Ag<sub>18</sub>(μ<sub>8</sub>-S)(p-TBBT)<sub>16</sub>(PPh<sub>3</sub>)<sub>8</sub>: symmetry breaking induced by the core to generate chirality.
Tian, Fan; Chen, Rong; Chemical communications (Cambridge, England) 56 (2020) 2719–2722; doi:10.1039/c9cc10045h

data_7125878
_publ_section_title
;
 Ag<sub>18</sub>(\m<sub>8</sub>-S)(p-TBBT)<sub>16</sub>(PPh<sub>3</sub>)<sub>8</sub>:
 symmetry breaking induced by the core to generate chirality.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2719
_journal_page_last               2722
_journal_paper_doi               10.1039/c9cc10045h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C320 H360 Ag18 P8 S17, 29.675[CH4O]'
_chemical_formula_sum            'C349.68 H478.7 Ag18 O29.68 P8 S17'
_chemical_formula_weight         7891.48
_chemical_name_common            'chiral Ag18S'
_chemical_name_systematic        Ag18(\m8-S)(p-TBBT)16(PPh3)8
_space_group_crystal_system      tetragonal
_space_group_IT_number           130
_space_group_name_Hall           '-P 4a 2ac'
_space_group_name_H-M_alt        'P 4/n c c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-01-24
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-01-24 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.69470(10)
_cell_length_b                   26.69470(10)
_cell_length_c                   50.0946(3)
_cell_measurement_reflns_used    96272
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.8470
_cell_measurement_theta_min      3.3260
_cell_volume                     35697.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     43.00  69.00   0.50    0.60    --    0.00  38.00-150.00   52
  2  \w    -16.00  29.00   0.50    0.60    --    0.00 -82.00  30.00   90
  3  \w    -14.00  12.00   0.50    0.60    --    0.00 -82.00-150.00   52
  4  \w      9.00  83.00   0.50    0.60    --    0.00  38.00-120.00  148
  5  \w    -32.00  19.00   0.50    0.60    --    0.00 -82.00-180.00  102
  6  \w      7.00 114.00   0.50    3.00    --   94.60 -77.00 120.00  214
  7  \w      5.00 114.00   0.50    3.00    --   94.60 -45.00 -60.00  218
  8  \w     49.00  87.00   0.50    3.00    --   94.60 -30.00-180.00   76
  9  \w      7.00  44.00   0.50    3.00    --   94.60 -30.00-180.00   74
 10  \w    154.00 183.00   0.50    3.00    --   94.60  77.00   0.00   58
 11  \w     12.00 117.00   0.50    3.00    --   94.60 -61.00 120.00  210
 12  \w    114.00 158.00   0.50    3.00    --   94.60  30.00 -90.00   88
 13  \w     85.00 183.00   0.50    3.00    --   94.60  15.00-150.00  196
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            202082
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.007
_diffrn_reflns_theta_min         2.341
_exptl_absorpt_coefficient_mu    9.456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull reddish black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             16209
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.332
_refine_diff_density_min         -1.750
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         18035
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0839P)^2^+91.1623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15399
_reflns_number_total             18035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc10045h2.cif
_cod_data_source_block           20190429_1
_cod_depositor_comments          'Adding full bibliography for 7125878.cif.'
