The fcc structure isomerization in gold nanoclusters
Zhuang, Shengli; Liao, Lingwen; Li, Man-Bo; Yao, Chuanhao; Zhao, Yan; Dong, Hongwei; Li, Jin; Deng, Haiteng; Li, Lingling; Wu, Zhikun; Nanoscale  (2017) –; doi:10.1039/C7NR05239A

data_1547467
_publ_section_title
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 The fcc structure isomerization in gold nanoclusters
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_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/C7NR05239A
_journal_year                    2017
_chemical_formula_moiety         'C256 H188 Au52 S32'
_chemical_formula_sum            'C256 H288 Au52 S32'
_chemical_formula_weight         14633.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-14 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                116.588(2)
_cell_angle_beta                 95.458(2)
_cell_angle_gamma                95.019(2)
_cell_formula_units_Z            1
_cell_length_a                   19.2220(8)
_cell_length_b                   19.8976(8)
_cell_length_c                   21.4243(9)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.53
_cell_measurement_theta_min      2.52
_cell_volume                     7216.1(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            96113
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.561
_diffrn_reflns_theta_min         2.333
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    50.734
_exptl_absorpt_correction_T_max  0.1665
_exptl_absorpt_correction_T_min  0.0411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1518 before and 0.0911 after correction.
The Ratio of minimum to maximum transmission is 0.2468.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.367
_exptl_crystal_description       block
_exptl_crystal_F_000             6444
_refine_diff_density_max         11.313
_refine_diff_density_min         -5.684
_refine_diff_density_rms         0.961
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.458
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1339
_refine_ls_number_reflns         24899
_refine_ls_number_restraints     1747
_refine_ls_restrained_S_all      1.876
_refine_ls_R_factor_all          0.1836
_refine_ls_R_factor_gt           0.1352
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3636
_refine_ls_wR_factor_ref         0.4084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14707
_reflns_number_total             24899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nr05239a2.cif
_cod_data_source_block           16520
_cod_database_code               1547467
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S7-C49 = S6-C41 = S5-C33 = S3-C17 = S4-C25 = S14-C105 = S13-C97 = S12-C89 =
 S11-C81 = S10-C73 = S9-C65 = S8-C57 = S1-C1 = S2-C9
 1.78 with sigma of 0.02
 C74-C75 = C74-C73 = C83-C82 = C81-C82 = C89-C90 = C91-C90 = C97-C98 = C106-
 C107 = C105-C106 = C26-C27 = C26-C25 = C18-C19 = C17-C18 = C9-C10 = C10-C11 =
 C3-C2 = C2-C1 = C66-C65 = C66-C67 = C34-C33 = C35-C34
 1.51 with sigma of 0.02
 C36-C34
 2.3 with sigma of 0.02
 C26-C32
 2.3 with sigma of 0.02
 C49-C50 = C51-C50
 1.51 with sigma of 0.02
 C105-C107
 2.4 with sigma of 0.02
 C97-C98 = C98-C99
 1.5 with sigma of 0.02
 C123-C128
 1.5 with sigma of 0.02
 C104-C98
 2.3 with sigma of 0.02
 C58-C59
 1.51 with sigma of 0.02
 C57-C58
 1.51 with sigma of 0.02
 S7-C50
 2.5 with sigma of 0.02
 C106-C108
 2.3 with sigma of 0.02
 C114-C115 = C113-C114
 1.51 with sigma of 0.02
 S15-C113
 1.78 with sigma of 0.02
 C42-C43 = C42-C41
 1.51 with sigma of 0.02
 S16-C121
 1.78 with sigma of 0.02
 C123-C122
 1.51 with sigma of 0.02
 C121-C122
 1.51 with sigma of 0.02
 C121-C122
 1.51 with sigma of 0.02
 C120-C114
 2.3 with sigma of 0.02
 C115-C113
 2.4 with sigma of 0.02
 S15-C114
 2.4 with sigma of 0.02
 C121-C123
 2.4 with sigma of 0.02
 C43-C41
 2.4 with sigma of 0.02
 C42-S6
 2.5 with sigma of 0.02
 C49-C51
 2.4 with sigma of 0.02
 Au20-C48
 3.8 with sigma of 0.02
 C42-C48
 2.3 with sigma of 0.02
 C50-C56
 2.3 with sigma of 0.02
 S16-C122
 2.5 with sigma of 0.02
 C121-C128
 2.3 with sigma of 0.02
 C123-C122
 1.51 with sigma of 0.02
 C122-C124
 2.3 with sigma of 0.02
 C27-C25
 2.4 with sigma of 0.02
 C27-C25
 2.4 with sigma of 0.02
 C15_$1-C125_$2 = C118_$3-C116_$4 = C118_$4-C116_$3 = C15_$2-C125_$1 = C118_$1-
 C116 = C118-C116_$1 = C127_$5-C126 = C127-C126_$5 = C127_$5-C127
 3 with sigma of 0.02
 C40_$1-C100_$5 = C118_$3-C116_$4 = C118_$4-C116_$3 = C118_$1-C116 = C118-
 C116_$1
 3 with sigma of 0.02
 C40_$6-C100
 3 with sigma of 0.02
 C15-C125_$4
 3 with sigma of 0.02
 C40_$6-C100
 3 with sigma of 0.01
 C39_$6-C100 = C40_$6-C101
 3 with sigma of 0.02
 C40_$6-C100 = C99-C39_$6
 3 with sigma of 0.02
 C10-C16 \\sim C10-C12
 with sigma of 0.02
3. Restrained planarity
 C114, C115, C116, C117, C118, C119, C120
 with sigma of 0.1
 C50, C51, C52, C53, C54, C55, C56
