Carbazole-based bis-imidazole ligand-involved synthesis of inorganic–organic hybrid polyoxometalates as electrochemical sensors for detecting bromate and efficient catalysts for selective oxidation of thioether
Wang, Xiang; Lin, Jiafeng; Li, Huan; Wang, Chenying; Wang, Xiuli; RSC Advances 12 (2022) 4437–4445; doi:10.1039/D1RA08861K

data_7244342
_publ_section_title
;
 Carbazole-based bis-imidazole ligand-involved synthesis of
 inorganic--organic hybrid polyoxometalates as electrochemical sensors for
 detecting bromate and efficient catalysts for selective oxidation of
 thioether
;
_journal_issue                   8
_journal_name_full               'RSC Advances'
_journal_page_first              4437
_journal_page_last               4445
_journal_paper_doi               10.1039/D1RA08861K
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety
'C36 H40 Cr Mo6 N10 Ni2 O29.50, 2.5(O), 2(H2 O)'
_chemical_formula_sum            'C36 H44 Cr Mo6 N10 Ni2 O34'
_chemical_formula_weight         1905.83
_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_creation_date             2022-01-19
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6115)
;
_audit_update_record
;
2022-01-25 deposited with the CCDC.	2022-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                95.1090(10)
_cell_angle_beta                 91.5670(10)
_cell_angle_gamma                97.2660(10)
_cell_formula_units_Z            1
_cell_length_a                   7.8269(4)
_cell_length_b                   10.4537(5)
_cell_length_c                   17.1966(8)
_cell_measurement_reflns_used    3225
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.278
_cell_volume                     1389.12(12)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0198
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10351
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.342
_diffrn_reflns_theta_min         1.972
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.265
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.388
_exptl_crystal_description       block
_exptl_crystal_F_000             934.0
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.623
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6894
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0414P)^2^+2.9528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5501
_reflns_number_total             6942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra08861k2.cif
_cod_data_source_block           3
_cod_database_code               7244342
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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(O5WB) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4WB) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O4WB(0.25) O5WB(0.5) O5WA(0.5) O4WA(0.75)
4.a Free rotating group:
 O3W(H3WA,H3WB)
4.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.c Ternary CH refined with riding coordinates:
 O10(H10), O11(H11), O12(H12)
4.d Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C3(H3A), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9),
 C10(H10A), C11(H11A), C14(H14), C17(H17)
;
_shelx_res_checksum              97652
_olex2_submission_special_instructions 'No special instructions were received'