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_4132483
_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         'C120 H179 Au14 Cd S12, 3(C H2 Cl2)'
_chemical_formula_sum            'C123 H185 Au14 Cd Cl6 S12'
_chemical_formula_weight         5131.05
_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     dual
_audit_creation_date             2018-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_cell_angle_alpha                80.994(2)
_cell_angle_beta                 82.064(2)
_cell_angle_gamma                62.481(2)
_cell_formula_units_Z            2
_cell_length_a                   16.476(2)
_cell_length_b                   16.719(2)
_cell_length_c                   30.157(4)
_cell_measurement_reflns_used    6832
_cell_measurement_temperature    170
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.35
_cell_volume                     7255.9(16)
_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      170
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.1622
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            48378
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.371
_exptl_absorpt_coefficient_mu    14.558
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.349
_exptl_crystal_description       block
_exptl_crystal_F_000             4742
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_refine_diff_density_max         5.410
_refine_diff_density_min         -4.223
_refine_diff_density_rms         0.417
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1405
_refine_ls_number_reflns         25553
_refine_ls_number_restraints     3297
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0650P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14051
_reflns_number_total             25553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04257_si_004.cif
_cod_data_source_block           mo_dm16342_0m_sq
_cod_database_code               4132483
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.122
_shelx_estimated_absorpt_t_min   0.097
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Au1, Cd1}
{Au2, Cd2}
3. Restrained distances
 C01S-C02P
 1.55 with sigma of 0.02
 C03E-C03B
 1.55 with sigma of 0.02
 C12-C1AA
 1.55 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C0AA \\sim C01A \\sim C1AA \\sim C01B \\sim C01C \\sim C01D \\sim C01E \\sim
C01G \\sim C01H \\sim C01I \\sim C01J \\sim C01K \\sim C01L \\sim C01M \\sim
C01N \\sim C01O \\sim C01P \\sim C01R \\sim C01S \\sim C01T \\sim C01U \\sim
C01V \\sim C01W \\sim C01X \\sim C01Y \\sim C01Z \\sim C02A \\sim C02B \\sim
C02C \\sim C02D \\sim C02E \\sim C02F \\sim C02G \\sim C02H \\sim C02I \\sim
C02J \\sim C02K \\sim C02L \\sim C02M \\sim C02N \\sim C02O \\sim C02P \\sim
C02Q \\sim C02R \\sim C02S \\sim C02T \\sim C02U \\sim C02V \\sim C02W \\sim
C02X \\sim C02Y \\sim C02Z \\sim C03A \\sim C03B \\sim C03C \\sim C03D \\sim
C03E \\sim C03F \\sim C03G \\sim C03H \\sim C03I \\sim C03J \\sim C03K \\sim
C03L \\sim C03M \\sim C03N \\sim C03O \\sim C03P \\sim C03Q \\sim C03R \\sim
C03S \\sim C03T \\sim C03V \\sim C03W \\sim C03X \\sim C03Y \\sim C03Z \\sim
C04A \\sim C04B \\sim C04C \\sim C11 \\sim C011 \\sim C12 \\sim C012 \\sim C013
\\sim C014 \\sim C015 \\sim C016 \\sim C017 \\sim C018 \\sim C18 \\sim C019
\\sim C020 \\sim C021 \\sim C022 \\sim C023 \\sim C024 \\sim C025 \\sim C026
\\sim C027 \\sim C028 \\sim C029 \\sim C030 \\sim C031 \\sim C032 \\sim C033
\\sim C034 \\sim C035 \\sim C036 \\sim C037 \\sim C038 \\sim C039 \\sim C040
\\sim C041 \\sim C042 \\sim C043 \\sim C044 \\sim C046 \\sim C047 \\sim C048
\\sim C16 \\sim C13 \\sim C31: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Cl3 \\sim Cl4 \\sim C13: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.005
Cl5 \\sim Cl8 \\sim C31: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.005
Uanis(Au1) = Uanis(Cd1)
Uanis(Au2) = Uanis(Cd2)
5. Others
 Fixed Sof: Au1(0.5) Cd2(0.5) Au2(0.5) Cd1(0.5)
6.a Ternary CH refined with riding coordinates:
 C01C(H01E), C01D(H01F), C01G(H01I), C01N(H01R), C01X(H2AA), C01Y(H3AA),
 C02A(H02A), C02F(H02J), C02T(H7AA), C02V(H9AA), C02W(H0BA), C02Y(H2BA),
 C02Z(H3BA), C03A(H03A), C03G(H03H), C03R(H03Z), C03S(H03), C03X(H7BA),
 C03Z(H9BA), C04B(H04C), C04C(H04D), C12(H12), C017(H017), C018(H018),
 C025(H025), C027(H027), C028(H028), C029(H029), C032(H032), C035(H035),
 C038(H038), C040(H040), C041(H041), C044(H044), C046(H046), C047(H047)
6.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C01A(H01A,H01B), C1AA(H1AA,H1AB), C01B(H01C,H01D), C01E(H01G,
 H01H), C01I(H01J,H01K), C01K(H01L,H01M), C01L(H01N,H01O), C01M(H01P,H01Q),
 C01P(H01S,H01T), C01R(H01U,H01V), C01T(H01W,H01X), C01U(H01Y,H), C01V(H01Z,HA),
  C01W(H01,HB), C01Z(H4AA,HC), C02B(H02B,H02C), C02C(H02D,H02E), C02D(H02F,
 H02G), C02E(H02H,H02I), C02G(H02K,H02L), C02H(H02M,H02N), C02I(H02O,H02P),
 C02J(H02Q,H02R), C02K(H02S,H02T), C02L(H02U,H02V), C02N(H02W,H02X), C02O(H02Y,
 HD), C02P(H02Z,HE), C02Q(H02,HF), C02R(H5AA,HG), C02S(H6AA,HH), C02U(H8AA,HI),
 C02X(H1BA,HJ), C03B(H03B,H03C), C03C(H03D,H03E), C03D(H03F,H03G), C03H(H03I,
 H03J), C03J(H03K,H03L), C03K(H03M,H03N), C03L(H03O,H03P), C03M(H03Q,H03R),
 C03N(H03S,H03T), C03O(H03U,H03V), C03P(H03W,H03X), C03Q(H03Y,HK), C03T(H4BA,
 HL), C03V(H5BA,HM), C03W(H6BA,HN), C03Y(H8BA,HO), C04A(H04A,H04B), C11(H11A,
 H11B), C012(H0CA,HP), C013(H1CA,HQ), C016(H2CA,HR), C18(H18A,H18B), C019(H3CA,
 HS), C020(H4CA,HT), C021(H5CA,HU), C022(H6CA,HV), C024(H7CA,HW), C026(H8CA,HX),
  C030(H9CA,HY), C031(H0DA,HZ), C033(H1DA,H5DA), C036(H2DA,H6DA), C037(H3DA,
 H7DA), C039(H4DA,H8DA), C042(H04E,H04F), C043(H04G,H04H), C048(H04I,H04J),
 C16(H16A,H16B), C13(H13A,H13B), C31(H31A,H31B)
6.c Aromatic/amide H refined with riding coordinates:
 C034(H034)
;
_shelx_res_checksum              74406
_shelx_hkl_checksum              98123
_shelx_fab_checksum              23625
_olex2_submission_special_instructions 'No special instructions were received'