Synthesis and luminescence properties of two silver cluster-assembled materials for selective Fe<sup>3+</sup> sensing.
Sakai, Jin; Biswas, Sourav; Irie, Tsukasa; Mabuchi, Haruna; Sekine, Taishu; Niihori, Yoshiki; Das, Saikat; Negishi, Yuichi; Nanoscale 15 (2023) 12227–12234; doi:10.1039/d3nr01920a

data_1569357
_publ_section_title
;
 Synthesis and luminescence properties of two silver cluster-assembled
 materials for selective Fe<sup>3+</sup> sensing.
;
_journal_issue                   29
_journal_name_full               Nanoscale
_journal_page_first              12227
_journal_page_last               12234
_journal_paper_doi               10.1039/d3nr01920a
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C234 H204 Ag24 F36 N12 O24 S12'
_chemical_formula_sum            'C234 H204 Ag24 F36 N12 O24 S12'
_chemical_formula_weight         7225.68
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-07
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-04-16 deposited with the CCDC.	2023-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   59.1396(19)
_cell_length_b                   59.1396(19)
_cell_length_c                   32.143(3)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      21.330
_cell_measurement_theta_min      2.346
_cell_volume                     97358(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1201
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -70
_diffrn_reflns_limit_k_max       66
_diffrn_reflns_limit_k_min       -70
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            367620
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.121
_diffrn_reflns_theta_max         25.121
_diffrn_reflns_theta_min         1.822
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.168
_exptl_absorpt_correction_T_max  0.0912
_exptl_absorpt_correction_T_min  0.0663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1444 before and 0.0647 after correction.
The Ratio of minimum to maximum transmission is 0.7270.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       block
_exptl_crystal_F_000             31752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.204
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         19291
_refine_ls_number_restraints     3130
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1492P)^2^+612.8511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2372
_refine_ls_wR_factor_ref         0.2813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10675
_reflns_number_total             19291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr01920a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1569357--1569358.cif.'
_cod_original_cell_volume        97359(10)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               1569357
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.800
_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
 C57-C44
 1.45 with sigma of 0.001
 C50-F7
 1.29 with sigma of 0.02
 C50-F2
 1.36 with sigma of 0.02
 C50-F9
 1.27 with sigma of 0.02
 C25-F4
 1.27 with sigma of 0.02
 C25-C16
 1.45 with sigma of 0.01
 C25-F3
 1.36 with sigma of 0.02
 C25-F6
 1.29 with sigma of 0.02
 C77-C29
 1.45 with sigma of 0.001
 C55-C73
 2.2 with sigma of 0.001
 C55-C37
 2.5 with sigma of 0.001
 C29-C73
 1.5 with sigma of 0.001
 C29-C27
 1.5 with sigma of 0.001
 C35-C77
 1.5 with sigma of 0.001
 C77-C15
 1.5 with sigma of 0.001
 C29-C9
 2.1 with sigma of 0.001
 C29-C55
 2.2 with sigma of 0.001
 C61-C65
 2.5 with sigma of 0.001
 C65-C61
 2.6 with sigma of 0.001
 C58-C22
 1.55 with sigma of 0.01
 C58-C40
 1.55 with sigma of 0.01
 C56-C58
 1.55 with sigma of 0.01
 C50-F7 \\sim C50-F2 \\sim C50-F9
 with sigma of 0.02
 F7-F2 \\sim F2-F9 \\sim F9-F7
 with sigma of 0.03
 C25-F6 \\sim C25-F3 \\sim C25-F4
 with sigma of 0.02
 F6-F3 \\sim F3-F4 \\sim F4-F6
 with sigma of 0.03
 C58-C40 \\sim C58-C22 \\sim C58-C56
 with sigma of 0.02
3. Restrained planarity
 C73, C29, C27, C77, C15, C35
 with sigma of 0.1
 C15, C77, C35, C29, C73, C27
 with sigma of 0.01
4. Rigid bond restraints
 O2, C16, F3, O4, F4, C25, F6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C1 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C8 \\sim C10 \\sim C11 \\sim C12
\\sim C13 \\sim C53 \\sim C27 \\sim C55 \\sim C7 \\sim C57 \\sim C14 \\sim C16
\\sim C18 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26
\\sim C28 \\sim C29 \\sim C30 \\sim C32 \\sim C34 \\sim C36 \\sim C38 \\sim C39
\\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47
\\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C54 \\sim C56 \\sim C58
\\sim C59 \\sim C15 \\sim C61 \\sim C31 \\sim C63 \\sim C2 \\sim C60 \\sim C62
\\sim C64 \\sim C65 \\sim C33 \\sim C67 \\sim C17 \\sim C69 \\sim C35 \\sim C66
\\sim C68 \\sim C70 \\sim C72 \\sim C74 \\sim C76 \\sim C78 \\sim C71 \\sim C9
\\sim C73 \\sim C37 \\sim C75 \\sim C19 \\sim C77 \\sim N1 \\sim N3 \\sim N2
\\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim
F9: within 5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 5A
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Fixed Sof: C13(0.25) H13(0.25) C53(0.25) H53(0.25) C27(0.25) C55(0.25)
 H55(0.25) C7(0.25) H7(0.25) C57(0.25) C29(0.25) C59(0.25) H59(0.25) C15(0.25)
 C61(0.25) H61(0.25) C31(0.25) H31(0.25) C63(0.25) C2(0.25) H2(0.25) C65(0.25)
 H65(0.25) C33(0.25) H33(0.25) C67(0.25) C17(0.25) H17(0.25) C69(0.25)
 H69(0.25) C35(0.25) C71(0.25) H71(0.25) C9(0.25) H9(0.25) C73(0.25) C37(0.25)
 H37(0.25) C75(0.25) C19(0.25) H19(0.25) C77(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C12(H12), C13(H13), C53(H53), C55(H55), C7(H7), C18(H18),
 C24(H24), C28(H28), C30(H30), C32(H32), C34(H34), C36(H36), C38(H38), C39(H39),
  C41(H41), C43(H43), C47(H47), C48(H48), C59(H59), C61(H61), C31(H31), C2(H2),
 C65(H65), C33(H33), C17(H17), C69(H69), C70(H70), C74(H74), C76(H76), C78(H78),
  C71(H71), C9(H9), C37(H37), C19(H19)
7.b Fitted hexagon refined as free rotating group:
 C13(C53,C27,C55,C7,C57), C59(C15,C61,C31,C63,C2), C65(C33,C67,C17,C69,C35),
 C70(C72,C74,C76,N2,C78), C71(C9,C73,C37,C75,C19)
7.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C40(H40A,H40B,H40C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C62(H62A,H62B,H62C), C66(H66A,
 H66B,H66C), C68(H68A,H68B,H68C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67350
_shelx_hkl_checksum              27716
_shelx_fab_checksum              99437
_olex2_submission_special_instructions 'No special instructions were received'