Multifunctional photoelectric sensors and catalysts for CO2RR and Cr(vi) solution based on a series of POM-based materials
Wang, Chen; Ying, Jun; Zhang, Xin-yue; Zhang, Bao-yue; Tian, Ai-xiang; Wang, Xiu-li; CrystEngComm 23 (2021) 2424–2431; doi:10.1039/D0CE01811B

data_7242272
_publ_section_title
;
 Multifunctional photoelectric sensors and catalysts for CO2RR and Cr(vi)
 solution based on a series of POM-based materials
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              2424
_journal_page_last               2431
_journal_paper_doi               10.1039/D0CE01811B
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C64 H68 Co4 N16 O82 S16 Si2 W24'
_chemical_formula_sum            'C64 H68 Co4 N16 O82 S16 Si2 W24'
_chemical_formula_weight         7590.60
_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     iterative
_audit_creation_date             2020-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-27 deposited with the CCDC.	2021-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                86.760(4)
_cell_angle_beta                 87.368(4)
_cell_angle_gamma                69.774(3)
_cell_formula_units_Z            1
_cell_length_a                   12.3151(19)
_cell_length_b                   15.487(2)
_cell_length_c                   19.695(3)
_cell_measurement_reflns_used    1089
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.26
_cell_measurement_theta_min      2.16
_cell_volume                     3517.7(9)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0984
_diffrn_reflns_av_unetI/netI     0.2318
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20280
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.403
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.335
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4675
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1143 before and 0.0454 after correction.
The Ratio of minimum to maximum transmission is 0.6269.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    3.583
_exptl_crystal_description       block
_exptl_crystal_F_000             3388
_refine_diff_density_max         3.395
_refine_diff_density_min         -2.508
_refine_diff_density_rms         0.494
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         12430
_refine_ls_number_restraints     4174
_refine_ls_restrained_S_all      0.794
_refine_ls_R_factor_all          0.1893
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0587P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5457
_reflns_number_total             12430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01811b2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7242268--7242272.cif.'
_cod_database_code               7242272
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H1Wa-H32b
 2 with sigma of 0.02
3. Rigid bond restraints
 S4, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S8, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W6A, W6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 W7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O22 \\sim O9 \\sim O39 \\sim O24 \\sim O10 \\sim O38 \\sim O26 \\sim O20 \\sim
O4 \\sim O31 \\sim O27 \\sim O11 \\sim O14 \\sim O17 \\sim O35 \\sim O7 \\sim
O34 \\sim O19 \\sim O13 \\sim O18 \\sim O21 \\sim O5 \\sim O16 \\sim O23 \\sim
O12 \\sim O28 \\sim O29 \\sim O30 \\sim O2 \\sim O40 \\sim O3 \\sim O1 \\sim
O15 \\sim O8 \\sim O36 \\sim O32 \\sim O6 \\sim O37 \\sim O1W \\sim O33 \\sim
O25: within 7A with sigma of 0.01 and sigma for terminal atoms of 0.02
W6A \\sim W6: within 2A with sigma of 0.0001 and sigma for terminal atoms of
0.0002
W7: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C7) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C32) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C16)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O6) \\sim
Ueq, Uanis(N6) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N8)
\\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N5) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O22) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O24)
\\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O26) \\sim Ueq,
Uanis(O20) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O27)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O17) \\sim Ueq,
Uanis(O35) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O19)
\\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O21) \\sim Ueq,
Uanis(O5) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O12)
\\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O30) \\sim Ueq,
Uanis(O2) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1) \\sim
Ueq, Uanis(O15) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O37) \\sim Ueq,
Uanis(O1W) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(O25) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(W2A) \\sim Ueq, Uanis(W2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(W6A) \\sim Ueq, Uanis(W6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(W7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 W6A, W6
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
 W7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Others
 Sof(W6A)=1-FVAR(1)
 Sof(W6)=FVAR(1)
 Fixed Sof: W2(0.5) W2A(0.5)
7.a Rotating group:
 O1W(H1Wa,H1Wb)
7.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C22(H22), C6(H6), C14(H14), C4(H4), C19(H19), C30(H30), C27(H27)
7.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C1(H1a,H1b,H1c), C32(H32a,H32b,H32c), C24(H24a,H24b,H24c),
 C25(H25a,H25b,H25c), C17(H17a,H17b,H17c), C9(H9a,H9b,H9c), C16(H16a,H16b,H16c)
;
_shelx_res_checksum              29566
_shelx_hkl_checksum              1392
_shelx_fab_checksum              96759
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'