Efficient synthesis of Au<sub>36</sub>(SR)<sub>24</sub> nanoclusters <i>via</i> the cluster-from-cluster approach.
Lin, Yan-Yan; Nan, Zi-Ang; Lei, Zhen; Wang, Quan-Ming; Nanoscale 17 (2025) 8724–8730; doi:10.1039/d5nr00203f

data_1574035
_publ_section_title
;
 Efficient synthesis of Au<sub>36</sub>(SR)<sub>24</sub> nanoclusters
 <i>via</i> the cluster-from-cluster approach.
;
_journal_issue                   14
_journal_name_full               Nanoscale
_journal_page_first              8724
_journal_page_last               8730
_journal_paper_doi               10.1039/d5nr00203f
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'C144 H96 Au36 Cl24 S24'
_chemical_formula_sum            'C144 H96 Au36 Cl24 S24'
_chemical_formula_weight         10537.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-05-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2025-01-15 deposited with the CCDC.	2025-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                81.994(3)
_cell_angle_beta                 87.439(2)
_cell_angle_gamma                66.468(3)
_cell_formula_units_Z            2
_cell_length_a                   19.0323(4)
_cell_length_b                   19.2290(6)
_cell_length_c                   30.6431(9)
_cell_measurement_reflns_used    16802
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      65.6270
_cell_measurement_theta_min      3.8760
_cell_volume                     10180.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (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)'
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_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   -114.00  -8.00   1.00    7.50    --  -40.81 -77.00  60.00  106
  2  \w   -115.00 -26.00   1.00    7.50    --  -40.81 -38.00 -60.00   89
  3  \w    -92.00  -2.00   1.00    7.50    --  -40.81 125.00 150.00   90
  4  \w     68.00 161.00   1.00   25.00    --   89.35  61.00-180.00   93
  5  \w     64.00  89.00   1.00   25.00    --   89.35  30.00 150.00   25
  6  \w     44.00 120.00   1.00   25.00    --   89.35-125.00 -30.00   76
  7  \w     29.00  92.00   1.00   25.00    --   89.35-125.00  60.00   63
  8  \w     15.00 118.00   1.00   25.00    --   89.35 -77.00 120.00  103
  9  \w     20.00  65.00   1.00   25.00    --   89.35 -77.00 -30.00   45
 10  \w     77.00 102.00   1.00   25.00    --   89.35 -77.00 -30.00   25
 11  \w      8.00 126.00   1.00   25.00    --   89.35 -15.00-180.00  118
 12  \w    103.00 164.00   1.00   25.00    --   89.35  30.00 150.00   61
 13  \w     17.00  64.00   1.00   25.00    --   89.35 -45.00  30.00   47
 14  \w     28.00  55.00   1.00   25.00    --   89.35-125.00 120.00   27
 15  \w     66.00 114.00   1.00   25.00    --   89.35-125.00 120.00   48
 16  \w    122.00 149.00   1.00   25.00    --   89.35 125.00 -30.00   27
 17  \w     27.00  67.00   1.00   25.00    --   89.35 -77.00-120.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            68318
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        65.917
_diffrn_reflns_theta_max         65.917
_diffrn_reflns_theta_min         3.596
_exptl_absorpt_coefficient_mu    52.853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.437
_exptl_crystal_description       block
_exptl_crystal_F_000             9192
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.655
_refine_diff_density_min         -3.712
_refine_diff_density_rms         0.389
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2194
_refine_ls_number_reflns         33855
_refine_ls_number_restraints     1512
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0812
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1119P)^2^+308.4854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2077
_refine_ls_wR_factor_ref         0.2379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22274
_reflns_number_total             33855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr00203f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1574029--1574035.cif.'
