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_7242268
_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         'Ge O40 W12, 4(C16 H16 Cu N4 S4)'
_chemical_formula_sum            'C64 H64 Cu4 Ge N16 O40 S16 W12'
_chemical_formula_weight         4743.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-09 deposited with the CCDC.	2021-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.791(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0266(10)
_cell_length_b                   24.0079(16)
_cell_length_c                   16.5999(12)
_cell_measurement_reflns_used    1377
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.48
_cell_measurement_theta_min      2.27
_cell_volume                     5491.2(7)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1533
_diffrn_reflns_av_unetI/netI     0.1701
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31258
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         1.510
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.921
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5620
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0990 before and 0.0392 after correction.
The Ratio of minimum to maximum transmission is 0.7542.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    2.869
_exptl_crystal_description       block
_exptl_crystal_F_000             4344
_refine_diff_density_max         1.862
_refine_diff_density_min         -2.202
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         9676
_refine_ls_number_restraints     3491
_refine_ls_restrained_S_all      0.870
_refine_ls_R_factor_all          0.1851
_refine_ls_R_factor_gt           0.0695
_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^)+(0.0543P)^2^+8.5996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4356
_reflns_number_total             9676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01811b2.cif
_cod_data_source_block           compound1
_cod_depositor_comments
'Adding full bibliography for 7242268--7242272.cif.'
_cod_database_code               7242268
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 S8A, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S8A, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S3, C11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N4, C15
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 Cu2, N5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W4, O16A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W6, O15
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O20A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 W6, O17
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 W5, O17
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 W4, O17
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 W2, O18
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 W6, O20
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 W2, O20
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 W1, O20
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Ge1, O17
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Ge1, O18
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S4, C14
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim C7 \\sim C12 \\sim C13 \\sim C16 \\sim C15 \\sim C1 \\sim C10
\\sim C14 \\sim C3 \\sim C9 \\sim C2 \\sim C11 \\sim C4 \\sim C8 \\sim C26
\\sim C28 \\sim C17 \\sim C21 \\sim C27 \\sim C18 \\sim C22 \\sim C23 \\sim C19
\\sim C25 \\sim C31 \\sim C32 \\sim C30 \\sim C20 \\sim C24 \\sim C29: within
7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Ge1: within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.04
S3 \\sim C11: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
N4 \\sim C15: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
W6 \\sim O15: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
O20A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
W6 \\sim O17: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
W5 \\sim O17: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
W4 \\sim O17: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
W2 \\sim O18: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
W6 \\sim O20: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
W2 \\sim O20: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
W1 \\sim O20: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
Ge1 \\sim O17: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
O6 \\sim O22 \\sim O14 \\sim O1 \\sim O3 \\sim O9 \\sim O7 \\sim O19 \\sim O4
\\sim O11 \\sim O5 \\sim O15 \\sim O21 \\sim O2 \\sim O17 \\sim O20 \\sim O18
\\sim O16 \\sim O12 \\sim O10 \\sim O13 \\sim O8: within 7A with sigma of 0.01
and sigma for terminal atoms of 0.02
O6 \\sim O22 \\sim O14 \\sim O1 \\sim O3 \\sim O9 \\sim O7 \\sim O19 \\sim O4
\\sim O11 \\sim O5 \\sim O15 \\sim O21 \\sim O2 \\sim O17 \\sim O20 \\sim O18
\\sim O16 \\sim O12 \\sim O10 \\sim O13 \\sim O8 \\sim O16A \\sim O11A \\sim
O20A: within 7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ge1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S8) \\sim Ueq, Uanis(S7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O20A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16A) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O20A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Fixed Sof: O11(0.5) O15(0.5) O21(0.5) O17(0.5) O20(0.5) O18(0.5) O16(0.5)
 S7(0.5) S8(0.5) H27(0.5) H27A(0.5) H29(0.5) H29A(0.5) S8A(0.5) S7A(0.5)
 O16A(0.5) O11A(0.5) O20A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C3(H3), C11(H11), C21(H21), C27(H27), C27(H27A), C22(H22),
 C29(H29), C29(H29A)
6.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C32(H32A,H32B,H32C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              37696
_shelx_hkl_checksum              10684
_olex2_submission_special_instructions 'No special instructions were received'