A Correlated Series of Au/Ag Nanoclusters Revealing the Evolutionary Patterns of Asymmetric Ag Doping.
Li, Yingwei; Luo, Tian-Yi; Zhou, Meng; Song, Yongbo; Rosi, Nathaniel L.; Jin, Rongchao; Journal of the American Chemical Society 140 (2018) 14235–14243; doi:10.1021/jacs.8b08335

data_4133066
_publ_section_title
;
 A Correlated Series of Au/Ag Nanoclusters Revealing the Evolutionary
 Patterns of Asymmetric Ag Doping.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14235
_journal_page_last               14243
_journal_paper_doi               10.1021/jacs.8b08335
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C150 H225 Ag5.76 Au17.24 S15'
_chemical_formula_sum            'C150 H225 Ag5.76 Au17.24 S15'
_chemical_formula_weight         6526.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.945(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4350(8)
_cell_length_b                   34.747(2)
_cell_length_c                   31.2829(15)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      40.09
_cell_measurement_theta_min      2.54
_cell_volume                     18906.7(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      230.01
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'APEX II CCD'
_diffrn_measured_fraction_theta_full 0.337
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker X8 Prospector Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1285
_diffrn_reflns_av_unetI/netI     0.1093
_diffrn_reflns_Laue_measured_fraction_full 0.337
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50213
_diffrn_reflns_point_group_measured_fraction_full 0.337
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         40.169
_diffrn_reflns_theta_min         1.903
_diffrn_source                   'IMuS micro-focus source'
_diffrn_source_target            Cu
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    30.920
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.2869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1530 before and 0.0819 after correction.
The Ratio of minimum to maximum transmission is 0.3836.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.293
_exptl_crystal_description       rod
_exptl_crystal_F_000             11990
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.736
_refine_diff_density_min         -1.587
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1701
_refine_ls_number_reflns         11517
_refine_ls_number_restraints     2358
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0945
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1037P)^2^+2750.2397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2418
_refine_ls_wR_factor_ref         0.2617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8412
_reflns_number_total             11517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08335_si_004.cif
_cod_data_source_block           ltylyw20170918_0m_a
_cod_original_cell_volume        18906.9(17)
_cod_database_code               4133066
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.747
_shelx_estimated_absorpt_t_min   0.063
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Au2, Ag2}
{Au3, Ag3}
{Au4, Ag4}
{Au5, Ag5}
{Au6, Ag6}
{Au7, Ag7}
{Au8, Ag8}
{Au9, Ag9}
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim
C19 \\sim C20: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim
C29 \\sim C30: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim
C39 \\sim C40: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
C49 \\sim C50: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim
C59 \\sim C60: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim
C69 \\sim C70: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim
C79 \\sim C80: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim
C89 \\sim C90: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim C98 \\sim
C99 \\sim C100: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim
C108 \\sim C109 \\sim C110: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim
C118 \\sim C119 \\sim C120: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim C127 \\sim
C128 \\sim C129 \\sim C130: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C131 \\sim C132 \\sim C133 \\sim C134 \\sim C135 \\sim C136 \\sim C137 \\sim