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_original_formula_sum        'C349.68 H478.70 Ag18 O29.68 P8 S17'
_cod_database_code               7125878
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.451
_shelx_estimated_absorpt_t_min   0.254
_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
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C39S-C38S
 1.6 with sigma of 0.02
 C39S-C36S
 1.6 with sigma of 0.02
 C5S-C8S \\sim C5S-C12S
 with sigma of 0.02
 C10S-C8S \\sim C11S-C12S
 with sigma of 0.02
 C15S-C8S \\sim C14S-C12S
 with sigma of 0.02
 C8S-C9S \\sim C12S-C13S
 with sigma of 0.02
 C5S-C10S \\sim C5S-C11S
 with sigma of 0.04
 C5S-C15S \\sim C5S-C14S
 with sigma of 0.04
 C5S-C9S \\sim C5S-C13S
 with sigma of 0.04
 C10S-C15S \\sim C11S-C14S
 with sigma of 0.04
 C10S-C9S \\sim C11S-C13S
 with sigma of 0.04
 C15S-C9S \\sim C14S-C13S
 with sigma of 0.04
 C27S-C28S \\sim C27S-C43S
 with sigma of 0.02
 C33S-C32S \\sim C44S-C45S
 with sigma of 0.02
 C33S-C28S \\sim C44S-C43S
 with sigma of 0.02
 C32S-C31S \\sim C45S-C40S
 with sigma of 0.02
 C31S-C30S \\sim C40S-C41S
 with sigma of 0.02
 C31S-C34S \\sim C40S-C39S
 with sigma of 0.02
 C30S-C29S \\sim C41S-C42S
 with sigma of 0.02
 C29S-C28S \\sim C42S-C43S
 with sigma of 0.02
 C27S-C33S \\sim C27S-C44S
 with sigma of 0.04
 C27S-C29S \\sim C27S-C42S
 with sigma of 0.04
 C33S-C31S \\sim C44S-C40S
 with sigma of 0.04
 C33S-C29S \\sim C44S-C42S
 with sigma of 0.04
 C32S-C30S \\sim C45S-C41S
 with sigma of 0.04
 C32S-C28S \\sim C45S-C43S
 with sigma of 0.04
 C32S-C34S \\sim C45S-C39S
 with sigma of 0.04
 C31S-C29S \\sim C40S-C42S
 with sigma of 0.04
 C30S-C28S \\sim C41S-C43S
 with sigma of 0.04
 C30S-C34S \\sim C41S-C39S
 with sigma of 0.04
 C7S-C2S \\sim C7T-C2S
 with sigma of 0.02
 C7S-C6S \\sim C7T-C6T
 with sigma of 0.02
 C2S-C3S \\sim C2S-C3T
 with sigma of 0.02
 C3S-C4S \\sim C3T-C4T
 with sigma of 0.02
 C4S-C5S \\sim C4T-C5T
 with sigma of 0.02
 C5S-C6S \\sim C5T-C6T
 with sigma of 0.02
 C5S-C8S \\sim C5T-C8S
 with sigma of 0.02
 C5S-C12S \\sim C5T-C12S
 with sigma of 0.02
 C7S-C5S \\sim C7T-C5T
 with sigma of 0.04
 C2S-C4S \\sim C2S-C4T
 with sigma of 0.04
 C2S-C6S \\sim C2S-C6T
 with sigma of 0.04
 C3S-C5S \\sim C3T-C5T
 with sigma of 0.04
 C4S-C6S \\sim C4T-C6T
 with sigma of 0.04
 C4S-C8S \\sim C4T-C8S
 with sigma of 0.04
 C4S-C12S \\sim C4T-C12S
 with sigma of 0.04
 C6S-C8S \\sim C6T-C8S
 with sigma of 0.04
 C6S-C12S \\sim C6T-C12S
 with sigma of 0.04
3. Rigid bond restraints
 C12S, C6S
 with sigma for 1-2 distances of 2.5 and sigma for 1-3 distances of 2.5
4. Uiso/Uaniso restraints and constraints
Uanis(C38S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27P) = Uanis(C28P) = Uanis(C29P) = Uanis(C30P) = Uanis(C25P) =
Uanis(C26P)
