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_7061184
_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 Mo4 N12 Ni O14, Mo4 O13, 4(H2 O)'
_chemical_formula_sum            'C26 H40 Mo8 N12 Ni O31'
_chemical_formula_weight         1842.93
_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.cc28v33c
_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                106.9050(10)
_cell_angle_beta                 107.5780(10)
_cell_angle_gamma                89.9400(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9807(3)
_cell_length_b                   12.6328(4)
_cell_length_c                   18.3167(5)
_cell_measurement_reflns_used    9231
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.384
_cell_measurement_theta_min      2.342
_cell_volume                     2517.12(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.0148
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18885
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.383
_diffrn_reflns_theta_min         1.692
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    2.395
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0460 before and 0.0241 after correction.
The Ratio of minimum to maximum transmission is 0.8859.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.432
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.764
_refine_diff_density_min         -1.550
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         12519
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0255P)^2^+3.7058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10755
_reflns_number_total             12519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05316g2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7061181--7061184.cif.'
_cod_original_cell_volume        2517.11(12)
_cod_database_code               7061184
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.659
_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
 N7A-C13A = C13A-N6A
 1.4 with sigma of 0.02
 C10A-C9A = C9A-C8A
 1.5 with sigma of 0.02
 C12A-N6A
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C10A)
\\sim Ueq, Uanis(N6A) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C12A) \\sim Ueq,
Uanis(N7A) \\sim Ueq, Uanis(C13A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N3, N6, N6A, N7, N7A, C8, C8A, C9, C9A, C10, C10A, C11, C11A, C12, C12A, C13,
 C13A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10C)=
 Sof(H10D)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=FVAR(1)
 Sof(N6A)=Sof(H6A)=Sof(N7A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=
 Sof(H13A)=1-FVAR(2)
 Sof(N6)=Sof(H6)=Sof(N7)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=
 FVAR(2)
 Sof(O30A)=Sof(H30C)=Sof(H30D)=1-FVAR(3)
 Sof(O30)=Sof(H30A)=Sof(H30B)=FVAR(3)
6.a Riding coordinates:
 O28(H28A,H28B), O29(H29A,H29B)
6.b Free rotating group:
 O27(H27A,H27B), O30(H30A,H30B), O30A(H30C,H30D)
6.c Rotating group:
 O1W(H1WA,H1WB)
6.d Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C8A(H8AA,H8AB), C9(H9A,H9B), C9A(H9AA,H9AB), C10(H10A,H10B),
 C10A(H10C,H10D), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
6.e Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), N6A(H6A), C1(H1), C2(H2), C4(H4), C5(H5A), C7(H7), C11(H11),
 C11A(H11A), C12(H12), C12A(H12A), C13(H13), C13A(H13A), C14(H14), C15(H15),
 C16(H16), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26)
;
_shelx_res_checksum              31997
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'