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_7710111
_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 H46 Al2 Co2 Mo12 N8 O58, 5(H2 O)'
_chemical_formula_sum            'C50 H56 Al2 Co2 Mo12 N8 O63'
_chemical_formula_weight         3100.12
_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             2021-12-09
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-09 deposited with the CCDC.	2022-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                81.7570(10)
_cell_angle_beta                 80.9080(10)
_cell_angle_gamma                75.0090(10)
_cell_formula_units_Z            1
_cell_length_a                   12.4682(5)
_cell_length_b                   12.4968(5)
_cell_length_c                   14.3152(6)
_cell_measurement_reflns_used    3925
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     2115.19(15)
_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      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 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.0235
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15697
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.293
_diffrn_reflns_theta_min         1.449
_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    2.236
_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    2.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         10429
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.557
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0350P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7821
_reflns_number_total             10429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04341b2.cif
_cod_data_source_block           1_CCDC3
_cod_database_code               7710111
_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
 H1WB-H4WB
 2.1 with sigma of 0.01
 O4W-H4WB
 0.851 with sigma of 0.002
 H4WB-O4W
 0.95 with sigma of 0.002
 H4WA-H18_$1
 2.2 with sigma of 0.001
 H4WB-H1WB
 3.2 with sigma of 0.001
 H18_$1-H4WB
 3.1 with sigma of 0.001
3. Others
 Fixed Sof: O4W(0.5) H4WA(0.5) H4WB(0.5)
4.a Free rotating group:
 O3W(H3WA,H3WB), O5W(H5WA,H5WB), O4W(H4WA,H4WB)
4.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N2(H2), N3(H3), C1(H1), C6(H6), C12(H12), C14(H14), C18(H18),
 C20(H20), C22(H22), C25(H25), C13(H13), C15(H15), C2(H2A), C5(H5), C21(H21),
 C11(H11), C23(H23), C3(H3A)
;
_shelx_res_checksum              1733
_olex2_submission_special_instructions 'No special instructions were received'