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_7708736
_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
'C20 H18 Cu2 N4 O41 W12 Zn0.5, C10 H12 Cu N2 O2, 2(H2 O)'
_chemical_formula_sum            'C30 H34 Cu3 N6 O45 W12 Zn0.5'
_chemical_formula_weight         3628.14
_chemical_name_systematic        monoclinic
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-18 deposited with the CCDC.	2021-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.479(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.566(4)
_cell_length_b                   19.243(5)
_cell_length_c                   22.630(6)
_cell_measurement_reflns_used    4400
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      25.058
_cell_measurement_theta_min      2.301
_cell_volume                     5890(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33664
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.095
_diffrn_reflns_theta_max         25.095
_diffrn_reflns_theta_min         1.815
_exptl_absorpt_coefficient_mu    24.697
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ad
_exptl_crystal_colour            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    4.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.580
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.350
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         10441
_refine_ls_number_restraints     1561
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0237P)^2^+28.2442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9018
_reflns_number_total             10441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02618f2.cif
_cod_data_source_block           xul20091007_1_0m
_cod_original_cell_volume        5889(3)
_cod_original_formula_sum        'C30 H34 Cu3 N6 O45 W12 Zn0.50'
_cod_database_code               7708736
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.243
_shelx_estimated_absorpt_t_min   0.083
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H6B-H22
 1.93 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O17 \\sim O15 \\sim O18 \\sim O41 \\sim O40 \\sim O20 \\sim O11 \\sim O28 \\sim
O3 \\sim O14 \\sim O13 \\sim O33 \\sim O42 \\sim O39 \\sim O26 \\sim O43 \\sim
O2 \\sim O12 \\sim O30 \\sim O31 \\sim O24 \\sim O16 \\sim O35 \\sim O29 \\sim
O22 \\sim O32 \\sim O1 \\sim O7 \\sim O4 \\sim O10 \\sim O21 \\sim O25 \\sim
O23 \\sim O8 \\sim O19 \\sim O34 \\sim O9 \\sim O27 \\sim O38 \\sim O5 \\sim
O36 \\sim O37 \\sim O6 \\sim O44 \\sim O45: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N1 \\sim N2 \\sim N6 \\sim N3 \\sim N4 \\sim N5: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02
C01S \\sim C01U \\sim C01V \\sim C01W \\sim C01Z \\sim C020 \\sim C021 \\sim
C022 \\sim C023 \\sim C024 \\sim C025 \\sim C026 \\sim C027 \\sim C028 \\sim
C029 \\sim C2 \\sim C3 \\sim C4 \\sim C6 \\sim C7 \\sim C9 \\sim C10 \\sim C11
\\sim C12 \\sim C13 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C22: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Zn1(0.5)
5.a Free rotating group:
 O44(H44A,H44B), O45(H45A,H45B)
5.b Rotating group:
 O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B)
5.c Aromatic/amide H refined with riding coordinates:
 C01V(H01V), C01W(H01W), C01Z(H01Z), C020(H020), C021(H021), C022(H022),
 C024(H024), C026(H026), C029(H029), C2(H2), C3(H3), C4(H4), C6(H6), C7(H7),
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18),
 C19(H19), C22(H22)
;
_shelx_res_checksum              64306
_shelx_hkl_checksum              65435
_olex2_submission_special_instructions 'No special instructions were received'