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_4133065
_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 Ag4 Au19 S15'
_chemical_formula_sum            'C150 H225 Ag4 Au19 S15'
_chemical_formula_weight         6683.03
_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     dual
_audit_creation_date             2018-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.106(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4011(6)
_cell_length_b                   44.214(2)
_cell_length_c                   30.3350(13)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      36.43
_cell_measurement_theta_min      2.47
_cell_volume                     23304.6(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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      230.01
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II CCD'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'APEX II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1404
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            98840
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        36.672
_diffrn_reflns_theta_max         36.672
_diffrn_reflns_theta_min         1.768
_diffrn_source                   'IMuS micro-focus source'
_diffrn_source_target            Cu
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.953
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.3246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1453 before and 0.0849 after correction. The Ratio of minimum to maximum transmission is 0.4344. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_description       Rod
_exptl_crystal_F_000             12216
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         8.927
_refine_diff_density_min         -2.451
_refine_diff_density_rms         0.376
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         11229
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.1317
_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^)+(0.0893P)^2^+7451.8389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3186
_refine_ls_wR_factor_ref         0.3306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9218
_reflns_number_total             11229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08335_si_003.cif
_cod_data_source_block           ltylyw20171014_8to1_0m
_cod_original_cell_volume        23304.5(17)
_cod_database_code               4133065
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.625
_shelx_estimated_absorpt_t_min   0.048
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S1-C1
 1.8 with sigma of 0.02
 C1-C2
 1.55 with sigma of 0.02
 C4-C10
 2.44 with sigma of 0.02
 C2-C7
 2.44 with sigma of 0.02
 C48-C43 = C50-C48
 1.55 with sigma of 0.02
 C9-C8 = C9-C3
 1.55 with sigma of 0.02
 C44-C48 = C49-C48
 2.54 with sigma of 0.04
 C9-C10 = C4-C9
 2.54 with sigma of 0.04
 C80-C71 \\sim C72-C71
 with sigma of 0.02
 C118-C120 \\sim C111-C116 \\sim C113-C114
 with sigma of 0.02
 C88-C90 \\sim C88-C87 \\sim C88-C89
 with sigma of 0.02
 C140-C135 \\sim C131-C137 \\sim C133-C139
 with sigma of 0.02
 S2-C11 \\sim S3-C21
 with sigma of 0.02
 C96-C94 \\sim C92-C94
 with sigma of 0.02
 C95-C94 \\sim C94-C93
 with sigma of 0.02
 C99-C98 \\sim C96-C95 \\sim C93-C92
 with sigma of 0.02
 C47-C50 \\sim C45-C46
 with sigma of 0.02
 C47-C46 \\sim C50-C45
 with sigma of 0.02
 C43-C45 \\sim C42-C46
 with sigma of 0.02
 C43-C42 \\sim C44-C43
 with sigma of 0.02
 C42-C41 \\sim C45-C44
 with sigma of 0.02
 C15-C14 \\sim C20-C15 \\sim C16-C15
 with sigma of 0.02
