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_7708737
_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 H22 Cu2 N4 O43 W12 Zn0.6, C10 H14 Cu N2 O3, 5(H2 O)'
_chemical_formula_sum            'C30 H46 Cu3 N6 O51 W12 Zn0.6'
_chemical_formula_weight         3742.77
_chemical_name_systematic        triclinic
_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             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                71.753(4)
_cell_angle_beta                 75.881(4)
_cell_angle_gamma                70.816(3)
_cell_formula_units_Z            2
_cell_length_a                   12.961(3)
_cell_length_b                   14.589(3)
_cell_length_c                   19.640(4)
_cell_measurement_reflns_used    3432
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.867
_cell_measurement_theta_min      2.212
_cell_volume                     3289.6(12)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.1063
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18956
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.528
_exptl_absorpt_coefficient_mu    22.155
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ad
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.779
_exptl_crystal_description       block
_exptl_crystal_F_000             3338
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.789
_refine_diff_density_min         -3.242
_refine_diff_density_rms         0.391
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         11572
_refine_ls_number_restraints     1802
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+31.6796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8302
_reflns_number_total             11572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02618f2.cif
_cod_data_source_block           xul200729_1_0m
_cod_original_cell_volume        3289.6(13)
_cod_original_formula_sum        'C30 H46 Cu3 N6 O51 W12 Zn0.60'
_cod_database_code               7708737
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.136
_shelx_estimated_absorpt_t_min   0.095
_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
 O41-H41A
 0.85 with sigma of 0.01
 O41-H41B
 0.85 with sigma of 0.01
 O51-H51A
 0.85 with sigma of 0.01
 O51-H51B
 0.85 with sigma of 0.01
 H49B-O38
 1.8 with sigma of 0.01
 O50-H50A
 0.85 with sigma of 0.01
 O50-H50B
 0.85 with sigma of 0.01
 O13-H50B
 2.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C5 \\sim C25 \\sim C26 \\sim C6 \\sim C27 \\sim C24 \\sim C16 \\sim C2 \\sim
C23 \\sim C3 \\sim C21 \\sim C13 \\sim C17 \\sim C20 \\sim C29 \\sim C9 \\sim
C12 \\sim C30 \\sim C8 \\sim C4 \\sim C1 \\sim C18 \\sim C15 \\sim C10 \\sim
C19 \\sim C7 \\sim C22 \\sim C28 \\sim C11 \\sim C14: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
O40 \\sim O18 \\sim O36 \\sim O1 \\sim O8 \\sim O2 \\sim O15 \\sim O35 \\sim
O38 \\sim O7 \\sim O39 \\sim O37 \\sim O19 \\sim O21 \\sim O16 \\sim O24 \\sim
O30 \\sim O20 \\sim O9 \\sim O33 \\sim O3 \\sim O32 \\sim O29 \\sim O6 \\sim
O34 \\sim O22 \\sim O17 \\sim O5 \\sim O23 \\sim O42 \\sim O28 \\sim O13 \\sim
O31 \\sim O14 \\sim O11 \\sim O51 \\sim O12 \\sim O41 \\sim O10 \\sim O25 \\sim
O4 \\sim O44 \\sim O26 \\sim O27 \\sim O45 \\sim O43 \\sim O50 \\sim O49 \\sim
O47 \\sim O48 \\sim O46: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O10) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(N3) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C28) \\sim Ueq,
Uanis(N6) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: Zn1(0.6)
5.a Riding coordinates:
 O49(H49A,H49B), O48(H48A,H48B), O46(H46A,H46B)
5.b Free rotating group:
 O50(H50A,H50B), O47(H47A,H47B)
5.c Rotating group:
 O42(H42A,H42B), O51(H51A,H51B), O41(H41A,H41B), O44(H44A,H44B), O45(H45A,
 H45B), O43(H43A,H43B)
5.d Aromatic/amide H refined with riding coordinates:
 C27(H27), C24(H24), C2(H2), C23(H23), C3(H3), C21(H21), C13(H13), C17(H17),
 C20(H20), C29(H29), C9(H9), C12(H12), C30(H30), C8(H8), C4(H4), C1(H1),
 C18(H18), C10(H10), C19(H19), C7(H7), C22(H22), C28(H28), C11(H11), C14(H14)
;
_shelx_res_checksum              26184
_shelx_hkl_checksum              65663
_olex2_submission_special_instructions 'No special instructions were received'