Ru(iii) -based polyoxometalate tetramers as highly efficient heterogeneous catalysts for alcohol oxidation reactions at room temperature
Zou, Yan; Li, Huafeng; Zhao, Xue; Song, Junpeng; Wang, Yaqiong; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Dalton Transactions  (2021) –; doi:10.1039/D1DT01819A

data_7708090
_publ_section_title
;
 Ru(iii) -based polyoxometalate tetramers as highly efficient
 heterogeneous catalysts for alcohol oxidation reactions at room
 temperature
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01819A
_journal_year                    2021
_chemical_formula_moiety
'0.5(C12 H12 As8 K8 N8 Na18 O308 Ru6.4 W80), 4(H2O), 54[H2O]'
_chemical_formula_sum            'C6 H122 As4 K4 N4 Na9 O212 Ru3.2 W40'
_chemical_formula_weight         11982.94
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc27wnd6
_audit_creation_date             2021-08-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-05 deposited with the CCDC.	2021-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.7922(4)
_cell_length_b                   19.7922(4)
_cell_length_c                   26.1324(6)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.305
_cell_measurement_theta_min      2.429
_cell_volume                     10236.9(4)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            41367
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.306
_diffrn_reflns_theta_min         2.429
_diffrn_source_type              Microfocus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.427
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.1794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1860 before and 0.0990 after correction. The Ratio of minimum to maximum transmission is 0.2406. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.570
_exptl_crystal_description       block
_exptl_crystal_F_000             9485
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.565
_refine_diff_density_min         -1.878
_refine_diff_density_rms         0.294
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.205(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         12357
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0441P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0959
_reflns_Friedel_coverage         0.899
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                11507
_reflns_number_total             12357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01819a2.cif
_cod_data_source_block           2082158
_cod_original_cell_volume        10236.9(5)
_cod_database_code               7708090
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.227
_shelx_estimated_absorpt_t_min   0.138
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.795(13)
 0.205(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O3W)
\\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq,
Uanis(O23) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O30)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(O1W) \\sim Ueq,
Uanis(O33) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O27)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O15) \\sim Ueq,
Uanis(O19) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O22) \\sim Ueq,
Uanis(O14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
;
_shelx_res_checksum              81285
_shelx_fab_checksum              44117
_olex2_submission_special_instructions 'No special instructions were received'