Gold-doped silver nanocluster [Au3Ag38(SCH2Ph)24X5](2-) (X = Cl or Br).
Wang, Zhi; Senanayake, Ravithree; Aikens, Christine M.; Chen, Wen-Miao; Tung, Chen-Ho; Sun, Di; Nanoscale 8 (2016) 18905–18911; doi:10.1039/c6nr06615a

data_1544250
_publ_section_title
;
 Gold-doped silver nanocluster [Au3Ag38(SCH2Ph)24X5](2-) (X = Cl or Br).
;
_journal_issue                   45
_journal_name_full               Nanoscale
_journal_page_first              18905
_journal_page_last               18911
_journal_paper_doi               10.1039/c6nr06615a
_journal_volume                  8
_journal_year                    2016
_chemical_formula_moiety
'C168 H168 Ag38 Au3 Br1.9 Cl3.1 S24, 2(C24 H20 P), 4(C2 H2 Cl4), 2(C H Cl3)'
_chemical_formula_sum            'C226 H218 Ag38 Au3 Br1.9 Cl25.1 P2 S24'
_chemical_formula_weight         9496.96
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-06-18 deposited with the CCDC.
2016-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.595(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.113(4)
_cell_length_b                   34.407(4)
_cell_length_c                   24.991(3)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.498
_cell_volume                     29678(6)
_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      120.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.1179
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            121553
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.427
_exptl_absorpt_coefficient_mu    4.619
_exptl_crystal_density_diffrn    2.125
_exptl_crystal_description       diamond
_exptl_crystal_F_000             18017
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.437
_refine_diff_density_min         -2.111
_refine_diff_density_rms         0.295
_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     2696
_refine_ls_number_reflns         51586
_refine_ls_number_restraints     883
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1507
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1617P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2695
_refine_ls_wR_factor_ref         0.2929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28716
_reflns_number_total             51586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nr06615a2.cif
_cod_data_source_block           p
_cod_depositor_comments          'Adding full bibliography for 1544250.cif.'
_cod_original_formula_sum        'C226 H218 Ag38 Au3 Br1.90 Cl25.10 P2 S24'
_cod_database_code               1544250
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.769
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Br1, Cl1A}
{Br2, Cl2A}
{Br3, Cl3A}
{Br4, Cl4A}
{Br5, Cl5A}
{Ag13, Au13}
{Ag30, Au30}
3. Restrained distances
 C170-Cl2
 1.75 with sigma of 0.01
 C170-Cl3
 1.75 with sigma of 0.01
 C170-Cl1
 1.75 with sigma of 0.01
 C43-C44
 1.55 with sigma of 0.01
 C43-C49
 2.35 with sigma of 0.01
 C43-S12
 1.85 with sigma of 0.01
 Cl2-Cl1
 2.9 with sigma of 0.01
 C43-C49
 2.4 with sigma of 0.01
 C43-C45
 2.4 with sigma of 0.01
 C141-C142
 1.55 with sigma of 0.01
4. Restrained planarity
 C43, C44, C45, C49
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
C155 \\sim C156 \\sim C157 \\sim C158 \\sim C159 \\sim C160 \\sim C161: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C169 \\sim Cl4 \\sim Cl5 \\sim Cl6 \\sim C170 \\sim Cl1 \\sim Cl2 \\sim Cl3:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim S12:
within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.08
C89 \\sim C88 \\sim C87 \\sim C86 \\sim C91 \\sim C84 \\sim C79 \\sim C80 \\sim
C81 \\sim C82 \\sim C83 \\sim C68 \\sim C69 \\sim C70 \\sim C23 \\sim C24 \\sim
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C14 \\sim C13 \\sim C12 \\sim C11 \\sim
C10 \\sim C37 \\sim C42 \\sim C41 \\sim C40 \\sim C39 \\sim C38 \\sim C122
\\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim C121 \\sim C119 \\sim C118
\\sim C117 \\sim C116 \\sim C115 \\sim C168 \\sim C167 \\sim C166 \\sim C165
\\sim C164 \\sim C35 \\sim C34 \\sim C33 \\sim C32 \\sim C31 \\sim C71 \\sim
C73 \\sim C77 \\sim C76 \\sim C75 \\sim C74 \\sim C72 \\sim C112 \\sim C111