Uanis(C37S) = Uanis(C36S) = Uanis(C39S) = Uanis(C38S) = Uanis(C34S) =
Uanis(C35S)
5. Others
 Sof(H27C)=Sof(H27D)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(H37D)=Sof(H37E)=
 Sof(H37F)=Sof(C39S)=Sof(C40S)=Sof(C41S)=Sof(H41S)=Sof(C42S)=Sof(H42S)=
 Sof(C43S)=Sof(C44S)=Sof(H44S)=Sof(C45S)=Sof(H45S)=1-FVAR(1)
 Sof(H27A)=Sof(H27B)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(H37A)=Sof(H37B)=
 Sof(H37C)=Sof(C33S)=Sof(H33S)=Sof(C32S)=Sof(H32S)=Sof(C31S)=Sof(C30S)=
 Sof(H30S)=Sof(C29S)=Sof(H29S)=Sof(C28S)=Sof(C34S)=FVAR(1)
 Fixed Sof: C7S(0.515) H7S(0.515) C3S(0.515) H3S(0.515) C4S(0.515) H4S(0.515)
 C5S(0.515) C6S(0.515) H6S(0.515) C8S(0.515) C9S(0.515) H9SA(0.515) H9SB(0.515)
 H9SC(0.515) C10S(0.515) H10A(0.515) H10B(0.515) H10C(0.515) C15S(0.515)
 H15A(0.515) H15B(0.515) H15C(0.515) C35S(0.45788) H35A(0.45788) H35B(0.45788)
 H35C(0.45788) C11S(0.485) H11A(0.485) H11B(0.485) H11C(0.485) C12S(0.485)
 C13S(0.485) H13A(0.485) H13B(0.485) H13C(0.485) C14S(0.485) H14A(0.485)
 H14B(0.485) H14C(0.485) C38S(0.54212) H38A(0.54212) H38B(0.54212)
 H38C(0.54212) C5T(0.485) C6T(0.485) H6T(0.485) C7T(0.485) H7T(0.485)
 C3T(0.485) H3T(0.485) C4T(0.485) H4T(0.485)
6.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C16S(H16A,H16B), C27S(H27A,H27B), C27S(H27C,H27D), C46S(H46A,
 H46B)
6.b Aromatic/amide H refined with riding coordinates:
 C2P(H2P), C3P(H3P), C4P(H4P), C5P(H5P), C6P(H6P), C7S(H7S), C3S(H3S),
 C4S(H4S), C6S(H6S), C8P(H8P), C9P(H9P), C10P(H10P), C11P(H11P), C12P(H12P),
 C14P(H14P), C15P(H15P), C16P(H16P), C17P(H17P), C18P(H18P), C18S(H18S),
 C19S(H19S), C21S(H21S), C22S(H22S), C20P(H20P), C21P(H21P), C22P(H22P),
 C23P(H23P), C24P(H24P), C28P(H28P), C29P(H29P), C30P(H30P), C26P(H26P),
 C27P(H27P), C36P(H36P), C35P(H35P), C34P(H34P), C33P(H33P), C32P(H32P),
 C49S(H49S), C48S(H48S), C52S(H52S), C51S(H51S), C33S(H33S), C32S(H32S),
 C30S(H30S), C29S(H29S), C41S(H41S), C42S(H42S), C44S(H44S), C45S(H45S),
 C6T(H6T), C7T(H7T), C3T(H3T), C4T(H4T)
6.c Fitted hexagon refined as free rotating group:
 C7S(C2S,C3S,C4S,C5S,C6S), C18S(C19S,C20S,C21S,C22S,C17S), C28P(C29P,C30P,C25P,
 C26P,C27P), C31P(C36P,C35P,C34P,C33P,C32P), C50S(C49S,C48S,C47S,C52S,C51S),
 C33S(C32S,C31S,C30S,C29S,C28S)
6.d Idealised Me refined as rotating group:
 C24S(H24A,H24B,H24C), C25S(H25A,H25B,H25C), C26S(H26A,H26B,H26C), C36S(H36A,
 H36B,H36C), C36S(H36D,H36E,H36F), C37S(H37A,H37B,H37C), C37S(H37D,H37E,H37F),
 C54S(H54A,H54B,H54C), C55S(H55A,H55B,H55C), C56S(H56A,H56B,H56C), C9S(H9SA,
 H9SB,H9SC), C10S(H10A,H10B,H10C), C15S(H15A,H15B,H15C), C35S(H35A,H35B,H35C),
 C11S(H11A,H11B,H11C), C13S(H13A,H13B,H13C), C14S(H14A,H14B,H14C), C38S(H38A,
 H38B,H38C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23628
_shelx_fab_checksum              5646
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;