Synthesis, characterization and electronic properties of an icosahedral Zintl cluster [Ag@Pb 12 ] 3-
Qingxue, Ma; Shu, Cong-Cong; Qiao, Jiao-Yang; Dong, Caixia; Sun, Zhong-Ming; Chemical Communications  (2026) –; doi:10.1039/D6CC01018K

data_7135745
_publ_section_title
;
 Synthesis, characterization and electronic properties of the icosahedral
 Zintl cluster [Ag@Pb<sub>12</sub>]<sup>3</sup>.
;
_journal_issue                   37
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9473
_journal_page_last               9476
_journal_paper_doi               10.1039/d6cc01018k
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         '3(C18 H36 K N2 O6), Ag Pb12, 3(C7 H8)'
_chemical_formula_sum            'C75 H132 Ag K3 N6 O18 Pb12'
_chemical_formula_weight         4117.680
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_Int_Tables_number      148
_atom_sites_solution_primary     dual
_audit_creation_date             2026-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2026-03-22 deposited with the CCDC.	2026-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   24.9000(3)
_cell_length_b                   24.9000(3)
_cell_length_c                   29.8591(4)
_cell_measurement_reflns_used    20606
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.8930
_cell_measurement_theta_min      2.5820
_cell_volume                     16032.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.44.123a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.123a 64-bit (release 06-10-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.123a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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-Arc 150'
_diffrn_measured_fraction_theta_full 0.9964
_diffrn_measured_fraction_theta_max 0.9016
_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     12.00  52.00   0.50    6.36    --   -0.39  38.00   0.00   80
  2  \w     11.00  42.00   0.50    6.36    --   -0.39  64.00  25.00   62
  3  \w     16.00  51.00   0.50    6.36    --   -0.39  19.00 -90.00   70
  4  \w     14.00  44.00   0.50    6.36    --   -0.39  58.00-143.30   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, SynergyCustom DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0022002000
_diffrn_orient_matrix_UB_12      0.0111797000
_diffrn_orient_matrix_UB_13      0.0213616000
_diffrn_orient_matrix_UB_21      -0.0043040000
_diffrn_orient_matrix_UB_22      0.0232044000
_diffrn_orient_matrix_UB_23      -0.0103697000
_diffrn_orient_matrix_UB_31      -0.0325532000
_diffrn_orient_matrix_UB_32      -0.0204587000
_diffrn_orient_matrix_UB_33      -0.0000713000
_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  0.0215
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.9964
_diffrn_reflns_Laue_measured_fraction_max 0.9016
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            38175
_diffrn_reflns_point_group_measured_fraction_full 0.9964
_diffrn_reflns_point_group_measured_fraction_max 0.9016
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         34.07
_diffrn_reflns_theta_min         2.01
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.179
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.123a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.559
_exptl_crystal_description       block
_exptl_crystal_F_000             10953.582
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.8646
_refine_diff_density_min         -2.3385
_refine_diff_density_rms         0.3156
_refine_ls_d_res_high            0.6343
_refine_ls_d_res_low             10.1411
_refine_ls_goodness_of_fit_ref   1.0254
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     458
_refine_ls_number_reflns         13176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0254
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+183.5713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              33
_reflns_limit_h_min              0
_reflns_limit_k_max              33
_reflns_limit_k_min              0
_reflns_limit_l_max              45
_reflns_limit_l_min              -44
_reflns_number_gt                11081
_reflns_number_total             13176
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d6cc01018k2.cif
_cod_data_source_block           37-MR-20251021-59F_auto
_cod_depositor_comments          'Adding full bibliography for 7135745.cif.'
_cod_original_cell_volume        16032.7(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7135745
_chemical_oxdiff_formula         CHNOKPbAg
_cell_oxdiff_angle_alpha         89.9730(10)
_cell_oxdiff_angle_beta          90.0104(9)
_cell_oxdiff_angle_gamma         120.0160(12)
_cell_oxdiff_length_a            24.8909(3)
_cell_oxdiff_length_b            24.9033(3)
_cell_oxdiff_length_c            29.8708(4)
_cell_oxdiff_measurement_reflns_used 20618
_cell_oxdiff_volume              16032.7(3)
_exptl_crystal_mounting_method
;
 Crystals were removed from the crystallisation vial and immediately coated
 with PDMS (polydimethylsiloxane/Dimethicone, CAS: 9006-65-9 on a glass slide.
 A suitable single crystal was selected and mounted on a glass fiber using
 vacuum silicone grease as adhesive. The glass fiber with single crystal was
 mounted on copper pin with solid paraffin. Operator: DJ_Tokyo.
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name 37-MR-20251021-59F.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C1(H1a,H1b), C3(H3a,H3b), C13(H13a,H13b), C7(H7a,H7b), C4(H4a,
 H4b), C14(H14a,H14b), C8(H8a,H8b), C6(H6a,H6b), C5(H5a,H5b), C9(H9a,H9b),
 C18(H18a,H18b), C16(H16a,H16b), C15(H15a,H15b), C12(H12a,H12b), C17(H17a,H17b),
  C10(H10a,H10b), C11(H11a,H11b)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C23(H23), C22(H22), C24(H24)
2.c Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c)
;
_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 2.279
_oxdiff_exptl_absorpt_empirical_full_min 0.674