Sc(OTf)3-Induced, Selective Removal of Alkynyl Ligands from Heteroleptic Au13 and Au38 Nanoclusters
Huang, Zengguang; Takano, Shinjiro; Tsukuda, Tatsuya; Nanoscale  (2025) –; doi:10.1039/D5NR03977K

data_1576388
_publ_section_title
;
 Sc(OTf)3-Induced, Selective Removal of Alkynyl Ligands from Heteroleptic
 Au13 and Au38 Nanoclusters
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/D5NR03977K
_journal_year                    2025
_chemical_formula_sum            'C154 H139 Au13 F6 N3 O6 P10 S2'
_chemical_formula_weight         5176.06
_chemical_name_common            'Au13(dppe)5(PA)2(OTf)3 big xtal CH3CN/Ether'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2025-09-02 deposited with the CCDC.	2025-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.0640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.5630(6)
_cell_length_b                   21.6738(6)
_cell_length_c                   30.9636(7)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      25.3464
_cell_measurement_theta_min      2.2998
_cell_volume                     17025.1(7)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service v8.5.1.2 Release'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_diffrn_ambient_temperature      100.0(5)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8VENTURE with PHOTON 3'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            132753
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         2.26
_diffrn_source                   'Microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.326
_exptl_absorpt_correction_T_max  0.24
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_type   'Numerical Mu From Formula'
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.019
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             9580
_exptl_crystal_size_max          0.634
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.176
_refine_diff_density_max         1.895
_refine_diff_density_min         -1.508
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         15563
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0137P)^2^+460.1683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14286
_reflns_number_total             15563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr03977k2.cif
_cod_data_source_block           20240322Au13dppe5PA2_OTf
_cod_database_code               1576388
_shelx_res_checksum              31271
_shelx_fab_checksum              1767