Bicarbonate insertion triggered self-assembly of chiral octa-gold nanoclusters into helical superstructures in the crystalline state
Si, Wei-Dan; Sheng, Kai; Zhang, Chengkai; Wang, Zhi; Zhang, Shan-Shan; Dou, Jian-Min; Feng, Lei; Gao, Zhi-Yong; Tung, Chen-Ho; Sun, Di; Chemical Science 13 (2022) 10523–10531; doi:10.1039/D2SC03463H

data_1567722
_publ_section_title
;
 Bicarbonate insertion triggered self-assembly of chiral octa-gold
 nanoclusters into helical superstructures in the crystalline state
;
_journal_issue                   35
_journal_name_full               'Chemical Science'
_journal_page_first              10523
_journal_page_last               10531
_journal_paper_doi               10.1039/D2SC03463H
_journal_volume                  13
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C146 H104 Au8 O4 P6 S2'
_chemical_formula_sum            'C146 H104 Au8 O4 P6 S2'
_chemical_formula_weight         3747.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-06-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-15 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5564(14)
_cell_length_b                   25.7288(16)
_cell_length_c                   26.0976(17)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      69.876
_cell_measurement_theta_min      3.231
_cell_volume                     13802.8(16)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            80987
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         3.231
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    16.890
_exptl_absorpt_correction_T_max  0.3220
_exptl_absorpt_correction_T_min  0.1452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1228 before and 0.0724 after correction.
The Ratio of minimum to maximum transmission is 0.4509.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       needle
_exptl_crystal_F_000             7064
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.206
_refine_diff_density_min         -1.896
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details
;
 Flack x determined using 9812 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.041(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1495
_refine_ls_number_reflns         24480
_refine_ls_number_restraints     1050
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0459P)^2^+152.9039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                23184
_reflns_number_total             24480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03463h2.cif
_cod_data_source_block           R_Au8d
_cod_database_code               1567722
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.486
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
S1 \\sim C7 \\sim C27 \\sim C28 \\sim C82 \\sim C83 \\sim C107 \\sim C120:
within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
P4 \\sim P6 \\sim C6 \\sim C8 \\sim C9 \\sim C12 \\sim C14 \\sim C15 \\sim C16
\\sim C19 \\sim C20 \\sim C25 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C40
\\sim C41 \\sim C47 \\sim C52 \\sim C56 \\sim C57 \\sim C62 \\sim C64 \\sim C68
\\sim C72 \\sim C74 \\sim C76 \\sim C78 \\sim C84 \\sim C96 \\sim C98 \\sim
C101 \\sim C102 \\sim C106 \\sim C108 \\sim C116 \\sim C118 \\sim C121 \\sim
C126 \\sim C133 \\sim C136 \\sim C138 \\sim C139 \\sim C144: within 2A with
sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
P3 \\sim P5 \\sim C2 \\sim C4 \\sim C10 \\sim C11 \\sim C13 \\sim C22 \\sim C23
\\sim C30 \\sim C31 \\sim C33 \\sim C42 \\sim C44 \\sim C49 \\sim C51 \\sim C54
\\sim C55 \\sim C58 \\sim C65 \\sim C67 \\sim C71 \\sim C75 \\sim C79 \\sim C85
\\sim C86 \\sim C88 \\sim C90 \\sim C92 \\sim C93 \\sim C95 \\sim C100 \\sim
C105 \\sim C110 \\sim C114 \\sim C117 \\sim C122 \\sim C123 \\sim C127 \\sim
C129 \\sim C131 \\sim C134 \\sim C137 \\sim C141 \\sim C143 \\sim C146: within
2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
P1 \\sim P2 \\sim C5 \\sim C17 \\sim C18 \\sim C21 \\sim C24 \\sim C26 \\sim
C29 \\sim C32 \\sim C38 \\sim C39 \\sim C43 \\sim C45 \\sim C46 \\sim C48 \\sim
C50 \\sim C53 \\sim C60 \\sim C61 \\sim C63 \\sim C66 \\sim C70 \\sim C77 \\sim
C80 \\sim C81 \\sim C87 \\sim C91 \\sim C94 \\sim C97 \\sim C99 \\sim C103
\\sim C104 \\sim C109 \\sim C112 \\sim C113 \\sim C115 \\sim C119 \\sim C124
\\sim C128 \\sim C130 \\sim C132 \\sim C135 \\sim C140 \\sim C145 \\sim C148:
within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
S2 \\sim O1 \\sim O4 \\sim C1 \\sim C3 \\sim C59 \\sim C69 \\sim C89 \\sim C111
\\sim C125: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008
within 2A
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24),
  C25(H25), C27(H27), C29(H29), C31(H31), C33(H33), C35(H35), C36(H36),
 C37(H37), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C47(H47), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C58(H58),
 C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66),
  C67(H67), C69(H69), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76),
 C79(H79), C80(H80), C81(H81), C84(H84), C85(H85), C88(H88), C90(H90), C91(H91),
  C92(H92), C94(H94), C98(H98), C99(H99), C101(H101), C102(H102), C105(H105),
 C106(H106), C107(H107), C108(H108), C109(H109), C110(H110), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C118(H118), C119(H119),
 C120(H120), C121(H121), C122(H122), C123(H123), C125(H125), C126(H126),
 C127(H127), C129(H129), C130(H130), C131(H131), C132(H132), C135(H135),
 C137(H137), C138(H138), C139(H139), C140(H140), C141(H141), C142(H142),
 C143(H143), C144(H144), C145(H145), C146(H146), C148(H148)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20387
_shelx_fab_checksum              20179
_olex2_submission_special_instructions 'No special instructions were received'