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_7061181
_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         'C52 H62 Co Ge2 Mo24 N24 O80, 4(H2 O)'
_chemical_formula_sum            'C52 H70 Co Ge2 Mo24 N24 O84'
_chemical_formula_weight         4881.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc28n3ln
_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                90
_cell_angle_beta                 101.2500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4694(5)
_cell_length_b                   22.2327(9)
_cell_length_c                   21.1800(8)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.279
_cell_measurement_theta_min      2.476
_cell_volume                     5758.9(4)
_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 0.997
_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  0.0262
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.312
_diffrn_reflns_theta_min         1.342
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.286
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0537 before and 0.0289 after correction.
The Ratio of minimum to maximum transmission is 0.8345.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.815
_exptl_crystal_description       block
_exptl_crystal_F_000             4642
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         14293
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0222P)^2^+10.3461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12153
_reflns_number_total             14293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05316g2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7061181--7061184.cif.'
_cod_database_code               7061181
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.638
_shelx_estimated_absorpt_t_min   0.574
_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. Uiso/Uaniso restraints and constraints
N9: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(N9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N9, N11, N11A, N12, N12A, 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
4. Others
 Sof(N11A)=Sof(N12A)=Sof(H12A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12C)=
 Sof(C13A)=Sof(H13A)=Sof(O42A)=Sof(H42C)=Sof(H42D)=1-FVAR(1)
 Sof(N11)=Sof(N12)=Sof(H12)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12B)=Sof(C13)=
 Sof(H13)=Sof(O42)=Sof(H42A)=Sof(H42B)=FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10C)=
 Sof(H10D)=1-FVAR(2)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=FVAR(2)
5.a Riding coordinates:
 O41(H41A,H41B), O42(H42A,H42B), O42A(H42C,H42D)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C8A(H8AA,H8AB), C9(H9A,H9B), C9A(H9AA,H9AB), C10(H10A,H10B),
 C10A(H10C,H10D), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 N7(H7), N10(H10), N12(H12), N12A(H12A), C1(H1), C4(H4), C5(H5), C6(H6),
 C7(H7A), C11(H11), C11A(H11A), C12(H12B), C12A(H12C), C13(H13), C13A(H13A),
 C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C25(H25), C26(H26)
;
_shelx_res_checksum              13171
_olex2_submission_special_instructions 'No special instructions were received'