A series of polyoxometalate compounds: syntheses, characterization, electrochemical sensing and photocatalytic properties
Gong, Yuan; Liu, Tao; Tian, Aixiang; Ying, Jun; Yang, Mengle; CrystEngComm 26 (2024) 6155–6160; doi:10.1039/D4CE00897A

data_7249425
_publ_section_title
;
 A series of polyoxometalate compounds: syntheses, characterization,
 electrochemical sensing and photocatalytic properties
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6155
_journal_page_last               6160
_journal_paper_doi               10.1039/D4CE00897A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'2(Mo12 O40 Si), 2(C26 H40 Cu N8 O5), 7.5(H2 O)'
_chemical_formula_sum            'C52 H95 Cu2 Mo24 N16 O97.5 Si2'
_chemical_formula_weight         4990.25
_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     iterative
_audit_creation_date             2024-06-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-10 deposited with the CCDC.	2024-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                89.2190(10)
_cell_angle_beta                 83.5790(10)
_cell_angle_gamma                62.0770(10)
_cell_formula_units_Z            1
_cell_length_a                   12.5392(3)
_cell_length_b                   13.1412(3)
_cell_length_c                   21.0778(5)
_cell_measurement_reflns_used    9242
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.52
_cell_measurement_theta_min      2.52
_cell_volume                     3046.62(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_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  0.0792
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            75398
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.986
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.860
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6055
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1351 before and 0.0938 after correction.
The Ratio of minimum to maximum transmission is 0.8120.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    2.720
_exptl_crystal_description       block
_exptl_crystal_F_000             2393
_refine_diff_density_max         1.937
_refine_diff_density_min         -1.539
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     984
_refine_ls_number_reflns         11914
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0680
_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^)+53.0968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1450
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9539
_reflns_number_total             11914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00897a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7249423--7249426.cif.'
_cod_original_cell_volume        3046.63(13)
_cod_original_formula_sum        'C52 H95 Cu2 Mo24 N16 O97.50 Si2'
_cod_database_code               7249425
_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) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C11-H11A
 1.14 with sigma of 0.02
 H11B-C11
 1.12 with sigma of 0.02
 Cu1-H3WA \\sim Cu1-H3WB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O49)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(O50) \\sim Ueq, Uanis(O27)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O54) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O35)
\\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O53) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Mo8(0.5) O54(0.5) O33(0.5) O56(0.5) O53(0.5) O19(0.5) O43(0.5)
 O11(0.5) O45(0.5) O57(0.5) O47(0.5) O3(0.5) O25(0.5) O51(0.5) O7(0.5) Mo3(0.5)
 O39(0.5) O52(0.5) O55(0.5) O21(0.5) O23(0.5) O38(0.5) C25(0.5) H25A(0.5)
 H25B(0.5) C27(0.5) H27A(0.5) H27B(0.5)
5.a Free rotating group:
 O3W(H3WA,H3WB), O17(H17A,H17B), O1(H1A,H1B)
5.b Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
5.c Ternary CH refined with riding coordinates:
 C22(H22), C5(H5)
5.d Secondary CH2 refined with riding coordinates:
 N29(H29A,H29B), C18(H18A,H18B), C24(H24A,H24B), C26(H26A,H26B), C7(H7A,H7B),
 C19(H19A,H19B), C21(H21A,H21B), C23(H23A,H23B), C3(H3A,H3B), C25(H25A,H25B),
 C27(H27A,H27B)
5.e Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C12(H12), C14(H14), C16(H16), C13(H13), C15(H15), C2(H2),
 C17(H17), C9(H9)
;
_shelx_res_checksum              15291
_shelx_hkl_checksum              97102
_shelx_fab_checksum              15498
_platon_squeeze_special_details
;
A solvent mask was calculated and 36 electrons were 
found in a volume of 97\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3.5[H2O] per Unit Cell 
which account for 35 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'