Unexpected structural transformation into noria-like Ag<sub>13</sub> metal clusters and a copper-doping induced boost in photoluminescence.
Peng, Su-Kao; Lu, Zhou; Xie, Mo; Huang, Yong-Liang; Luo, Dong; Wang, Jia-Nan; Zhu, Xiao-Wei; Li, Xue; Zhou, Xiao-Ping; Li, Dan; Chemical communications (Cambridge, England) 56 (2020) 4789–4792; doi:10.1039/c9cc09818f

data_7126065
_publ_section_title
;
 Unexpected structural transformation into noria-like Ag<sub>13</sub>
 metal clusters and a copper-doping induced boost in photoluminescence.
;
_journal_issue                   35
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4789
_journal_page_last               4792
_journal_paper_doi               10.1039/c9cc09818f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C94 H46 Ag11.5 Cu1.5 F36 N12'
_chemical_formula_sum            'C94 H46 Ag11.5 Cu1.5 F36 N12'
_chemical_formula_weight         3363.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-26 deposited with the CCDC.	2020-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                61.283(2)
_cell_angle_beta                 67.640(2)
_cell_angle_gamma                61.420(2)
_cell_formula_units_Z            1
_cell_length_a                   15.4952(4)
_cell_length_b                   15.5896(3)
_cell_length_c                   15.5997(3)
_cell_measurement_reflns_used    15973
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.2340
_cell_measurement_theta_min      5.0790
_cell_volume                     2846.14(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.963
_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    -65.00   3.00   0.50    0.50    --   -2.20 -64.00 -68.00  136
  2  \w     18.00  43.00   0.50    0.50    --   -2.20  64.00  67.00   50
  3  \w    -39.00 -12.00   0.50    0.50    --    2.20 -64.00 -68.00   54
  4  \w     33.00  58.00   0.50    0.50    --    2.20  64.00  67.00   50
  5  \w     64.00  97.00   0.50    0.50    --  106.30 -64.00 -68.00   66
  6  \w     80.00 195.00   0.50    0.50    --  106.30  64.00  67.00  230
  7  \w    -38.00  31.00   0.50    0.50    --   -2.20 -82.00 150.00  138
  8  \w    -29.00  -2.00   0.50    0.50    --   -2.20  82.00 120.00   54
  9  \w    -36.00  38.00   0.50    0.50    --   -2.20  82.00 -30.00  148
 10  \w    -38.00  31.00   0.50    0.50    --   -2.20 -82.00  30.00  138
 11  \w    -37.00  32.00   0.50    0.50    --    2.20 -82.00-120.00  138
 12  \w    -30.00  -3.00   0.50    0.50    --    2.20  82.00-120.00   54
 13  \w     47.00 111.00   0.50    0.50    --  106.30 -82.00-120.00  128
 14  \w     58.00 139.00   0.50    0.50    --  106.30 -82.00  60.00  162
 15  \w     17.00 123.00   0.50    0.50    --  106.30 -38.00 -60.00  212
 16  \w     19.00 129.00   0.50    0.50    --  106.30 -82.00 -30.00  220
 17  \w     75.00 174.00   0.50    0.50    --  106.30  19.00  60.00  198
 18  \w     26.00  52.00   0.50    0.50    --  106.30 -82.00  60.00   52
 19  \w     82.00 107.00   0.50    0.50    --  106.30 -82.00-180.00   50
 20  \w     27.00 140.00   0.50    0.50    --  106.30 -82.00 -90.00  226
 21  \w     83.00 163.00   0.50    0.50    --  106.30  57.00  90.00  160
 22  \w     54.00 131.00   0.50    0.50    --  106.30 -57.00 120.00  154
 23  \w     39.00 104.00   0.50    0.50    --  106.30 -19.00  60.00  130
 24  \w     40.00 140.00   0.50    0.50    --  106.30 -82.00 120.00  200
 25  \w     33.00 128.00   0.50    0.50    --  106.30 -38.00  90.00  190
;
_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      -0.0513843000
_diffrn_orient_matrix_UB_12      0.0419038000
_diffrn_orient_matrix_UB_13      0.0855486000
_diffrn_orient_matrix_UB_21      0.1006308000
_diffrn_orient_matrix_UB_22      -0.0024901000
_diffrn_orient_matrix_UB_23      -0.0000934000
_diffrn_orient_matrix_UB_31      -0.0236796000
_diffrn_orient_matrix_UB_32      0.1134862000
_diffrn_orient_matrix_UB_33      -0.0765861000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33504
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.223
_diffrn_reflns_theta_min         5.111
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    16.724
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_description       block
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.193
_refine_diff_density_min         -2.049
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         11751
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0831P)^2^+21.6957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10484
_reflns_number_total             11751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09818f2.cif
_cod_data_source_block           Ag113Cu17
_cod_depositor_comments
'Adding full bibliography for 7126064--7126066.cif.'
_cod_original_formula_sum        'C94 H46 Ag11.50 Cu1.50 F36 N12'
_cod_database_code               7126065
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N F Ag Cu'
_shelx_estimated_absorpt_t_max   0.489
_shelx_estimated_absorpt_t_min   0.286
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C34, C39, C35, C36, C37, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C39 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C39) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C42) = Uanis(C45)
Uanis(C34) = Uanis(C35)
4. Others
 Fixed Sof: Ag06(0.75) Cu1(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C29(H29), C11(H11), C24(H24), C8(H8), C5(H5), C17(H17), C19(H19),
 C21(H21), C20(H20), C6(H6), C18(H18), C7(H7), C39(H39), C35(H35), C36(H36),
 C37(H37), C38(H38), C46(H46), C45(H45), C44(H44), C43(H43), C47(H47)
5.b Fitted hexagon refined as free rotating group:
 C39(C34,C35,C36,C37,C38), C46(C45,C44,C43,C42,C47)
;
_shelx_res_checksum              62807
_platon_squeeze_void_probe_radius 1.20
_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 1.895
_oxdiff_exptl_absorpt_empirical_full_min 0.569