A series of polyoxometalate compounds by tuning N sites and numbers of ligands: syntheses, characterization and electrochemical sensing, and photocatalytic and supercapacitor properties
Jin, Liang; Ying, Jun; Zhang, Yanping; Sun, Chenxi; Tian, Aixiang; Wang, Xiuli; New Journal of Chemistry 46 (2022) 8422–8432; doi:10.1039/D2NJ00674J

data_7061416
_publ_section_title
;
 A series of polyoxometalate compounds by tuning N sites and numbers of
 ligands: syntheses, characterization and electrochemical sensing, and
 photocatalytic and supercapacitor properties
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8422
_journal_page_last               8432
_journal_paper_doi               10.1039/D2NJ00674J
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C13 H26 Cr Mo6 N5 Ni O26, 4.5(H2 O)'
_chemical_formula_sum            'C13 H35 Cr Mo6 N5 Ni O30.5'
_chemical_formula_weight         1435.81
_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_block_doi                 10.5517/ccdc.csd.cc28wgtg
_audit_creation_date             2022-03-19
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-03-25 deposited with the CCDC.	2022-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                104.7480(10)
_cell_angle_beta                 117.5640(10)
_cell_angle_gamma                92.4810(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5532(5)
_cell_length_b                   13.0752(5)
_cell_length_c                   13.5524(6)
_cell_measurement_reflns_used    4695
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.277
_cell_measurement_theta_min      2.328
_cell_volume                     1873.01(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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  0.0211
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13874
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.842
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.820
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0485 before and 0.0283 after correction.
The Ratio of minimum to maximum transmission is 0.8835.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.546
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_refine_diff_density_max         1.469
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         9216
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+2.0840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7070
_reflns_number_total             9216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00674j2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7061415--7061421.cif.'
_cod_original_formula_sum        'C13 H35 Cr Mo6 N5 Ni O30.50'
_cod_database_code               7061416
_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) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O6W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O5W(0.5) H5WA(0.5) H5WB(0.5) O6W(0.5) H6WA(0.5) H6WB(0.5) O7W(0.5)
 H7WA(0.5) H7WB(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O6(H6), O7(H7), O8(H8), O21(H21), O22(H22), O23(H23),
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB),
  O7W(H7WA,H7WB)
4.b Ternary CH refined with riding coordinates:
 N5(H5)
4.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7A)
;
_shelx_res_checksum              83053
_olex2_submission_special_instructions 'No special instructions were received'