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_1574033
_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         'C168 H162 Au36 S24'
_chemical_formula_sum            'C168 H168 Au36 S24'
_chemical_formula_weight         10047.25
_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             2021-05-13
_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                82.1999(18)
_cell_angle_beta                 75.0794(19)
_cell_angle_gamma                88.5290(14)
_cell_formula_units_Z            2
_cell_length_a                   18.9703(3)
_cell_length_b                   19.2923(4)
_cell_length_c                   28.0221(7)
_cell_measurement_reflns_used    12828
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      65.2450
_cell_measurement_theta_min      3.7540
_cell_volume                     9817.6(4)
_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 5.2137
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0895
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            66135
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        65.511
_diffrn_reflns_theta_max         65.511
_diffrn_reflns_theta_min         3.549
_exptl_absorpt_coefficient_mu    51.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47748
_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    3.399
_exptl_crystal_description       block
_exptl_crystal_F_000             8808
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.872
_refine_diff_density_min         -3.187
_refine_diff_density_rms         0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1974
_refine_ls_number_reflns         32938
_refine_ls_number_restraints     1452
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+168.9699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20614
_reflns_number_total             32938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr00203f2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 1574029--1574035.cif.'
_cod_database_code               1574033
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C247-C242 \\sim C247-C244
 with sigma of 0.02
 C248-C244 \\sim C248-C246
 with sigma of 0.02
 C108-C104 \\sim C108-C106
 with sigma of 0.02
 C107-C102 \\sim C107-C104
 with sigma of 0.02
 C57-C56 \\sim C57-C54
 with sigma of 0.02
 C137-C136 \\sim C137-C134
 with sigma of 0.02
 C87-C85 \\sim C77-C75 \\sim C137-C135 \\sim C17-C15 \\sim C47-C45 \\sim
C207-C205 \\sim C217-C215 ~
 C57-C55 \\sim C67-C65 \\sim C197-C195 \\sim C177-C175 \\sim C127-C125 \\sim
C187-C185 \\sim C117-C115
 \\sim C247-C243 \\sim C248-C245 \\sim C27-C25 \\sim C28-C23 \\sim C227-C225
\\sim C37-C35 \\sim C167-C165
 \\sim C97-C95 \\sim C237-C235 \\sim C107-C103 \\sim C108-C105 \\sim C157-C155
\\sim C147-C145
 with sigma of 0.01
2. Restrained planarity
 S5, C51, C52, C53, C54, C55, C56, C57
 with sigma of 0.1
 S6, C61, C62, C63, C64, C65, C66, C67
 with sigma of 0.1
 S24, C241, C242, C243, C244, C245, C246, C247, C248
 with sigma of 0.1
 S10, C101, C102, C103, C104, C105, C106, C107, C108
 with sigma of 0.1
 S8, C81, C82, C83, C84, C85, C86, C87
 with sigma of 0.1
 S2, C21, C22, C23, C24, C25, C26, C27, C28
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
S1 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
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
S3 \\sim C31 \\sim C36 \\sim C35 \\sim C34 \\sim C33 \\sim C32 \\sim C37:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
S5 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
S6 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Au5 \\sim Au6 \\sim Au15 \\sim Au32 \\sim S7 \\sim S8 \\sim S9 \\sim C71 \\sim
C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C81 \\sim C82 \\sim
C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C91 \\sim C92 \\sim C93 \\sim
C94 \\sim C95 \\sim C96 \\sim C97: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
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
S11 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim
C117: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
