Single Crystal XRD Structure and Theoretical Analysis of the Chiral Au30S(S-t-Bu)18 Cluster.
Crasto, David; Malola, Sami; Brosofsky, Grace; Dass, Amala; Häkkinen, Hannu; Journal of the American Chemical Society 136 (2014) 5000–5005; doi:10.1021/ja412141j

data_4121607
_publ_section_title
;
 Single Crystal XRD Structure and Theoretical Analysis of the Chiral
 Au30S(S-t-Bu)18 Cluster.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5000
_journal_page_last               5005
_journal_paper_doi               10.1021/ja412141j
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C72 H162 Au30 S19'
_chemical_formula_sum            'C72 H162 Au30 S19'
_chemical_formula_weight         7546.14
_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
_audit_creation_date             2014-02-25
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                81.352(7)
_cell_angle_beta                 78.546(6)
_cell_angle_gamma                69.930(7)
_cell_formula_units_Z            2
_cell_length_a                   14.982(5)
_cell_length_b                   19.899(7)
_cell_length_c                   28.215(10)
_cell_measurement_temperature    173(2)
_cell_volume                     7713(5)
_computing_cell_refinement       'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 Verr. 2013.2-0 (Buker-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      173.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.498
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.50\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_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  0.1267
_diffrn_reflns_av_unetI/netI     0.1274
_diffrn_reflns_Laue_measured_fraction_full 0.498
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57513
_diffrn_reflns_point_group_measured_fraction_full 0.498
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         19.782
_diffrn_reflns_theta_min         0.739
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_exptl_absorpt_coefficient_mu    28.681
_exptl_absorpt_correction_T_max  0.0870
_exptl_absorpt_correction_T_min  0.0366
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6536
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.962
_refine_diff_density_min         -2.729
_refine_diff_density_rms         0.577
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         13890
_refine_ls_number_restraints     1530
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0916P)^2^+124.7198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8334
_reflns_number_total             13890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja412141j_si_002.cif
_cod_data_source_block           sep9
_cod_database_code               4121607
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Same fragment restrains
{S1, C1, C2, C3, C4}
{S2, C5, C6, C7, C8}
{S3, C9, C10, C11, C12}
{S4, C13, C14, C15, C16}
{S5, C17, C18, C19, C20}
{S6, C21, C22, C23, C24}
{S7, C25, C26, C27, C28}
{S8, C29, C30, C31, C32}
{S10, C37, C38, C39, C40}
{S11, C41, C42, C43, C44}
{S12, C45, C46, C47, C48}
{S13, C49, C50, C51, C52}
{S14, C53, C54, C55, C56}
{S15, C57, C58, C59, C60}
{S16, C61, C62, C63, C64}
{S17, C65, C66, C67, C68}
{S18, C69, C70, C71, C72}
as
{S9, C33, C34, C35, C36}
3.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), C8(H8a,H8b,H8c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C12(H12a,
 H12b,H12c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c),
 C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C22(H22a,H22b,
 H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C26(H26a,H26b,H26c), C27(H27a,
 H27b,H27c), C28(H28a,H28b,H28c), C30(H30a,H30b,H30c), C31(H31a,H31b,H31c),
 C32(H32a,H32b,H32c), C34(H34a,H34b,H34c), C35(H35a,H35b,H35c), C36(H36a,H36b,
 H36c), C38(H38a,H38b,H38c), C39(H39a,H39b,H39c), C40(H40a,H40b,H40c), C42(H42a,
 H42b,H42c), C43(H43a,H43b,H43c), C44(H44a,H44b,H44c), C46(H46a,H46b,H46c),
 C47(H47a,H47b,H47c), C48(H48a,H48b,H48c), C50(H50a,H50b,H50c), C51(H51a,H51b,
 H51c), C52(H52a,H52b,H52c), C54(H54a,H54b,H54c), C55(H55a,H55b,H55c), C56(H56a,
 H56b,H56c), C58(H58a,H58b,H58c), C59(H59a,H59b,H59c), C60(H60a,H60b,H60c),
 C62(H62a,H62b,H62c), C63(H63a,H63b,H63c), C64(H64a,H64b,H64c), C66(H66a,H66b,
 H66c), C67(H67a,H67b,H67c), C68(H68a,H68b,H68c), C70(H70a,H70b,H70c), C71(H71a,
 H71b,H71c), C72(H72a,H72b,H72c)
;
_shelx_estimated_absorpt_t_max   0.352
_shelx_estimated_absorpt_t_min   0.099
_shelxl_version_number           2013-4