A series of POM compounds constructed using a flexible ligand containing three coordination groups: electrocatalytic and photocatalytic reduction and amperometric detection of Cr(vi)
Sun, Chenxi; Zhang, Yanping; Ying, Jun; Jin, Liang; Tian, Aixiang; Wang, Xiuli; New Journal of Chemistry 46 (2022) 2798–2807; doi:10.1039/D1NJ05316G

data_7061183
_publ_section_title
;
 A series of POM compounds constructed using a flexible ligand containing
 three coordination groups: electrocatalytic and photocatalytic reduction
 and amperometric detection of Cr(vi)
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2798
_journal_page_last               2807
_journal_paper_doi               10.1039/D1NJ05316G
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C26 H32 Co Mo4 N12 O14, Mo4 O13, 4(H2 O)'
_chemical_formula_sum            'C26 H40 Co Mo8 N12 O31'
_chemical_formula_weight         1843.15
_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.cc28v15c
_audit_creation_date             2021-12-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2021-12-08 deposited with the CCDC.	2022-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                73.018(2)
_cell_angle_beta                 72.311(2)
_cell_angle_gamma                89.9470(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0040(14)
_cell_length_b                   12.6182(14)
_cell_length_c                   18.381(2)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.348
_cell_measurement_theta_min      2.345
_cell_volume                     2525.0(5)
_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 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18710
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.348
_diffrn_reflns_theta_min         1.695
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0703 before and 0.0287 after correction.
The Ratio of minimum to maximum transmission is 0.7794.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.424
_exptl_crystal_description       block
_exptl_crystal_F_000             1782
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.471
_refine_diff_density_min         -2.191
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         12471
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0285P)^2^+15.5911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10812
_reflns_number_total             12471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05316g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7061181--7061184.cif.'
_cod_database_code               7061183
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.720
_shelx_estimated_absorpt_t_min   0.664
_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,H) groups
2. Restrained distances
 C21-C22 = C22-C23
 1.5 with sigma of 0.02
 C21-N9 = N9-C21A
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C21A) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C22A)
\\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N9, N11, N11A, N12, N12A, C21, C21A, C22, C22A, C23, C23A, C24, C24A, C25,
 C25A, C26, C26A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N11A)=Sof(H11A)=Sof(N12A)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=
 Sof(H22C)=Sof(H22D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=1-FVAR(1)
 Sof(N11)=Sof(N12)=Sof(H12)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=
 Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=
 Sof(C26)=Sof(H26)=FVAR(1)
 Sof(O30A)=Sof(H30C)=Sof(H30D)=1-FVAR(2)
 Sof(O30)=Sof(H30A)=Sof(H30B)=FVAR(2)
6.a Riding coordinates:
 O28(H28A,H28B), O29(H29A,H29B), O30A(H30C,H30D)
6.b Free rotating group:
 O27(H27A,H27B), O30(H30A,H30B)
6.c Rotating group:
 O1W(H1WA,H1WB)
6.d Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C21(H21A,H21B), C21A(H21C,H21D),
 C22(H22A,H22B), C22A(H22C,H22D), C23(H23A,H23B), C23A(H23C,H23D)
6.e Aromatic/amide H refined with riding coordinates:
 N10(H10), N11A(H11A), N12(H12), C1(H1), C2(H2), C3(H3), C7(H7), C10(H10A),
 C11(H11), C12(H12A), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19),
 C20(H20), C24(H24), C24A(H24A), C25(H25), C25A(H25A), C26(H26), C26A(H26A)
;
_shelx_res_checksum              13770
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'