Assembly of sandwiched-type ruthenium-containing polyoxometalates for efficient construction of C-C bonds
Xiong, Lijuan; Liu, Sen; Chen, Wenjing; Yang, Mengnan; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Chemical Communications  (2026) –; doi:10.1039/D6CC00285D

data_7135630
_publ_section_title
;
 Assembly of sandwich-type ruthenium-containing polyoxometalates for
 efficient construction of C-C bonds.
;
_journal_issue                   28
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7353
_journal_page_last               7356
_journal_paper_doi               10.1039/d6cc00285d
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'H47 K8 Na3 O98.5 Ru4 W18, 1.5(H2 O)'
_chemical_formula_sum            'H50 K8 Na3 O100 Ru4 W18'
_chemical_formula_weight         5745.75
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2025-11-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-11-19 deposited with the CCDC.	2026-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                84.1350(10)
_cell_angle_beta                 81.9160(10)
_cell_angle_gamma                73.4810(10)
_cell_formula_units_Z            1
_cell_length_a                   11.9922(3)
_cell_length_b                   12.0664(3)
_cell_length_c                   15.9420(4)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    150.01
_cell_measurement_theta_max      28.328
_cell_measurement_theta_min      2.325
_cell_volume                     2184.95(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27258
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.255
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              Microfocus
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    24.778
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1079 before and 0.0610 after correction. The Ratio of minimum to maximum transmission is 0.6013. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    4.367
_exptl_crystal_description       needle
_exptl_crystal_F_000             2543
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.243
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         7766
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.256
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0213P)^2^+33.8018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7359
_reflns_number_total             7766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cc00285d2.cif
_cod_data_source_block           m7412_0m
_cod_depositor_comments          'Adding full bibliography for 7135630.cif.'
_cod_database_code               7135630
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.242
_shelx_estimated_absorpt_t_min   0.083
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups, H4 of O4, H10W of O10W, H39 of O39
 At 1.2 times of:
  H5W of O5W, H3W of O3W, H2W of O2W, H4W of O4W, H12W of O12W, H14W of O14W,
  H11W of O11W, H40 of O40
2. Restrained distances
 Ru1-H17B_$8 \\sim Ru1-H17A_$8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O38 \\sim O12W: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(Na1) \\sim Ueq, Uanis(O11W) \\sim Ueq, Uanis(O13W) \\sim Ueq, Uanis(O14W)
\\sim Ueq, Uanis(O6W) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O12W) \\sim Ueq, Uanis(O38) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: K4A(0.8) K4B(0.2) Na1(0.5) O6W(0.75) H6WA(0.75) H6WB(0.75)
 O12W(0.5) H12W(0.5) O13W(0.5) H13A(0.5) H13B(0.5) O14W(0.75) H14W(0.75)
 O36(0.5) H36A(0.5) H36B(0.5) O37(0.75) H37A(0.75) H37B(0.75) O38(0.5)
 H38A(0.5) H38B(0.5) O39(0.25) H39(0.25) O40(0.5) H40(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2W), O3W(H3W), O4(H4), O4W(H4W), O5W(H5W), O6W(H6WA,
 H6WB), O7W(H7WA,H7WB), O8W(H8WA,H8WB), O9W(H9WA,H9WB), O10W(H10W), O11W(H11W),
 O12W(H12W), O13W(H13A,H13B), O14W(H14W), O17(H17A,H17B), O36(H36A,H36B),
 O37(H37A,H37B), O38(H38A,H38B), O39(H39), O40(H40)
;
_shelx_res_checksum              39572
_shelx_hkl_checksum              85135
_olex2_submission_special_instructions 'No special instructions were received'