A tetranuclear Pr-W heterometal cluster-imbedded antimotungstate for the catalytic synthesis of benzimidazoles.
Zheng, Zhijian; Jiang, Song; Chen, Xuejiao; Liu, Haoqi; Liu, Yufeng; Dong, Yayu; Sun, Xiaopeng; Yang, Guoping; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9291–9295; doi:10.1039/d5dt00386e

data_7718694
_publ_section_title
;
 A tetranuclear Pr-W heterometal cluster-imbedded antimotungstate for the
 catalytic synthesis of benzimidazoles.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9291
_journal_page_last               9295
_journal_paper_doi               10.1039/d5dt00386e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C14 H9 Cl0.5 Na5 O177 Pr4 Sb4 W42, 0.5[]'
_chemical_formula_sum            'C14 H9 Cl0.5 Na5 O177 Pr4 Sb4 W42'
_chemical_formula_weight         11914.23
_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             2024-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-08-02 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                85.183(2)
_cell_angle_beta                 85.802(2)
_cell_angle_gamma                69.864(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5636(8)
_cell_length_b                   19.4915(11)
_cell_length_c                   48.477(3)
_cell_measurement_reflns_used    9317
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.099
_cell_measurement_theta_min      2.259
_cell_volume                     11976.8(12)
_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      100
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_unetI/netI     0.0899
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            123886
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.225
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    21.410
_exptl_absorpt_correction_T_max  0.0109
_exptl_absorpt_correction_T_min  0.0003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1698 before and 0.0983 after correction.
The Ratio of minimum to maximum transmission is 0.0275.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.304
_exptl_crystal_description       block
_exptl_crystal_F_000             10241
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.33
_refine_diff_density_max         6.062
_refine_diff_density_min         -3.646
_refine_diff_density_rms         0.859
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2252
_refine_ls_number_reflns         41574
_refine_ls_number_restraints     3358
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.1018
_refine_ls_shift/su_max          0.002
_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          0.2731
_refine_ls_wR_factor_ref         0.2823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                34676
_reflns_number_total             41574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00386e2.cif
_cod_data_source_block           Pr4tar3_sq
_cod_depositor_comments          'Adding full bibliography for 7718694.cif.'
_cod_original_cell_volume        11976.9(12)
_cod_original_formula_sum        'C14 H9 Cl0.50 Na5 O177 Pr4 Sb4 W42'
_cod_database_code               7718694
_shelx_shelxl_version_number     2018/3
_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
2. Restrained distances
 C7-C8
 1.55 with sigma of 0.02
 C11-C10
 1.55 with sigma of 0.02
 W34-O110
 1.65 with sigma of 0.02
 W41-O130
 1.65 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim O1L \\sim O1W \\sim O2 \\sim O2L \\sim O2W \\sim O3 \\sim O3L \\sim
O3W \\sim O4 \\sim O4L \\sim O4W \\sim O5 \\sim O5L \\sim O5W \\sim O6 \\sim
O6L \\sim O6W \\sim O7 \\sim O7L \\sim O7W \\sim O8 \\sim O8L \\sim O8W \\sim
O9 \\sim O9L \\sim O9W \\sim O10 \\sim O10L \\sim O10W \\sim O11 \\sim O11L
\\sim O12 \\sim O12L \\sim O15W \\sim O13 \\sim O13L \\sim O13W \\sim O14 \\sim
O14L \\sim O15 \\sim O15L \\sim O16 \\sim O16L \\sim O17 \\sim O17L \\sim O18
\\sim O18L \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim
O25 \\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim
O33 \\sim O34 \\sim O35 \\sim O36 \\sim O37 \\sim O38 \\sim O39 \\sim O40 \\sim
O41 \\sim O42 \\sim O43 \\sim O44 \\sim O45 \\sim O46 \\sim O47 \\sim O48 \\sim
O49 \\sim O50 \\sim O51 \\sim O52 \\sim O53 \\sim O54 \\sim O55 \\sim O56 \\sim
O57 \\sim O58 \\sim O59 \\sim O60 \\sim O61 \\sim O62 \\sim O63 \\sim O64 \\sim
O65 \\sim O66 \\sim O67 \\sim O68 \\sim O69 \\sim O70 \\sim O71 \\sim O72 \\sim
O73 \\sim O74 \\sim O75 \\sim O76 \\sim O77 \\sim O78 \\sim O79 \\sim O80 \\sim
O81 \\sim O82 \\sim O83 \\sim O84 \\sim O85 \\sim O86 \\sim O87 \\sim O88 \\sim
O89 \\sim O90 \\sim O91 \\sim O92 \\sim O93 \\sim O94 \\sim O95 \\sim O96 \\sim
O97 \\sim O98 \\sim O99 \\sim O100 \\sim O101 \\sim O102 \\sim O103 \\sim O104
\\sim O105 \\sim O106 \\sim O107 \\sim O108 \\sim O109 \\sim O110 \\sim O111
\\sim O112 \\sim O113 \\sim O114 \\sim O115 \\sim O116 \\sim O117 \\sim O118
\\sim O119 \\sim O120 \\sim O121 \\sim O122 \\sim O123 \\sim O124 \\sim O125
\\sim O126 \\sim O127 \\sim O128 \\sim O129 \\sim O130 \\sim O131 \\sim O132
\\sim O133 \\sim O134 \\sim O135 \\sim O136 \\sim O137 \\sim O138 \\sim O139
\\sim O140 \\sim O141 \\sim O142 \\sim O143 \\sim O144 \\sim O145 \\sim O146
\\sim O14W \\sim O12W \\sim O15X: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3A
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(Cl1) \\sim Ueq, Uanis(O12W) \\sim Ueq, Uanis(O14W) \\sim Ueq, Uanis(O15W)
\\sim Ueq, Uanis(O15X) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(W33A) \\sim Ueq, Uanis(W33) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: W33(0.98) Cl1(0.5) O15W(0.5) O14W(0.5) O12W(0.5) W33A(0.02)
 O15X(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              71158
_shelx_hkl_checksum              74306
_shelx_fab_checksum              6033
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'