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_7244370
_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         'O40 Si W12, C26 H26 Co N8 O4'
_chemical_formula_sum            'C26 H26 Co N8 O44 Si W12'
_chemical_formula_weight         3447.77
_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
_audit_creation_date             2021-12-20
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-20 deposited with the CCDC.	2022-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                86.843(2)
_cell_angle_beta                 73.656(2)
_cell_angle_gamma                85.335(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4696(14)
_cell_length_b                   13.3599(14)
_cell_length_c                   20.487(2)
_cell_measurement_reflns_used    5197
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.21
_cell_volume                     3262.4(6)
_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 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23686
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.285
_diffrn_reflns_theta_min         1.530
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.421
_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    3.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3038
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.295
_refine_diff_density_min         -2.014
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         16004
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      6.499
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0219P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11020
_reflns_number_total             16004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01619a2.cif
_cod_data_source_block           1_CCDC2
_cod_database_code               7244370
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 O11-N6
 3 with sigma of 0.02
 O11-N6
 3.3 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N8(H8), N4(H4), N5(H5), C6(H6A), C14(H14), C16(H16), C20(H20),
  C22(H22), C13(H13), C2(H2), C17(H17), C9(H9), C19(H19), N7(H7), C5(H5A),
 C21(H21), C11(H11), C23(H23), C3(H3A), C25(H25)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56208
_shelx_fab_checksum              15477
_olex2_submission_special_instructions 'No special instructions were received'