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_7244127
_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 H28 Cu2 Mo12 N12 O45 P, 5(H2 O), 2(H O0.25)'
_chemical_formula_sum            'C24 H40 Cu2 Mo12 N12 O50.5 P'
_chemical_formula_weight         2614.01
_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             2021-11-25
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-25 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                89.7710(10)
_cell_angle_beta                 86.3930(10)
_cell_angle_gamma                81.1880(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9002(5)
_cell_length_b                   11.5504(5)
_cell_length_c                   14.7377(7)
_cell_measurement_reflns_used    3953
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     1829.94(14)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f 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  0.0217
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13731
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.497
_diffrn_reflns_theta_min         2.275
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.675
_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    2.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1249
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.822
_refine_diff_density_min         -2.293
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         9163
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0748
_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^)+(0.0326P)^2^+33.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1630
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7595
_reflns_number_total             9163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01403j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7244127--7244130.cif.'
_cod_original_formula_sum        'C24 H40 Cu2 Mo12 N12 O50.50 P'
_cod_database_code               7244127
_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(O16) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O24) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O3(0.5) O3A(0.5) O6(0.5) O6A(0.5) O16(0.5) O16A(0.5) O17(0.5)
 O17A(0.5) O18(0.5) O18A(0.5) O19(0.5) O19A(0.5) O20(0.5) O20A(0.5) O22(0.5)
 O23(0.5) O24(0.5) O25(0.5) O6W(0.5) H6WA(0.5) H6WB(0.5) O7W(0.5) H7WA(0.5)
 H7WB(0.5) O2W(0.5) H2WA(0.5) H2WB(0.5) O3W(0.5) H3WA(0.5) H3WB(0.5) O5W(0.5)
 H5WA(0.5) H5WB(0.5) O4W(0.25) H4WA(0.5) H4WB(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O6W(H6WA,H6WB), O7W(H7WA,H7WB), O2W(H2WA,H2WB), O3W(H3WA,
 H3WB), O5W(H5WA,H5WB), O4W(H4WA,H4WB)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C4(H4A), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'