\\sim C110 \\sim C106 \\sim C107 \\sim C92 \\sim C93 \\sim C98 \\sim C97 \\sim
C96 \\sim C95 \\sim C94 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C58 \\sim C63 \\sim C62 \\sim C61 \\sim C60 \\sim C59 \\sim
C131 \\sim C132 \\sim C133 \\sim C128 \\sim C129 \\sim C130 \\sim C151 \\sim
C152 \\sim C153 \\sim C154 \\sim C150 \\sim C149 \\sim C120 \\sim C113 \\sim C2
\\sim C7 \\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C90: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C134 \\sim C135 \\sim C140 \\sim C138 \\sim C139 \\sim C136: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.08
C215 \\sim C220 \\sim C219 \\sim C218 \\sim C217 \\sim C216 \\sim C197 \\sim
C202 \\sim C201 \\sim C200 \\sim C199 \\sim C192 \\sim C191 \\sim C196 \\sim
C182 \\sim C181 \\sim C180 \\sim C188 \\sim C187 \\sim C186: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.08
C208 \\sim C203 \\sim C204 \\sim C206 \\sim C226 \\sim C221 \\sim C225 \\sim
C224 \\sim C223 \\sim C222: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.08
C173 \\sim C174 \\sim C176 \\sim C175 \\sim C177 \\sim C178 \\sim C171 \\sim
C172: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
S7 \\sim C141 \\sim C142 \\sim C147 \\sim C144 \\sim C145 \\sim C143 \\sim
C146: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
Uanis(Br4) = Uanis(Cl4A)
Uanis(Ag13) = Uanis(Au13)
Uanis(Ag30) = Uanis(Au30)
Uanis(Br3) = Uanis(Cl3A)
Uanis(Br5) = Uanis(Cl5A)
Uanis(Br1) = Uanis(Cl1A)
Uanis(Br2) = Uanis(Cl2A)
6. Others
 Fixed Sof: Ag4(0.8) Ag13(0.5) Au13(0.5) Ag30(0.5) Au30(0.5) Br1(0.35)
 Br2(0.35) Br3(0.35) Br4(0.5) Br5(0.35) Cl1A(0.65) Cl2A(0.65) Cl3A(0.65)
 Cl4A(0.5) Cl5A(0.65) Ag4A(0.2)
7.a Ternary CH refined with riding coordinates:
 C177(H177), C178(H178), C171(H171), C172(H172), C175(H175), C176(H176),
 C173(H173), C174(H174), C169(H169), C170(H170)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C22(H22A,H22B), C29(H29A,H29B),
 C36(H36A,H36B), C43(H43A,H43B), C50(H50A,H50B), C57(H57A,H57B), C64(H64A,H64B),
  C71(H71A,H71B), C78(H78A,H78B), C85(H85A,H85B), C92(H92A,H92B), C99(H99A,
 H99B), C106(H10A,H10B), C113(H11A,H11B), C120(H12A,H12B), C127(H12C,H12D),
 C134(H13A,H13B), C148(H14A,H14B), C155(H15C,H15D), C162(H16A,H16B), C141(H14C,
 H14D)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C45(H45),
  C49(H49), C48(H48), C47(H47), C46(H46), C55(H55), C56(H56), C52(H52),
 C53(H53), C54(H54), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C66(H66),
  C67(H67), C68(H68), C69(H69), C70(H70), C73(H73), C74(H74), C75(H75),
 C76(H76), C77(H77), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C91(H91),
  C90(H90), C89(H89), C88(H88), C87(H87), C94(H94), C95(H95), C96(H96),
 C97(H97), C98(H98), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105),
  C108(H108), C109(H109), C110(H110), C111(H111), C112(H112), C115(H115),
 C116(H116), C117(H117), C118(H118), C119(H119), C124(H124), C125(H125),
 C126(H126), C122(H122), C123(H123), C129(H129), C130(H130), C131(H131),
 C132(H132), C133(H133), C136(H136), C137(H137), C138(H138), C139(H139),
 C140(H140), C150(H150), C151(H151), C152(H152), C153(H153), C154(H154),
 C160(H160), C161(H161), C157(H157), C158(H158), C159(H159), C164(H164),
 C165(H165), C166(H166), C167(H167), C168(H168), C203(H203), C204(H204),
 C205(H205), C206(H206), C207(H207), C210(H210), C211(H211), C212(H212),
 C213(H213), C214(H214), C220(H220), C219(H219), C218(H218), C217(H217),
 C216(H216), C222(H222), C223(H223), C224(H224), C225(H225), C226(H226),
 C180(H180), C181(H181), C182(H182), C183(H183), C184(H184), C186(H186),
 C187(H187), C188(H188), C189(H189), C190(H190), C192(H192), C193(H193),
 C194(H194), C195(H195), C196(H196), C198(H198), C199(H199), C200(H200),
 C201(H201), C202(H202), C143(H143), C144(H144), C145(H145), C146(H146),
 C147(H147)
7.d Fitted hexagon refined as free rotating group:
 C45(C44,C49,C48,C47,C46), C55(C56,C51,C52,C53,C54), C86(C91,C90,C89,C88,C87),
 C124(C125,C126,C121,C122,C123), C160(C161,C156,C157,C158,C159), C215(C220,C219,
 C218,C217,C216), C142(C143,C144,C145,C146,C147)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'