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_1570614
_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, 1(Cl), 1[B1F4]'
_chemical_formula_sum            'C72 H108 Ag14 B Cl F4'
_chemical_formula_weight         2606.02
_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   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2hpf4s
_audit_creation_date             2023-12-15
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.04.09 svn.r3586 for OlexSys, GUI svn.r5731)
;
_audit_update_record
;
2023-12-15 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                   16.5410(9)
_cell_length_b                   16.5410(9)
_cell_length_c                   29.8249(19)
_cell_measurement_reflns_used    6390
_cell_measurement_temperature    200.01(10)
_cell_measurement_theta_max      26.9460
_cell_measurement_theta_min      2.9780
_cell_volume                     7067.0(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      200.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.865
_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    -11.00  79.00   0.50    4.00    --  -10.60  38.00  30.00  180
  2  \w    -20.00  59.00   0.50    4.00    --   10.90  57.00 150.00  158
;
_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      -0.0099316000
_diffrn_orient_matrix_UB_12      -0.0413869000
_diffrn_orient_matrix_UB_13      -0.0115953000
_diffrn_orient_matrix_UB_21      0.0470637000
_diffrn_orient_matrix_UB_22      0.0111110000
_diffrn_orient_matrix_UB_23      0.0027454000
_diffrn_orient_matrix_UB_31      -0.0118586000
_diffrn_orient_matrix_UB_32      -0.0248046000
_diffrn_orient_matrix_UB_33      0.0205775000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            9459
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.757
_diffrn_reflns_theta_min         1.971
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (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    1.837
_exptl_crystal_description       block
_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.00092(8)
_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   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3550
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0862P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2404
_reflns_number_total             3550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr05409h2.cif
_cod_data_source_block           cl@ag14-bf4
_cod_depositor_comments
'Adding full bibliography for 1570610--1570618.cif.'
_cod_original_cell_volume        7067.0(9)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1570614
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.594
_shelx_estimated_absorpt_t_min   0.530
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C3 = C5-C3 = C6-C3 = C10A-C9 = C12-C9 = C11A-C9 = C10-C9 = C11-C9 = C12A-C9
 1.54 with sigma of 0.02
 C4A-C3 = C5A-C3 = C6A-C3
 1.54 with sigma of 0.02
 C4-C5 \\sim C5-C6 \\sim C6-C4
 with sigma of 0.02
 C10-C11 \\sim C11-C12 \\sim C12-C10
 with sigma of 0.02
 C10A-C11A \\sim C11A-C12A \\sim C12A-C10A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C12A) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C9, C10A, C12, C11A, C10, C12A, C11, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 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(1)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=1-FVAR(2)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(2)
6.a Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C5(H5A,H5B,
 H5C), C12A(H12D,H12E,H12F), C11A(H11D,H11E,H11F), C5A(H5AA,H5AB,H5AC)
6.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C10A(H10D,H10E,H10F), C6A(H6AA,H6AB,H6AC),
 C4A(H4AA,H4AB,H4AC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87225
_shelx_hkl_checksum              1973
_shelx_fab_checksum              85302
_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 8.677
_oxdiff_exptl_absorpt_empirical_full_min 0.409