_length_c                   21.5233(12)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.343
_cell_measurement_theta_min      2.336
_cell_volume                     5029.8(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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35829
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.359
_diffrn_reflns_theta_min         1.354
_exptl_absorpt_coefficient_mu    3.446
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4357
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.013
_exptl_crystal_description       block
_exptl_crystal_F_000             4316
_refine_diff_density_max         0.698
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         12562
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0196P)^2^+15.4553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10978
_reflns_number_total             12562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03485a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7060005--7060009.cif.'
_cod_database_code               7060009
_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,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H1WB-O34_$1
 2.4 with sigma of 0.02
 H1WA-O14_$2
 2.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O17 \\sim O17A \\sim O22 \\sim O22A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(O17) \\sim Ueq, Uanis(O17A) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O22A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: O17(0.5) O17A(0.5) O22(0.5) O22A(0.5) H1A(0.83333) H1B(0.83333)
 H1C(0.83333) H8A(0.83333) H8B(0.83333) H8C(0.83333)
5.a Free rotating group:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C13(H13A,H13B), C20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18)
5.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N8(H8A,H8B,H8C)
;
_shelx_res_checksum              37062
_olex2_submission_special_instructions 'No special instructions were received'