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_7244340
_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 H32 Cu Mo8 N10 O28, H2 O'
_chemical_formula_sum            'C36 H42 Cu Mo8 N10 O29'
_chemical_formula_weight         1901.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-01-20
_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                90
_cell_angle_beta                 95.4410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4459(4)
_cell_length_b                   24.3390(11)
_cell_length_c                   24.7639(11)
_cell_measurement_reflns_used    2849
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.35
_cell_volume                     5067.6(4)
_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    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16628
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.677
_diffrn_reflns_theta_min         1.652
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.427
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3668.0
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.619
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5364
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0329P)^2^+1.5361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3871
_reflns_number_total             5367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra08861k2.cif
_cod_data_source_block           2
_cod_database_code               7244340
_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,H) groups
2. Restrained distances
 H2WA-N4
 2.5 with sigma of 0.02
 H2WA-O2W
 0.95 with sigma of 0.02
3. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5)
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C17(H17), C14(H14), C13(H13), C11(H11), C10(H10), C9(H9),
 C8(H8), C5(H5), C4(H4), C3(H3), C2(H2A), C1(H1A)
;
_shelx_res_checksum              47468
_olex2_submission_special_instructions 'No special instructions were received'