Snapshots of key intermediates unveiling the growth from silver ions to Ag70 nanoclusters
Luo, Xi-Ming; Huang, Shuo; Luo, Peng; Ma, Kai; Wang, Zhao-Yang; Dong, Xi-Yan; Zang, Shuang-Quan; Chemical Science 13 (2022) 11110–11118; doi:10.1039/D2SC04204E

data_1567539
_publ_section_title
;
 Snapshots of key intermediates unveiling the growth from silver ions to
 Ag70 nanoclusters
;
_journal_issue                   37
_journal_name_full               'Chemical Science'
_journal_page_first              11110
_journal_page_last               11118
_journal_paper_doi               10.1039/D2SC04204E
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         '0.5(C104 H168 Ag28 F48 N12 O44 S12)'
_chemical_formula_sum            'C52 H84 Ag14 F24 N6 O22 S6'
_chemical_formula_weight         3303.79
_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   mixed
_audit_creation_date             2021-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-28 deposited with the CCDC.	2022-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.945(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4916(4)
_cell_length_b                   18.1316(4)
_cell_length_c                   23.7184(4)
_cell_measurement_reflns_used    12259
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.3950
_cell_measurement_theta_min      3.6830
_cell_volume                     9237.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -29.00  15.00   0.50    0.50    --    0.00  57.00  30.00   88
  2  \w    -87.00 -16.00   0.50    0.50    --    0.00 -38.00 -90.00  142
  3  \w      4.00  29.00   0.50    0.50    --    0.00 -38.00 -90.00   50
  4  \w     57.00  84.00   0.50    0.50    --    0.00  57.00  30.00   54
  5  \w     87.00 147.00   0.50    2.00    --   98.80  61.00 150.00  120
  6  \w     14.00 111.00   0.50    2.00    --   98.80 -45.00   0.00  194
  7  \w      9.00 106.00   0.50    2.00    --   98.80 -61.00   0.00  194
  8  \w    103.00 141.00   0.50    2.00    --   98.80  45.00-150.00   76
  9  \w     21.00 107.00   0.50    2.00    --   98.80 -82.00   0.00  172
 10  \w     68.00 148.00   0.50    2.00    --   98.80  82.00 120.00  160
 11  \w    160.00 185.00   0.50    2.00    --   98.80  45.00-150.00   50
 12  \w     68.00 149.00   0.50    2.00    --   98.80  61.00-150.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0040841000
_diffrn_orient_matrix_UB_12      0.0581767000
_diffrn_orient_matrix_UB_13      -0.0470372000
_diffrn_orient_matrix_UB_21      0.0321955000
_diffrn_orient_matrix_UB_22      0.0537455000
_diffrn_orient_matrix_UB_23      0.0420043000
_diffrn_orient_matrix_UB_31      0.0639684000
_diffrn_orient_matrix_UB_32      -0.0307723000
_diffrn_orient_matrix_UB_33      -0.0156681000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13218
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.499
_diffrn_reflns_theta_max         66.499
_diffrn_reflns_theta_min         3.660
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.507
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.376
_exptl_crystal_description       block
_exptl_crystal_F_000             6336
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.876
_refine_diff_density_min         -3.667
_refine_diff_density_rms         0.399
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         13218
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.1149
_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^)+(0.2000P)^2^+300.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3121
_refine_ls_wR_factor_ref         0.3217
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11516
_reflns_number_total             13218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04204e4.cif
_cod_data_source_block           ag14
_cod_depositor_comments
'Adding full bibliography for 1567539--1567541.cif.'
_cod_database_code               1567539
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.185
_shelx_estimated_absorpt_t_min   0.150
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7784(16)
 0.2216(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2-C21 = N2-C22 = N2-C23
 1.45 with sigma of 0.02
 O10-C24 = O10-C21
 1.2 with sigma of 0.02
 O11-C27
 1.2 with sigma of 0.02
 O11-C28
 1.2 with sigma of 0.02
 N3-C28 = N3-C27
 1.4 with sigma of 0.02
 C27-C32
 2.3 with sigma of 0.04
 N2-C23 \\sim N2-C21 \\sim N2-C24 \\sim N2-C26 \\sim N2-C22 \\sim N2-C25_$1
 with sigma of 0.02
 N3-C30 \\sim N3-C29 \\sim N3-C32 \\sim N3-C31
 with sigma of 0.02
4. Rigid bond restraints
 C31, C27, O11, C28, N3, C32, C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, C10, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, Ag2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(F7) \\sim Ueq,
Uanis(O1) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F10) \\sim
Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=1-FVAR(1)
 Sof(C27)=Sof(H27)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C32)=Sof(H32A)=
 Sof(H32B)=Sof(H32C)=FVAR(1)
 Fixed Sof: C21(0.5) H21(0.5) C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C23(0.5)
 H23A(0.5) H23B(0.5) H23C(0.5) C24(0.5) H24(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 H25C(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
7.a Riding coordinates:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
7.b Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7)
7.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C21(H21), C24(H24), C27(H27), C28(H28)
7.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              2551
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.064
_oxdiff_exptl_absorpt_empirical_full_min 0.458