_cod_database_code               1574035
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained planarity
 Cl27, S27, C271, C276, C275, C274, C273, C272
 with sigma of 0.1
 Cl25, S25, C253, C252, C251, C256, C255, C254
 with sigma of 0.1
 Cl26, S26, C261, C266, C265, C264, C263, C262
 with sigma of 0.1
 Cl2, S2, C21, C22, C24, C25, C26
 with sigma of 0.1
 Cl27, C274, C273, C272, C271, C276, C275, S27
 with sigma of 0.1
2. Uiso/Uaniso restraints and constraints
Cl4 \\sim S4 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Cl7 \\sim S7 \\sim C75 \\sim C74 \\sim C73 \\sim C72 \\sim C71 \\sim C76:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Cl8 \\sim S8 \\sim C81 \\sim C86 \\sim C85 \\sim C84 \\sim C83 \\sim C82:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Cl28 \\sim S8 \\sim C281 \\sim C286 \\sim C285 \\sim C284 \\sim C283 \\sim
C282: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl9 \\sim S9 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Cl18 \\sim S18 \\sim C181 \\sim C182 \\sim C183 \\sim C184 \\sim C185 \\sim
C186: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl11 \\sim S11 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim
C116: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl3 \\sim S3 \\sim C34 \\sim C33 \\sim C32 \\sim C31 \\sim C36 \\sim C35:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Cl16 \\sim S16 \\sim C161 \\sim C162 \\sim C163 \\sim C164 \\sim C165 \\sim
C166: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl12 \\sim S12 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim
C126: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl21 \\sim S21 \\sim C213 \\sim C214 \\sim C215 \\sim C216 \\sim C211 \\sim
C212: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl24 \\sim S24 \\sim C241 \\sim C246 \\sim C245 \\sim C244 \\sim C243 \\sim
C242: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl23 \\sim S23 \\sim C235 \\sim C236 \\sim C231 \\sim C232 \\sim C233 \\sim
C234: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Au36 \\sim Cl23 \\sim S23 \\sim C235 \\sim C236 \\sim C231 \\sim C232 \\sim
C233 \\sim C234: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Cl17 \\sim S17 \\sim C171 \\sim C172 \\sim C173 \\sim C174 \\sim C175 \\sim
C176: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl1 \\sim S1 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Cl20 \\sim S20 \\sim C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim
C206: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl15 \\sim S15 \\sim C154 \\sim C155 \\sim C156 \\sim C151 \\sim C152 \\sim
C153: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl5 \\sim S5 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Cl6 \\sim S6 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Cl10 \\sim S10 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim
C106: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl13 \\sim S13 \\sim C131 \\sim C132 \\sim C133 \\sim C134 \\sim C135 \\sim
C136: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl14 \\sim S14 \\sim C141 \\sim C142 \\sim C143 \\sim C144 \\sim C145 \\sim
C146: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl19 \\sim S19 \\sim C191 \\sim C192 \\sim C193 \\sim C194 \\sim C195 \\sim
C196: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl22 \\sim S22 \\sim C221 \\sim C226 \\sim C225 \\sim C224 \\sim C223 \\sim
C222: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Au35 \\sim Au36 \\sim Cl23 \\sim S23 \\sim C235 \\sim C236 \\sim C231 \\sim
C232 \\sim C233 \\sim C234: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Au27 \\sim Au36 \\sim Cl24 \\sim S24 \\sim C241 \\sim C246 \\sim C245 \\sim
C244 \\sim C243 \\sim C242: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Cl2 \\sim S2 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Cl27 \\sim S27 \\sim C271 \\sim C276 \\sim C275 \\sim C274 \\sim C273 \\sim