S12 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim
C127: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
S14 \\sim C141 \\sim C146 \\sim C145 \\sim C144 \\sim C143 \\sim C142 \\sim
C147: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
S16 \\sim C161 \\sim C162 \\sim C163 \\sim C164 \\sim C165 \\sim C166 \\sim
C167: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
S17 \\sim C171 \\sim C172 \\sim C173 \\sim C174 \\sim C175 \\sim C176 \\sim
C177: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
S18 \\sim C181 \\sim C182 \\sim C183 \\sim C184 \\sim C185 \\sim C186 \\sim
C187: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
S19 \\sim C191 \\sim C192 \\sim C193 \\sim C194 \\sim C195 \\sim C196 \\sim
C197: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
S20 \\sim C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim C206 \\sim
C207: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
S21 \\sim C211 \\sim C212 \\sim C213 \\sim C214 \\sim C215 \\sim C216 \\sim
C217: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
S22 \\sim C221 \\sim C223 \\sim C224 \\sim C225 \\sim C226 \\sim C227: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
S23 \\sim C231 \\sim C232 \\sim C233 \\sim C234 \\sim C235 \\sim C236 \\sim
C237: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
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
S13 \\sim C131 \\sim C132 \\sim C133 \\sim C134 \\sim C135 \\sim C136 \\sim
C137: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
4. Others
 Fixed Sof: C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C28(0.5) H28A(0.5)
 H28B(0.5) H28C(0.5) C107(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C108(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) C247(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 C248(0.5) H24D(0.5) H24E(0.5) H24F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C16(H16), C22(H22), C24(H24), C26(H26),
 C36(H36), C34(H34), C33(H33), C32(H32), C42(H42), C43(H43), C44(H44), C46(H46),
  C52(H52), C53(H53), C54(H54), C56(H56), C66(H66), C64(H64), C63(H63),
 C62(H62), C76(H76), C74(H74), C73(H73), C72(H72), C86(H86), C82(H82), C83(H83),
  C84(H84), C94(H94), C93(H93), C92(H92), C96(H96), C106(H106), C104(H104),
 C102(H102), C112(H112), C116(H116), C114(H114), C113(H113), C122(H122),
 C123(H123), C124(H124), C126(H126), C136(H136), C132(H132), C133(H133),
 C134(H134), C142(H142), C143(H143), C144(H144), C146(H146), C152(H152),
 C153(H153), C154(H154), C156(H156), C162(H162), C163(H163), C164(H164),
 C166(H166), C172(H172), C173(H173), C174(H174), C176(H176), C182(H182),
 C183(H183), C184(H184), C186(H186), C192(H192), C193(H193), C194(H194),
 C196(H196), C202(H202), C203(H203), C204(H204), C206(H206), C212(H212),
 C213(H213), C214(H214), C216(H216), C222(H222), C223(H223), C224(H224),
 C226(H226), C232(H232), C233(H233), C234(H234), C236(H236), C244(H244),
 C246(H246), C242(H242)
5.b Fitted hexagon refined as free rotating group:
 C31(C36,C35,C34,C33,C32), C51(C52,C53,C54,C55,C56), C61(C66,C65,C64,C63,C62),
 C76(C75,C74,C73,C72,C71), C86(C81,C82,C83,C84,C85), C95(C94,C93,C92,C91,C96),
 C101(C106,C105,C104,C103,C102), C112(C111,C116,C115,C114,C113), C135(C136,C131,
 C132,C133,C134), C191(C192,C193,C194,C195,C196), C244(C245,C246,C241,C242,C243)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C37(H37A,H37B,
 H37C), C47(H47A,H47B,H47C), C57(H57A,H57B,H57C), C67(H67A,H67B,H67C), C77(H77A,
 H77B,H77C), C87(H87A,H87B,H87C), C97(H97A,H97B,H97C), C107(H10A,H10B,H10C),
 C108(H10D,H10E,H10F), C117(H11A,H11B,H11C), C127(H12A,H12B,H12C), C147(H14A,
 H14B,H14C), C157(H15A,H15B,H15C), C167(H16A,H16B,H16C), C177(H17D,H17E,H17F),
 C187(H18A,H18B,H18C), C197(H19A,H19B,H19C), C207(H20A,H20B,H20C), C217(H21A,
 H21B,H21C), C227(H22A,H22B,H22C), C237(H23A,H23B,H23C), C247(H24A,H24B,H24C),
 C248(H24D,H24E,H24F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61918
_shelx_hkl_checksum              44022
_shelx_fab_checksum              20132
_olex2_submission_special_instructions 'No special instructions were received'