Four Keggin-type polyoxometalate-based complexes derived from bis(pyrazine)–bis(amide) ligands for electrochemical sensing of multiple analytes and adsorbing dye molecules
Cui, Zi-Wei; Lu, Jun-Jun; Lin, Hong-Yan; Luan, Jian; Chang, Zhi-Han; Li, Xiao-Hui; Wang, Xiu-Li; CrystEngComm 24 (2022) 828–836; doi:10.1039/D1CE01403J

data_7244130
_publ_section_title
;
 Four Keggin-type polyoxometalate-based complexes derived from
 bis(pyrazine)--bis(amide) ligands for electrochemical sensing of multiple
 analytes and adsorbing dye molecules
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              828
_journal_page_last               836
_journal_paper_doi               10.1039/D1CE01403J
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C28 H32 Cu2 N12 O44 Si W12, 8(H2 O)'
_chemical_formula_sum            'C28 H48 Cu2 N12 O52 Si W12'
_chemical_formula_weight         3746.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-20
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6427)
;
_audit_update_record
;
2021-11-25 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.218(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1453(7)
_cell_length_b                   17.1380(11)
_cell_length_c                   19.2588(12)
_cell_measurement_reflns_used    1283
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      21.88
_cell_measurement_theta_min      2.34
_cell_volume                     3328.8(4)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_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_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1145
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19979
_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         25.696
_diffrn_reflns_theta_min         1.595
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.398
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    3.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.868
_refine_diff_density_min         -2.327
_refine_diff_density_rms         0.380
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         6339
_refine_ls_number_restraints     744
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+115.4300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3916
_reflns_number_total             6339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01403j3.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7244127--7244130.cif.'
_cod_database_code               7244130
_shelx_shelxl_version_number     2018/3
_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 C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O15) \\sim Ueq, Uanis(O15A) \\sim Ueq, Uanis(O18A) \\sim Ueq, Uanis(O18)
\\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O16) \\sim Ueq,
Uanis(O10A) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O5(0.5) O5A(0.5) O10(0.5) O10A(0.5) O11(0.5) O11A(0.5) O12(0.5)
 O12A(0.5) O14(0.5) O14A(0.5) O15(0.5) O15A(0.5) O16(0.5) O16A(0.5) O18(0.5)
 O18A(0.5) O21(0.5) O22(0.5) O23(0.5) O24(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B)
5.c Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C12(H12A,H12B,H12C)
5.d Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C2(H2), C3(H3A), C8(H8), C9(H9)
;
_shelx_res_checksum              31817
_shelx_hkl_checksum              15561
_olex2_submission_special_instructions 'No special instructions were received'