Photoluminescence control by atomically precise surface metallization of C-centered hexagold(i) clusters using N-heterocyclic carbenes.
Lei, Zhen; Zhao, Pei; Pei, Xiao-Li; Ube, Hitoshi; Ehara, Masahiro; Shionoya, Mitsuhiko; Chemical science 14 (2023) 6207–6215; doi:10.1039/d3sc01976d

data_1569121
_publ_section_title
;
 Photoluminescence control by atomically precise surface metallization of
 C-centered hexagold(i) clusters using N-heterocyclic carbenes.
;
_journal_issue                   23
_journal_name_full               'Chemical science'
_journal_page_first              6207
_journal_page_last               6215
_journal_paper_doi               10.1039/d3sc01976d
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C16 H18 N3, Cl'
_chemical_formula_sum            'C16 H18 Cl N3'
_chemical_formula_weight         287.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-09-21 deposited with the CCDC.	2023-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.3536(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.26934(12)
_cell_length_b                   14.15286(15)
_cell_length_c                   12.30478(15)
_cell_measurement_reflns_used    7056
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      72.7440
_cell_measurement_theta_min      4.9590
_cell_volume                     1503.42(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_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    -59.00 -16.00   0.20    0.20    --    0.00 -19.00 120.00  215
  2  \w     25.00  87.00   0.20    0.20    --    0.00  38.00 -90.00  310
  3  \w     64.00 183.00   0.20    0.60    --   93.30  77.00 -60.00  595
  4  \w     80.00 158.00   0.20    0.60    --   93.30  30.00  90.00  390
  5  \w     31.00  90.00   0.20    0.60    --   93.30 -45.00 150.00  295
  6  \w    123.00 181.00   0.20    0.60    --   93.30  45.00-180.00  290
  7  \w     94.00 119.00   0.20    0.60    --   93.30  15.00 -60.00  125
  8  \w    -16.00  59.00   0.20    0.20    --    0.00  38.00 120.00  375
  9  \w     68.00 103.00   0.20    0.60    --   93.30 -30.00 120.00  175
 10  \w     82.00 112.00   0.20    0.60    --   93.30  61.00 150.00  150
 11  \w      8.00  34.00   0.20    0.60    --   93.30 -45.00 -60.00  130
 12  \w     39.00  65.00   0.20    0.60    --   93.30 -45.00 -60.00  130
 13  \w     85.00 112.00   0.20    0.60    --   93.30 -45.00 -60.00  135
 14  \w     18.00  70.00   0.20    0.60    --   93.30 -61.00-120.00  260
 15  \w    117.00 176.00   0.20    0.60    --   93.30  61.00 150.00  295
 16  \w     66.00 116.80   0.20    0.60    --   93.30  82.00 150.00  254
;
_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      0.0182960000
_diffrn_orient_matrix_UB_12      -0.0633193000
_diffrn_orient_matrix_UB_13      -0.0959762000
_diffrn_orient_matrix_UB_21      -0.1722598000
_diffrn_orient_matrix_UB_22      0.0148887000
_diffrn_orient_matrix_UB_23      -0.0750638000
_diffrn_orient_matrix_UB_31      0.0427625000
_diffrn_orient_matrix_UB_32      0.0873017000
_diffrn_orient_matrix_UB_33      -0.0568282000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9271
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.225
_diffrn_reflns_theta_min         4.966
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    2.184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0533P)^2^+0.5303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2797
_reflns_number_total             2931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01976d2.cif
_cod_data_source_block           BIPc-HCl
_cod_depositor_comments
'Adding full bibliography for 1569121--1569126.cif.'
_cod_database_code               1569121
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              41640
_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 2.436
_oxdiff_exptl_absorpt_empirical_full_min 0.648