Structure of Chiral Au44(2,4-DMBT)26 Nanocluster with an 18-Electron Shell Closure.
Liao, Lingwen; Zhuang, Shengli; Yao, Chuanhao; Yan, Nan; Chen, Jishi; Wang, Chengming; Xia, Nan; Liu, Xu; Li, Man-Bo; Li, Lingling; Bao, Xiaoli; Wu, Zhikun; Journal of the American Chemical Society 138 (2016) 10425–10428; doi:10.1021/jacs.6b07178

data_4130822
_publ_section_title
;
 Structure of Chiral Au44(2,4-DMBT)26 Nanocluster with an 18-Electron
 Shell Closure.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10425
_journal_page_last               10428
_journal_paper_doi               10.1021/jacs.6b07178
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C205 H215 Au44 S26'
_chemical_formula_sum            'C208 H234 Au44 S26'
_chemical_formula_weight         12234.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                88.620(2)
_cell_angle_beta                 89.464(2)
_cell_angle_gamma                71.411(2)
_cell_formula_units_Z            2
_cell_length_a                   19.0970(10)
_cell_length_b                   24.0131(13)
_cell_length_c                   29.8101(15)
_cell_measurement_reflns_used    9462
_cell_measurement_temperature    150
_cell_measurement_theta_max      66.629
_cell_measurement_theta_min      2.469
_cell_volume                     12953.3(12)
_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      150.0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            232123
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.878
_diffrn_reflns_theta_max         66.878
_diffrn_reflns_theta_min         2.417
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    47.736
_exptl_absorpt_correction_T_max  0.1643
_exptl_absorpt_correction_T_min  0.0268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1664 before and 0.1031 after correction.
The Ratio of minimum to maximum transmission is 0.1631.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.137
_exptl_crystal_description       block
_exptl_crystal_F_000             10748
_refine_diff_density_max         11.107
_refine_diff_density_min         -7.718
_refine_diff_density_rms         0.965
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.644
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2234
_refine_ls_number_reflns         45135
_refine_ls_number_restraints     1973
_refine_ls_restrained_S_all      1.609
_refine_ls_R_factor_all          0.1666
_refine_ls_R_factor_gt           0.1398
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3650
_refine_ls_wR_factor_ref         0.4009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33225
_reflns_number_total             45135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b07178_si_002.cif
_cod_data_source_block           160421anhui2_0m
_cod_database_code               4130822
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C199-C198
 1.52 with sigma of 0.01
 C144-C140
 1.52 with sigma of 0.01
 C15-C14
 1.52 with sigma of 0.01
 C96-C92
 1.52 with sigma of 0.01
 C16-C12
 1.52 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C129 \\sim C130 \\sim C131 \\sim C132 \\sim C133 \\sim C134: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
C193 \\sim C198 \\sim C197 \\sim C196 \\sim C195 \\sim C194 \\sim C200 \\sim
C199: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C153 \\sim C158 \\sim C157 \\sim C156 \\sim C155 \\sim C154 \\sim C160 \\sim
C159: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C161 \\sim C162 \\sim C163 \\sim C164 \\sim C165 \\sim C166 \\sim C167: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
C137 \\sim C138 \\sim C139 \\sim C140 \\sim C141 \\sim C142 \\sim C143 \\sim
C144: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim C206 \\sim C207 \\sim
