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_7244128
_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         'C24 H24 Cu2 Mo12 N12 O44 Si, 3(H2 O)'
_chemical_formula_sum            'C24 H30 Cu2 Mo12 N12 O47 Si'
_chemical_formula_weight         2545.05
_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_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                 96.972(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0460(11)
_cell_length_b                   20.6074(14)
_cell_length_c                   18.8644(13)
_cell_measurement_reflns_used    2952
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.95
_cell_measurement_theta_min      2.39
_cell_volume                     6191.7(7)
_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      293
_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 0.999
_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  0.0871
_diffrn_reflns_av_unetI/netI     0.0938
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35168
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.469
_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    3.148
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4840
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.206
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         10904
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0898P)^2^+32.2075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6831
_reflns_number_total             10904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01403j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7244127--7244130.cif.'
_cod_database_code               7244128
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2W) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N4)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: O3W(0.5) H3WA(0.5) H3WB(0.5) O4W(0.5) H4WA(0.5) H4WB(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C14(H14A,H14B), C16(H16A,H16B), C20(H20A,H20B)
4.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N5(H5), N7(H7), N8(H8), C6(H6), C8(H8A), C9(H9), C10(H10), C13(H13),
 C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              7386
_shelx_hkl_checksum              12261
_olex2_submission_special_instructions 'No special instructions were received'