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_7249424
_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         'C26 H32 Cu2 Mo4 N8 O15, H2 O'
_chemical_formula_sum            'C26 H34 Cu2 Mo4 N8 O16'
_chemical_formula_weight         1225.45
_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             2023-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-11 deposited with the CCDC.	2024-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                95.939(2)
_cell_angle_beta                 109.007(2)
_cell_angle_gamma                112.422(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7451(7)
_cell_length_b                   12.7628(8)
_cell_length_c                   13.4678(7)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.73
_cell_volume                     1848.57(19)
_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 0.980
_diffrn_measured_fraction_theta_max 0.956
_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  0.0854
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            52521
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.330
_diffrn_reflns_theta_min         2.730
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.527
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5895
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1341 before and 0.0750 after correction.
The Ratio of minimum to maximum transmission is 0.7905.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    2.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         8814
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0361P)^2^+6.7241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5765
_reflns_number_total             8814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00897a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7249423--7249426.cif.'
_cod_original_cell_volume        1848.57(18)
_cod_database_code               7249424
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0005
3. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Free rotating group:
 O17(H17C,H17D)
4.b Ternary CH refined with riding coordinates:
 C15(H15), C9(H9)
4.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B), C17(H17A,H17B), C19(H19A,H19B), C5(H5A,H5B),
 C21(H21A,H21B), C11(H11A,H11B), C23(H23A,H23B), C3(H3A,H3B), C25(H25A,H25B)
4.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C12(H12), C16(H16), C24(H24), C26(H26), C13(H13), C7(H7),
 C2(H2)
;
_shelx_res_checksum              20731
_shelx_hkl_checksum              31675
_olex2_submission_special_instructions 'No special instructions were received'