Structural Evolution of Atomically Precise Thiolated Bimetallic [Au12+nCu32(SR)30+n](4-) (n = 0, 2, 4, 6) Nanoclusters.
Yang, Huayan; Wang, Yu; Yan, Juanzhu; Chen, Xi; Zhang, Xin; Häkkinen, Hannu; Zheng, Nanfeng; Journal of the American Chemical Society 136 (2014) 7197–7200; doi:10.1021/ja501811j

data_4121796
_publ_section_title
;
 Structural Evolution of Atomically Precise Thiolated Bimetallic
 [Au12+nCu32(SR)30+n](4-) (n = 0, 2, 4, 6) Nanoclusters.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7197
_journal_page_last               7200
_journal_paper_doi               10.1021/ja501811j
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'C135.94 H76.85 Au13 Cu12 F61.03 S20, 4(C24 H20 P), 0.78(C6)'
_chemical_formula_sum            'C238 H164 Au13 Cl4 Cu12 F60 O4 P4 S20'
_chemical_formula_weight         8457.62
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-04
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                63.599(5)
_cell_angle_beta                 82.266(4)
_cell_angle_gamma                80.078(4)
_cell_formula_units_Z            1
_cell_length_a                   18.0621(8)
_cell_length_b                   19.5128(9)
_cell_length_c                   20.8568(10)
_cell_measurement_reflns_used    17829
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.0050
_cell_measurement_theta_min      4.2940
_cell_volume                     6471.7(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector_area_resol_mean 10.3415
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9608
_diffrn_measurement_details
;
  1 omega  -50.00   35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7424   38.0000 -180.0000 85

  2 omega  -49.00   23.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7424   38.0000  -90.0000 72

  3 omega -128.00  -78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7424  178.0000   90.0000 50

  4 omega -115.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7424  -57.0000   30.0000 103

  5 omega   62.00  121.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7424 -178.0000   90.0000 59

  6 omega -145.00  -89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -94.0000  150.0000 56

  7 omega   28.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -94.0000  -60.0000 77

  8 omega   33.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940 -125.0000 -120.0000 88

  9 omega   30.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -77.0000   30.0000 112

 10 omega   90.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940   45.0000   30.0000 77

 11 omega   32.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000   90.0000 48

 12 omega   59.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -97.0000   19.0000 51

 13 omega   60.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000   30.0000 27

 14 omega   52.00   84.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000 -180.0000 32

 15 omega   37.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000    0.0000 52

 16 omega   34.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -45.0000  -90.0000 64

 17 omega   25.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -94.0000 -120.0000 70

 18 omega   44.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940    0.0000 -180.0000 130
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0557203000
_diffrn_orient_matrix_UB_12      0.0364894000
_diffrn_orient_matrix_UB_13      0.0215013000
_diffrn_orient_matrix_UB_21      0.0026651000
_diffrn_orient_matrix_UB_22      -0.0689682000
_diffrn_orient_matrix_UB_23      0.0746835000
_diffrn_orient_matrix_UB_31      0.0664685000
_diffrn_orient_matrix_UB_32      -0.0425231000
_diffrn_orient_matrix_UB_33      -0.0281071000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40869
_diffrn_reflns_theta_full        61.17
_diffrn_reflns_theta_max         61.17
_diffrn_reflns_theta_min         3.55
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.427
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    2.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3987
_platon_squeeze_details
;
SQUEEZE removed 2 disordered dichloromethane and four water molecules per formula unit.
;
_refine_diff_density_max         3.825
_refine_diff_density_min         -2.754
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1490
_refine_ls_number_reflns         19869
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.178
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+37.0670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                16951
_reflns_number_total             19869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja501811j_si_006.cif
_cod_data_source_block           (AuCu)25
_cod_depositor_comments
'Adding full bibliography for 4121793--4121797.cif.'
_cod_original_cell_volume        6471.6(5)
_cod_database_code               4121796
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F27-C63 = F26-C63 = F25-C63
 1.3 with sigma of 0.02
 F22A-C128 = F119-C128
 1.35 with sigma of 0.02
3. Rigid bond restraints
 F3, C7
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F5, C14
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F7, C21
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F14, C35
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F27, C63
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C25, C26
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C32, C35
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C43, C44
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 P1, C71
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C72, C73
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C77, C82
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C91, C92
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 P2, C95
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C96, C97
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C97, C98
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C101, C102
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C103, C104
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C105, C106
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C110, C111
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C108) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F22A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Sof(S8A)=Sof(H52A)=Sof(H55A)=Sof(H54A)=1-FVAR(1)
 Sof(S8)=FVAR(1)
 Sof(F22A)=1-FVAR(2)
 Sof(F22)=Sof(F23)=FVAR(2)
 Sof(C53B)=Sof(C50B)=Sof(C52B)=Sof(C51B)=Sof(C54B)=Sof(C55B)=1-FVAR(3)
 Sof(C53A)=Sof(C52A)=Sof(C51A)=Sof(C50A)=Sof(C55A)=Sof(C54A)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C30(H30), C27(H27), C16(H16), C62(H62),
 C20(H20), C17(H17), C61(H61), C23(H23), C26(H26), C40(H40), C19(H19), C24(H24),
  C76(H76), C75(H75), C74(H74), C73(H73), C72(H72), C13(H13), C12(H12),
 C10(H10), C9(H9), C41(H41), C38(H38), C31(H31), C48(H48), C33(H33), C66(H66),
 C65(H65), C37(H37), C68(H68), C84(H84), C86(H86), C85(H85), C87(H87), C88(H88),
  C69(H69), C47(H47), C45(H45), C34(H34), C93(H93), C92(H92), C91(H91),
 C90(H90), C94(H94), C44(H44), C82(H82), C78(H78), C79(H79), C80(H80),
 C106(H106), C105(H105), C104(H104), C103(H103), C102(H102), C58(H58), C59(H59),
  C100(H100), C96(H96), C97(H97), C98(H98), C99(H99), C81(H81), C114(H114),
 C118(H118), C117(H117), C116(H116), C115(H115), C112(H112), C111(H111),
 C110(H110), C109(H109), C108(H108), C52A(H52A), C51A(H51A), C55A(H55A),
 C54A(H54A)
6.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C71(C76,C75,C74,C73,C72), C8(C13,C12,C11,C10,C9), C83(C84,
 C86,C85,C87,C88), C93(C92,C91,C90,C89,C94), C101(C106,C105,C104,C103,C102),
 C100(C95,C96,C97,C98,C99), C114(C113,C118,C117,C116,C115), C112(C111,C110,C109,
 C108,C107), C53A(C52A,C51A,C50A,C55A,C54A)
;