X-ray Crystal Structure and Theoretical Analysis of Au25‒xAgx(SCH2CH2Ph)18‒Alloy
Kumara, Chanaka; Aikens, Christine M.; Dass, Amala; The Journal of Physical Chemistry Letters 5 (2014) 461–; doi:10.1021/jz402441d

data_8000197
_publ_section_title
;
 X-ray Crystal Structure and Theoretical Analysis of
 Au25--xAgx(SCH2CH2Ph)18--Alloy
;
_journal_issue                   3
_journal_name_full               'The Journal of Physical Chemistry Letters'
_journal_page_first              461
_journal_paper_doi               10.1021/jz402441d
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C144 H162 Ag6.66 Au18.34 S18'
_chemical_formula_sum            'C144 H162 Ag6.66 Au18.34 S18'
_chemical_formula_weight         6800.70
_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     direct
_audit_creation_date             2013-07-29
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                105.871(12)
_cell_angle_beta                 106.252(13)
_cell_angle_gamma                90.74(2)
_cell_formula_units_Z            1
_cell_length_a                   16.191(7)
_cell_length_b                   17.244(7)
_cell_length_c                   18.613(7)
_cell_measurement_reflns_used    9092
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.36
_cell_volume                     4776(3)
_computing_cell_refinement       'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_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  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58305
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.359
_diffrn_reflns_theta_min         1.190
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.917
_exptl_absorpt_correction_T_max  0.1689
_exptl_absorpt_correction_T_min  0.0946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1036 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.5601.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3076
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.637
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         23796
_refine_ls_number_restraints     509
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0550P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16319
_reflns_number_total             23796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz402441d_si_002.cif
_cod_data_source_block           dass01_sq_s
_cod_database_code               8000197
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Shared sites
{Au2, Ag2}
{Au3, Ag3}
{Au4, Ag4}
{Au5, Ag5}
{Au6, Ag6}
{Au10, Ag10}
3. Restrained distances
 C51A-C50 \\sim C51-C50
 with sigma of 0.004
 S1-C1 \\sim S2-C9 \\sim S3-C17 \\sim S4-C25 \\sim S5-C33 \\sim S6-C41 \\sim S7-C49 \\sim S8-C57 \\sim S9-C65
 \\sim S4A-C25A
 with sigma of 0.01
 C2-C1 \\sim C18-C17 \\sim C9-C10 \\sim C58-C57 \\sim C42-C41 \\sim C66-C65 \\sim C34-C33 \\sim C50-C49 ~
 C26-C25 \\sim C25A-C26A
 with sigma of 0.01
 C3-C2 \\sim C19-C18 \\sim C59-C58 \\sim C11-C10 \\sim C43-C42 \\sim C67-C66 \\sim C35-C34 \\sim C51-C50 ~
 C51A-C50 \\sim C27-C26 \\sim C26A-C27A
 with sigma of 0.01
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(Au2) = Uanis(Ag2)
Uanis(Au3) = Uanis(Ag3)
Uanis(Au4) = Uanis(Ag4)
Uanis(Au5) = Uanis(Ag5)
Uanis(Au6) = Uanis(Ag6)
Uanis(Au10) = Uanis(Ag10)
Uiso(C51) = Uiso(C52) = Uiso(C53) = Uiso(C54) = Uiso(C55) = Uiso(C56) = Uiso(C51A) = Uiso(C52A) = Uiso(C53A) = Uiso(C54A) = Uiso(C55A) = Uiso(C56A)
Uiso(C25) = Uiso(C26) = Uiso(C27) = Uiso(C28) = Uiso(C29) = Uiso(C30) = Uiso(C31) = Uiso(C32) = Uiso(C27A) = Uiso(C28A) = Uiso(C29A) = Uiso(C30A) = Uiso(C31A) = Uiso(C32A) = Uiso(C26A) = Uiso(C25A)
6. Others
 Sof(Ag2)=1-FVAR(1)
 Sof(Au2)=FVAR(1)
 Sof(Ag3)=1-FVAR(2)
 Sof(Au3)=FVAR(2)
 Sof(Ag4)=1-FVAR(3)
 Sof(Au4)=FVAR(3)
 Sof(Ag5)=1-FVAR(4)
 Sof(Au5)=FVAR(4)
 Sof(Ag6)=1-FVAR(5)
 Sof(Au6)=FVAR(5)
 Sof(Ag10)=1-FVAR(6)
 Sof(Au10)=FVAR(6)
 Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(H53A)=
 Sof(C54A)=Sof(H54A)=Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=1-FVAR(7)
 Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53)=Sof(C54)=
 Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=FVAR(7)
 Sof(S4A)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=
 Sof(C27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=
 Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=1-FVAR(8)
 Sof(S4)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=
 Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=
 Sof(C32)=Sof(H32)=FVAR(8)
7.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C25A(H25C,H25D), C26A(H26C,H26D), C1(H1A,H1B),
  C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C17(H17A,H17B), C18(H18A,H18B),
 C33(H33A,H33B), C34(H34A,H34B), C41(H41A,H41B), C42(H42A,H42B), C49(H49A,H49B),
  C50(H50A,H50B), C50(H50C,H50D), C57(H57A,H57B), C58(H58A,H58B), C65(H65A,
 H65B), C66(H66A,H66B)
7.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C28A(H28A), C29A(H29A),
 C30A(H30A), C31A(H31A), C32A(H32A), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
 C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C52(H52), C53(H53), C54(H54),
  C55(H55), C56(H56), C52A(H52A), C53A(H53A), C54A(H54A), C55A(H55A),
 C56A(H56A), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C68(H68),
 C69(H69), C70(H70), C71(H71), C72(H72)
7.c Fitted hexagon refined as free rotating group:
 C27(C28,C29,C30,C31,C32), C27A(C28A,C29A,C30A,C31A,C32A), C3(C4,C5,C6,C7,C8),
 C11(C12,C13,C14,C15,C16), C19(C20,C21,C22,C23,C24), C35(C36,C37,C38,C39,C40),
 C43(C44,C45,C46,C47,C48), C51(C52,C53,C54,C55,C56), C51A(C52A,C53A,C54A,C55A,
 C56A), C59(C60,C61,C62,C63,C64), C67(C68,C69,C70,C71,C72)
;
_shelx_estimated_absorpt_t_max   0.755
_shelx_estimated_absorpt_t_min   0.382
_shelx_fab_checksum              27433
_shelx_hkl_checksum              4652
_shelx_res_checksum              724
_shelxl_version_number           2013-3