Designed construction of two new atom-precise three-dimensional and two-dimensional Ag<sub>12</sub> cluster-assembled materials.
Nakatani, Riki; Sakai, Jin; Saha, Aishik; Kondo, Ayumu; Tomioka, Rina; Kawawaki, Tokuhisa; Das, Saikat; Negishi, Yuichi; Nanoscale 17 (2025) 813–822; doi:10.1039/d4nr03992k

data_1573240
_publ_section_title
;
 Designed construction of two new atom-precise three-dimensional and
 two-dimensional Ag<sub>12</sub> cluster-assembled materials.
;
_journal_issue                   2
_journal_name_full               Nanoscale
_journal_page_first              813
_journal_page_last               822
_journal_paper_doi               10.1039/d4nr03992k
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'C15 H14 Ag2 F3 N O2 S, 1.5[C2H5OH]'
_chemical_formula_sum            'C18 H23 Ag2 F3 N O3.5 S'
_chemical_formula_weight         614.17
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-24 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   24.5604(4)
_cell_length_b                   24.5604(4)
_cell_length_c                   21.6065(6)
_cell_measurement_reflns_used    7622
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.5530
_cell_measurement_theta_min      2.9010
_cell_volume                     11287.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_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      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.956
_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     96.00 178.00   0.50    0.33    --  105.20  30.00   0.00  164
  2  \w     30.00  55.00   0.50    0.33    --  105.20 -45.00-120.00   50
  3  \w     29.00  55.00   0.50    0.33    --  105.20 -44.00-136.00   52
  4  \w     48.00 105.00   0.50    0.33    --  105.20 -77.00   0.00  114
  5  \w     31.00  56.00   0.50    0.33    --  105.20 -45.00  90.00   50
  6  \w    -17.00  63.00   0.50    0.08    --   41.30 -99.00  94.00  160
  7  \w     39.00 106.00   0.50    0.33    --  105.20 -99.00  94.00  134
  8  \w      3.00  38.00   0.50    0.08    --  -41.30  19.00 -30.00   70
  9  \w    -59.00 -32.00   0.50    0.33    -- -104.00  61.00 -30.00   54
 10  \w    -24.00  35.00   0.50    0.08    --  -41.30  19.00  90.00  118
 11  \w    -63.00 -37.00   0.50    0.33    -- -104.00  61.00 120.00   52
 12  \w   -117.00 -80.00   0.50    0.33    -- -104.00 134.00 176.00   74
 13  \w    -68.00 -42.00   0.50    0.33    -- -104.00 134.00 176.00   52
;
_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      0.0577347000
_diffrn_orient_matrix_UB_12      0.0383179000
_diffrn_orient_matrix_UB_13      -0.0416824000
_diffrn_orient_matrix_UB_21      -0.0437263000
_diffrn_orient_matrix_UB_22      -0.0088705000
_diffrn_orient_matrix_UB_23      -0.0548166000
_diffrn_orient_matrix_UB_31      0.0004783000
_diffrn_orient_matrix_UB_32      0.0609275000
_diffrn_orient_matrix_UB_33      0.0182507000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12388
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.530
_diffrn_reflns_theta_min         2.915
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.672
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       block
_exptl_crystal_F_000             5454
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4922
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0553P)^2^+89.2830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4397
_reflns_number_total             4922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr03992k2.cif
_cod_data_source_block           230111_rn_scam_90k_auto
_cod_depositor_comments
'Adding full bibliography for 1573239--1573240.cif.'
_cod_original_cell_volume        11287.2(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C18 H23 Ag2 F3 N O3.50 S'
_cod_database_code               1573240
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.218
_shelx_estimated_absorpt_t_min   0.218
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(S1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C8(H8), C10(H10), C7(H7), C11(H11)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 705 electrons were 
found in a volume of 4622\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.551[C2H5OH] per Unit Cell 
which account for 702 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13591
_shelx_fab_checksum              3391
_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 1.830
_oxdiff_exptl_absorpt_empirical_full_min 0.743