X-ray-triggered through-space charge transfer and photochromism in silver nanoclusters.
Ren, Zhen; Sun, Jun-Jun; Xu, Long; Luo, Peng; Ma, Zi-Wei; Li, Si; Si, Yu-Bing; Dong, Xi-Yan; Pan, Fangfang; Nanoscale 16 (2024) 2662–2671; doi:10.1039/d3nr05409h

data_1570610
_publ_section_title
;
 X-ray-triggered through-space charge transfer and photochromism in silver
 nanoclusters.
;
_journal_issue                   5
_journal_name_full               Nanoscale
_journal_page_first              2662
_journal_page_last               2671
_journal_paper_doi               10.1039/d3nr05409h
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C72 H108 Ag14, Cl'
_chemical_formula_sum            'C72 H109 Ag14 Cl O'
_chemical_formula_weight         2536.22
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2gp1nw
_audit_creation_date             2023-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-25 deposited with the CCDC.	2023-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.3155(3)
_cell_length_b                   16.3155(3)
_cell_length_c                   29.6131(5)
_cell_measurement_reflns_used    3881
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.0970
_cell_measurement_theta_min      4.3300
_cell_volume                     6826.8(2)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      199.99(10)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.956
_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    -12.00  44.00   0.50    0.50    --    0.00  38.00-150.00  112
  2  \w     53.00  85.00   0.50    0.50    --    0.00  38.00-150.00   64
  3  \w     11.00 113.00   0.50    4.50    --   95.80 -82.00 150.00  204
  4  \w    115.00 171.00   0.50    4.50    --   95.80  45.00 -60.00  112
  5  \w     26.00 119.00   0.50    4.50    --   95.80 -61.00 150.00  186
  6  \w     83.00 134.00   0.50    4.50    --   95.80  45.00 -30.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            6732
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.288
_diffrn_reflns_theta_min         3.466
_exptl_absorpt_coefficient_mu    24.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09778
_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            violet
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.959
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2964
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+20.3275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2482
_reflns_number_total             2964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr05409h2.cif
_cod_data_source_block           cl@ag14-cu-ray_sq
_cod_depositor_comments
'Adding full bibliography for 1570610--1570618.cif.'
_cod_original_cell_volume        6826.8(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1570610
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.086
_shelx_estimated_absorpt_t_min   0.065
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5A-C3 = C4A-C3 = C6A-C3 = C11A-C9A = C10A-C9A = C12A-C9A
 1.53 with sigma of 0.01
 C9-C11 = C9-C10 = C9-C12 = C6-C3 = C5-C3 = C4-C3
 1.53 with sigma of 0.01
 C8A-C9A = C9-C8
 1.5 with sigma of 0.02
 C4A-C5A \\sim C4A-C6A \\sim C5A-C6A \\sim C11A-C12A \\sim C12A-C10A \\sim
C10A-C11A
 with sigma of 0.02
 C10-C11 \\sim C10-C12 \\sim C11-C12 \\sim C4-C5 \\sim C4-C6 \\sim C5-C6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C7A)
\\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C10A) \\sim Ueq,
Uanis(C11A) \\sim Ueq, Uanis(C12A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Ag3) = Uanis(Ag3A)
Uanis(C7A) = Uanis(C7)
4. Rigid body (RIGU) restrains
 C4A, C3, C6
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C9, C12
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Sof(Ag3A)=1-FVAR(1)
 Sof(Ag3)=FVAR(1)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=1-FVAR(2)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=
 Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(2)
 Sof(C7A)=Sof(C8A)=Sof(C9A)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C11A)=
 Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(3)
 Sof(C7)=Sof(C8)=Sof(C9)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=
 Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(3)
6.a Riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C4A(H4AA,H4AB,H4AC),
 C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F)
6.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C5A(H5AA,H5AB,
 H5AC), C6A(H6AA,H6AB,H6AC), C12A(H12D,H12E,H12F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 225 electrons were 
found in a volume of 783\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
3[OH] and 10[CH3OH] per Unit Cell 
which account for 207 electrons 
per unit cell.
;
_shelx_res_checksum              20351
_shelx_hkl_checksum              75896
_shelx_fab_checksum              49083
_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
;