Au25(SEt)18, a Nearly Naked Thiolate-Protected Au25 Cluster: Structural Analysis by Single Crystal X-ray Crystallography and Electron Nuclear Double Resonance.
Dainese, Tiziano; Antonello, Sabrina; Gascón, José A; Pan, Fangfang; Perera, Neranjan V.; Ruzzi, Marco; Venzo, Alfonso; Zoleo, Alfonso; Rissanen, Kari; Maran, Flavio; ACS nano 8 (2014) 3904–3912; doi:10.1021/nn500805n

data_4510222
_publ_section_title
;
 Au25(SEt)18, a Nearly Naked Thiolate-Protected Au25 Cluster: Structural
 Analysis by Single Crystal X-ray Crystallography and Electron Nuclear
 Double Resonance.
;
_journal_issue                   4
_journal_name_full               'ACS nano'
_journal_page_first              3904
_journal_page_last               3912
_journal_paper_doi               10.1021/nn500805n
_journal_volume                  8
_journal_year                    2014
_chemical_formula_moiety         'C36 H90 Au25 S18'
_chemical_formula_sum            'C36 H90 Au25 S18'
_chemical_formula_weight         6024.32
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                104.383(3)
_cell_angle_beta                 101.406(3)
_cell_angle_gamma                119.292(4)
_cell_formula_units_Z            1
_cell_length_a                   13.7727(6)
_cell_length_b                   13.8864(6)
_cell_length_c                   14.1519(5)
_cell_measurement_reflns_used    4938
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      76.4800
_cell_measurement_theta_min      4.1510
_cell_volume                     2116.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      123.0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13182
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         76.647
_diffrn_reflns_theta_min         3.706
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    83.388
_exptl_absorpt_correction_T_max  0.553
_exptl_absorpt_correction_T_min  0.342
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2569
_exptl_crystal_size_max          0.0738
_exptl_crystal_size_mid          0.0418
_exptl_crystal_size_min          0.0412
_refine_diff_density_max         2.671
_refine_diff_density_min         -2.557
_refine_diff_density_rms         0.438
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         8455
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0608
_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^)+(0.1026P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6681
_reflns_number_total             8455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nn500805n_si_002.cif
_cod_data_source_block           au25_131031_abs_ana
_cod_depositor_comments          'Adding full bibliography for 4510222.cif.'
_cod_original_cell_volume        2116.91(16)
_cod_database_code               4510222
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-C2 \\sim C3-C4 \\sim C5-C6 \\sim C7-C8 \\sim C9-C10 \\sim C11-C12 \\sim
C13-C14 \\sim C15-C16 \\sim C17-C18
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C7 \\sim C8: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C7 \\sim C8: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C5) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C10)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B)
4.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C14(H14A,H14B,H14C)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              77599
_shelx_hkl_checksum              23436