Total Structure Determination of Au<sub>16</sub>(S-Adm)<sub>12</sub> and Cd<sub>1</sub>Au<sub>14</sub>(S tBu)<sub>12</sub> and Implications for the Structure of Au<sub>15</sub>(SR)<sub>13</sub>.
Yang, Sha; Chen, Shuang; Xiong, Lin; Liu, Chong; Yu, Haizhu; Wang, Shuxin; Rosi, Nathaniel L.; Pei, Yong; Zhu, Manzhou; Journal of the American Chemical Society 140 (2018) 10988–10994; doi:10.1021/jacs.8b04257

data_4132482
_publ_section_title
;
 Total Structure Determination of Au<sub>16</sub>(S-Adm)<sub>12</sub> and
 Cd<sub>1</sub>Au<sub>14</sub>(S tBu)<sub>12</sub> and Implications for
 the Structure of Au<sub>15</sub>(SR)<sub>13</sub>.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10988
_journal_page_last               10994
_journal_paper_doi               10.1021/jacs.8b04257
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C48 H108 Au14 Cd S12'
_chemical_formula_sum            'C48 H108 Au14 Cd S12'
_chemical_formula_weight         3940.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.508(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.960(4)
_cell_length_b                   20.862(3)
_cell_length_c                   19.584(3)
_cell_measurement_reflns_used    7186
_cell_measurement_temperature    296
_cell_measurement_theta_max      25.616
_cell_measurement_theta_min      2.216
_cell_volume                     9300(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1074
_diffrn_reflns_av_unetI/netI     0.1124
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_number            9615
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.330
_diffrn_reflns_theta_min         1.324
_exptl_absorpt_coefficient_mu    22.503
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.1929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1809 before and 0.0792 after correction.
The Ratio of minimum to maximum transmission is 0.2588.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.814
_exptl_crystal_description       block
_exptl_crystal_F_000             6720
_refine_diff_density_max         2.310
_refine_diff_density_min         -1.706
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     357
_refine_ls_number_reflns         9615
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0495P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5240
_reflns_number_total             9615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04257_si_003.cif
_cod_data_source_block           20160403a_0m
_cod_database_code               4132482
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Au8, Cd8}
3. Restrained distances
 C17-C20 = C17-C19 = C24-C21 = C22-C21 = C23-C21 = C3-C1 = C2-C1 = C1-C4 = C10-
 C9 = C12-C9 = C11-C9 = C7-C5 = C6-C5 = C13-C16 = C15-C13 = C13-C14
 1.52 with sigma of 0.02
 C18-C17
 1.52 with sigma of 0.02
 C8-C5
 1.52 with sigma of 0.02
4. Rigid bond restraints
 C9, C12
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
C17 \\sim C19 \\sim C20 \\sim C18: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C5 \\sim C6 \\sim C7 \\sim C8: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C3) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C18) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Au8) = Uanis(Cd8)
6. Others
 Fixed Sof: Au8(0.5) Cd8(0.5)
7.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'