Dual tuning of nodes and functional guests of polyoxometalate@metal-organic frameworks for enhanced photocatalytic oxidative coupling.
Jiang, Zhiqiang; Zhao, Qixin; Zeng, Yang; Gong, Tengfei; Huang, Zhenxuan; Chen, Zeyu; Shen, Jiefeng; Xuan, Weimin; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9338–9345; doi:10.1039/d5dt00655d

data_7718663
_publ_section_title
;
 Dual tuning of nodes and functional guests of
 polyoxometalate@metal-organic frameworks for enhanced photocatalytic
 oxidative coupling.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9338
_journal_page_last               9345
_journal_paper_doi               10.1039/d5dt00655d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C38.019 H29.009 Br Cd2 N13.009 O6.991, O40 P V2 W10, 0.991(H2 O1), 23[H2O]'
_chemical_formula_sum            'C38.02 H76.99 Br Cd2 N13.01 O70.98 P V2 W10'
_chemical_formula_weight         4128.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-04-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-04-24 deposited with the CCDC.	2025-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.727(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2114(15)
_cell_length_b                   21.527(2)
_cell_length_c                   25.359(3)
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.488
_cell_measurement_theta_min      2.328
_cell_volume                     8228.6(15)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68883
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            69912
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.412
_diffrn_reflns_theta_max         24.617
_diffrn_reflns_theta_min         1.571
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    13.992
_exptl_absorpt_correction_T_max  0.0904
_exptl_absorpt_correction_T_min  0.0349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1550 before and 0.1106 after correction.
The Ratio of minimum to maximum transmission is 0.3861.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             7584
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.242
_refine_diff_density_min         -1.885
_refine_diff_density_rms         0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         7555
_refine_ls_number_restraints     1031
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0715P)^2^+424.9328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7251
_reflns_number_total             7555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00655d2.cif
_cod_data_source_block           pomof3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7718662--7718664.cif.
;
_cod_database_code               7718663
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.487
_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
 C20-C19
 1.46 with sigma of 0.02
 N8-C20
 1.16 with sigma of 0.02
 N8-C19
 2.62 with sigma of 0.02
 Cd1-H4A \\sim Cd1-H4B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N8 \\sim C19 \\sim C20: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O2 \\sim W1 \\sim W3 \\sim O9 \\sim O11 \\sim O12 \\sim O16 \\sim O19 \\sim V1A
\\sim V3A \\sim O9A \\sim O11A \\sim O12A \\sim O16A \\sim O19A \\sim W6 \\sim
O10 \\sim O14 \\sim O15 \\sim O17 \\sim V6A \\sim O10A \\sim O14A \\sim O15A
\\sim O17A \\sim O13 \\sim O13A \\sim O7 \\sim W2 \\sim W4 \\sim O3 \\sim O5
\\sim O20 \\sim O21 \\sim O22 \\sim O24 \\sim V2A \\sim V4A \\sim O3A \\sim O5A
\\sim O20A \\sim O21A \\sim O22A \\sim O24A \\sim W5 \\sim O25 \\sim V5A \\sim
O25A \\sim O23 \\sim O23A \\sim O26: within 2.5A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2.5A
Cd1 \\sim O8 \\sim N8 \\sim C19 \\sim C20 \\sim O1A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 1*[Sof(W1)+Sof(V1A)]+1*[Sof(W2)+Sof(V2A)]+1*[Sof(W3)+Sof(V3A)]+1*[Sof(W4)+
 Sof(V4A)]+1*[Sof(W5)+Sof(V5A)]+1*[Sof(W6)+Sof(V6A)]=5 with esd of 0
 Sof(N8)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=1-FVAR(1)
 Sof(O8)=Sof(H8A)=Sof(H8B)=Sof(O1A)=Sof(H1AA)=Sof(H1AB)=FVAR(1)
 Sof(O3A)=Sof(O5A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=Sof(O13A)=Sof(O14A)=
 Sof(O15A)=Sof(O16A)=Sof(O17A)=Sof(O19A)=Sof(O20A)=Sof(O21A)=Sof(O22A)=
 Sof(O23A)=Sof(O24A)=Sof(O25A)=1-FVAR(2)
 Sof(O3)=Sof(O5)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(O13)=Sof(O14)=Sof(O15)=
 Sof(O16)=Sof(O17)=Sof(O19)=Sof(O20)=Sof(O21)=Sof(O22)=Sof(O23)=Sof(O24)=
 Sof(O25)=FVAR(2)
 Sof(V1A)=1-FVAR(3)
 Sof(W1)=FVAR(3)
 Sof(V2A)=1-FVAR(4)
 Sof(W2)=FVAR(4)
 Sof(V3A)=1-FVAR(5)
 Sof(W3)=FVAR(5)
 Sof(V4A)=1-FVAR(6)
 Sof(W4)=FVAR(6)
 Sof(V5A)=1-FVAR(7)
 Sof(W5)=FVAR(7)
 Sof(V6A)=1-FVAR(8)
 Sof(W6)=FVAR(8)
 Fixed Sof: O2(0.5) O7(0.5) O18(0.5) O26(0.5)
5.a Riding coordinates:
 O8(H8A,H8B), O1A(H1AA,H1AB)
5.b Free rotating group:
 O4(H4A,H4B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C17(H17)
5.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 922 electrons were 
found in a volume of 1600\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
23[H2O] per Asymmetric Unit 
which account for 920 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              72911
_shelx_hkl_checksum              20523
_shelx_fab_checksum              3892
_olex2_submission_special_instructions 'No special instructions were received'