C272: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl25 \\sim S25 \\sim C253 \\sim C252 \\sim C251 \\sim C256 \\sim C255 \\sim
C254: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl26 \\sim S26 \\sim C261 \\sim C266 \\sim C265 \\sim C264 \\sim C263 \\sim
C262: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Au27 \\sim Au38 \\sim Cl27 \\sim S27 \\sim C271 \\sim C276 \\sim C275 \\sim
C274 \\sim C273 \\sim C272: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Au27 \\sim Au36 \\sim Au38 \\sim Cl24 \\sim Cl27 \\sim S24 \\sim S27 \\sim C241
\\sim C246 \\sim C245 \\sim C244 \\sim C243 \\sim C242 \\sim C271 \\sim C276
\\sim C275 \\sim C274 \\sim C273 \\sim C272: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
3. Others
 Fixed Sof: Au35(0.75) Au36(0.75) Au37(0.25) Au38(0.25) Cl8(0.5) Cl22(0.75)
 Cl23(0.75) Cl24(0.75) Cl25(0.25) Cl26(0.25) Cl27(0.25) Cl28(0.5) S22(0.75)
 S23(0.75) S24(0.75) S25(0.25) S26(0.25) S27(0.25) C81(0.5) C86(0.5) H86(0.5)
 C85(0.5) H85(0.5) C84(0.5) C83(0.5) H83(0.5) C82(0.5) H82(0.5) C221(0.75)
 C226(0.75) H226(0.75) C225(0.75) H225(0.75) C224(0.75) C223(0.75) H223(0.75)
 C222(0.75) H222(0.75) C235(0.75) H235(0.75) C236(0.75) H236(0.75) C231(0.75)
 C232(0.75) H232(0.75) C233(0.75) H233(0.75) C234(0.75) C241(0.75) C246(0.75)
 H246(0.75) C245(0.75) H245(0.75) C244(0.75) C243(0.75) H243(0.75) C242(0.75)
 H242(0.75) C253(0.25) H253(0.25) C252(0.25) H252(0.25) C251(0.25) C256(0.25)
 H256(0.25) C255(0.25) H255(0.25) C254(0.25) C261(0.25) C266(0.25) H266(0.25)
 C265(0.25) H265(0.25) C264(0.25) C263(0.25) H263(0.25) C262(0.25) H262(0.25)
 C271(0.25) C276(0.25) H276(0.25) C275(0.25) H275(0.25) C274(0.25) C273(0.25)
 H273(0.25) C272(0.25) H272(0.25) C281(0.5) C286(0.5) H286(0.5) C285(0.5)
 H285(0.5) C284(0.5) C283(0.5) H283(0.5) C282(0.5) H282(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C33(H33), C32(H32), C36(H36), C35(H35), C42(H42), C43(H43), C45(H45),
  C46(H46), C52(H52), C53(H53), C55(H55), C56(H56), C62(H62), C63(H63),
 C65(H65), C66(H66), C75(H75), C73(H73), C72(H72), C76(H76), C86(H86), C85(H85),
  C83(H83), C82(H82), C92(H92), C93(H93), C95(H95), C96(H96), C102(H102),
 C103(H103), C105(H105), C106(H106), C112(H112), C113(H113), C115(H115),
 C116(H116), C122(H122), C123(H123), C125(H125), C126(H126), C132(H132),
 C133(H133), C135(H135), C136(H136), C142(H142), C143(H143), C145(H145),
 C146(H146), C155(H155), C156(H156), C152(H152), C153(H153), C162(H162),
 C163(H163), C165(H165), C166(H166), C172(H172), C173(H173), C175(H175),
 C176(H176), C182(H182), C183(H183), C185(H185), C186(H186), C192(H192),
 C193(H193), C195(H195), C196(H196), C202(H202), C203(H203), C205(H205),
 C206(H206), C213(H213), C215(H215), C216(H216), C212(H212), C226(H226),
 C225(H225), C223(H223), C222(H222), C235(H235), C236(H236), C232(H232),
 C233(H233), C246(H246), C245(H245), C243(H243), C242(H242), C253(H253),
 C252(H252), C256(H256), C255(H255), C266(H266), C265(H265), C263(H263),
 C262(H262), C276(H276), C275(H275), C273(H273), C272(H272), C286(H286),
 C285(H285), C283(H283), C282(H282)
4.b Fitted hexagon refined as free rotating group:
 C34(C33,C32,C31,C36,C35), C51(C52,C53,C54,C55,C56), C75(C74,C73,C72,C71,C76),
 C81(C86,C85,C84,C83,C82), C154(C155,C156,C151,C152,C153), C213(C214,C215,C216,
 C211,C212), C221(C226,C225,C224,C223,C222), C235(C236,C231,C232,C233,C234),
 C241(C246,C245,C244,C243,C242), C253(C252,C251,C256,C255,C254), C261(C266,C265,
 C264,C263,C262), C271(C276,C275,C274,C273,C272), C281(C286,C285,C284,C283,C282)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              89843
_shelx_hkl_checksum              22869
_shelx_fab_checksum              23138
_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
;