Facile synthesis of a Ru-based polyoxometalate for efficient reduction of nitrobenzene.
Zhang, Shihao; Sun, Yahao; Chen, Wenjing; Li, Huafeng; Li, Kunhong; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9352–9358; doi:10.1039/d5dt00020c

data_7718687
_publ_section_title
;
 Facile synthesis of a Ru-based polyoxometalate for efficient reduction of
 nitrobenzene.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9352
_journal_page_last               9358
_journal_paper_doi               10.1039/d5dt00020c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C20 H16 Cl2 N4 O40 P Ru2 W11, 1[Na+], 2[H+], 10[H2O]'
_chemical_formula_sum            'C20 H38 Cl2 N4 Na O50 P Ru2 W11'
_chemical_formula_weight         3483.89
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-04-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-21 deposited with the CCDC.	2025-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                89.7310(10)
_cell_angle_beta                 76.2710(10)
_cell_angle_gamma                63.0070(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7139(5)
_cell_length_b                   13.8151(5)
_cell_length_c                   23.4730(9)
_cell_measurement_reflns_used    8283
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.30
_cell_volume                     3822.1(2)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47946
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.097
_diffrn_reflns_theta_max         25.097
_diffrn_reflns_theta_min         2.302
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              Microfocus
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.044
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1133 before and 0.0676 after correction. The Ratio of minimum to maximum transmission is 0.6833. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.027
_exptl_crystal_description       block
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.970
_refine_diff_density_min         -2.269
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         13572
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0314P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8850
_reflns_number_total             13572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00020c2.cif
_cod_data_source_block           2367306
_cod_depositor_comments          'Adding full bibliography for 7718687.cif.'
_cod_database_code               7718687
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.549
_shelx_estimated_absorpt_t_min   0.343
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O41) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(O44) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: O11(0.8) O22(0.8) O24(0.8) O39(0.8) O41(0.2) O42(0.2) O43(0.2)
 O44(0.2)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 453 electrons were 
found in a volume of 1626\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[Na+],2[H+], 10[H2O] per formula unit 
which account for 226 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23307
_shelx_hkl_checksum              82356
_shelx_fab_checksum              41946
_olex2_submission_special_instructions 'No special instructions were received'