Synthesis and crystallization of a carboxylate functionalized <i>N</i>-heterocyclic carbene-based Au<sub>13</sub> cluster with strong photo-luminescence.
Yuan, Xiting; Ye, Zichen; Malola, Sami; Shekhah, Osama; Jiang, Hao; Hu, Xinyan; Wang, Jian-Xin; Wang, Hong; Shkurenko, Aleksander; Jia, Jiangtao; Guillerm, Vincent; Mohammed, Omar F.; Chen, Xiaolan; Zheng, Nanfeng; Häkkinen, Hannu; Eddaoudi, Mohamed; Chemical science 15 (2024) 16112–16117; doi:10.1039/d4sc04594g

data_1572603
_publ_section_title
;
 Synthesis and crystallization of a carboxylate functionalized
 <i>N</i>-heterocyclic carbene-based Au<sub>13</sub> cluster with strong
 photo-luminescence.
;
_journal_issue                   39
_journal_name_full               'Chemical science'
_journal_page_first              16112
_journal_page_last               16117
_journal_paper_doi               10.1039/d4sc04594g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'((Na (H2 O)3)0.67) H6.33 (Au13 (C33 H26 N4 O4)5 Cl2), 2.42(H2 O)'
_chemical_formula_sum            'C165 H145.17 Au13 Cl2 N20 Na0.67 O24.42'
_chemical_formula_weight         5445.71
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-04-06 deposited with the CCDC.	2024-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.118(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.064(1)
_cell_length_b                   27.538(1)
_cell_length_c                   35.319(1)
_cell_measurement_reflns_used    9444
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      64.68
_cell_measurement_theta_min      2.50
_cell_volume                     25345.4(15)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 v2018.7-2 (Bruker AXS Inc., 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            291486
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        62.385
_diffrn_reflns_theta_max         65.850
_diffrn_reflns_theta_min         3.851
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    14.342
_exptl_absorpt_correction_T_max  0.0999
_exptl_absorpt_correction_T_min  0.0156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1168 before and 0.0829 after correction.
The Ratio of minimum to maximum transmission is 0.1562.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       prism
_exptl_crystal_F_000             10156
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.143
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2095
_refine_ls_number_reflns         41296
_refine_ls_number_restraints     2655
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0615
_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^)+(0.1224P)^2^+69.4463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1860
_refine_ls_wR_factor_ref         0.2176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28907
_reflns_number_total             41296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04594g2.cif
_cod_data_source_block           KME_1502_sq
_cod_depositor_comments          'Adding full bibliography for 1572603.cif.'
_cod_original_cell_volume        25345(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1572603
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.480
_shelx_estimated_absorpt_t_max   0.534
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              14271
_shelx_hkl_checksum              94984
_shelx_fab_checksum              98057