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_1574031
_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         'C192 H186 Au36 S24'
_chemical_formula_sum            'C192 H216 Au36 S24'
_chemical_formula_weight         10383.87
_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
_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                90
_cell_angle_beta                 94.218(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5790(7)
_cell_length_b                   30.2707(11)
_cell_length_c                   37.2286(11)
_cell_measurement_reflns_used    2489
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      52.8580
_cell_measurement_theta_min      3.6840
_cell_volume                     22004.5(13)
_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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector_area_resol_mean 10.4273
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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    -73.00  35.00   1.00    6.00    --  -40.81  77.00 -60.00  108
  2  \w    -94.00 -25.00   1.00    6.00    --  -40.81 -57.00 150.00   69
  3  \w    -54.00 -27.00   1.00    6.00    --  -40.81 125.00   0.00   27
  4  \w    106.00 139.00   1.00   21.00    --   89.35 125.00 -30.00   33
  5  \w    102.00 129.00   1.00   21.00    --   89.35 125.00 -90.00   27
  6  \w     99.00 152.00   1.00   21.00    --   89.35 125.00  90.00   53
  7  \w     60.00 166.00   1.00   21.00    --   89.35  77.00-120.00  106
  8  \w     23.00  99.00   1.00   21.00    --   89.35 -77.00 150.00   76
  9  \w     14.00  89.00   1.00   21.00    --   89.35 -77.00   0.00   75
 10  \w     96.00 139.00   1.00   21.00    --   89.35 125.00-180.00   43
;
_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  0.2376
_diffrn_reflns_av_unetI/netI     0.3187
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            72592
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        59.143
_diffrn_reflns_theta_max         59.143
_diffrn_reflns_theta_min         3.695
_exptl_absorpt_coefficient_mu    46.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52558
_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_colour_primary    black
_exptl_crystal_density_diffrn    3.134
_exptl_crystal_description       plate
_exptl_crystal_F_000             18384
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.446
_refine_diff_density_min         -2.986
_refine_diff_density_rms         0.426
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2019
_refine_ls_number_reflns         31211
_refine_ls_number_restraints     2568
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.2292
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.2410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11316
_reflns_number_total             31211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr00203f2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 1574029--1574035.cif.'
_cod_original_cell_volume        22004.4(13)
_cod_database_code               1574031
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C58-C54 \\sim C57-C55 \\sim C208-C204 \\sim C207-C205 \\sim C47-C45 \\sim
C48-C44 \\sim C228-C224 ~
 C127-C125 \\sim C227-C225 \\sim C128-C124 \\sim C238-C234 \\sim C248-C244
\\sim C237-C235 \\sim C247-
 C245 \\sim C187-C185 \\sim C188-C184 \\sim C38-C34 \\sim C28-C24 \\sim C27-C25
\\sim C37-C35 \\sim C167-
 C165 \\sim C168-C164 \\sim C148-C144 \\sim C147-C145 \\sim C137-C135 \\sim
C138-C134 \\sim C98-C94 ~
 C97-C95 \\sim C87-C85 \\sim C88-C84 \\sim C157-C155 \\sim C158-C154 \\sim
C178-C174 \\sim C177-C175 ~
 C68-C64 \\sim C67-C65 \\sim C218-C214 \\sim C217-C215 \\sim C107-C105 \\sim
C108-C104 \\sim C118-C114
 \\sim C117-C115 \\sim C18-C14 \\sim C17-C15 \\sim C197-C195 \\sim C198-C194
\\sim C77-C75 \\sim C78-C74
 with sigma of 0.01
2. Restrained planarity
 S1, C11, C12, C13, C14, C15, C16, C17, C18
 with sigma of 0.1
 S3, C31, C32, C33, C34, C35, C36, C37, C38
 with sigma of 0.1
 S2, C21, C22, C23, C24, C25, C26, C27, C28
