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_7061182
_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
'C13 H30 Mo6.167 N6 Ni2 O31.5 Te, 2.5(H2 O), 1[H2O]'
_chemical_formula_sum            'C13 H37 Mo6.17 N6 Ni2 O35 Te'
_chemical_formula_weight         1674.45
_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.cc28qbp1
_audit_creation_date             2021-12-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2021-12-24 deposited with the CCDC.	2022-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.778(2)
_cell_angle_beta                 96.280(2)
_cell_angle_gamma                112.573(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2559(9)
_cell_length_b                   10.2674(11)
_cell_length_c                   27.104(3)
_cell_measurement_reflns_used    8187
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.176
_cell_measurement_theta_min      2.692
_cell_volume                     2104.9(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 0.975
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            12289
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         0.757
_exptl_absorpt_coefficient_mu    3.443
_exptl_absorpt_correction_T_max  0.2627
_exptl_absorpt_correction_T_min  0.1938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0710 before and 0.0285 after correction.
The Ratio of minimum to maximum transmission is 0.7377.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.642
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.434
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         7631
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0586P)^2^+28.3513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6857
_reflns_number_total             7631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05316g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7061181--7061184.cif.'
_cod_database_code               7061182
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.626
_shelx_estimated_absorpt_t_min   0.561
_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
Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O25) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(O28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O28A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 O26, N4, N5, N6, C8, C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Mo7(0.16667) O25(0.5) H25A(0.5) H25B(0.5) O28(0.5) H28A(0.5)
 H28B(0.5) O28A(0.5) H28C(0.5) H28D(0.5) O29(0.5) H29A(0.5) H29B(0.5)
5.a Riding coordinates:
 O2W(H2WA,H2WB), O5W(H5WA,H5WB), O6W(H6W,H6WA), O25(H25A,H25B), O26(H26A,H26B),
  O28(H28A,H28B), O28A(H28C,H28D), O29(H29A,H29B)
5.b Free rotating group:
 O27(H27A,H27B)
5.c Rotating group:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
5.d Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
5.e Aromatic/amide H refined with riding coordinates:
 N6(H6), C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 24 electrons were 
found in a volume of 92\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[H2O] per Asymmetric Unit 
which account for 20 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              28841
_shelx_fab_checksum              20424
_olex2_submission_special_instructions 'No special instructions were received'