Electrocrystallization of Monolayer-Protected Gold Clusters: Opening the Door to Quality, Quantity, and New Structures.
Antonello, Sabrina; Dainese, Tiziano; Pan, Fangfang; Rissanen, Kari; Maran, Flavio; Journal of the American Chemical Society 139 (2017) 4168–4174; doi:10.1021/jacs.7b00568

data_4125889
_publ_section_title
;
 Electrocrystallization of Monolayer-Protected Gold Clusters: Opening the
 Door to Quality, Quantity, and New Structures.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4168
_journal_page_last               4174
_journal_paper_doi               10.1021/jacs.7b00568
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C144 H162 Au25 S18'
_chemical_formula_sum            'C144 H162 Au25 S18'
_chemical_formula_weight         7393.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ac 2bc'
_space_group_name_H-M_alt        'P n a a'
_symmetry_space_group_name_Hall  '-P 2ac 2bc'
_symmetry_space_group_name_H-M   'P n a a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5677(2)
_cell_length_b                   31.2061(8)
_cell_length_c                   26.9907(3)
_cell_measurement_reflns_used    36128
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.3270
_cell_measurement_theta_min      3.1460
_cell_volume                     15639.1(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_details
;
  1 omega   23.00   61.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       20.6883  -96.0000 -133.0000 38

  2 omega  -42.00   48.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       20.6883  -77.0000  -30.0000 90

  3 omega   -2.00   92.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       20.6883   37.0000 -120.0000 94

  4 omega   -5.00   90.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       20.6883   77.0000   90.0000 95
;
_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      -0.0243517000
_diffrn_orient_matrix_UB_12      0.0039574000
_diffrn_orient_matrix_UB_13      -0.0197193000
_diffrn_orient_matrix_UB_21      0.0063065000
_diffrn_orient_matrix_UB_22      -0.0208973000
_diffrn_orient_matrix_UB_23      -0.0093401000
_diffrn_orient_matrix_UB_31      -0.0287511000
_diffrn_orient_matrix_UB_32      -0.0079931000
_diffrn_orient_matrix_UB_33      0.0146617000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            101709
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         29.601
_diffrn_reflns_theta_min         2.834
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    23.629
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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)
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    3.140
_exptl_crystal_description
;
;
_exptl_crystal_F_000             13156
_exptl_crystal_size_max          0.2243
_exptl_crystal_size_mid          0.1624
_exptl_crystal_size_min          0.0505
_refine_diff_density_max         4.505
_refine_diff_density_min         -3.237
_refine_diff_density_rms         0.443
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.300
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         19817
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.291
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0048P)^2^+752.2776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17274
_reflns_number_total             19817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00568_si_002.cif
_cod_data_source_block           au25_sc2ph_18
_cod_database_code               4125889
_chemical_oxdiff_formula         'Au25 S18 C144 H162'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. Restrained distances
 C40B-C35B \\sim C36B-C35B \\sim C36-C35 \\sim C40-C35 \\sim C39-C38 \\sim
C40-C39 \\sim C40B-C39B ~
 C39B-C38B \\sim C38B-C37B \\sim C38-C37 \\sim C37-C36 \\sim C37B-C36B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C37B) \\sim Ueq, Uanis(C36B) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C55) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C39B) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C62)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C19) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C38) \\sim Ueq, Uanis(C35B) \\sim Ueq, Uanis(C40B) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C64B) \\sim Ueq, Uanis(C61B) \\sim Ueq, Uanis(C60B) \\sim Ueq,
Uanis(C59) \\sim Ueq, Uanis(C59B) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C58B) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C57) \\sim Ueq,
Uanis(C74) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(S8) \\sim Ueq, Uanis(S8B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Au11) = Uanis(Au11)
Uanis(Au11) = Uanis(Au12)
Uanis(C35B) = Uanis(C35)
Uanis(C38B) = Uanis(C38)
4. Others
 Sof(Au11)=1-FVAR(1)
 Sof(Au12)=FVAR(1)
 Fixed Sof: H34A(0.5) H34B(0.5) H34C(0.5) H34D(0.5) C35(0.5) C36(0.5) H36(0.5)
 C36B(0.5) H36B(0.5) C37(0.5) H37(0.5) C37B(0.5) H37B(0.5) C38(0.5) H38(0.5)
 C35B(0.5) C38B(0.5) H38B(0.5) C39(0.5) H39(0.5) C39B(0.5) H39B(0.5) C40(0.5)
 H40(0.5) C40B(0.5) H40B(0.5) C57(0.5) H57A(0.5) H57B(0.5) C58(0.5) H58A(0.5)
 H58B(0.5) C58B(0.5) H58C(0.5) H58D(0.5) C59(0.5) C59B(0.5) C60(0.5) H60(0.5)
 C60B(0.5) H60B(0.5) C61(0.5) H61(0.5) C61B(0.5) H61B(0.5) C62(0.5) H62(0.5)
 C62B(0.5) H62B(0.5) C63(0.5) H63(0.5) C63B(0.5) H63B(0.5) C64(0.5) H64(0.5)
 C64B(0.5) H64B(0.5) C74(0.5) H74A(0.5) H74B(0.5) S8(0.5) S8B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C17(H17A,H17B),
 C18(H18A,H18B), C25(H25A,H25B), C26(H26A,H26B), C33(H33A,H33B), C34(H34A,H34B),
  C34(H34C,H34D), C41(H41A,H41B), C42(H42A,H42B), C49(H49A,H49B), C50(H50A,
 H50B), C57(H57A,H57B), C58(H58A,H58B), C58B(H58C,H58D), C65(H65A,H65B),
 C66(H66A,H66B), C74(H74A,H74B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C36(H36), C36B(H36B), C37(H37),
 C37B(H37B), C38(H38), C38B(H38B), C39(H39), C39B(H39B), C40(H40), C40B(H40B),
 C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C52(H52), C53(H53), C54(H54),
  C55(H55), C56(H56), C60(H60), C60B(H60B), C61(H61), C61B(H61B), C62(H62),
 C62B(H62B), C63(H63), C63B(H63B), C64(H64), C64B(H64B), C68(H68), C69(H69),
 C70(H70), C71(H71), C72(H72)
;
_shelx_res_checksum              2451
_shelx_hkl_checksum              67393
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'