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_7126064
_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 Ag13 F36 N12'
_chemical_formula_sum            'C94 H46 Ag13 F36 N12'
_chemical_formula_weight         3429.74
_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             2018-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-25 deposited with the CCDC.	2020-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                61.894(3)
_cell_angle_beta                 68.689(2)
_cell_angle_gamma                61.905(3)
_cell_formula_units_Z            1
_cell_length_a                   15.3728(4)
_cell_length_b                   15.4794(4)
_cell_length_c                   15.4872(4)
_cell_measurement_reflns_used    33431
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.2900
_cell_measurement_theta_min      2.5250
_cell_volume                     2819.87(16)
_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 0.999
_diffrn_measured_fraction_theta_max 0.896
_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      5.00  30.00   0.50   60.00    --   -2.60  30.00  -5.00   50
  2  \w    -69.00 -34.00   0.50   60.00    --   -2.60 -30.00-165.00   70
  3  \w    -53.00 -28.00   0.50   60.00    --    2.90 -30.00-165.00   50
  4  \w    -38.00  31.00   0.50   60.00    --   -2.60 -82.00 -30.00  138
  5  \w    -14.00  36.00   0.50   60.00    --   -2.60  77.00 -90.00  100
  6  \w    -84.00  26.00   0.50   60.00    --    2.90 -38.00  30.00  220
  7  \w     40.00  65.00   0.50   60.00    --    2.90  38.00-150.00   50
  8  \w    -13.00  36.00   0.50   60.00    --    2.90  38.00-150.00   98
  9  \w    -92.00 -21.00   0.50   12.00    --   -2.40 -51.00 -79.00  142
 10  \w     37.00  87.00   0.50   12.00    --   -2.40  23.00-121.97  100
 11  \w    -32.00  -5.00   0.50   12.00    --   -2.40  23.00-121.97   54
 12  \w    -42.00 -16.00   0.50   12.00    --    2.70 -80.00 -70.50   52
 13  \w     -9.00  26.00   0.50   12.00    --    2.70 -38.00 -30.00   70
 14  \w    -22.00  56.00   0.50   12.00    --    2.70 -12.00  51.43  156
 15  \w    -74.00 -25.00   0.50   12.00    --    2.70 -12.00  51.43   98
 16  \w     -1.00  37.00   0.50   12.00    --    2.70 -80.00 -70.50   76
 17  \w    -79.00 -20.00   0.50   12.00    --    2.70 -38.00 -30.00  118
 18  \w     11.00  37.00   0.50   12.00    --    2.70 -80.00-175.79   52
 19  \w    -42.00 -17.00   0.50   12.00    --    2.70 -80.00-175.79   50
 20  \w    -48.00  -4.00   0.50   12.00    --   -2.40 -51.00 -79.00   88
 21  \w    -71.00 -45.00   0.50   12.00    --    2.70 -51.00 -79.00   52
 22  \w    -54.00 -29.00   0.50   12.00    --    2.70 -51.00 -79.00   50
 23  \w    -54.00 -29.00   0.50   12.00    --    2.70 -51.00 -79.00   50
;
_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      0.0297204000
_diffrn_orient_matrix_UB_12      -0.0119203000
_diffrn_orient_matrix_UB_13      0.0328650000
_diffrn_orient_matrix_UB_21      0.0286525000
_diffrn_orient_matrix_UB_22      -0.0502187000
_diffrn_orient_matrix_UB_23      -0.0037559000
_diffrn_orient_matrix_UB_31      0.0335442000
_diffrn_orient_matrix_UB_32      0.0211833000
_diffrn_orient_matrix_UB_33      -0.0411544000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            112942
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.067
_diffrn_reflns_theta_min         2.340
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    2.308
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80370
_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            colorless
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_description       lump
_exptl_crystal_F_000             1629
_refine_diff_density_max         2.348
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         16203
_refine_ls_number_restraints     143
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0282P)^2^+7.9141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13645
_reflns_number_total             16203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09818f2.cif
_cod_data_source_block           Ag13
_cod_depositor_comments
'Adding full bibliography for 7126064--7126066.cif.'
_cod_database_code               7126064
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Ag N H C F'
_chemical_oxdiff_usercomment     Ag13
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C37, C36, C35, C34, C39, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43, C42, C41, C40, C39, 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
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C40 \\sim C41 \\sim C39 \\sim C38 \\sim C43 \\sim C42: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C33) = Uanis(C34)
4. Others
 Fixed Sof: C34(0.5) C39(0.5) H39(0.5) C38(0.5) H38(0.5) C37(0.5) H37(0.5)
 C36(0.5) H36(0.5) C35(0.5) H35(0.5) C40(0.5) C45(0.5) H45(0.5) C44(0.5)
 H44(0.5) C43(0.5) H43(0.5) C42(0.5) H42(0.5) C41(0.5) H41(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C53(H53), C13(H13), C21(H21), C49(H49), C16(H16), C52(H52), C9(H9), C12(H12),
 C3(H3), C50(H50), C11(H11), C51(H51), C10(H10), C27(H27), C31(H31), C28(H28),
 C29(H29), C30(H30), C39(H39), C38(H38), C37(H37), C36(H36), C35(H35), C45(H45),
  C44(H44), C43(H43), C42(H42), C41(H41)
5.b Fitted hexagon refined as free rotating group:
 C34(C39,C38,C37,C36,C35), C40(C45,C44,C43,C42,C41)
;
_shelx_res_checksum              91496
_shelx_fab_checksum              57471
_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 1.317
_oxdiff_exptl_absorpt_empirical_full_min 0.778