Structural Oscillation Revealed in Gold Nanoparticles.
Xia, Nan; Yuan, Jinyun; Liao, Lingwen; Zhang, Wenhao; Li, Jin; Deng, Haiteng; Yang, Jinlong; Wu, Zhikun; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c02117

data_4135099
_publ_section_title
;
 Structural Oscillation Revealed in Gold Nanoparticles.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c02117
_journal_year                    2020
_chemical_formula_moiety         'C100 H180 Au28 S20'
_chemical_formula_sum            'C100 H180 Au28 S20'
_chemical_formula_weight         7538.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.017(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.7979(13)
_cell_length_b                   18.4577(7)
_cell_length_c                   26.0404(11)
_cell_measurement_reflns_used    9701
_cell_measurement_temperature    170
_cell_measurement_theta_max      54.87
_cell_measurement_theta_min      3.69
_cell_volume                     15246.0(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1015
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67021
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        52.977
_diffrn_reflns_theta_max         52.977
_diffrn_reflns_theta_min         2.872
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    35.671
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.3963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1868 before and 0.1236 after correction. The Ratio of minimum to maximum transmission is 0.2676. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.284
_exptl_crystal_description       block
_exptl_crystal_F_000             13248
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         8.515
_refine_diff_density_min         -8.606
_refine_diff_density_rms         0.914
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         13384
_refine_ls_number_restraints     575
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.1046
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2646
_refine_ls_wR_factor_ref         0.2812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10764
_reflns_number_total             13384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02117_si_003.cif
_cod_data_source_block           190425xn_1_0m_sq_sq
_cod_database_code               4135099
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.269
_shelx_estimated_absorpt_t_min   0.100
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C9-C37 = C37-C28
 1.5 with sigma of 0.02
 C40-C17
 1.5 with sigma of 0.02
 C44-C45
 1.5 with sigma of 0.02
 C44-C46 = C50-C49
 1.5 with sigma of 0.02
 C46-C50
 1.5 with sigma of 0.02
 C50-C44 = C44-C49
 2.5 with sigma of 0.02
 C46-C45
 2.5 with sigma of 0.02
 C32-C39
 1.5 with sigma of 0.02
 C13-C32
 1.5 with sigma of 0.02
 C49-C45
 1.5 with sigma of 0.02
 C39A-C32A = C39-C32
 1.5 with sigma of 0.02
 C39A-C16
 1.5 with sigma of 0.02
 C45A-C44 = C44-C45
 1.5 with sigma of 0.02
 C45A-C46
 2.5 with sigma of 0.02
 C31A-C40A = C31-C40
 1.5 with sigma of 0.02
 C31A-C15 = C15-C31
 1.5 with sigma of 0.02
 C38-C36
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C32) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C39A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C45) \\sim Ueq, Uanis(C45A) \\sim Ueq, Uanis(C49A) \\sim Ueq, Uanis(C49)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq, Uanis(C37A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C31) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C40A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C25) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, C37, C38, C39, C40, C42, C41, C43, C44, C45, C46, C48, C47,
 C50, C49, C37A, C32A, C39A, C49A, C45A, C31A, C40A, C25A, S1, S2, S3, S4, S5,
 S6, S7, S8, S9, S10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H9AA(0.5) H9AB(0.5) H9BC(0.5) H9BD(0.5) H13A(0.5) H13B(0.5)
 H13C(0.5) H13D(0.5) H15A(0.5) H15B(0.5) H15C(0.5) H15D(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5) H16D(0.5) H17A(0.5) H17B(0.5) H17C(0.5) H17D(0.5)
 H22A(0.5) H22B(0.5) H22C(0.5) H22D(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 H23D(0.5) C25(0.5) H25A(0.5) H25B(0.5) H28A(0.5) H28B(0.5) H28C(0.5) H28D(0.5)
 C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5) H32B(0.5) C37(0.5) H37A(0.5)
 H37B(0.5) C39(0.5) H39A(0.5) H39B(0.5) C40(0.5) H40A(0.5) H40B(0.5) H44(0.5)
 H44A(0.5) C45(0.5) H45A(0.5) H45B(0.5) H50A(0.5) H50B(0.5) H50C(0.5) H50D(0.5)
 C49(0.5) H49A(0.5) H49B(0.5) C37A(0.5) H37C(0.5) H37D(0.5) C32A(0.5) H32C(0.5)
 H32D(0.5) C39A(0.5) H39C(0.5) H39D(0.5) C49A(0.5) H49C(0.5) H49D(0.5)
 C45A(0.5) H45C(0.5) H45D(0.5) C31A(0.5) H31C(0.5) H31D(0.5) C40A(0.5)
 H40C(0.5) H40D(0.5) C25A(0.5) H25C(0.5) H25D(0.5)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C8(H8), C12(H12), C20(H20), C27(H27), C34(H34),
 C42(H42), C44(H44), C44(H44A)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9AA,H9AB), C9(H9BC,
 H9BD), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C13(H13C,H13D),
 C14(H14A,H14B), C15(H15A,H15B), C15(H15C,H15D), C16(H16A,H16B), C16(H16C,H16D),
  C17(H17A,H17B), C17(H17C,H17D), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,
 H21B), C22(H22A,H22B), C22(H22C,H22D), C23(H23A,H23B), C23(H23C,H23D),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C28(H28C,H28D),
  C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B),
  C46(H46A,H46B), C48(H48A,H48B), C47(H47A,H47B), C50(H50A,H50B), C50(H50C,
 H50D), C49(H49A,H49B), C37A(H37C,H37D), C32A(H32C,H32D), C39A(H39C,H39D),
 C49A(H49C,H49D), C45A(H45C,H45D), C31A(H31C,H31D), C40A(H40C,H40D), C25A(H25C,
 H25D)
;
_shelx_res_checksum              16649
_shelx_hkl_checksum              32037
_shelx_fab_checksum              54538
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'