Gold Nanowired: A Linear (Au25)n Polymer from Au25 Molecular Clusters.
De Nardi, Marco; Antonello, Sabrina; Jiang, De-En; Pan, Fangfang; Rissanen, Kari; Ruzzi, Marco; Venzo, Alfonso; Zoleo, Alfonso; Maran, Flavio; ACS nano 8 (2014) 8505–8512; doi:10.1021/nn5031143

data_4511748
_publ_section_title
;
 Gold Nanowired: A Linear (Au25)n Polymer from Au25 Molecular Clusters.
;
_journal_issue                   8
_journal_name_full               'ACS nano'
_journal_page_first              8505
_journal_page_last               8512
_journal_paper_doi               10.1021/nn5031143
_journal_volume                  8
_journal_year                    2014
_chemical_formula_moiety         'C72 H162 Au25 S18'
_chemical_formula_sum            'C72 H162 Au25 S18'
_chemical_formula_weight         6529.25
_chemical_name_systematic
;
 ?
;
_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   mixed
_audit_creation_date             2014-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                92.101(2)
_cell_angle_beta                 106.955(3)
_cell_angle_gamma                106.132(3)
_cell_formula_units_Z            2
_cell_length_a                   16.1305(5)
_cell_length_b                   17.9824(5)
_cell_length_c                   22.1697(7)
_cell_measurement_reflns_used    17145
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      75.1110
_cell_measurement_theta_min      4.2150
_cell_volume                     5860.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0223235000
_diffrn_orient_matrix_UB_12      -0.0436708000
_diffrn_orient_matrix_UB_13      0.0545153000
_diffrn_orient_matrix_UB_21      0.0000996000
_diffrn_orient_matrix_UB_22      -0.0764397000
_diffrn_orient_matrix_UB_23      -0.0336703000
_diffrn_orient_matrix_UB_31      0.1023241000
_diffrn_orient_matrix_UB_32      0.0183285000
_diffrn_orient_matrix_UB_33      0.0354968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40949
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         66.749
_diffrn_reflns_theta_min         3.111
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    60.357
_exptl_absorpt_correction_T_max  0.195
_exptl_absorpt_correction_T_min  0.017
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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    3.700
_exptl_crystal_description       needle
_exptl_crystal_F_000             5714
_exptl_crystal_size_max          0.1601
_exptl_crystal_size_mid          0.0417
_exptl_crystal_size_min          0.0373
_refine_diff_density_max         3.376
_refine_diff_density_min         -4.015
_refine_diff_density_rms         0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         20784
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0939P)^2^+21.7386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17251
_reflns_number_total             20784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nn5031143_si_002.cif
_cod_data_source_block           au25c4
_cod_depositor_comments          'Adding full bibliography for 4511748.cif.'
_cod_database_code               4511748
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Au25 S18 C72 H162'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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
 C13-C14 = C14-C15 = C15-C16 = C33-C34 = C34-C35 = C35-C36
 1.54 with sigma of 0.01
 C21-C22 = C22-C23 = C23-C24 = C57-C58 = C58-C59 = C59-C60
 1.54 with sigma of 0.01
 C41A-C42A = C42A-C43A = C43A-C44A = C41B-C42B = C42B-C43B = C43B-C44B
 1.54 with sigma of 0.01
 C69-C70 = C70-C71 = C71-C72
 1.54 with sigma of 0.01
 C37A-C38A = C38A-C39A = C39A-C40A
 1.54 with sigma of 0.01
 C37B-C38B = C38B-C39B = C39B-C40B
 1.54 with sigma of 0.01
 C41A-C43A = C41B-C43B = C42A-C44A = C42B-C44B
 2.5 with sigma of 0.04
 C13-C15 = C14-C16 = C57-C59 = C58-C60 = C69-C71 = C70-C72
 2.5 with sigma of 0.01
 C37A-C39A = C38A-C40A = C37B-C39B = C38B-C40B
 2.5 with sigma of 0.01
 C5-C6 \\sim C6-C7 \\sim C7-C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C55 \\sim C56: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C41A \\sim C42A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C35 \\sim C36: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C19 \\sim C20: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C46 \\sim C47: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C21 \\sim C22: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C23 \\sim C24: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C56) \\sim Ueq,
Uanis(C68) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C38A)
\\sim Ueq, Uanis(C41A) \\sim Ueq, Uanis(C42A) \\sim Ueq, Uanis(C43A) \\sim Ueq,
: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C55) \\sim Ueq, Uanis(C37B) \\sim Ueq, Uanis(C38B) \\sim Ueq, Uanis(C39B)
\\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C43B) \\sim Ueq, Uanis(C44A) \\sim Ueq,
: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(S12) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C8) = Uanis(C32)
Uanis(C7) = Uanis(C31)
Uanis(C6) = Uanis(C30)
Uanis(C5) = Uanis(C29)
Uanis(C37A) = Uanis(C37B)
Uanis(C38A) = Uanis(C38B)
Uanis(C39A) = Uanis(C39B)
Uanis(C41A) = Uanis(C41B)
Uanis(C42A) = Uanis(C42B)
Uanis(C43A) = Uanis(C43B)
Uanis(C44A) = Uanis(C44B)
Uanis(C40A) = Uanis(C40B)
4. Others
 Sof(S10B)=Sof(C37B)=Sof(H37C)=Sof(H37D)=Sof(C38B)=Sof(H38C)=Sof(H38D)=
 Sof(C39B)=Sof(H39C)=Sof(H39D)=Sof(C40B)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(1)
 Sof(S10A)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(C38A)=Sof(H38A)=Sof(H38B)=
 Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Sof(S11B)=Sof(C41B)=Sof(H41C)=Sof(H41D)=Sof(C42B)=Sof(H42C)=Sof(H42D)=
 Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(2)
 Sof(S11A)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(C42A)=Sof(H42A)=Sof(H42B)=
 Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(2)
 Fixed Uiso: C14(0.12) C15(0.15) C16(0.18) C48(0.2) C57(0.1) C58(0.12)
 C59(0.15) C60(0.18) C70(0.14) C71(0.16) C72(0.18)
5.a Riding coordinates:
 C37A(H37A,H37B), C37B(H37C,H37D), C38A(H38A,H38B), C38B(H38C,H38D), C39A(H39A,
 H39B), C39B(H39C,H39D), C40A(H40A,H40B,H40C), C40B(H40D,H40E,H40F), C41A(H41A,
 H41B), C41B(H41C,H41D), C42A(H42A,H42B), C42B(H42C,H42D), C43A(H43A,H43B),
 C43B(H43C,H43D), C44A(H44A,H44B,H44C), C44B(H44D,H44E,H44F), C72(H72A,H72B,
 H72C)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
  C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
 C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C65(H65A,H65B), C66(H66A,H66B),
  C67(H67A,H67B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C),
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C32(H32A,H32B,
 H32C), C36(H36A,H36B,H36C), C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C56(H56A,
 H56B,H56C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C68(H68A,H68B,H68C)
;