Dual-nodes bridged cobalt-modified Keggin-type polyoxometalate-based chains for highly efficient CO<sub>2</sub> photoconversion.
Chen, Xin-Lian; Wu, Jie; Wang, Ji-Lei; Liu, Xiao-Mei; Mei, Hua; Xu, Yan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12943–12950; doi:10.1039/d4dt01757a

data_7716637
_publ_section_title
;
 Dual-nodes bridged cobalt-modified Keggin-type polyoxometalate-based
 chains for highly efficient CO<sub>2</sub> photoconversion.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12943
_journal_page_last               12950
_journal_paper_doi               10.1039/d4dt01757a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C48 H36 Co2 N12 O40 Si W12, 2(C2 H6 O)'
_chemical_formula_sum            'C52 H48 Co2 N12 O42 Si W12'
_chemical_formula_weight         3865.17
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-05-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-02 deposited with the CCDC.	2024-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                101.102(9)
_cell_angle_beta                 98.930(10)
_cell_angle_gamma                108.668(9)
_cell_formula_units_Z            1
_cell_length_a                   11.981(9)
_cell_length_b                   12.240(9)
_cell_length_c                   14.091(11)
_cell_measurement_reflns_used    5924
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.201
_cell_measurement_theta_min      2.542
_cell_volume                     1868(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       SAINT
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.0940
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13284
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.515
_diffrn_source_current           25.0
_diffrn_source_power             1.125
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    18.937
_exptl_absorpt_correction_T_max  0.230
_exptl_absorpt_correction_T_min  0.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            orange-red
_exptl_crystal_colour_primary    orange-red
_exptl_crystal_density_diffrn    3.436
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.808
_refine_diff_density_min         -2.816
_refine_diff_density_rms         0.468
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         6532
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0729
_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^)+(0.0308P)^2^+124.8066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5772
_reflns_number_total             6532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01757a2.cif
_cod_data_source_block           Co
_cod_depositor_comments
'Adding full bibliography for 7716637--7716639.cif.'
_cod_database_code               7716637
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.230
_shelx_estimated_absorpt_t_min   0.192
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N1-C5 = N1-C7 = N2-C7 = N2-C4 = N3-C12 = N3-C8 = N4-C19 = N4-C18
 1.35 with sigma of 0.0002
 N6-C19 = N6-C17 = C1-C2 = C1-C6 = C2-C3 = C3-C4 = C4-C5 = C5-C6 = C8-C9
 1.35 with sigma of 0.0002
 C9-C10 = C10-C11 = C11-C12 = C13-C14 = C13-C18 = C15-C16 = C16-C17
 1.35 with sigma of 0.0002
 C21-C22 = C23-C24 = N5-C20 = N5-C24 = C20-C21
 1.35 with sigma of 0.0002
 C7-C8 = C14-C15 = C17-C18 = C19-C20 = C22-C23
 1.45 with sigma of 0.0002
 H6A-H23A
 2.2 with sigma of 0.02
 C25-O23
 1.3 with sigma of 0.001
 C25-C26
 1.55 with sigma of 0.001
3. Rigid bond restraints
 C15, C16
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C21, C22
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C25 \\sim C26 \\sim O23: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O12 \\sim O15: within 10A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 10A
O20 \\sim O2: within 10A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 10A
O21 \\sim O5: within 10A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 10A
Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O7) \\sim
Ueq, Uanis(O8) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O13) \\sim Ueq,
Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O18)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O21) \\sim Ueq,
Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O14) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Others
 Fixed Sof: O12(0.5) O20(0.5) O21(0.5) O22(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1A), N6(H6A), C1(H1), C2(H2), C3(H3), C6(H6), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C21(H21), C22(H22), C23(H23),
  C24(H24)
6.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
6.d Idealised tetrahedral OH refined as rotating group:
 O23(H23A)
;
_shelx_res_checksum              13143
_shelx_hkl_checksum              24395
_olex2_submission_special_instructions 'No special instructions were received'