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_1567721
_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   geom
_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                   18.8119(2)
_cell_length_b                   27.6970(2)
_cell_length_c                   31.3398(3)
_cell_measurement_reflns_used    30322
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.5660
_cell_measurement_theta_min      2.6960
_cell_volume                     16329.1(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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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   -119.00 -65.00   1.00    0.50    --  -48.45-135.00 -60.00   54
  2  \w   -120.00 -70.00   1.00    0.50    --  -48.45-125.00-180.00   50
  3  \w    -23.00  61.00   1.00    0.50    --   48.45 -38.00 -60.00   84
  4  \w    -81.00 -13.00   1.00    3.20    --  -86.25  36.00 -38.00   68
  5  \w     87.00 158.00   1.00    3.20    --  106.49 134.00-173.00   71
  6  \w     98.00 176.00   1.00    3.20    --  106.49  85.00 121.00   78
  7  \w     37.00 121.00   1.00    3.20    --  106.49 -57.00  90.00   84
  8  \w     93.00 177.00   1.00    3.20    --  106.49 125.00-150.00   84
  9  \w     92.00 167.00   1.00    3.20    --  106.49 125.00  60.00   75
;
_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      -0.0173744000
_diffrn_orient_matrix_UB_12      -0.0227613000
_diffrn_orient_matrix_UB_13      -0.0435780000
_diffrn_orient_matrix_UB_21      -0.0336678000
_diffrn_orient_matrix_UB_22      -0.0437305000
_diffrn_orient_matrix_UB_23      0.0226918000
_diffrn_orient_matrix_UB_31      -0.0726737000
_diffrn_orient_matrix_UB_32      0.0257224000
_diffrn_orient_matrix_UB_33      -0.0000936000
_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  0.0863
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            70011
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         2.740
_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    14.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09039
_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    1.575
_exptl_crystal_description       needle
_exptl_crystal_F_000             7320
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.335
_refine_diff_density_min         -3.181
_refine_diff_density_rms         0.260
_refine_ls_abs_structure_details
;
 Flack x determined using 9624 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1399
_refine_ls_number_reflns         28707
_refine_ls_number_restraints     973
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0815
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1510P)^2^+172.2397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2257
_refine_ls_wR_factor_ref         0.2437
_reflns_Friedel_coverage         0.842
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                25197
_reflns_number_total             28707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03463h2.cif
_cod_data_source_block           SD_R_Au8c
_cod_database_code               1567721
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AuP
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.534
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H7 of O7
 At 1.5 times of:
  H2 of O2, H4A of O4, H5A of O5
2. Restrained distances
 O10-C119 = O6-C118
 1.25 with sigma of 0.01
 C1-C47
 1.45 with sigma of 0.01
 C16-C137
 1.45 with sigma of 0.01
 O5-O8 \\sim O5-O10 \\sim O8-O10
 with sigma of 0.02
 C118-O3 \\sim C118-O4 \\sim C118-O6
 with sigma of 0.01
 C119-O5 \\sim C119-O8 \\sim C119-O10
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C148 \\sim C29: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 2A
C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105: within 2A with
sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
C30 \\sim C57 \\sim C66 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim
C84 \\sim C113: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 2A
C16 \\sim C27 \\sim C44 \\sim C62 \\sim C74 \\sim C77 \\sim C90 \\sim C115
\\sim C128 \\sim C129 \\sim C130 \\sim C131 \\sim C132 \\sim C133 \\sim C134
\\sim C135 \\sim C136 \\sim C137 \\sim C149 \\sim C150: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 2A
C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim C127: within 2A with
sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 2A
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 2A
C60 \\sim C75 \\sim C86 \\sim C99 \\sim C110 \\sim C112: within 2A with sigma
of 0.004 and sigma for terminal atoms of 0.008 within 2A
C5 \\sim C43 \\sim C63 \\sim C67 \\sim C88 \\sim C145: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 2A
C33 \\sim C45 \\sim C53 \\sim C56 \\sim C78 \\sim C98: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 2A
C2 \\sim C3 \\sim C64 \\sim C108 \\sim C114 \\sim C144: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 2A
C138 \\sim C139 \\sim C140 \\sim C141 \\sim C142 \\sim C143: within 2A with
sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
C13 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim
C24 \\sim C25 \\sim C26 \\sim C31 \\sim C41 \\sim C55 \\sim C61 \\sim C65 \\sim
C76 \\sim C85 \\sim C109 \\sim C147: within 2A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 2A
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 2A
C6 \\sim C15 \\sim C40 \\sim C49 \\sim C52 \\sim C54 \\sim C87 \\sim C106 \\sim
C116 \\sim C117: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 2A
O3 \\sim O4 \\sim O5 \\sim O6 \\sim O8 \\sim O10 \\sim C118 \\sim C119: within
2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
O1 \\sim O2 \\sim C1 \\sim C14 \\sim C28 \\sim C47 \\sim C48 \\sim C51 \\sim
C89: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within
2A
O7 \\sim O9 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim
C107: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008
within 2A
C146 \\sim C50: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 2A
Uanis(C143) \\sim Ueq, Uanis(C125) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.008
Uanis(C37) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.008
Uanis(C119) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.2
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), C7(H7A), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C30(H30), C31(H31), C34(H34), C36(H36), C37(H37), C38(H38),
 C39(H39), C41(H41), C42(H42), C45(H45), C48(H48), C49(H49), C50(H50), C51(H51),
  C53(H53), C54(H54), C55(H55), C56(H56), C59(H59), C62(H62), C63(H63),
 C64(H64), C65(H65), C66(H66), C67(H67), C69(H69), C70(H70), C71(H71), C72(H72),
  C73(H73), C78(H78), C81(H81), C82(H82), C83(H83), C84(H84), C87(H87),
 C88(H88), C89(H89), C90(H90), C94(H94), C95(H95), C96(H96), C97(H97), C98(H98),
  C99(H99), C75(H75), C86(H86), C112(H112), C110(H110), C100(H100), C101(H101),
 C102(H102), C104(H104), C105(H105), C106(H106), C108(H108), C109(H109),
 C114(H114), C115(H115), C116(H116), C117(H117), C122(H122), C123(H123),
 C125(H125), C126(H126), C127(H127), C128(H128), C129(H129), C130(H130),
 C131(H131), C134(H134), C135(H135), C138(H138), C139(H139), C140(H140),
 C142(H142), C143(H143), C145(H145), C146(H146), C148(H148), C58(H58),
 C111(H111), C91(H91), C32(H32), C149(H149), C150(H150)
4.b Fitted hexagon refined as free rotating group:
 C7(C8,C9,C10,C11,C12), C34(C35,C36,C37,C38,C39), C68(C69,C70,C71,C72,C73),
 C79(C80,C81,C82,C83,C84), C92(C93,C94,C95,C96,C97), C99(C60,C75,C86,C112,C110),
  C100(C101,C102,C103,C104,C105), C122(C123,C124,C125,C126,C127), C138(C139,
 C140,C141,C142,C143), C148(C58,C111,C91,C32,C29)
4.c Tetrahedral OH refined with riding coordinates:
 O2(H2), O4(H4A), O5(H5A), O7(H7)
4.d Naphthalene refined as free rotating group:
 C17(C18,C19,C20,C21,C22,C23,C24,C25,C26), C128(C129,C130,C131,C132,C133,C134,
 C135,C136,C137)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              41892
_shelx_fab_checksum              36096
_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 4.704
_oxdiff_exptl_absorpt_empirical_full_min 0.505