Template-Assisted Alloying of Atom-Precise Silver Nanocluster: A New Approach to Generate Cluster Functionality
Mandal, Sukhendu; Biswas, Sourav; Das, Anish Kumar; Manna, Surya Sekhar; Pathak, Biswarup; Chemical Science  (2022) –; doi:10.1039/D2SC04390D

data_1567592
_publ_section_title
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 Template-Assisted Alloying of Atom-Precise Silver Nanocluster: A New
 Approach to Generate Cluster Functionality
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC04390D
_journal_year                    2022
_chemical_formula_moiety         'C64 H102 Ag20 F24 N4 O16 S10, 2(C2 H6 O), S'
_chemical_formula_sum            'C68 H114 Ag20 F24 N4 O18 S11'
_chemical_formula_weight         4241.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-07-04 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.3970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3357(12)
_cell_length_b                   16.1055(12)
_cell_length_c                   23.5813(17)
_cell_measurement_reflns_used    8577
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.41
_cell_volume                     6185.9(8)
_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      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0959
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            89860
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.439
_diffrn_reflns_theta_min         2.415
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.356
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.277
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             4052
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.038
_refine_diff_density_max         5.121
_refine_diff_density_min         -3.332
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         15437
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1295
_refine_ls_R_factor_gt           0.0717
_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^)+(0.1021P)^2^+60.1172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9045
_reflns_number_total             15437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04390d1.cif
_cod_data_source_block           agcutbtea
_cod_database_code               1567592
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.741
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C3 \\sim C2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Ag06 \\sim C2 \\sim Ag07 \\sim C3 \\sim F1 \\sim F3 \\sim F2: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C21 \\sim C01D: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C2 \\sim C3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C2 \\sim C3 \\sim F1 \\sim F3 \\sim F2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C2 \\sim O1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Ag04 \\sim Ag06 \\sim Ag0A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C01X \\sim C01D: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
S00F \\sim Ag09 \\sim S00D: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C3 \\sim F3 \\sim F2 \\sim F1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
S1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
3. Others
 Fixed Sof: O1(0.33333) O3(0.33333) O2(0.33333)
 Fixed U11: C3(0.089793) F1(0.140624) F2(0.149074) F3(0.178836)
 Fixed U12: C3(0.031426) F1(0.018004) F2(0.019661) F3(0.037734)
 Fixed U13: C3(0.010766) F1(-0.037496) F2(-0.000183) F3(-0.001049)
 Fixed U22: C3(0.07593) F1(0.10283) F2(0.1089) F3(0.10468)
 Fixed U23: C3(0.02434) F1(0.02347) F2(0.031) F3(0.00883)
 Fixed U33: C3(0.05772) F1(0.06203) F2(0.11064) F3(0.09281)
4.a Secondary CH2 refined with riding coordinates:
 C01T(H6,HL)
4.b Idealised Me refined as rotating group:
 C017(H01A,H01B,H01C), C018(H01D,H01E,H01F), C01B(H01G,H01H,H01I), C01E(H01J,
 H01K,H01L), C01F(H01M,H01N,H01O), C01H(H01P,H01Q,H01R), C01I(H01S,H01T,H01U),
 C01J(H01V,H01W,H01X), C01K(H01Y,H,HA), C01L(H01Z,HB,HC), C01M(H01,HD,HE),
 C01N(H1,HF,HG), C01Q(H2,HH,HI), C01R(H3,HJ,HK), C01U(H4,HM,HN), C01X(H5,HO,HP),
  C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
4.c Idealised tetrahedral OH refined as rotating group:
 O00Z(H00Z)
;
_shelx_res_checksum              27145
_shelx_hkl_checksum              8623
_olex2_submission_special_instructions 'No special instructions were received'