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_7244129
_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         'O40 Si W12, C28 H38 Co2 N12 O8, 1.5(H2 O)'
_chemical_formula_sum            'C28 H41 Co2 N12 O49.5 Si W12'
_chemical_formula_weight         3689.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2021-11-25 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.134(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.8588(14)
_cell_length_b                   21.3036(14)
_cell_length_c                   10.4152(8)
_cell_measurement_reflns_used    2640
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     3483.4(5)
_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 1.5 (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      296.15
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10045
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.033
_diffrn_reflns_theta_max         25.033
_diffrn_reflns_theta_min         1.611
_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
_exptl_absorpt_coefficient_mu    20.309
_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            Pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    3.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3290
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.581
_refine_diff_density_min         -2.043
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         3158
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0356P)^2^+63.8128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2529
_reflns_number_total             3158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01403j3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'Pink' was changed to
'pink' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7244127--7244130.cif.
;
_cod_original_formula_sum        'C28 H41 Co2 N12 O49.50 Si W12'
_cod_database_code               7244129
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.106
_shelx_estimated_absorpt_t_min   0.085
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1WA,H1WB} of O1W, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H2WA,H2WB} of O2W, {H3WA,H3WB} of O3W
2. Restrained distances
 Si1-O14
 1.535 with sigma of 0.0005
3. Uiso/Uaniso restraints and constraints
Uanis(O2W) \\sim Ueq, Uanis(O3W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O1, C9, N4, O19, C5, C6, N3, C8, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O19(0.5) O3(0.5) O6(0.5) C5(0.5) O7(0.5) C6(0.5) H6A(0.5) H6B(0.5)
 N3(0.5) O11(0.25) O13(0.25) O14(0.25) O15(0.5) O16(0.5) C8(0.5) H8A(0.5)
 H8B(0.5) O9(0.5) O4(0.5) O3A(0.5) O16A(0.5) O6A(0.5) O7A(0.5) O11A(0.25)
 O2(0.25) O2A(0.25) O2W(0.25) H2WA(0.25) H2WB(0.25) O3W(0.125) H3WA(0.125)
 H3WB(0.125) O1(0.5) C9(0.5) N4(0.5) H4(0.5)
6.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B)
6.c Me refined with riding coordinates:
 C7(H7A,H7B,H7C)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), N4(H4)
;
_shelx_res_checksum              18297
_shelx_hkl_checksum              63621
_olex2_submission_special_instructions 'No special instructions were received'