pH-controlled assembly of [ZnW12O40]6–based hybrids from 0D dimer to 2D network: synthesis, crystal structure, and photocatalytic performance in transformation of toluene into benzaldehyde
Guo, Keke; Yang, Yanli; Dong, Si-Meng; Li, Fengyan; Jiang, Xin-Ye; Xu, Lin; Dalton Transactions  (2021) –; doi:10.1039/D1DT02618F

data_7708738
_publ_section_title
;
 pH-controlled assembly of [ZnW12O40]6--based hybrids from 0D dimer to 2D
 network: synthesis, crystal structure, and photocatalytic performance in
 transformation of toluene into benzaldehyde
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02618F
_journal_year                    2021
_chemical_formula_moiety
'C10 H10 Cu N2 O41 W12 Zn, C10 H14 Cu N2 O3, 2(C4 H12 N), 3(H2 O)'
_chemical_formula_sum            'C28 H54 Cu2 N6 O47 W12 Zn'
_chemical_formula_weight         3625.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-29 deposited with the CCDC.	2021-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4367(16)
_cell_length_b                   23.8076(17)
_cell_length_c                   26.7171(17)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      63.798
_cell_measurement_theta_min      3.713
_cell_volume                     13635.2(17)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.11
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57426
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        63.860
_diffrn_reflns_theta_max         63.860
_diffrn_reflns_theta_min         3.230
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    38.178
_exptl_absorpt_correction_T_max  0.0611
_exptl_absorpt_correction_T_min  0.0043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1295 before and 0.0900 after correction.
The Ratio of minimum to maximum transmission is 0.0704.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    3.532
_exptl_crystal_description       block
_exptl_crystal_F_000             12928
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.798
_refine_diff_density_min         -1.327
_refine_diff_density_rms         0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         11135
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0703
_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^)+(0.0753P)^2^+662.4064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8211
_reflns_number_total             11135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02618f2.cif
_cod_data_source_block           cu_xul200722_2_0m
_cod_database_code               7708738
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.251
_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
 C21-C24
 2.38 with sigma of 0.02
 C23-C24
 2.38 with sigma of 0.02
 O42-H42A
 0.85 with sigma of 0.02
 O42-H42B
 0.85 with sigma of 0.02
 O44-H44B
 0.8 with sigma of 0.01
 O44-H44A
 0.8 with sigma of 0.01
 O32-H46B
 2 with sigma of 0.01
 H43B-O43
 0.85 with sigma of 0.01
 O43-H43A
 0.85 with sigma of 0.01
 O41-H41A
 0.85 with sigma of 0.01
 O41-H41B
 0.85 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O45 \\sim O48 \\sim O47: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O48) \\sim Ueq, Uanis(O47) \\sim Ueq, Uanis(O45) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: O45(0.5) H45A(0.5) H45B(0.5) O48(0.5) H48A(0.5) H48B(0.5)
5.a Riding coordinates:
 O47(H47A,H47B), O45(H45A,H45B), O48(H48A,H48B)
5.b Free rotating group:
 O46(H46A,H46B)
5.c Rotating group:
 O43(H43A,H43B), O44(H44A,H44B), O41(H41A,H41B), O42(H42A,H42B)
5.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C8(H8), C20(H20), C1(H1), C14(H14), C18(H18), C19(H19), C17(H17),
 C2(H2), C10(H10), C3(H3), C12(H12), C9(H9), C11(H11), C7(H7), C4(H4)
5.e Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C23(H23A,H23B,
 H23C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C21(H21A,H21B,H21C), C24(H24A,
 H24B,H24C)
;
_shelx_res_checksum              45882
_shelx_hkl_checksum              31244
_olex2_submission_special_instructions 'No special instructions were received'