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_7249426
_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         'Mo12 O40 Si, C52 H72 N16 Ni2 O8, 2.5[H2O]'
_chemical_formula_sum            'C52 H77 Mo12 N16 Ni2 O50.5 Si'
_chemical_formula_weight         3031.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-04-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-17 deposited with the CCDC.	2024-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5205(4)
_cell_length_b                   15.3929(6)
_cell_length_c                   23.5897(8)
_cell_measurement_reflns_used    9643
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.18
_cell_volume                     4543.6(3)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0563
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            115231
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.176
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.115
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5915
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1131 before and 0.0669 after correction.
The Ratio of minimum to maximum transmission is 0.7932.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_description       block
_exptl_crystal_F_000             2958
_refine_diff_density_max         0.890
_refine_diff_density_min         -1.810
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         8006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+17.4281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7178
_reflns_number_total             8006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00897a2.cif
_cod_data_source_block           2_sq
_cod_depositor_comments
'Adding full bibliography for 7249423--7249426.cif.'
_cod_original_formula_sum        'C52 H77 Mo12 N16 Ni2 O50.50 Si'
_cod_database_code               7249426
_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
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O30(0.5) O17(0.5) O5(0.5) O28(0.5) O36(0.5) O33(0.5) O31(0.5)
 O35(0.5) O23(0.5) O25(0.5) O11(0.5) O27(0.5) O22(0.5) O9(0.5) O15(0.5) O3(0.5)
 O32(0.5) O7(0.5) O29(0.5) O34(0.5) O24(0.5) O19(0.5)
3.a Rotating group:
 O1(H1A,H1B), O4(H4A,H4B)
3.b Ternary CH refined with riding coordinates:
 C2(H2), C17(H17)
3.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C13(H13A,H13B), C9(H9A,H9B), C19(H19A,H19B), C5(H5A,H5B),
 C21(H21A,H21B), C11(H11A,H11B), C23(H23A,H23B), C3(H3A,H3B), C25(H25A,H25B)
3.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C12(H12), C14(H14), C20(H20), C22(H22), C24(H24), C26(H26),
 C7(H7), C15(H15)
;
_shelx_res_checksum              72610
_shelx_hkl_checksum              5786
_shelx_fab_checksum              1549
_platon_squeeze_special_details
;
A solvent mask was calculated and 54 electrons were 
found in a volume of 490\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
2.5[H2O] per Unit Cell 
which account for 50 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'