A Magnetic Look into the Protecting Layer of Au25Clusters
Agrachev, Mikhail; Antonello, Sabrina; Dainese, Tiziano; Gascon, Jose; Pan, Fangfang; Rissanen, Kari; Ruzzi, Marco; Venzo, Alfonso; Zoleo, Alfonso; Maran, Flavio; Chem. Sci.  (2016) –; doi:10.1039/C6SC03691K

data_1544157
_publ_section_title
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 A Magnetic Look into the Protecting Layer of Au25Clusters
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C6SC03691K
_journal_year                    2016
_chemical_formula_moiety         'C54 H126 Au25 S18'
_chemical_formula_sum            'C54 H126 Au25 S18'
_chemical_formula_weight         6276.78
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-12 deposited with the CCDC.
2016-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.771(2)
_cell_length_b                   17.771(2)
_cell_length_c                   27.217(2)
_cell_measurement_reflns_used    1165
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.0530
_cell_measurement_theta_min      2.7420
_cell_volume                     7443.8(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measurement_details
;
  1 omega  -77.00   16.00   1.0000  260.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.6221  -19.0000    0.0000 93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0077614000
_diffrn_orient_matrix_UB_12      0.0174411000
_diffrn_orient_matrix_UB_13      0.0215904000
_diffrn_orient_matrix_UB_21      0.0340917000
_diffrn_orient_matrix_UB_22      -0.0024233000
_diffrn_orient_matrix_UB_23      0.0120994000
_diffrn_orient_matrix_UB_31      0.0300242000
_diffrn_orient_matrix_UB_32      0.0425733000
_diffrn_orient_matrix_UB_33      -0.0081473000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.812
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            4883
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.972
_diffrn_reflns_theta_min         1.998
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    37.189
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.550
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    4.201
_exptl_crystal_description       plate
_exptl_crystal_F_000             8139
_exptl_crystal_size_max          0.0619
_exptl_crystal_size_mid          0.0405
_exptl_crystal_size_min          0.0144
_refine_diff_density_max         1.608
_refine_diff_density_min         -2.034
_refine_diff_density_rms         0.326
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3240
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0288P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2181
_reflns_number_total             3240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc03691k2.cif
_cod_data_source_block           Au25_SPr_18
_cod_original_cell_volume        7444(2)
_cod_database_code               1544157
_chemical_oxdiff_formula         'Au25 C300 H900 S18'
_reflns_odcompleteness_completeness 92.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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
 C1-C2 = C2-C3 = C4-C5 = C5-C6 = C7-C8 = C8-C9
 1.54 with sigma of 0.02
 H5A_$1-H2A
 2.2 with sigma of 0.02
 C2B-C1 \\sim C2B-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3 \\sim C2B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C2) = Uanis(C2B)
4. Others
 Sof(Au2B)=Sof(Au3B)=Sof(Au4B)=Sof(Au5B)=1-FVAR(1)
 Sof(Au2A)=Sof(Au3A)=Sof(Au4A)=Sof(Au5A)=FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(H3BD)=Sof(H3BE)=Sof(H3BF)=Sof(C2B)=Sof(H2BA)=
 Sof(H2BB)=1-FVAR(2)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=
 FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,
 H7B), C8(H8A,H8B), C2B(H2BA,H2BB)
5.b Me refined with riding coordinates:
 C3(H3AA,H3AB,H3AC), C3(H3BD,H3BE,H3BF)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'