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_7061415
_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_absolute_configuration ad
_chemical_formula_moiety         'C26 H51 Co Cr2 Mo12 N10 O51, 2(H2 O)'
_chemical_formula_sum            'C26 H55 Co Cr2 Mo12 N10 O53'
_chemical_formula_weight         2670.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc28r45c
_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                90
_cell_angle_beta                 110.347(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.751(3)
_cell_length_b                   25.890(6)
_cell_length_c                   19.146(3)
_cell_measurement_reflns_used    1668
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.442
_cell_measurement_theta_min      2.369
_cell_volume                     6856(2)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0727
_diffrn_reflns_av_unetI/netI     0.1235
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19539
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.573
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.767
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0687 before and 0.0473 after correction.
The Ratio of minimum to maximum transmission is 0.8119.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.587
_exptl_crystal_description       block
_exptl_crystal_F_000             5136
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.752
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.253
_refine_ls_abs_structure_details
;
 Flack x determined using 2555 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         11448
_refine_ls_number_restraints     1146
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0656
_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^)+(0.0776P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1699
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    0.894
_reflns_Friedel_fraction_max     0.894
_reflns_number_gt                7907
_reflns_number_total             11448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00674j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7061415--7061421.cif.'
_cod_database_code               7061415
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.698
_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(O48) \\sim Ueq, Uanis(O49) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Riding coordinates:
 O1W(H1WA,H1WB), O7(H7), O11(H11), O15(H15), O19(H19), O27(H27), O30(H30),
 O34(H34), O37(H37), O48(H48), O49(H49), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
4.b Ternary CH refined with riding coordinates:
 N5(H5), N10(H10)
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), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
  C20(H20A,H20B), C21(H21A,H21B)
4.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N7(H7A), C1(H1), C2(H2A), C3(H3), C4(H4A), C7(H7B), C14(H14),
 C22(H22), C24(H24), C25(H25), C26(H26)
;
_shelx_res_checksum              30038
_olex2_submission_special_instructions 'No special instructions were received'