 with sigma of 0.1
 S5, C51, C52, C53, C54, C55, C56, C57, C58
 with sigma of 0.1
 S4, C41, C42, C43, C44, C45, C46, C47, C48
 with sigma of 0.1
 S7, C71, C72, C73, C74, C75, C76, C77, C78
 with sigma of 0.1
 S6, C61, C62, C63, C64, C65, C66, C67, C68
 with sigma of 0.1
 S9, C91, C92, C93, C94, C95, C96, C97, C98
 with sigma of 0.1
 S8, C81, C82, C83, C84, C85, C86, C87, C88
 with sigma of 0.1
 S10, C101, C102, C103, C104, C105, C106, C107, C108
 with sigma of 0.1
 S18, C181, C182, C183, C184, C185, C186, C187, C188
 with sigma of 0.1
 S19, C191, C192, C193, C194, C195, C196, C197, C198
 with sigma of 0.1
 S11, C111, C112, C113, C114, C115, C116, C117, C118
 with sigma of 0.1
 S17, C171, C172, C173, C174, C175, C176, C177, C178
 with sigma of 0.1
 S12, C121, C122, C123, C124, C125, C126, C127, C128
 with sigma of 0.1
 S13, C131, C132, C133, C134, C135, C136, C137, C138
 with sigma of 0.1
 S14, C141, C142, C143, C144, C145, C146, C147, C148
 with sigma of 0.1
 S16, C161, C162, C163, C164, C165, C166, C167, C168
 with sigma of 0.1
 S15, C151, C152, C153, C154, C155, C156, C157, C158
 with sigma of 0.1
 S20, C201, C202, C203, C204, C205, C206, C207, C208
 with sigma of 0.1
 S21, C211, C212, C213, C214, C215, C216, C217, C218
 with sigma of 0.1
 S22, C221, C222, C223, C224, C225, C226, C227, C228
 with sigma of 0.1
 S24, C241, C242, C243, C244, C245, C246, C247, C248
 with sigma of 0.1
 S23, C231, C232, C233, C234, C235, C236, C237, C238
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Au1 \\sim Au11 \\sim S1 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim
C16 \\sim C17 \\sim C18: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Au2 \\sim Au25 \\sim S3 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim
C36 \\sim C37 \\sim C38: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Au1 \\sim Au2 \\sim S2 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim
C26 \\sim C27 \\sim C28: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Au3 \\sim Au4 \\sim S5 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim
C56 \\sim C57 \\sim C58: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Au3 \\sim Au12 \\sim S4 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim
C46 \\sim C47 \\sim C48: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Au4 \\sim Au28 \\sim S6 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim
C66 \\sim C67 \\sim C68: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Au5 \\sim Au32 \\sim S7 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim
C76 \\sim C77 \\sim C78: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Au5 \\sim Au6 \\sim S8 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim
C86 \\sim C87 \\sim C88: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Au6 \\sim Au15 \\sim S9 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim
C96 \\sim C97 \\sim C98: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Au7 \\sim Au35 \\sim S10 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105
\\sim C106 \\sim C107 \\sim C108: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Au7 \\sim Au8 \\sim S11 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115
\\sim C116 \\sim C117 \\sim C118: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Au8 \\sim Au22 \\sim S12 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125
\\sim C126 \\sim C127 \\sim C128: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Au9 \\sim Au10 \\sim S13 \\sim C131 \\sim C132 \\sim C133 \\sim C134 \\sim C135
\\sim C136 \\sim C137 \\sim C138: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Au9 \\sim Au16 \\sim S14 \\sim C141 \\sim C142 \\sim C143 \\sim C144 \\sim C145
\\sim C146 \\sim C147 \\sim C148: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Au10 \\sim Au18 \\sim S15 \\sim C151 \\sim C152 \\sim C153 \\sim C154 \\sim
C155 \\sim C156 \\sim C157 \\sim C158: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Au23 \\sim Au31 \\sim S16 \\sim C161 \\sim C162 \\sim C163 \\sim C164 \\sim