 with sigma of 0.1
 C122, C123, C124, C125, C126, C127, C128
 with sigma of 0.1
 C34, C35, C40, C39, C38, C37, C36
 with sigma of 0.1
 C10, C11, C16, C15, C14, C13, C12
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
S1 \\sim C1 \\sim C2 \\sim C3 \\sim C8 \\sim C7 \\sim C6 \\sim C5 \\sim C4:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S2 \\sim C9 \\sim C10 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C11: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S3 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim
C24: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S4 \\sim C25 \\sim C26 \\sim C27 \\sim C32 \\sim C31 \\sim C30 \\sim C29 \\sim
C28: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S5 \\sim C33 \\sim C34 \\sim C35 \\sim C40 \\sim C39 \\sim C38 \\sim C37 \\sim
C36: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S6 \\sim C41 \\sim C42 \\sim C48 \\sim C47 \\sim C46 \\sim C45 \\sim C44 \\sim
C43: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S7 \\sim C49 \\sim C50 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim
C51: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S8 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim
C64: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S9 \\sim C65 \\sim C66 \\sim C67 \\sim C72 \\sim C71 \\sim C70 \\sim C69 \\sim
C68: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S10 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim
C80: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S11 \\sim C81 \\sim C82 \\sim C83 \\sim C88 \\sim C87 \\sim C86 \\sim C85 \\sim
C84: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S12 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim
C96: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S13 \\sim C97 \\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103
\\sim C104: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
S14 \\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim
C111 \\sim C112: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
S15 \\sim C113 \\sim C114 \\sim C115 \\sim C120 \\sim C119 \\sim C118 \\sim
C117 \\sim C116: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
S16 \\sim C121 \\sim C122 \\sim C123 \\sim C128 \\sim C127 \\sim C126 \\sim
C125 \\sim C124: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(C36) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq,
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C72) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq,
Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C87)
\\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C84) \\sim Ueq,
Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92)
\\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C95) \\sim Ueq,
Uanis(C96) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C99)
\\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq,
Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C111) \\sim Ueq,
Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C115) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C119) \\sim Ueq,
Uanis(C118) \\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(C116) \\sim Ueq,
Uanis(C121) \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq,
Uanis(C128) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C126) \\sim Ueq,
Uanis(C125) \\sim Ueq, Uanis(C124) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B),
 C33(H33A,H33B), C41(H41A,H41B), C49(H49A,H49B), C50(H50A,H50B), C57(H57A,H57B),
  C58(H58A,H58B), C65(H65A,H65B), C73(H73A,H73B), C81(H81A,H81B), C82(H82A,
 H82B), C89(H89A,H89B), C90(H90A,H90B), C105(H10A,H10B), C113(H11A,H11B),
 C114(H11C,H11D), C121(H12A,H12B), C122(H12C,H12D)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C6(H6), C5(H5), C4(H4), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24), C32(H32), C31(H31), C30(H30), C29(H29), C28(H28), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56), C60(H60), C61(H61), C62(H62),
 C63(H63), C64(H64), C72(H72), C71(H71), C70(H70), C69(H69), C68(H68), C76(H76),
  C77(H77), C78(H78), C79(H79), C80(H80), C88(H88), C87(H87), C86(H86),
 C85(H85), C84(H84), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96),
 C108(H108), C109(H109), C110(H110), C111(H111), C112(H112)
5.c Fitted hexagon refined as free rotating group:
 C3(C8,C7,C6,C5,C4), C12(C13,C14,C15,C16,C11), C19(C20,C21,C22,C23,C24),
 C27(C32,C31,C30,C29,C28), C35(C40,C39,C38,C37,C36), C48(C47,C46,C45,C44,C43),
 C52(C53,C54,C55,C56,C51), C59(C60,C61,C62,C63,C64), C67(C72,C71,C70,C69,C68),
 C75(C76,C77,C78,C79,C80), C83(C88,C87,C86,C85,C84), C91(C92,C93,C94,C95,C96),
 C99(C100,C101,C102,C103,C104), C107(C108,C109,C110,C111,C112), C115(C120,C119,
 C118,C117,C116), C123(C128,C127,C126,C125,C124)
;
_shelx_res_checksum              96776
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'