C208: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C169 \\sim C174 \\sim C173 \\sim C172 \\sim C171 \\sim C170 \\sim C175 \\sim
C176: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C17 \\sim C22 \\sim C21 \\sim C20 \\sim C19 \\sim C18 \\sim C23 \\sim C24:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C161 \\sim C162 \\sim C163 \\sim C164 \\sim C165 \\sim C166 \\sim C167 \\sim
C168: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C2 \\sim C1 \\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C7 \\sim C8: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01
C177 \\sim C182 \\sim C181 \\sim C180 \\sim C178 \\sim C179 \\sim C184 \\sim
C183: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C57 \\sim C62 \\sim C61 \\sim C60 \\sim C59 \\sim C58 \\sim C63 \\sim C64:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C81 \\sim C86 \\sim C85 \\sim C84 \\sim C83 \\sim C82 \\sim C87 \\sim C88:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C102 \\sim C103: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C54) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C130) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(C158) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C58) \\sim Ueq,
Uanis(C60) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C90)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C70) \\sim Ueq,
Uanis(C159) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C153) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C113) \\sim Ueq,
Uanis(C97) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C114)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C78) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq,
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq,
Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq,
Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C77) \\sim Ueq,
Uanis(C76) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq,
Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86)
\\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C89) \\sim Ueq,
Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C93)
\\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C96) \\sim Ueq,
Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C100)
\\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq,
Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C106) \\sim Ueq,
Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C109) \\sim Ueq,
Uanis(C110) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C115) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C117) \\sim Ueq,
Uanis(C118) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq,
Uanis(C121) \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq,
Uanis(C124) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C126) \\sim Ueq,
Uanis(C129) \\sim Ueq, Uanis(C130) \\sim Ueq, Uanis(C131) \\sim Ueq,
Uanis(C132) \\sim Ueq, Uanis(C133) \\sim Ueq, Uanis(C134) \\sim Ueq,
Uanis(C135) \\sim Ueq, Uanis(C136) \\sim Ueq, Uanis(C137) \\sim Ueq,
Uanis(C138) \\sim Ueq, Uanis(C139) \\sim Ueq, Uanis(C140) \\sim Ueq,
Uanis(C141) \\sim Ueq, Uanis(C142) \\sim Ueq, Uanis(C143) \\sim Ueq,
Uanis(C144) \\sim Ueq, Uanis(C145) \\sim Ueq, Uanis(C146) \\sim Ueq,
Uanis(C147) \\sim Ueq, Uanis(C148) \\sim Ueq, Uanis(C149) \\sim Ueq,
Uanis(C150) \\sim Ueq, Uanis(C151) \\sim Ueq, Uanis(C152) \\sim Ueq,
Uanis(C153) \\sim Ueq, Uanis(C158) \\sim Ueq, Uanis(C157) \\sim Ueq,
Uanis(C156) \\sim Ueq, Uanis(C155) \\sim Ueq, Uanis(C154) \\sim Ueq,
Uanis(C159) \\sim Ueq, Uanis(C160) \\sim Ueq, Uanis(C161) \\sim Ueq,
Uanis(C162) \\sim Ueq, Uanis(C163) \\sim Ueq, Uanis(C164) \\sim Ueq,
Uanis(C165) \\sim Ueq, Uanis(C166) \\sim Ueq, Uanis(C167) \\sim Ueq,
