Trinuclear ruthenium core-containing polyoxometalate-based hybrids: preparation, characterization and catalytic behavior.
Li, Huafeng; He, Peipei; Wan, Rong; Zou, Yan; Zhao, Xue; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2895–2904; doi:10.1039/c9dt04616j

data_7703402
_publ_section_title
;
 Trinuclear ruthenium core-containing polyoxometalate-based hybrids:
 preparation, characterization and catalytic behavior.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2895
_journal_page_last               2904
_journal_paper_doi               10.1039/c9dt04616j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'As4 K Na O144 W42, 2(C12 H18 Cl3 N18 O Ru3), 8(O)'
_chemical_formula_sum            'C24 H36 As4 Cl6 K N36 Na O154 Ru6 W42'
_chemical_formula_weight         12195.48
_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     dual
_audit_creation_date             2019-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-27 deposited with the CCDC.	2020-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                89.231(2)
_cell_angle_beta                 72.661(2)
_cell_angle_gamma                80.351(2)
_cell_formula_units_Z            2
_cell_length_a                   20.0498(11)
_cell_length_b                   24.3323(11)
_cell_length_c                   25.4119(12)
_cell_measurement_reflns_used    9750
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.18
_cell_volume                     11657.8(10)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 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  0.0686
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            171590
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.105
_diffrn_source_type              Microfocus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.739
_exptl_absorpt_correction_T_max  0.0017
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1296 before and 0.0790 after correction. The Ratio of minimum to maximum transmission is 0.0000. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.474
_exptl_crystal_description       block
_exptl_crystal_F_000             10600
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.180
_refine_diff_density_min         -2.043
_refine_diff_density_rms         0.811
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2466
_refine_ls_number_reflns         41423
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.1042
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2754
_refine_ls_wR_factor_ref         0.3173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27183
_reflns_number_total             41423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04616j2.cif
_cod_data_source_block           njy1_a
_cod_depositor_comments
'Adding full bibliography for 7703402--7703403.cif.'
_cod_database_code               7703402
_shelx_shelxl_version_number     2018/3
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N35-C11
 1.38 with sigma of 0.02
 N35-C24
 1.38 with sigma of 0.02
 N36-C8
 1.38 with sigma of 0.02
 C4-N27
 1.38 with sigma of 0.02
 C10-N27
 1.38 with sigma of 0.02
 C1-N19
 1.38 with sigma of 0.02
 N19-C2
 1.38 with sigma of 0.02
 C11-C24
 2.4 with sigma of 0.04
 C10-C4
 2.4 with sigma of 0.04
 O91-O78 \\sim O78-O100
 with sigma of 0.02
 O136-O126 \\sim O126-O132
 with sigma of 0.02
 O8-O35 \\sim O35-O126
 with sigma of 0.02
3. Rigid bond restraints
 N19, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O55) \\sim Ueq, Uanis(O57) \\sim Ueq, Uanis(O76) \\sim Ueq, Uanis(O77)
\\sim Ueq, Uanis(O78) \\sim Ueq, Uanis(O80) \\sim Ueq, Uanis(O84) \\sim Ueq,
Uanis(O85) \\sim Ueq, Uanis(O88) \\sim Ueq, Uanis(O97) \\sim Ueq, Uanis(O105)
\\sim Ueq, Uanis(O106) \\sim Ueq, Uanis(O113) \\sim Ueq, Uanis(O142) \\sim Ueq,
Uanis(O145) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(N30) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O4W) \\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O6W) \\sim Ueq, Uanis(O8W)
\\sim Ueq, Uanis(N34) \\sim Ueq, Uanis(N35) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(Cl6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: O35(0.7) O35B(0.3)
6.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N8(H8), N11(H11), N13(H13), N16(H16), N19(H19), N24(H24), N27(H27),
 N30(H30), N31(H31), N34(H34), N35(H35), C1(H1), C2(H2), C3(H3A), C4(H4),
 C5(H5), C6(H6), C7(H7), C8(H8A), C9(H9), C10(H10), C11(H11A), C12(H12),
 C13(H13A), C14(H14), C15(H15), C16(H16A), C17(H17), C18(H18), C19(H19A),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24A)
;
_shelx_res_checksum              10334
_shelx_fab_checksum              85116
_olex2_submission_special_instructions 'No special instructions were received'