Polyoxometalate-mediated syntheses of three structurally new silver clusters.
Zhang, Jing; Dong, Yuanyuan; Deng, Lan; Chi, Manzhou; Feng, Yeqin; Zhao, Mengyun; Lv, Hongjin; Yang, Guo-Yu; Nanoscale 16 (2024) 11518–11523; doi:10.1039/d4nr02016b

data_1571725
_publ_section_title
;
 Polyoxometalate-mediated syntheses of three structurally new silver
 clusters.
;
_journal_issue                   24
_journal_name_full               Nanoscale
_journal_page_first              11518
_journal_page_last               11523
_journal_paper_doi               10.1039/d4nr02016b
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'Ag16 C242 Co8 O82 P16 S6 Si2 W18, 4(C2 N)'
_chemical_formula_sum            'C250 Ag16 Co8 N4 O82 P16 S6 Si2 W18'
_chemical_formula_weight         10621.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_audit_creation_date             2023-12-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-02-29 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                67.8510(10)
_cell_angle_beta                 66.9270(10)
_cell_angle_gamma                78.9240(10)
_cell_formula_units_Z            1
_cell_length_a                   18.6002(2)
_cell_length_b                   22.9769(3)
_cell_length_c                   23.2397(3)
_cell_measurement_reflns_used    46554
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5450
_cell_measurement_theta_min      2.2050
_cell_volume                     8451.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_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    -86.00 -61.00   0.50    1.50    --  -17.50 152.00 151.00   50
  2  \w     13.00  65.00   0.50    1.50    --  -17.50  19.00 150.00  104
  3  \w    -55.00 -12.00   0.50    1.50    --  -17.50 122.00  -8.00   86
  4  \w    -24.00  58.00   0.50    1.50    --  -17.50  19.00 -90.00  164
  5  \w    -59.00  44.00   0.50    1.50    --   14.06 -57.00-180.00  206
  6  \w    -16.00   9.00   0.50    1.50    --   14.06 -99.00 -30.00   50
  7  \w     19.00  44.00   0.50    1.50    --   14.06 -99.00 -30.00   50
  8  \w     45.00  72.00   0.50    1.50    --   14.06-122.00 -90.00   54
  9  \w     45.00  70.00   0.50    1.50    --   14.06-178.00 -60.00   50
 10  \w     37.00  92.00   0.50    1.50    --   14.06-152.00 109.00  110
 11  \w    -62.00  44.00   0.50    1.50    --   14.06 -57.00  90.00  212
 12  \w    -73.00 -43.00   0.50    1.50    --  -17.50-178.00  30.00   60
 13  \w    -17.00  30.00   0.50    1.50    --  -17.50 -99.00 -90.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            113256
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.158
_exptl_absorpt_coefficient_mu    7.561
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.86a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.087
_exptl_crystal_description       block
_exptl_crystal_F_000             4848
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.227
_refine_diff_density_min         -1.655
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1802
_refine_ls_number_reflns         37761
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0597P)^2^+109.7717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27411
_reflns_number_total             37761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr02016b2.cif
_cod_data_source_block           1213-1_auto_sq
_cod_depositor_comments
'Adding full bibliography for 1571724--1571726.cif.'
_cod_database_code               1571725
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.328
_shelx_estimated_absorpt_t_min   0.300
_olex2_refinement_description
;
1. Restrained distances
 C124-C61
 1.54 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C118 \\sim C79 \\sim C119 \\sim C60 \\sim C121 \\sim C81: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C31 \\sim C110 \\sim C45 \\sim C124 \\sim C61: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(N2) = Uanis(N1)
3. Others
 Sof(Ag7)=1-FVAR(1)
 Sof(Ag3)=FVAR(1)
4.a Fitted hexagon refined as free rotating group:
 C118(C79,C119,C60,C121,C81)
;
_shelx_res_checksum              11450
_shelx_hkl_checksum              33723
_shelx_fab_checksum              75759
_platon_squeeze_void_probe_radius 1.20
_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
;