Linker driven site-specific catalysis in atomically precise silver cluster assemblies.
Chandrashekar, Priyanka; Karmakar, Arun; Aparna, Ravari Kandy; Singh, Laddi; Mondal, Pradip Kumar; Kundu, Subrata; Bhattacharyya, Kalishankar; Mandal, Sukhendu; Chemical science 16 (2025) 5726–5734; doi:10.1039/d4sc08408j

data_1574002
_publ_section_title
;
 Linker driven site-specific catalysis in atomically precise silver
 cluster assemblies.
;
_journal_issue                   13
_journal_name_full               'Chemical science'
_journal_page_first              5726
_journal_page_last               5734
_journal_paper_doi               10.1039/d4sc08408j
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C39 H45 Ag6 F9 N3 O6 S3'
_chemical_formula_sum            'C39 H45 Ag6 F9 N3 O6 S3'
_chemical_formula_weight         1566.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-08-24 deposited with the CCDC.	2025-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.946(5)
_cell_length_b                   27.850(6)
_cell_length_c                   18.982(4)
_cell_measurement_reflns_used    2956
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.1
_cell_measurement_theta_min      1.5
_cell_volume                     12130(5)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra Synchrotron - XRD1 BL'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
'Huber Kappa Goniometer, Pilatus 2M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            157382
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.944
_diffrn_reflns_theta_min         1.132
_exptl_absorpt_coefficient_mu    1.992
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       Plate
_exptl_crystal_F_000             6072
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.670
_refine_diff_density_min         -1.848
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.00028(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         12774
_refine_ls_number_restraints     835
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0848
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1364P)^2^+41.4224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2608
_refine_ls_wR_factor_ref         0.2755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9419
_reflns_number_total             12774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08408j2.cif
_cod_data_source_block           PC06
_cod_depositor_comments
'Adding full bibliography for 1573999--1574002.cif.'
_cod_original_cell_volume        12130(4)
_cod_database_code               1574002
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.826
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O20-C00L = O00Q-C00L
 1.2 with sigma of 0.02
 F01P-C17 = F01O-C17
 1.4 with sigma of 0.02
 F01W-C17
 1.4 with sigma of 0.02
 C01Z-C01Q
 1.5 with sigma of 0.02
 C27-C00S
 1.5 with sigma of 0.02
 C30-C00R
 1.5 with sigma of 0.02
 C17-C00L
 1.5 with sigma of 0.02
 O20-C00L \\sim O00Q-C00L
 with sigma of 0.02
 F01P-C17 \\sim F01O-C17
 with sigma of 0.02
 F01O-C17 \\sim F01W-C17
 with sigma of 0.02
 F01L-C30 \\sim F01J-C30 \\sim F20-C30
 with sigma of 0.02
 F01L-F01J \\sim F01J-F20 \\sim F01L-F20
 with sigma of 0.02
 F015-C27 \\sim F019-C27 \\sim F00K-C27
 with sigma of 0.02
 C8-C017 \\sim C8-C01Y \\sim C01Y-C01T \\sim C021-C01T \\sim C021-C01V \\sim
C01V-C017
 with sigma of 0.02
 C020-C018 \\sim C020-C01S \\sim C01S-C01I
 with sigma of 0.02
 C01Z-C01Q \\sim C2-C01Z \\sim C2-C1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Ag6A \\sim Ag6B: within 5A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 5A
O20 \\sim C00L \\sim O00Q \\sim C17 \\sim F01P \\sim F01O \\sim F01W: within 5A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 5A
C017 \\sim C8 \\sim C01Y \\sim C01T \\sim C021 \\sim C01V: within 5A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 5A
C018 \\sim C020 \\sim C01S \\sim C01I: within 5A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 5A
O00J \\sim C00R \\sim O00C \\sim C30 \\sim F01L \\sim F01J \\sim F20: within 5A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 5A
C00S \\sim C27 \\sim F00K \\sim F015 \\sim F019: within 5A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 5A
O00G \\sim C10 \\sim O17 \\sim C4 \\sim F2 \\sim F4: within 5A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 5A
C01Q \\sim C01Z \\sim C2 \\sim C1: within 5A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 5A
Ag01 \\sim O20: within 5A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 5A
Uanis(S00B) = Uanis(C017)
Uanis(S00A) = Uanis(C01Q)
4. Rigid body (RIGU) restrains
 O20, C00L, O00Q, C17, F01W, F01P, F01O
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Ag6A, Ag6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C017, C8, C01Y, C01T, C021, C01V
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C018, C020, C01S, C01I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O00J, C00R, O00C, C30, F01L, F01J, F20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00S, C27, F00K, F015, F019
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O00G, C10, O17, C4, F2, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C01Q, C01Z, C2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F01O)=0.5*(1-FVAR(2))
 Sof(F01W)=0.5*FVAR(2)
 Sof(F4)=1-FVAR(2)
 Sof(F1)=FVAR(2)
 Sof(Ag6B)=1-FVAR(3)
 Sof(Ag6A)=FVAR(3)
 Sof(Ag4B)=0.5*(1-FVAR(5))
 Sof(Ag4A)=0.5*FVAR(5)
 Fixed Sof: C10(0.5) O17(0.5)
 Fixed X: F2(0.285399) C4(0.2317) C10(0.2178) O17(0.1846)
 Fixed Y: F2(0.3851) C4(0.390901) C10(0.442669) O17(0.44)
 Fixed Z: F2(0.5) C4(0.5) C10(0.5204) O17(0.5737)
6.a Ternary CH refined with riding coordinates:
 C00I(H00I), C017(H017), C018(H018), C01Q(H01Q)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C00Y(H00A,H00B), C00Z(H00C,H00D), C2(H2A,H2B), C013(H01A,H01B),
 C01A(H01C,H01D), C01E(H01F,H01G), C01I(H01I,H01J), C01S(H01K,H01L), C01T(H01N,
 H01O), C01V(H01P,H01R), C01Y(H01S,H01T), C01Z(H01U,H01V), C020(H02A,H02B),
 C021(H02C,H02D), C8(H8A,H8B)
6.c Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00O(H00O), C00T(H00T), C00W(H00W), C010(H010), C011(H011),
 C012(H012), C014(H014), C016(H016), C01D(H01E), C01G(H01H), C01M(H01M)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82130
_shelx_fab_checksum              67757
_olex2_submission_special_instructions 'No special instructions were received'