Controllable syntheses of two structurally new {AsW<sub>9</sub>O<sub>33</sub>}-mediated silver alkynyl clusters.
Liu, Qingqing; Feng, Yeqin; Liu, Tianfu; Zhao, Mengyun; Li, Yurui; Lv, Hongjin; Yang, Guo-Yu; Nanoscale 17 (2025) 21475–21480; doi:10.1039/d5nr03313f

data_1575578
_publ_section_title
;
 Controllable syntheses of two structurally new
 {AsW<sub>9</sub>O<sub>33</sub>}-mediated silver alkynyl clusters.
;
_journal_issue                   37
_journal_name_full               Nanoscale
_journal_page_first              21475
_journal_page_last               21480
_journal_paper_doi               10.1039/d5nr03313f
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'C162 H258 Ag48 As2 N12 O90 W18'
_chemical_formula_sum            'C162 H258 Ag48 As2 N12 O90 W18'
_chemical_formula_weight         12450.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-05-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-06-25 deposited with the CCDC.	2025-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.926(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7989(12)
_cell_length_b                   23.745(3)
_cell_length_c                   35.279(12)
_cell_measurement_reflns_used    9358
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.0620
_cell_measurement_theta_min      2.1850
_cell_volume                     14020(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.126a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.126a 64-bit (release 11-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.126a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -107.00 -41.00   0.50    0.76    --  -17.62-178.00-150.00  132
  2  \w    -23.00  65.00   0.50    0.76    --  -17.62  19.00  60.00  176
  3  \w    -75.00 -50.00   0.50    0.76    --  -17.62 133.00  22.00   50
  4  \w    -87.00 -62.00   0.50    0.76    --  -17.62 137.00-159.00   50
  5  \w    -24.00  65.00   0.50    0.76    --  -17.62  19.00 -30.00  178
  6  \w     46.00  71.00   0.50    0.76    --   13.87-137.00 137.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0022939000
_diffrn_orient_matrix_UB_12      0.0293438000
_diffrn_orient_matrix_UB_13      -0.0035745000
_diffrn_orient_matrix_UB_21      0.0141270000
_diffrn_orient_matrix_UB_22      -0.0057120000
_diffrn_orient_matrix_UB_23      -0.0178595000
_diffrn_orient_matrix_UB_31      -0.0395142000
_diffrn_orient_matrix_UB_32      -0.0003333000
_diffrn_orient_matrix_UB_33      -0.0086295000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.808
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            93992
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.886
_diffrn_reflns_theta_min         2.103
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.911
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.126a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.949
_exptl_crystal_description       block
_exptl_crystal_F_000             11376
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.906
_refine_diff_density_min         -2.421
_refine_diff_density_rms         0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         32710
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0651
_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^)+(0.0869P)^2^+347.7025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20995
_reflns_number_total             32710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr03313f2.cif
_cod_data_source_block           exp_4503_auto_sq
_cod_depositor_comments
'Adding full bibliography for 1575578--1575579.cif.'
