An Intermetallic Au24Ag20 Superatom Nanocluster Stabilized by Labile Ligands.
Wang, Yu; Su, Haifeng; Xu, Chaofa; Li, Gang; Gell, Lars; Lin, Shuichao; Tang, Zichao; Häkkinen, Hannu; Zheng, Nanfeng; Journal of the American Chemical Society  (2015) 150327131618002–; doi:10.1021/jacs.5b01232

data_4123542
_publ_section_title
;
 An Intermetallic Au24Ag20 Superatom Nanocluster Stabilized by Labile
 Ligands.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              150327131618002
_journal_paper_doi               10.1021/jacs.5b01232
_journal_year                    2015
_chemical_formula_moiety         'C180 H116 Ag20 Au24 Cl2 N4 S4'
_chemical_formula_sum            'C180 H116 Ag20 Au24 Cl2 N4 O4 S4'
_chemical_formula_weight         9482.50
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.335(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.9728(5)
_cell_length_b                   18.7149(5)
_cell_length_c                   25.7811(7)
_cell_measurement_temperature    100(2)
_cell_volume                     10036.4(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-1997 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33041
_diffrn_reflns_theta_full        61.17
_diffrn_reflns_theta_max         61.17
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    48.227
_exptl_crystal_density_diffrn    3.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8380
_platon_squeeze_details
;
SQUEEZE removed 2 disordered water molecules per formula unit.
;
_refine_diff_density_max         4.863
_refine_diff_density_min         -2.941
_refine_diff_density_rms         0.393
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         15424
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+378.5172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.1932
_reflns_number_gt                13014
_reflns_number_total             15424
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b01232_si_002.cif
_cod_data_source_block           Au24Ag20
_cod_original_cell_volume        10036.3(5)
_cod_database_code               4123542
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 C30, C29, C28, C27, C32, C31, C26, C25
 with sigma of 0.1
 C77, C76, C75, C80, C79, C78, C74, C73
 with sigma of 0.1
3. Rigid bond restraints
 C61, C62
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C59, C58
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C54, C55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C35, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C83, C82
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C41, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Au11, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C86) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C13) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C90) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C63)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C90) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(C86) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C48) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C16) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C90) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C77(H77), C76(H76),
 C80(H80), C79(H79), C78(H78), C87(H87), C88(H88), C89(H89), C90(H90), C30(H30),
  C29(H29), C28(H28), C32(H32), C31(H31), C24(H24), C20(H20), C21(H21),
 C22(H22), C23(H23), C85(H85), C4(H4), C8(H8), C7(H7), C6(H6), C5(H5), C16(H16),
  C15(H15), C14(H14), C13(H13), C12(H12), C72(H72), C71(H71), C70(H70),
 C69(H69), C68(H68), C36(H36), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
  C37(H37), C60(H60), C64(H64), C63(H63), C62(H62), C61(H61), C38(H38),
 C39(H39), C83(H83), C82(H82), C84(H84), C40(H40)
5.b Fitted hexagon refined as free rotating group:
 C43(C44,C45,C46,C47,C48), C77(C76,C75,C80,C79,C78), N2(C86,C87,C88,C89,C90),
 C30(C29,C28,C27,C32,C31), C24(C19,C20,C21,C22,C23), C4(C3,C8,C7,C6,C5),
 C11(C16,C15,C14,C13,C12), C72(C71,C70,C69,C68,C67), C51(C52,C53,C54,C55,C56),
 C60(C59,C64,C63,C62,C61)
;
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20