Cobalt complexes tuned by Anderson-type polyoxometalates and bis-amide derivative ligands featuring a ‘V’-like connector for efficient ampere sensing and the visible-light catalytic reduction of Cr(vi)
Zhang, Yue; Wang, Xiang; Wang, Yue; Xu, Na; Wang, Xiu-Li; Dalton Transactions  (2022) –; doi:10.1039/D1DT04341B

data_7710109
_publ_section_title
;
 Cobalt complexes tuned by Anderson-type polyoxometalates and bis-amide
 derivative ligands featuring a &#x2018;V&#x2019;-like connector for
 efficient ampere sensing and the visible-light catalytic reduction of
 Cr(vi)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04341B
_journal_year                    2022
_chemical_formula_moiety         'C50 H54 Co2 Mo6 N8 O34 Te, 2(H2 O)'
_chemical_formula_sum            'C50 H58 Co2 Mo6 N8 O36 Te'
_chemical_formula_weight         2168.14
_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             2021-08-04
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-09 deposited with the CCDC.	2022-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                87.576(3)
_cell_angle_beta                 86.380(3)
_cell_angle_gamma                78.615(3)
_cell_formula_units_Z            1
_cell_length_a                   8.9146(11)
_cell_length_b                   10.3622(13)
_cell_length_c                   18.449(2)
_cell_measurement_reflns_used    830
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     1666.6(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0671
_diffrn_reflns_av_unetI/netI     0.1817
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12408
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.369
_diffrn_reflns_theta_min         1.106
_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    2.107
_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    2.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.138
_refine_diff_density_min         -1.658
_refine_diff_density_rms         0.331
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         8272
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1769
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0610P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3613
_reflns_number_total             8272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04341b2.cif
_cod_data_source_block           1_CCDC1
_cod_original_cell_volume        1666.5(4)
_cod_database_code               7710109
_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. Restrained distances
 Co1-H3WA \\sim Co1-H3WB
 with sigma of 0.02
 Co1-H1WA \\sim Co1-H1WB
 with sigma of 0.02
3.a Free rotating group:
 O3W(H3WA,H3WB), O1W(H1WA,H1WB), O4W(H4WA,H4WB)
3.b Rotating group:
 O2W(H2WA,H2WB)
3.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B)
3.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C3(H3A), N4(H4), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
  C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
 C23(H23), C24(H24), C25(H25)
;
_shelx_res_checksum              57277
_olex2_submission_special_instructions 'No special instructions were received'