C165 \\sim C166 \\sim C167 \\sim C168: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Au24 \\sim Au33 \\sim S17 \\sim C171 \\sim C172 \\sim C173 \\sim C174 \\sim
C175 \\sim C176 \\sim C177 \\sim C178: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Au31 \\sim Au34 \\sim S18 \\sim C181 \\sim C182 \\sim C183 \\sim C184 \\sim
C185 \\sim C186 \\sim C187 \\sim C188: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Au33 \\sim Au36 \\sim S19 \\sim C191 \\sim C192 \\sim C193 \\sim C194 \\sim
C195 \\sim C196 \\sim C197 \\sim C198: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Au14 \\sim Au21 \\sim S20 \\sim C201 \\sim C202 \\sim C203 \\sim C204 \\sim
C205 \\sim C206 \\sim C207 \\sim C208: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Au30 \\sim Au36 \\sim S21 \\sim C211 \\sim C212 \\sim C213 \\sim C214 \\sim
C215 \\sim C216 \\sim C217 \\sim C218: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Au29 \\sim Au34 \\sim S24 \\sim C241 \\sim C242 \\sim C243 \\sim C244 \\sim
C245 \\sim C246 \\sim C247 \\sim C248: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Au13 \\sim Au19 \\sim S23 \\sim C231 \\sim C232 \\sim C233 \\sim C234 \\sim
C235 \\sim C236 \\sim C237 \\sim C238: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Au13 \\sim Au14 \\sim S22 \\sim C221 \\sim C222 \\sim C223 \\sim C224 \\sim
C225 \\sim C226 \\sim C227 \\sim C228: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
4.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C16(H16), C12(H12), C26(H26), C23(H23), C22(H22), C36(H36),
 C32(H32), C33(H33), C43(H43), C46(H46), C42(H42), C53(H53), C52(H52), C56(H56),
  C66(H66), C62(H62), C63(H63), C76(H76), C72(H72), C73(H73), C86(H86),
 C82(H82), C83(H83), C96(H96), C92(H92), C93(H93), C106(H106), C102(H102),
 C103(H103), C116(H116), C113(H113), C112(H112), C123(H123), C122(H122),
 C126(H126), C132(H132), C133(H133), C136(H136), C146(H146), C142(H142),
 C143(H143), C153(H153), C152(H152), C156(H156), C163(H163), C162(H162),
 C166(H166), C173(H173), C172(H172), C176(H176), C186(H186), C182(H182),
 C183(H183), C192(H192), C196(H196), C193(H193), C206(H206), C203(H203),
 C202(H202), C216(H216), C212(H212), C213(H213), C226(H226), C223(H223),
 C222(H222), C233(H233), C236(H236), C232(H232), C246(H246), C242(H242),
 C243(H243)
4.b Fitted hexagon refined as free rotating group:
 C13(C14,C15,C16,C11,C12), C21(C26,C25,C24,C23,C22), C34(C35,C36,C31,C32,C33),
 C43(C44,C45,C46,C41,C42), C55(C54,C53,C52,C51,C56), C65(C66,C61,C62,C63,C64),
 C75(C76,C71,C72,C73,C74), C86(C81,C82,C83,C84,C85), C94(C95,C96,C91,C92,C93),
 C104(C105,C106,C101,C102,C103), C111(C116,C115,C114,C113,C112), C125(C124,C123,
 C122,C121,C126), C131(C132,C133,C134,C135,C136), C144(C145,C146,C141,C142,
 C143), C154(C153,C152,C151,C156,C155), C164(C163,C162,C161,C166,C165),
 C174(C173,C172,C171,C176,C175), C186(C181,C182,C183,C184,C185), C192(C191,C196,
 C195,C194,C193), C201(C206,C205,C204,C203,C202), C215(C216,C211,C212,C213,
 C214), C221(C226,C225,C224,C223,C222), C233(C234,C235,C236,C231,C232),
 C246(C241,C242,C243,C244,C245)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C47(H47A,H47B,H47C), C57(H57A,
 H57B,H57C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C77(H77A,H77B,H77C),
 C78(H78A,H78B,H78C), C88(H88A,H88B,H88C), C97(H97A,H97B,H97C), C98(H98A,H98B,
 H98C), C107(H10A,H10B,H10C), C108(H10D,H10E,H10F), C117(H11A,H11B,H11C),
 C127(H12A,H12B,H12C), C137(H13A,H13B,H13C), C138(H13D,H13E,H13F), C148(H14A,
 H14B,H14C), C157(H15A,H15B,H15C), C167(H16A,H16B,H16C), C168(H16D,H16E,H16F),
 C177(H17D,H17E,H17F), C178(H17G,H17H,H17I), C187(H18D,H18E,H18F), C188(H18G,
 H18H,H18I), C197(H19A,H19B,H19C), C198(H19D,H19E,H19F), C207(H20A,H20B,H20C),
 C217(H21A,H21B,H21C), C218(H21D,H21E,H21F), C228(H22A,H22B,H22C), C237(H23A,
 H23B,H23C), C238(H23D,H23E,H23F), C247(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              89551
_shelx_hkl_checksum              61097
_shelx_fab_checksum              63398
_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
;