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_1569124
_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         'C115 H96 Au6 N24, 2(B F4), C H2 Cl2'
_chemical_formula_sum            'C116 H98 Au6 B2 Cl2 F8 N24'
_chemical_formula_weight         3254.50
_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             2020-12-30
_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                 92.7197(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.44142(13)
_cell_length_b                   43.0804(4)
_cell_length_c                   17.47381(12)
_cell_measurement_reflns_used    32256
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      73.2980
_cell_measurement_theta_min      2.7220
_cell_volume                     10858.95(16)
_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 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 0.999
_diffrn_measured_fraction_theta_max 0.976
_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     -3.00  88.00   0.50    0.92    --    0.00  38.00-180.00  182
  2  \w    -14.00  83.00   0.50    0.92    --    0.00  57.00 -60.00  194
  3  \w    -18.00   7.00   0.50    0.92    --    0.00  38.00 150.00   50
  4  \w     70.00 130.00   0.50    3.70    --   98.20 -30.00  60.00  120
  5  \w     51.00 121.00   0.50    3.70    --   98.20 -30.00 150.00  140
  6  \w     69.00 187.00   0.50    3.70    --   98.20  15.00 -90.00  236
  7  \w     43.00 133.00   0.50    3.70    --   98.20 -77.00 -60.00  180
  8  \w     12.00 125.00   0.50    3.70    --   98.20 -45.00  90.00  226
  9  \w    107.00 133.00   0.50    3.70    --   98.20  45.00 -60.00   52
 10  \w      9.00 144.00   0.50    3.70    --   98.20 -15.00 -90.00  270
;
_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      0.0677356000
_diffrn_orient_matrix_UB_12      -0.0275733000
_diffrn_orient_matrix_UB_13      0.0081297000
_diffrn_orient_matrix_UB_21      -0.0062130000
_diffrn_orient_matrix_UB_22      0.0011580000
_diffrn_orient_matrix_UB_23      0.0877409000
_diffrn_orient_matrix_UB_31      -0.0822899000
_diffrn_orient_matrix_UB_32      -0.0227480000
_diffrn_orient_matrix_UB_33      -0.0053994000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59653
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.509
_diffrn_reflns_theta_min         2.732
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.935
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42977
_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            colorless
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_description       block
_exptl_crystal_F_000             6208
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.799
_refine_diff_density_min         -2.158
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1418
_refine_ls_number_reflns         21354
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+47.2881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18478
_reflns_number_total             21354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01976d2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 1569121--1569126.cif.'
_cod_database_code               1569124
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.91
_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
2. Restrained distances
 F8-B2 = F5-B2 = F6-B2 = F7-B2
 1.45 with sigma of 0.02
 F5-F6 = F5-F7 = F5-F8 = F6-F7 = F6-F8 = F7-F8
 2.35 with sigma of 0.02
 F9-B3 = F12-B3 = F10-B3 = F11-B3
 1.35 with sigma of 0.02
 F9-F10 = F9-F11 = F9-F12 = F10-F11 = F10-F12 = F11-F12
 2.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
F9 \\sim F10 \\sim F11 \\sim F12 \\sim B3: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
F5 \\sim F6 \\sim F7 \\sim F8 \\sim B2: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
N623 \\sim C618 \\sim C619 \\sim C620 \\sim C621 \\sim C622: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
N123 \\sim C117 \\sim C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
F5 \\sim F6 \\sim F7 \\sim F8 \\sim B2 \\sim F9 \\sim F10 \\sim F11 \\sim F12
\\sim B3: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
4. Others
 Fixed Sof: F5(0.5) F6(0.5) F7(0.5) F8(0.5) B2(0.5) F9(0.5) F10(0.5) F11(0.5)
 F12(0.5) B3(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C110(H11A,H11B), C117(H11C,H11D), C210(H21A,H21B), C217(H21C,H21D), C310(H31A,
 H31B), C317(H31C,H31D), C410(H41A,H41B), C417(H41C,H41D), C510(H51A,H51B),
 C517(H51C,H51D), C610(H61A,H61B), C617(H61C,H61D), C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C104(H104), C105(H105), C106(H106), C107(H107), C112(H112), C113(H113),
 C114(H114), C115(H115), C119(H119), C120(H120), C121(H121), C122(H122),
 C204(H204), C205(H205), C206(H206), C207(H207), C212(H212), C213(H213),
 C214(H214), C215(H215), C219(H219), C220(H220), C221(H221), C222(H222),
 C304(H304), C305(H305), C306(H306), C307(H307), C312(H312), C313(H313),
 C314(H314), C315(H315), C319(H319), C320(H320), C321(H321), C322(H322),
 C404(H404), C405(H405), C406(H406), C407(H407), C412(H412), C413(H413),
 C414(H414), C415(H415), C419(H419), C420(H420), C421(H421), C422(H422),
 C504(H504), C505(H505), C506(H506), C507(H507), C512(H512), C513(H513),
 C514(H514), C515(H515), C519(H519), C520(H520), C521(H521), C522(H522),
 C604(H604), C605(H605), C606(H606), C607(H607), C612(H612), C613(H613),
 C614(H614), C615(H615), C619(H619), C620(H620), C621(H621), C622(H622)
;
_shelx_res_checksum              45446
_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 1.810
_oxdiff_exptl_absorpt_empirical_full_min 0.731