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_1569123
_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         'C97 H102 Au6 N18, 2(B F4), C H2 Cl2'
_chemical_formula_sum            'C98 H104 Au6 B2 Cl2 F8 N18'
_chemical_formula_weight         2960.30
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-07
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-21 deposited with the CCDC.	2023-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9220(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.57251(16)
_cell_length_b                   22.5778(2)
_cell_length_c                   17.07448(17)
_cell_measurement_reflns_used    14075
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      73.3260
_cell_measurement_theta_min      3.8940
_cell_volume                     5154.00(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_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     10.00  36.00   0.50    0.77    --    0.00  38.00 120.00   52
  2  \w    -86.00 -23.00   0.50    0.77    --    0.00 -38.00-120.00  126
  3  \w    -28.00  86.00   0.50    0.77    --    0.00  57.00   0.00  228
  4  \w     10.00 100.00   0.50    3.07    --   98.20 -82.00-120.00  180
  5  \w    101.00 127.00   0.50    3.07    --   98.20 -82.00-180.00   52
  6  \w      9.00 128.00   0.50    3.07    --   98.20 -61.00 120.00  238
  7  \w     99.00 125.00   0.50    3.07    --   98.20 -82.00 -60.00   52
  8  \w     68.00  93.00   0.50    3.07    --   98.20 -82.00 -60.00   50
  9  \w     79.00 188.00   0.50    3.07    --   98.20  30.00-120.00  218
 10  \w     30.00 113.00   0.50    3.07    --   98.20 -77.00  60.00  166
 11  \w    131.00 188.00   0.50    3.07    --   98.20  82.00-150.00  114
 12  \w     64.00 123.00   0.50    3.07    --   98.20 -82.00 -90.00  118
 13  \w     79.00 187.00   0.50    3.07    --   98.20  30.00 -30.00  216
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0564634000
_diffrn_orient_matrix_UB_12      -0.0548307000
_diffrn_orient_matrix_UB_13      0.0380497000
_diffrn_orient_matrix_UB_21      0.0882595000
_diffrn_orient_matrix_UB_22      0.0397416000
_diffrn_orient_matrix_UB_23      0.0367764000
_diffrn_orient_matrix_UB_31      -0.0479065000
_diffrn_orient_matrix_UB_32      0.0083768000
_diffrn_orient_matrix_UB_33      0.0747710000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            31050
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.525
_diffrn_reflns_theta_min         3.277
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.684
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.647
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         10136
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0722P)^2^+32.7763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8499
_reflns_number_total             10136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01976d2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 1569121--1569126.cif.'
_cod_original_cell_volume        5153.99(10)
_cod_database_code               1569123
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.88
_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. Restrained distances
 Cl2-C2 \\sim Cl1-C2
 with sigma of 0.02
 N302-C320 \\sim N302-C317
 with sigma of 0.02
 C320-C321 \\sim C318-C317 \\sim C319-C317 \\sim C320-C322
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C317 \\sim C321 \\sim C322 \\sim C320 \\sim C318 \\sim C319: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
Cl1 \\sim Cl2 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
4. Others
 Fixed Sof: C317(0.5) H317(0.5) C321(0.5) H32A(0.5) H32B(0.5) H32C(0.5)
 C322(0.5) H32D(0.5) H32E(0.5) H32F(0.5) C320(0.5) H320(0.5) C318(0.5)
 H31C(0.5) H31D(0.5) H31E(0.5) C319(0.5) H31F(0.5) H31G(0.5) H31H(0.5) Cl1(0.5)
 Cl2(0.5) C2(0.5) H2A(0.5) H2B(0.5)
5.a Ternary CH refined with riding coordinates:
 C317(H317), C117(H117), C217(H217), C320(H320)
5.b Secondary CH2 refined with riding coordinates:
 C110(H11A,H11B), C210(H21A,H21B), C310(H31A,H31B), C2(H2A,H2B)
5.c Aromatic/amide H refined with riding coordinates:
 C204(H204), C205(H205), C206(H206), C207(H207), C104(H104), C105(H105),
 C106(H106), C107(H107), C112(H112), C113(H113), C114(H114), C115(H115),
 C215(H215), C214(H214), C213(H213), C212(H212), C307(H307), C306(H306),
 C305(H305), C304(H304), C312(H312), C313(H313), C314(H314), C315(H315)
5.d Idealised Me refined as rotating group:
 C321(H32A,H32B,H32C), C322(H32D,H32E,H32F), C119(H11C,H11D,H11E), C118(H11F,
 H11G,H11H), C218(H21C,H21D,H21E), C219(H21F,H21G,H21H), C318(H31C,H31D,H31E),
 C319(H31F,H31G,H31H)
;
_shelx_res_checksum              84688
_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 1.975
_oxdiff_exptl_absorpt_empirical_full_min 0.642