 C16-C11 \\sim C20-C18 \\sim C14-C13
 with sigma of 0.02
 C41-C43 \\sim C41-C50
 with sigma of 0.02
 C59-C57 \\sim C60-C57 \\sim C58-C57
 with sigma of 0.02
 C58-C59 \\sim C55-C53
 with sigma of 0.02
 C82-C84 \\sim C86-C84 \\sim C90-C84 \\sim C87-C84
 with sigma of 0.02
 C89-C81 \\sim C87-C83 \\sim C90-C85
 with sigma of 0.02
 C89-C88 \\sim C88-C87 \\sim C90-C88
 with sigma of 0.02
 C73-C72 \\sim C74-C73 \\sim C79-C73
 with sigma of 0.02
 C105-C104 \\sim C108-C105 \\sim C109-C108 \\sim C110-C109 \\sim C110-C103
\\sim C104-C103
 with sigma of 0.02
 C106-C105 \\sim C109-C107 \\sim C103-C102
 with sigma of 0.02
 C102-C101 \\sim C107-C101 \\sim C106-C101
 with sigma of 0.02
 C118-C115 \\sim C116-C115 \\sim C115-C114
 with sigma of 0.02
 C126-C121 \\sim C130-C121 \\sim C122-C121
 with sigma of 0.02
 C124-C123 \\sim C125-C124 \\sim C129-C123 \\sim C127-C125 \\sim C128-C127
\\sim C129-C128
 with sigma of 0.02
 C122-C124 \\sim C126-C124 \\sim C127-C124 \\sim C129-C124
 with sigma of 0.02
 C135-C134 \\sim C140-C135 \\sim C136-C135
 with sigma of 0.02
 C132-C131 \\sim C137-C131 \\sim C136-C131
 with sigma of 0.02
 C138-C131 \\sim C140-C136
 with sigma of 0.02
 C134-C140 \\sim C133-C138
 with sigma of 0.02
 C1-C2 \\sim C1-C7 \\sim C1-C6
 with sigma of 0.02
 C6-C7 \\sim C8-C5
 with sigma of 0.02
 C44-C49 \\sim C50-C43
 with sigma of 0.02
 C2-C6 \\sim C1-C3 \\sim C3-C5 \\sim C5-C1
 with sigma of 0.02
 C6-C1 \\sim C7-C1 \\sim C8-C7 \\sim C6-C5
 with sigma of 0.02
 C4-C5 \\sim C1-C2 \\sim C10-C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Ag1 \\sim S1 \\sim Au1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 Ag1, S1, Au1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C13(H13), C15(H15), C18(H18), C23(H23), C25(H25),
 C28(H28), C33(H33), C35(H35), C38(H38), C43(H43), C45(H45), C50(H50), C53(H53),
  C55(H55), C57(H57), C63(H63), C65(H65), C68(H68), C73(H73), C75(H75),
 C78(H78), C83(H83), C85(H85), C88(H88), C93(H93), C95(H95), C98(H98),
 C103(H103), C105(H105), C109(H109), C113(H113), C115(H115), C120(H120),
 C123(H123), C125(H125), C128(H128), C133(H133), C135(H135), C138(H138),
 C143(H143), C145(H145), C150(H150)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), 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),
  C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C34(H34A,H34B), C36(H36A,
 H36B), C37(H37A,H37B), C39(H39A,H39B), C40(H40A,H40B), C42(H42A,H42B),
 C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B),
  C52(H52A,H52B), C54(H54A,H54B), C56(H56A,H56B), C58(H58A,H58B), C59(H59A,
 H59B), C60(H60A,H60B), C62(H62A,H62B), C64(H64A,H64B), C66(H66A,H66B),
 C67(H67A,H67B), C69(H69A,H69B), C70(H70A,H70B), 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), C89(H89A,H89B),
 C90(H90A,H90B), C92(H92A,H92B), C94(H94A,H94B), C96(H96A,H96B), C97(H97A,H97B),
  C99(H99A,H99B), C100(H10C,H10D), C102(H10E,H10F), C104(H10G,H10H), C106(H10I,
 H10J), C107(H10K,H10L), C108(H10M,H10N), C110(H11A,H11B), C112(H11C,H11D),
 C114(H11E,H11F), C116(H11G,H11H), C117(H11I,H11J), C118(H11K,H11L), C119(H11M,
 H11N), C122(H12C,H12D), C124(H12E,H12F), C126(H12G,H12H), C127(H12I,H12J),
 C129(H12K,H12L), C130(H13A,H13B), C132(H13C,H13D), C134(H13E,H13F), C136(H13G,
 H13H), C137(H13I,H13J), C139(H13K,H13L), C140(H14C,H14D), C142(H14E,H14F),
 C144(H14G,H14H), C146(H14I,H14J), C147(H14K,H14L), C148(H14M,H14N), C149(H14O,
 H14P), C9(H9A,H9B)
;
_shelx_res_checksum              4319
_shelx_hkl_checksum              45582
_olex2_submission_special_instructions 'No special instructions were received'