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_1574001
_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 N6 O6 S3, C3 H7 N O'
_chemical_formula_sum            'C42 H52 Ag6 F9 N7 O7 S3'
_chemical_formula_weight         1681.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-24 deposited with the CCDC.	2025-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.57(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.994(5)
_cell_length_b                   14.021(3)
_cell_length_c                   29.259(6)
_cell_measurement_reflns_used    5367
_cell_measurement_temperature    90
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      1.6
_cell_volume                     11063(4)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0561
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            61389
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.612
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_exptl_absorpt_coefficient_mu    2.195
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.019
_exptl_crystal_description       block
_exptl_crystal_F_000             6560
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.762
_refine_diff_density_min         -1.415
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         9951
_refine_ls_number_restraints     744
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1172P)^2^+71.4546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1860
_refine_ls_wR_factor_ref         0.1931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8609
_reflns_number_total             9951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08408j2.cif
_cod_data_source_block           26_02_90K
_cod_depositor_comments
'Adding full bibliography for 1573999--1574002.cif.'
_cod_database_code               1574001
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.810
_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. Restrained distances
 N7-C41 \\sim N7-C23
 with sigma of 0.02
 C30-C29 \\sim C31-C30 \\sim C31-C19 \\sim C34-C19 \\sim C34-C33 \\sim C33-C29
 with sigma of 0.02
 C29-C31 \\sim C31-C34 \\sim C29-C34 \\sim C30-C19 \\sim C19-C33 \\sim C30-C33
 with sigma of 0.02
 F9-C42 \\sim F8-C42 \\sim F7-C42
 with sigma of 0.02
 F8-F9 \\sim F9-F7 \\sim F8-F7
 with sigma of 0.02
 C28-C27 \\sim C27-C26 \\sim C32-C28 \\sim C32-C18
 with sigma of 0.02
 N3-C26 \\sim N3-C18
 with sigma of 0.02
 N5-C9 \\sim N4-C28 \\sim N9-C28 \\sim N8-C9
 with sigma of 0.02
 N5-N4 \\sim N9-N8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5 \\sim C39 \\sim O6: within 5A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 5A
C29 \\sim C30 \\sim C33 \\sim C34 \\sim C19 \\sim C31: within 5A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 5A
O40 \\sim C7 \\sim N7 \\sim C23 \\sim C41: within 5A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 5A
F9 \\sim F7 \\sim F8 \\sim C42: within 5A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 5A
N3 \\sim C26 \\sim C27 \\sim C28 \\sim C32 \\sim C18: within 5A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 5A
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17: within 5A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 5A
N4 \\sim N5 \\sim N9 \\sim N8: within 5A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 5A
Uanis(O6) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C41) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(O40) \\sim Ueq: with sigma of 0.03 and sigma for terminal
atoms of 0.06
Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(C42) \\sim
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 O5, C39, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C29, C30, C31, C19, C34, C33
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O40, C7, N7, C23, C41
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F9, F7, F8, C42
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N3, C26, C27, C28, C32, C18
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C12, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N4, N9, N5, N8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(N9)=Sof(N8)=1-FVAR(1)
 Sof(N4)=Sof(N5)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C12(H12), C29(H29)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C13(H13A,
 H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C19(H19A,H19B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B)
6.c Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C41(H41A,H41B,H41C)
6.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C43(H43), C8(H8), C10(H10), C11(H11), C18(H18), C20(H20), C21(H21),
 C24(H24), C25(H25), C26(H26), C27(H27), C32(H32)
;
_shelx_res_checksum              69681
_olex2_submission_special_instructions 'No special instructions were received'