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_1573239
_publ_section_title
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 Designed construction of two new atom-precise three-dimensional and
 two-dimensional Ag<sub>12</sub> cluster-assembled materials.
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_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         'C36 H45 Ag6 F9 N4 O6 S3, 1[C4H9NO]'
_chemical_formula_sum            'C40 H54 Ag6 F9 N5 O7 S3'
_chemical_formula_weight         1631.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-07-23
_audit_creation_method
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Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
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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                90
_cell_formula_units_Z            8
_cell_length_a                   21.868(3)
_cell_length_b                   22.557(3)
_cell_length_c                   22.892(3)
_cell_measurement_reflns_used    4674
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.17
_cell_measurement_theta_min      2.54
_cell_volume                     11292(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      273.15
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2248
_diffrn_reflns_av_unetI/netI     0.1141
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            76830
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         2.070
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.227
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1833 before and 0.0985 after correction. 
The Ratio of minimum to maximum transmission is 0.8625. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_description       block
_exptl_crystal_F_000             6368
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.578
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9365
_refine_ls_number_restraints     506
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0382P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5705
_reflns_number_total             9365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr03992k2.cif
_cod_data_source_block           231021_rn_tus42_colorless_90k__a
_cod_depositor_comments
'Adding full bibliography for 1573239--1573240.cif.'
_cod_database_code               1573239
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.664
_shelx_estimated_absorpt_t_min   0.617
_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. 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
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18)
4.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 392 electrons were 
found in a volume of 2712\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C4H9NO] per formula unit 
which account for 384 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              709
_shelx_fab_checksum              31031
_olex2_submission_special_instructions 'No special instructions were received'