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_7242270
_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 Ge2 N16 Ni4 O82 S16 W24, 4(H2 O)'
_chemical_formula_sum            'C64 H76 Ge2 N16 Ni4 O86 S16 W24'
_chemical_formula_weight         7750.78
_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             2020-04-17
_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                86.664(5)
_cell_angle_beta                 87.320(5)
_cell_angle_gamma                69.631(5)
_cell_formula_units_Z            1
_cell_length_a                   12.315(3)
_cell_length_b                   15.474(4)
_cell_length_c                   19.504(5)
_cell_measurement_reflns_used    2653
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.47
_cell_volume                     3477.0(15)
_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      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0587
_diffrn_reflns_av_unetI/netI     0.1381
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25091
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.099
_diffrn_reflns_theta_min         1.714
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.047
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    3.701
_exptl_crystal_description       block
_exptl_crystal_F_000             3468
_refine_diff_density_max         3.818
_refine_diff_density_min         -3.369
_refine_diff_density_rms         0.450
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1100
_refine_ls_number_reflns         16787
_refine_ls_number_restraints     3942
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0429P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1282
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9240
_reflns_number_total             16787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01811b2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7242268--7242272.cif.'
_cod_original_cell_volume        3477.2(16)
_cod_database_code               7242270
_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. Rigid bond restraints
 W5, W10A, W4AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 W1, W2AB, W3AA, W2AC
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 W0AA, W9, W6AA, W7AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
W1 \\sim W2AB \\sim W3AA: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
W5 \\sim W10A \\sim W4AA: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
W1 \\sim W2AB \\sim W3AA \\sim W2AC: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
W0AA \\sim W9 \\sim W6AA \\sim W7AA: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
O15 \\sim O9 \\sim O34 \\sim O28 \\sim O7 \\sim O18 \\sim O14 \\sim O3 \\sim
O23 \\sim O32 \\sim O37 \\sim O13 \\sim O24 \\sim O6 \\sim O4 \\sim O33 \\sim
O8 \\sim O40 \\sim O21 \\sim O16 \\sim O35 \\sim O11 \\sim O5 \\sim O38 \\sim
O12 \\sim O26 \\sim O30 \\sim O36 \\sim O39 \\sim O29 \\sim O1W \\sim O22 \\sim
O2 \\sim O1 \\sim O20 \\sim O25 \\sim O31 \\sim O19 \\sim O17 \\sim O10 \\sim
O3W \\sim O2W: within 7A with sigma of 0.01 and sigma for terminal atoms of 0.02
O15 \\sim O9 \\sim O34 \\sim O28 \\sim O7 \\sim O18 \\sim O14 \\sim O3 \\sim
O23 \\sim O32 \\sim O37 \\sim O13 \\sim O24 \\sim O6 \\sim O4 \\sim O33 \\sim
O8 \\sim O40 \\sim O21 \\sim O16 \\sim O35 \\sim O11 \\sim O5 \\sim O38 \\sim
O12 \\sim O26 \\sim O30 \\sim O36 \\sim O39 \\sim O29 \\sim O1W \\sim O22 \\sim
O2 \\sim O1 \\sim O20 \\sim O25 \\sim O31 \\sim O19 \\sim O17 \\sim O10 \\sim
O3W \\sim O2W \\sim O2X: within 7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(O20) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C8A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(W8AA) \\sim Ueq, Uanis(W10) \\sim Ueq, Uanis(W1AA) \\sim Ueq, Uanis(W11B)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(W2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(W2) \\sim Ueq, Uanis(W1A) \\sim Ueq, Uanis(W1B) \\sim Ueq: with sigma of
0.0001 and sigma for terminal atoms of 0.0002
Uanis(W2) \\sim Ueq, Uanis(W1A) \\sim Ueq, Uanis(W1B) \\sim Ueq, Uanis(W1C)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(W1) \\sim Ueq, Uanis(W2AB) \\sim Ueq, Uanis(W3AA) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.001
Uanis(W5) \\sim Ueq, Uanis(W10A) \\sim Ueq, Uanis(W4AA) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(W5) \\sim Ueq, Uanis(W10A) \\sim Ueq, Uanis(W4AA) \\sim Ueq, Uanis(W5AA)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(W4) \\sim Ueq, Uanis(W6A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(W0AA) \\sim Ueq, Uanis(W9) \\sim Ueq, Uanis(W6AA) \\sim Ueq, Uanis(W7AA)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O2X) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 W2, W1A, W1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 W1, W2AB, W3AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 W5, W10A, W4AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 W1, W2AB, W3AA, W2AC
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 W0AA, W9, W6AA, W7AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: W4(0.5) W5(0.25) W2(0.25) W8AA(0.25) C8(0.5) H8A(0.5) H8B(0.5)
 H8C(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) O2W(0.5) H2WA(0.5) H2WB(0.5)
 O2X(0.5) H2XA(0.5) H2XB(0.5) W10(0.25) W1AA(0.25) W11B(0.25) W1A(0.25)
 W1B(0.25) W1C(0.25) W1(0.25) W2AB(0.25) W3AA(0.25) W6A(0.5) W10A(0.25)
 W4AA(0.25) W5AA(0.25) W2AC(0.25) W0AA(0.25) W9(0.25) W6AA(0.25) W7AA(0.25)
6.a Everything fixed:
 O3W, H3WA, H3WB, O2W, H2WA, H2WB, O2X, H2XA, H2XB
6.b Rotating group:
 O1W(H1WA,H1WB)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C27(H27), C30(H30), C14(H14), C3(H3), C19(H19), C22(H22), C11(H11)
6.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C32(H32A,H32B,
 H32C), C23(H23A,H23B,H23C), C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C9(H9A,H9B,
 H9C), C8A(H8AA,H8AB,H8AC)
;
_shelx_res_checksum              68355
_shelx_hkl_checksum              32557
_olex2_submission_special_instructions 'No special instructions were received'