C138 \\sim C139 \\sim C140: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C141 \\sim C142 \\sim C143 \\sim C144 \\sim C145 \\sim C146 \\sim C147 \\sim
C148 \\sim C149 \\sim C150: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(Au2) = Uanis(Ag2)
Uanis(Au3) = Uanis(Ag3)
Uanis(Au4) = Uanis(Ag4)
Uanis(Au5) = Uanis(Ag5)
Uanis(Au6) = Uanis(Ag6)
Uanis(Au7) = Uanis(Ag7)
Uanis(Au8) = Uanis(Ag8)
Uanis(Au9) = Uanis(Ag9)
4. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12, C13, C14, C15, C16, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C22, C23, C24, C25, C26, C27, C28, C29, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C32, C33, C34, C35, C36, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C42, C43, C44, C45, C46, C47, C48, C49, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, C52, C53, C54, C55, C56, C57, C58, C59, C60
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61, C62, C63, C64, C65, C66, C67, C68, C69, C70
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C71, C72, C73, C74, C75, C76, C77, C78, C79, C80
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C81, C82, C83, C84, C85, C86, C87, C88, C89, C90
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, C92, C93, C94, C95, C96, C97, C98, C99, C100
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C101, C102, C103, C104, C105, C106, C107, C108, C109, C110
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C111, C112, C113, C114, C115, C116, C117, C118, C119, C120
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C121, C122, C123, C124, C125, C126, C127, C128, C129, C130
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C131, C132, C133, C134, C135, C136, C137, C138, C139, C140
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C141, C142, C143, C144, C145, C146, C147, C148, C149, C150
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Ag2)=1-FVAR(1)
 Sof(Au2)=FVAR(1)
 Sof(Ag3)=1-FVAR(2)
 Sof(Au3)=FVAR(2)
 Sof(Ag4)=1-FVAR(3)
 Sof(Au4)=FVAR(3)
 Sof(Ag5)=1-FVAR(4)
 Sof(Au5)=FVAR(4)
 Sof(Ag6)=1-FVAR(5)
 Sof(Au6)=FVAR(5)
 Sof(Ag7)=1-FVAR(6)
 Sof(Au7)=FVAR(6)
 Sof(Ag8)=1-FVAR(7)
 Sof(Au8)=FVAR(7)
 Sof(Ag9)=1-FVAR(8)
 Sof(Au9)=FVAR(8)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C13(H13), C15(H15), C18(H18), C23(H23), C25(H25),
 C29(H29), C33(H33), C35(H35), C40(H40), C43(H43), C45(H45), C49(H49), C53(H53),
  C55(H55), C60(H60), C65(H65), C66(H66), C70(H70), C73(H73), C75(H75),
 C78(H78), C83(H83), C85(H85), C89(H89), C93(H93), C95(H95), C100(H100),
 C103(H103), C105(H105), C110(H110), C113(H113), C115(H115), C119(H119),
 C123(H123), C125(H125), C130(H130), C135(H135), C137(H137), C140(H140),
 C143(H143), C145(H145), C148(H148)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C4(H4a,H4b), C6(H6a,H6b), C7(H7a,H7b), C8(H8a,H8b), C10(H10a,
 H10b), C12(H12a,H12b), C14(H14a,H14b), C16(H16a,H16b), C17(H17a,H17b),
 C19(H19a,H19b), C20(H20a,H20b), C22(H22a,H22b), C24(H24a,H24b), C26(H26a,H26b),
  C27(H27a,H27b), C28(H28a,H28b), C30(H30a,H30b), C32(H32a,H32b), C34(H34a,
 H34b), C36(H36a,H36b), C37(H37a,H37b), C38(H38a,H38b), C39(H39a,H39b),
 C42(H42a,H42b), C44(H44a,H44b), C46(H46a,H46b), C47(H47a,H47b), C48(H48a,H48b),
  C50(H50a,H50b), C52(H52a,H52b), C54(H54a,H54b), C56(H56a,H56b), C57(H57a,
 H57b), C58(H58a,H58b), C59(H59a,H59b), C62(H62a,H62b), C63(H63a,H63b),
 C64(H64a,H64b), C67(H67a,H67b), C68(H68a,H68b), C69(H69a,H69b), C72(H72a,H72b),
  C74(H74a,H74b), C76(H76a,H76b), C77(H77a,H77b), C79(H79a,H79b), C80(H80a,
 H80b), C82(H82a,H82b), C84(H84a,H84b), C86(H86a,H86b), C87(H87a,H87b),
 C88(H88a,H88b), C90(H90a,H90b), C92(H92a,H92b), C94(H94a,H94b), C96(H96a,H96b),
  C97(H97a,H97b), C98(H98a,H98b), C99(H99a,H99b), C102(H10c,H10d), C104(H10e,
 H10f), C106(H10g,H10h), C107(H10i,H10j), C108(H10k,H10l), C109(H10m,H10n),
 C112(H11a,H11b), C114(H11c,H11d), C116(H11e,H11f), C117(H11g,H11h), C118(H11i,
 H11j), C120(H12c,H12d), C122(H12e,H12f), C124(H12g,H12h), C126(H12i,H12j),
 C127(H12k,H12l), C128(H12m,H12n), C129(H12o,H12p), C132(H13a,H13b), C133(H13c,
 H13d), C134(H13e,H13f), C136(H13g,H13h), C138(H13i,H13j), C139(H13k,H13l),
 C142(H14c,H14d), C144(H14e,H14f), C146(H14g,H14h), C147(H14i,H14j), C149(H14k,
 H14l), C150(H15a,H15b)
;
_shelx_res_checksum              77099
_shelx_hkl_checksum              10041
_olex2_submission_special_instructions 'No special instructions were received'