Various amide derivatives induced Keggin-type SiW12O404−-based cobalt complexes: assembly, structure, electrochemical sensing and dye adsorption properties
Li, Lei; Zhang, Yue; Wang, Xiang; Xu, Na; Li, Xiao-Hui; Wang, Xiu-Li; CrystEngComm 24 (2022) 1195–1202; doi:10.1039/D1CE01619A

data_7244368
_publ_section_title
;
 Various amide derivatives induced Keggin-type SiW12O404&#x2212;-based
 cobalt complexes: assembly, structure, electrochemical sensing and dye
 adsorption properties
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1195
_journal_page_last               1202
_journal_paper_doi               10.1039/D1CE01619A
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C42 H36 Co2 N12 O48 Si W12, 1[5H2O]'
_chemical_formula_sum            'C42 H36 Co2 N12 O48 Si W12'
_chemical_formula_weight         3828.98
_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             2021-11-17
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-17 deposited with the CCDC.	2022-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                100.9280(10)
_cell_angle_beta                 111.9070(10)
_cell_angle_gamma                99.1860(10)
_cell_formula_units_Z            1
_cell_length_a                   11.8442(7)
_cell_length_b                   12.6156(8)
_cell_length_c                   15.1270(10)
_cell_measurement_reflns_used    2877
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     1992.1(2)
_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      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 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14695
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.294
_diffrn_reflns_theta_min         1.508
_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    17.761
_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    3.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.744
_refine_diff_density_min         -4.520
_refine_diff_density_rms         0.497
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         9799
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+18.7866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6691
_reflns_number_total             9799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01619a2.cif
_cod_data_source_block           1
_cod_database_code               7244368
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.125
_shelx_estimated_absorpt_t_min   0.100
_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. Rigid bond restraints
 Si1, O23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Si1, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O9 \\sim W2 \\sim W5: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.001 within 2A
W2 \\sim O24 \\sim W4: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.01 within 2A
O19 \\sim W4 \\sim W6: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.01 within 2A
O24 \\sim W4 \\sim W2: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.001 within 2A
O17 \\sim W5 \\sim W3: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.001 within 2A
Uanis(O1) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O21) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O21) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O21(0.5) O11(0.5) O23(0.5) O6(0.5)
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N6(H6), N3(H3), C4(H4), C8(H8), C12(H12), C16(H16), C20(H20),
 C11(H11), C3(H3A), C15(H15), N5(H5), C2(H2), C17(H17), C19(H19), C5(H5A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91113
_shelx_fab_checksum              71242
_olex2_submission_special_instructions 'No special instructions were received'