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_1567723
_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 H106 Au8 O4 P6 S2, 2(C H O3)'
_chemical_formula_sum            'C148 H108 Au8 O10 P6 S2'
_chemical_formula_weight         3872.01
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-10-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-14 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                   18.4744(2)
_cell_length_b                   27.7085(3)
_cell_length_c                   31.2344(3)
_cell_measurement_reflns_used    16781
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.3680
_cell_measurement_theta_min      2.8220
_cell_volume                     15988.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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   -117.00 -70.00   1.00    1.12    --  -48.45-125.00 -60.00   47
  2  \w    -59.00  21.00   1.00    1.12    --  -48.45  38.00-150.00   80
  3  \w    -95.00 -38.00   1.00    8.00    --  -86.25 131.00-123.00   57
  4  \w     42.00 129.00   1.00    8.00    --  106.49-142.00  82.00   87
  5  \w     65.00 172.00   1.00    8.00    --  106.49   5.00 169.00  107
  6  \w     79.00 120.00   1.00    8.00    --  106.49 -57.00-120.00   41
  7  \w     34.00  60.00   1.00    8.00    --  106.49 -57.00-120.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0008924000
_diffrn_orient_matrix_UB_12      -0.0519935000
_diffrn_orient_matrix_UB_13      0.0174522000
_diffrn_orient_matrix_UB_21      -0.0051183000
_diffrn_orient_matrix_UB_22      -0.0196197000
_diffrn_orient_matrix_UB_23      -0.0460474000
_diffrn_orient_matrix_UB_31      0.0832379000
_diffrn_orient_matrix_UB_32      -0.0017417000
_diffrn_orient_matrix_UB_33      -0.0026307000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48414
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         2.829
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    14.631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.609
_exptl_crystal_description       needle
_exptl_crystal_F_000             7320
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.374
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.223
_refine_ls_abs_structure_details
;
 Flack x determined using 7353 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.041(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1483
_refine_ls_number_reflns         26263
_refine_ls_number_restraints     1057
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0816P)^2^+214.2552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1881
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    0.846
_reflns_Friedel_fraction_max     0.846
_reflns_number_gt                20735
_reflns_number_total             26263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03463h2.cif
_cod_data_source_block           SD_S_Au8c
_cod_database_code               1567723
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AuC
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.387
_reflns_odcompleteness_completeness 98.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 C122-C59
 1.39 with sigma of 0.01
 C59-C33
 1.39 with sigma of 0.01
 C33-C127
 1.39 with sigma of 0.01
 C127-C128
 1.39 with sigma of 0.01
 C128-C123
 1.39 with sigma of 0.01
 C123-C122
 1.39 with sigma of 0.01
 C122-C121
 1.39 with sigma of 0.01
 C121-C126
 1.39 with sigma of 0.01
 C126-C125
 1.39 with sigma of 0.01
 C125-C124
 1.39 with sigma of 0.01
 C124-C123
 1.39 with sigma of 0.01
 C107-C39