Uanis(C169) \\sim Ueq, Uanis(C170) \\sim Ueq, Uanis(C171) \\sim Ueq,
Uanis(C172) \\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(C174) \\sim Ueq,
Uanis(C175) \\sim Ueq, Uanis(C176) \\sim Ueq, Uanis(C177) \\sim Ueq,
Uanis(C182) \\sim Ueq, Uanis(C181) \\sim Ueq, Uanis(C180) \\sim Ueq,
Uanis(C179) \\sim Ueq, Uanis(C178) \\sim Ueq, Uanis(C183) \\sim Ueq,
Uanis(C184) \\sim Ueq, Uanis(C185) \\sim Ueq, Uanis(C186) \\sim Ueq,
Uanis(C187) \\sim Ueq, Uanis(C188) \\sim Ueq, Uanis(C189) \\sim Ueq,
Uanis(C190) \\sim Ueq, Uanis(C191) \\sim Ueq, Uanis(C192) \\sim Ueq,
Uanis(C193) \\sim Ueq, Uanis(C194) \\sim Ueq, Uanis(C195) \\sim Ueq,
Uanis(C196) \\sim Ueq, Uanis(C197) \\sim Ueq, Uanis(C198) \\sim Ueq,
Uanis(C199) \\sim Ueq, Uanis(C200) \\sim Ueq, Uanis(C201) \\sim Ueq,
Uanis(C206) \\sim Ueq, Uanis(C205) \\sim Ueq, Uanis(C204) \\sim Ueq,
Uanis(C203) \\sim Ueq, Uanis(C202) \\sim Ueq, Uanis(C208) \\sim Ueq,
Uanis(C112) \\sim Ueq, Uanis(C207) \\sim Ueq, Uanis(C168) \\sim Ueq, Uanis(C16)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C10(H10), C11(H11), C13(H13), C18(H18), C19(H19),
 C21(H21), C26(H26), C27(H27), C29(H29), C34(H34), C35(H35), C37(H37), C42(H42),
  C43(H43), C45(H45), C50(H50), C51(H51), C53(H53), C58(H58), C59(H59),
 C61(H61), C66(H66), C67(H67), C69(H69), C77(H77), C75(H75), C74(H74), C82(H82),
  C83(H83), C85(H85), C90(H90), C91(H91), C93(H93), C98(H98), C99(H99),
 C101(H101), C106(H106), C107(H107), C109(H109), C114(H114), C115(H115),
 C117(H117), C123(H123), C125(H125), C130(H130), C131(H131), C133(H133),
 C138(H138), C139(H139), C141(H141), C146(H146), C147(H147), C149(H149),
 C157(H157), C155(H155), C154(H154), C162(H162), C163(H163), C165(H165),
 C170(H170), C171(H171), C173(H173), C181(H181), C179(H179), C178(H178),
 C186(H186), C187(H187), C189(H189), C194(H194), C195(H195), C197(H197),
 C205(H205), C203(H203), C202(H202)
4.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C9(C10,C11,C12,C13,C14), C17(C18,C19,C20,C21,C22),
 C25(C26,C27,C28,C29,C30), C33(C34,C35,C36,C37,C38), C41(C42,C43,C44,C45,C46),
 C49(C50,C51,C52,C53,C54), C73(C78,C77,C76,C75,C74), C81(C82,C83,C84,C85,C86),
 C89(C90,C91,C92,C93,C94), C97(C98,C99,C100,C101,C102), C105(C106,C107,C108,
 C109,C110), C113(C114,C115,C116,C117,C118), C121(C122,C123,C124,C125,C126),
 C129(C130,C131,C132,C133,C134), C137(C138,C139,C140,C141,C142), C145(C146,C147,
 C148,C149,C150), C153(C158,C157,C156,C155,C154), C161(C162,C163,C164,C165,
 C166), C169(C170,C171,C172,C173,C174), C177(C182,C181,C180,C179,C178),
 C185(C186,C187,C188,C189,C190), C193(C194,C195,C196,C197,C198), C201(C206,C205,
 C204,C203,C202)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C48(H48A,
 H48B,H48C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C63(H63A,H63B,H63C),
 C64(H64A,H64B,H64C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C79(H79A,H79B,
 H79C), C80(H80A,H80B,H80C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C95(H95A,
 H95B,H95C), C96(H96A,H96B,H96C), C103(H10A,H10B,H10C), C104(H10D,H10E,H10F),
 C119(H11A,H11B,H11C), C120(H12A,H12B,H12C), C135(H13A,H13B,H13C), C136(H13D,
 H13E,H13F), C143(H14A,H14B,H14C), C144(H14D,H14E,H14F), C151(H15A,H15B,H15C),
 C152(H15D,H15E,H15F), C159(H15G,H15H,H15I), C160(H16A,H16B,H16C), C167(H16D,
 H16E,H16F), C175(H17A,H17B,H17C), C176(H17D,H17E,H17F), C183(H18A,H18B,H18C),
 C184(H18D,H18E,H18F), C191(H19A,H19B,H19C), C192(H19D,H19E,H19F), C199(H19G,
 H19H,H19I), C200(H20B,H20C,H20A), C208(H20D,H20E,H20F), C112(H11D,H11E,H11F),
 C207(H20G,H20H,H20I), C168(H16G,H16H,H16I), C16(H16J,H16K,H16L)
;
_shelx_res_checksum              56544
_shelx_hkl_checksum              59428
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'