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_1569122
_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         'C19 H17 N4, Cl, H2 O'
_chemical_formula_sum            'C19 H19 Cl N4 O'
_chemical_formula_weight         354.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-09-21 deposited with the CCDC.	2023-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.9170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3991(2)
_cell_length_b                   9.82400(10)
_cell_length_c                   13.8269(2)
_cell_measurement_reflns_used    7268
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      71.6740
_cell_measurement_theta_min      3.4680
_cell_volume                     1750.29(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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      2.00  28.00   0.50    0.50    --    0.00  38.00-180.00   52
  2  \w    -88.00  10.00   0.50    0.50    --    0.00 -57.00   0.00  196
  3  \w    -24.00  26.00   0.50    0.50    --    0.00 -57.00 120.00  100
  4  \w    -68.00 -35.00   0.50    0.50    --    0.00 -57.00 120.00   66
  5  \w    152.00 178.00   0.50    0.50    --   95.70  61.00-180.00   52
  6  \w      6.00  36.00   0.50    0.50    --   95.70 -45.00-150.00   60
  7  \w     46.00 129.00   0.50    0.50    --   95.70 -77.00-180.00  166
  8  \w    106.00 144.00   0.50    0.50    --   95.70  61.00-180.00   76
  9  \w      7.00 117.00   0.50    0.50    --   95.70 -61.00  30.00  220
 10  \w     87.00 120.00   0.50    0.50    --   95.70 -45.00-150.00   66
 11  \w     61.00 174.00   0.50    0.50    --   95.70  77.00 -30.00  226
 12  \w     72.00 122.00   0.50    0.50    --   95.70 -61.00-180.00  100
 13  \w     71.00 149.00   0.50    0.50    --   95.70 -15.00 150.00  156
 14  \w     26.00  51.00   0.50    0.50    --   95.70 -15.00 150.00   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      0.1078647000
_diffrn_orient_matrix_UB_12      0.0346863000
_diffrn_orient_matrix_UB_13      -0.0125115000
_diffrn_orient_matrix_UB_21      -0.0400151000
_diffrn_orient_matrix_UB_22      0.1410598000
_diffrn_orient_matrix_UB_23      -0.0419176000
_diffrn_orient_matrix_UB_31      0.0323356000
_diffrn_orient_matrix_UB_32      0.0591928000
_diffrn_orient_matrix_UB_33      0.1073051000
_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  0.0176
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8598
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.121
_diffrn_reflns_theta_min         4.070
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    2.047
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67967
_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    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0550P)^2^+1.1710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1045
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3247
_reflns_number_total             3359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01976d2.cif
_cod_data_source_block           BIPc2-HCl
_cod_depositor_comments
'Adding full bibliography for 1569121--1569126.cif.'
_cod_database_code               1569122
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Free rotating group:
 O1(H1A,H1B)
1.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C17(H17A,H17B)
1.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), C19(H19), C20(H20), C21(H21), C22(H22)
;
_shelx_res_checksum              50470
_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 2.047
_oxdiff_exptl_absorpt_empirical_full_min 0.643