Heteroatom Tracing Reveals the 30-Atom Au-Ag Bimetallic Nanocluster as a Dimeric Structure.
Li, Yingwei; Taylor, Michael G.; Luo, Tian-Yi; Song, Yongbo; Rosi, Nathaniel L.; Mpourmpakis, Giannis; Jin, Rongchao; The journal of physical chemistry letters 11 (2020) 7307–7312; doi:10.1021/acs.jpclett.0c01977

data_8000448
_publ_section_title
;
 Heteroatom Tracing Reveals the 30-Atom Au-Ag Bimetallic Nanocluster as a
 Dimeric Structure.
;
_journal_issue                   17
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              7307
_journal_page_last               7312
_journal_paper_doi               10.1021/acs.jpclett.0c01977
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C72 H162 Ag2.69 Au27.31 S18'
_chemical_formula_sum            'C72 H162 Ag2.68 Au27.31 S18'
_chemical_formula_weight         7274.86
_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             2018-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.777(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2662(5)
_cell_length_b                   51.5233(15)
_cell_length_c                   17.4781(5)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    230
_cell_measurement_theta_max      51.025
_cell_measurement_theta_min      3.02
_cell_volume                     13746.4(7)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      230.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'APEX II CCD'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1533
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            102654
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        51.355
_diffrn_reflns_theta_max         51.355
_diffrn_reflns_theta_min         1.715
_diffrn_source                   'IMuS micro-focus source'
_diffrn_source_target            Cu
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    58.953
_exptl_absorpt_correction_T_max  0.7501
_exptl_absorpt_correction_T_min  0.1478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1824 before and 0.0909 after correction. The Ratio of minimum to maximum transmission is 0.1970. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.515
_exptl_crystal_description       needle
_exptl_crystal_F_000             12664
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.310
_refine_diff_density_min         -2.097
_refine_diff_density_rms         0.467
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         14920
_refine_ls_number_restraints     813
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0865
_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^)+(0.0379P)^2^+2999.0439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11061
_reflns_number_total             14920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz0c01977_si_002.cif
_cod_data_source_block           ltylyw20180511_0m_a
_cod_depositor_comments          'Adding full bibliography for 8000448.cif.'
_cod_database_code               8000448
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.201
_shelx_estimated_absorpt_t_min   0.030
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Ag7, Au7}
{Ag19, Au19}
{Ag21, Au21}
{Ag22, Au22}
{Ag23, Au23}
{Ag24, Au24}
{Ag26, Au26}
{Ag27, Au27}
3. Restrained distances
 C42-C43 \\sim C43-C44 \\sim C44-C42
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
S1 \\sim C1 \\sim C2 \\sim C3 \\sim C4: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S2 \\sim C5 \\sim C6 \\sim C7 \\sim C8: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S3 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S4 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S5 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S6 \\sim C21 \\sim C22 \\sim C23 \\sim C24: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S7 \\sim C25 \\sim C26 \\sim C27 \\sim C28: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S8 \\sim C29 \\sim C30 \\sim C31 \\sim C32: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S9 \\sim C33 \\sim C34 \\sim C35 \\sim C36: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S10 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S11 \\sim C41 \\sim C42 \\sim C43 \\sim C44: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S12 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S13 \\sim C49 \\sim C50 \\sim C51 \\sim C52: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S15 \\sim C57 \\sim C58 \\sim C59 \\sim C60: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S16 \\sim C61 \\sim C62 \\sim C63 \\sim C64: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S17 \\sim C65 \\sim C66 \\sim C67 \\sim C68: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
S18 \\sim C69 \\sim C70 \\sim C71 \\sim C72: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(Ag7) = Uanis(Au7)
Uanis(Ag19) = Uanis(Au19)
Uanis(Ag21) = Uanis(Au21)
Uanis(Ag22) = Uanis(Au22)
Uanis(Ag23) = Uanis(Au23)
Uanis(Ag24) = Uanis(Au24)
Uanis(Ag26) = Uanis(Au26)
Uanis(Ag27) = Uanis(Au27)
5. Rigid body (RIGU) restrains
 S1, C1, C2, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S3, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S4, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S5, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S6, C21, C22, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S7, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S8, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S9, C33, C34, C35, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S10, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S11, C41, C42, C43, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S12, C45, C46, C47, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S13, C49, C50, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S15, C57, C58, C59, C60
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S16, C61, C62, C63, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S17, C65, C66, C67, C68
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S18, C69, C70, C71, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Ag7)=1-FVAR(1)
 Sof(Au7)=FVAR(1)
 Sof(Ag22)=1-FVAR(2)
 Sof(Au22)=FVAR(2)
 Sof(Au1A)=1-FVAR(3)
 Sof(Au25)=FVAR(3)
 Sof(A28B)=1-FVAR(4)
 Sof(Au28)=FVAR(4)
 Sof(Ag19)=1-FVAR(5)
 Sof(Au19)=FVAR(5)
 Sof(Ag21)=1-FVAR(6)
 Sof(Au21)=FVAR(6)
 Sof(Ag23)=1-FVAR(7)
 Sof(Au23)=FVAR(7)
 Sof(Ag24)=1-FVAR(8)
 Sof(Au24)=FVAR(8)
 Sof(Ag26)=1-FVAR(9)
 Sof(Au26)=FVAR(9)
 Sof(Ag27)=1-FVAR(10)
 Sof(Au27)=FVAR(10)
7.a Idealised Me refined with riding coordinates:
 C52(H52A,H52B,H52C)
7.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C58(H58A,
 H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C67(H67A,H67B,
 H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,
 H72B,H72C)
;
_olex2_submission_special_instructions 'No special instructions were received'