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_1567724
_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
_atom_sites_solution_primary     iterative
_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                   20.333(5)
_cell_length_b                   25.812(5)
_cell_length_c                   26.048(5)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.031
_cell_measurement_theta_min      2.768
_cell_volume                     13671(5)
_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  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0601
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            73670
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.070
_diffrn_reflns_theta_max         67.070
_diffrn_reflns_theta_min         3.246
_diffrn_source                   'microfocus sealed X-ray tube'
_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    17.053
_exptl_absorpt_correction_T_max  0.3220
_exptl_absorpt_correction_T_min  0.1330
_exptl_absorpt_correction_type   multi-scan
_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    1.821
_exptl_crystal_description       block
_exptl_crystal_F_000             7064
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.799
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Flack x determined using 9200 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.070(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1495
_refine_ls_number_reflns         23980
_refine_ls_number_restraints     426
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0448P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                22317
_reflns_number_total             23980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03463h2.cif
_cod_data_source_block           R_Au8e
_cod_database_code               1567724
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.483
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
O2 \\sim C69 \\sim O3 \\sim C137 \\sim C139 \\sim C17 \\sim C123 \\sim C119
\\sim C67 \\sim S2: within 2A with sigma of 0.004 and sigma for terminal atoms
of 0.008 within 2A
S1 \\sim C77 \\sim C86 \\sim C126 \\sim C52 \\sim C89 \\sim C75 \\sim C29 \\sim
O4 \\sim O1: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 2A
C43 \\sim C20 \\sim C14 \\sim C48 \\sim C30 \\sim C132 \\sim C45 \\sim C101
\\sim C92 \\sim C106 \\sim C25 \\sim C50 \\sim C109 \\sim C5 \\sim C55 \\sim
C115 \\sim C22 \\sim C116 \\sim C70 \\sim C57 \\sim P4 \\sim C24 \\sim C114
\\sim C81 \\sim C66 \\sim C58 \\sim C62 \\sim C13 \\sim C83 \\sim C37 \\sim
C134 \\sim C144 \\sim P1 \\sim C76 \\sim C87 \\sim C95 \\sim C103 \\sim C120
\\sim C49 \\sim C91 \\sim C72 \\sim C51 \\sim C47 \\sim C39 \\sim C56: within
2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C20(H20), C22(H22), C26(H26), C28(H28), C30(H30), C32(H32),
 C38(H38), C40(H40), C44(H44), C48(H48), C50(H50), C52(H52), C60(H60), C64(H64),
  C68(H68), C70(H70), C72(H72), C80(H80), C82(H82), C86(H86), C88(H88),
 C90(H90), C96(H96), C98(H98), C100(H100), C104(H104), C108(H108), C110(H110),
 C112(H112), C114(H114), C118(H118), C120(H120), C122(H122), C124(H124),
 C126(H126), C128(H128), C130(H130), C134(H134), C138(H138), C140(H140),
 C142(H142), C144(H144), C146(H146), C73(H73), C37(H37), C75(H75), C19(H19),
 C39(H39), C79(H79), C5(H5), C81(H81), C83(H83), C21(H21), C85(H85), C43(H43),
 C87(H87), C11(H11), C45(H45), C91(H91), C93(H93), C47(H47), C95(H95), C3(H3),
 C97(H97), C49(H49), C25(H25), C101(H101), C51(H51), C103(H103), C105(H105),
 C53(H53), C27(H27), C109(H109), C55(H55), C111(H111), C7(H7), C113(H113),
 C57(H57), C115(H115), C117(H117), C15(H15), C121(H121), C123(H123), C31(H31),
 C125(H125), C63(H63), C127(H127), C129(H129), C65(H65), C131(H131), C33(H33),
 C133(H133), C67(H67), C135(H135), C17(H17), C139(H139), C35(H35), C141(H141),
 C71(H71), C143(H143), C9(H9), C145(H145)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78968
_shelx_fab_checksum              43175
_olex2_submission_special_instructions 'No special instructions were received'