_cod_database_code               1575578
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'As W O Ag'
_chemical_oxdiff_usercomment     'As W O Ag'
_shelx_estimated_absorpt_t_max   0.244
_shelx_estimated_absorpt_t_min   0.198
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C61-C26 = C26-C73
 2.5 with sigma of 0.02
 C56-C12 = C12-C3
 2.5 with sigma of 0.02
 C62-C19 = C19-C16
 2.5 with sigma of 0.02
 C61-C6
 1.54 with sigma of 0.02
 C6-C73
 1.54 with sigma of 0.02
 C56-C34
 1.54 with sigma of 0.02
 C5-C31
 1.54 with sigma of 0.02
 C1-C65
 1.54 with sigma of 0.02
 C28-C80
 1.54 with sigma of 0.02
 C34-C56
 1.54 with sigma of 0.02
 C3-C34
 1.54 with sigma of 0.02
 C12-C34
 1.54 with sigma of 0.02
 C18-C44
 1.54 with sigma of 0.02
 C23-C42
 1.54 with sigma of 0.02
 C11-C4 = C4-C18
 2.5 with sigma of 0.02
 C18-C11 = C11-C4
 2.5 with sigma of 0.02
 C44-C4
 1.54 with sigma of 0.02
 C44-C18
 1.54 with sigma of 0.02
 C11-C44
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O28) = Uanis(C10) = Uanis(C70) = Uanis(O32) = Uanis(C4) = Uanis(O34) =
Uanis(C17) = Uanis(O8) = Uanis(O36) = Uanis(O10) = Uanis(C7) = Uanis(C39) =
Uanis(N4) = Uanis(C9) = Uanis(O18) = Uanis(C12) = Uanis(C24) = Uanis(C11) =
Uanis(C28) = Uanis(N6) = Uanis(N3) = Uanis(C42) = Uanis(C30) = Uanis(C22) =
Uanis(C35) = Uanis(C37) = Uanis(C40) = Uanis(C20) = Uanis(O19) = Uanis(C43) =
Uanis(C45) = Uanis(C3) = Uanis(C49) = Uanis(C47) = Uanis(C51) = Uanis(C18) =
Uanis(C32) = Uanis(C6) = Uanis(C54) = Uanis(C8) = Uanis(C55) = Uanis(C23) =
Uanis(C57) = Uanis(C64) = Uanis(C68) = Uanis(C71) = Uanis(C66) = Uanis(C77) =
Uanis(C72) = Uanis(C78) = Uanis(C41) = Uanis(C79) = Uanis(C25) = Uanis(C67) =
Uanis(C59) = Uanis(C74) = Uanis(C60) = Uanis(C2) = Uanis(C44) = Uanis(C5) =
Uanis(C33) = Uanis(C29) = Uanis(C46) = Uanis(C34) = Uanis(C27) = Uanis(C56) =
Uanis(C48) = Uanis(C16) = Uanis(C36) = Uanis(C62) = Uanis(C50) = Uanis(C21) =
Uanis(O5) = Uanis(C52) = Uanis(C65) = Uanis(C38) = Uanis(C1) = Uanis(C53) =
Uanis(C69) = Uanis(C31) = Uanis(C15) = Uanis(C80) = Uanis(C13) = Uanis(C81) =
Uanis(C75) = Uanis(C82) = Uanis(C19) = Uanis(C58)
Uanis(C14) = Uanis(C76) = Uanis(C6) = Uanis(C61) = Uanis(C26) = Uanis(C73) =
Uanis(C21) = Uanis(C46) = Uanis(C43) = Uanis(C20) = Uanis(C77) = Uanis(C2)
Uanis(N7) = Uanis(N5) = Uanis(N2)
4. Others
 Sof(Ag2B)=1-FVAR(1)
 Sof(Ag2A)=FVAR(1)
 Sof(Ag1B)=1-FVAR(2)
 Sof(Ag1A)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C33(H33), C70(H70), C47(H47)
5.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C27(H27A,H27B,H27C), C52(H52A,H52B,H52C), C53(H53A,H53B,
 H53C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C58(H58A,
 H58B,H58C), C42(H42A,H42B,H42C), C68(H68A,H68B,H68C), C71(H71A,H71B,H71C),
 C22(H22A,H22B,H22C), C39(H39A,H39B,H39C), C78(H78A,H78B,H78C), C37(H37A,H37B,
 H37C), C79(H79A,H79B,H79C), C17(H17A,H17B,H17C), C67(H67A,H67B,H67C), C20(H20A,
 H20B,H20C), C74(H74A,H74B,H74C), C9(H9A,H9B,H9C), C2(H2A,H2B,H2C), C43(H43A,
 H43B,H43C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C29(H29A,H29B,H29C), C3(H3A,
 H3B,H3C), C12(H12A,H12B,H12C), C56(H56A,H56B,H56C), C16(H16A,H16B,H16C),
 C62(H62A,H62B,H62C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C), C65(H65A,H65B,
 H65C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C69(H69A,H69B,H69C), C75(H75A,H75B,
 H75C), C19(H19A,H19B,H19C), C73(H73A,H73B,H73C), C61(H61A,H61B,H61C), C26(H26A,
 H26B,H26C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75779
_shelx_fab_checksum              80548
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.703
_oxdiff_exptl_absorpt_empirical_full_min 0.721