 1.39 with sigma of 0.01
 C95-C84
 1.39 with sigma of 0.01
 C84-C47
 1.39 with sigma of 0.01
 C107-C46
 1.39 with sigma of 0.01
 C140-C50
 1.39 with sigma of 0.02
 C46-C140
 1.39 with sigma of 0.02
 C47-C48
 1.39 with sigma of 0.02
 C48-C49
 1.39 with sigma of 0.02
 C46-C47
 1.39 with sigma of 0.02
 C101-C100
 1.39 with sigma of 0.02
 C85-C101
 1.39 with sigma of 0.02
 C53-C85
 1.39 with sigma of 0.02
 C30-C102
 1.39 with sigma of 0.02
 C99-C55
 1.39 with sigma of 0.02
 C99-C106
 1.39 with sigma of 0.02
 C106-C111
 1.39 with sigma of 0.02
 C111-C53
 1.39 with sigma of 0.02
 C108-C109
 1.39 with sigma of 0.02
 C131-C145
 1.39 with sigma of 0.02
 C143-C144
 1.39 with sigma of 0.02
 C129-C143
 1.39 with sigma of 0.02
 C94-C52
 1.39 with sigma of 0.02
 C94-C60
 1.39 with sigma of 0.02
 C60-C141
 1.39 with sigma of 0.02
 C137-C132
 1.39 with sigma of 0.02
 C141-C142
 1.39 with sigma of 0.02
 C52-C113
 1.39 with sigma of 0.02
 C113-C142
 1.39 with sigma of 0.02
 C60-C94
 1.39 with sigma of 0.02
 C145-C144
 1.39 with sigma of 0.01
 C130-C131
 1.39 with sigma of 0.01
 C130-C129
 1.39 with sigma of 0.01
 C41-C27
 1.39 with sigma of 0.01
 C27-C18
 1.39 with sigma of 0.01
 C18-C17
 1.39 with sigma of 0.01
 C38-C103
 1.39 with sigma of 0.01
 C81-C103
 1.39 with sigma of 0.01
 C81-C44
 1.39 with sigma of 0.01
 C132-C133
 1.39 with sigma of 0.02
 C137-C136
 1.39 with sigma of 0.02
 C133-C134
 1.39 with sigma of 0.02
 C136-C135
 1.39 with sigma of 0.02
 C112-C29
 1.39 with sigma of 0.02
 C59-C51
 1.39 with sigma of 0.02
 C65-C66
 1.39 with sigma of 0.02
 C66-C67
 1.39 with sigma of 0.02
 C68-C67
 1.39 with sigma of 0.02
 C69-C68
 1.39 with sigma of 0.02
 C69-C64
 1.39 with sigma of 0.02
 O6-C146
 1.3 with sigma of 0.01
 O7-C146
 1.35 with sigma of 0.01
 O5-C146
 1.3 with sigma of 0.01
 C45-C58
 1.39 with sigma of 0.01
 C58-C139
 1.39 with sigma of 0.02
 C104-C114
 1.39 with sigma of 0.01
 C138-C114
 1.39 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 1.7A
3.a Riding coordinates:
 O3(H3), O7(H7A), O9(H9A)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C28(H28), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39),
 C42(H42), C43(H43), C44(H44), C48(H48), C49(H49), C50(H50), C52(H52), C56(H56),
  C57(H57), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68),
 C69(H69), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78),
  C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C85(H85), C87(H87),
 C88(H88), C89(H89), C90(H90), C91(H91), C93(H93), C94(H94), C96(H96), C97(H97),
  C98(H98), C100(H100), C101(H101), C102(H102), C103(H103), C104(H104),
 C105(H105), C106(H106), C107(H107), C108(H108), C109(H109), C110(H110),
 C111(H111), C112(H112), C113(H113), C114(H114), C115(H115), C116(H116),
 C118(H118), C119(H119), C120(H120), C121(H121), C124(H124), C125(H125),
 C126(H126), C127(H127), C128(H128), C131(H131), C132(H132), C133(H133),
 C134(H134), C135(H135), C136(H136), C138(H138), C139(H139), C140(H140),
 C141(H141), C142(H142), C143(H143), C144(H144), C145(H145), C148(H148)
3.c Fitted hexagon refined as free rotating group:
 C5(C6,C7,C8,C9,C10), C21(C22,C23,C24,C25,C26), C64(C65,C66,C67,C68,C69),
 C71(C72,C73,C74,C75,C76), C87(C88,C89,C90,C91,C92), C115(C116,C117,C118,C119,
 C120), C132(C133,C134,C135,C136,C137)
3.d Tetrahedral OH refined with riding coordinates:
 O2(H2)
;
_shelx_res_checksum              98678
_shelx_fab_checksum              30577
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.231
_oxdiff_exptl_absorpt_empirical_full_min 0.518