Isomerization in Alkynyl-Protected Gold Nanoclusters.
Guan, Zong-Jie; Hu, Feng; Li, Jiao-Jiao; Wen, Zhao-Rui; Lin, Yu-Mei; Wang, Quan-Ming; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b11836

data_4134070
_publ_section_title
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 Isomerization in Alkynyl-Protected Gold Nanoclusters.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11836
_journal_year                    2020
_chemical_formula_moiety         'C90 H135 Au23'
_chemical_formula_sum            'C90 H135 Au23'
_chemical_formula_weight         5747.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-02
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                78.085(3)
_cell_angle_beta                 72.959(3)
_cell_angle_gamma                86.481(3)
_cell_formula_units_Z            2
_cell_length_a                   17.3791(5)
_cell_length_b                   19.0145(6)
_cell_length_c                   19.1440(6)
_cell_measurement_reflns_used    11742
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.0320
_cell_measurement_theta_min      3.5890
_cell_volume                     5918.2(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.1299
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39368
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.042
_diffrn_reflns_theta_max         25.042
_diffrn_reflns_theta_min         3.285
_exptl_absorpt_coefficient_mu    28.408
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00750
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_density_diffrn    3.225
_exptl_crystal_description       plate
_exptl_crystal_F_000             4984
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         4.600
_refine_diff_density_min         -4.506
_refine_diff_density_rms         0.483
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         20830
_refine_ls_number_restraints     582
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0701
_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^)+(0.0686P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14885
_reflns_number_total             20830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11836_si_003.cif
_cod_data_source_block           au23-2
_cod_database_code               4134070
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.132
_shelx_estimated_absorpt_t_min   0.043
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16-C13
 1.54 with sigma of 0.02
 C14-C13
 1.54 with sigma of 0.02
 C15-C13
 1.54 with sigma of 0.02
 C13-C12
 1.54 with sigma of 0.02
 C12-C14
 2.56 with sigma of 0.02
 C12-C16
 2.56 with sigma of 0.02
 C12-C15
 2.56 with sigma of 0.02
 C15-C16
 2.56 with sigma of 0.02
 C16-C14
 2.56 with sigma of 0.02
 C14-C15
 2.56 with sigma of 0.02
 C42-C46
 2.56 with sigma of 0.02
 C42-C45
 2.56 with sigma of 0.02
 C42-C44
 2.56 with sigma of 0.02
 C44-C46
 2.56 with sigma of 0.02
 C46-C45
 2.56 with sigma of 0.02
 C45-C44
 2.56 with sigma of 0.02
 C43-C42
 1.54 with sigma of 0.02
 C46-C43
 1.54 with sigma of 0.02
 C45-C43
 1.54 with sigma of 0.02
 C44-C43
 1.54 with sigma of 0.02
 C153-C152
 1.54 with sigma of 0.02
 C154-C153
 1.54 with sigma of 0.02
 C153-C156
 1.54 with sigma of 0.02
 C155-C153
 1.54 with sigma of 0.02
 C152-C154
 2.56 with sigma of 0.02
 C152-C156
 2.56 with sigma of 0.02
 C152-C155
 2.56 with sigma of 0.02
 C155-C154
 2.56 with sigma of 0.02
 C154-C156
 2.56 with sigma of 0.02
 C156-C155
 2.56 with sigma of 0.02
 C32-C34
 2.56 with sigma of 0.02
 C32-C35
 2.56 with sigma of 0.02
 C32-C36
 2.56 with sigma of 0.02
 C36-C34
 2.56 with sigma of 0.02
 C34-C35
 2.56 with sigma of 0.02
 C35-C36
 2.56 with sigma of 0.02
 C34-C33
 1.54 with sigma of 0.02
 C33-C35
 1.54 with sigma of 0.02
 C36-C33
 1.54 with sigma of 0.02
 Au17-C32
 3.1 with sigma of 0.02
 C33-C32
 1.54 with sigma of 0.02
 Au17-C31
 1.89 with sigma of 0.02
 C32-C31
 1.2 with sigma of 0.02
 C31-C33
 2.74 with sigma of 0.02
 C21-Au17
 1.89 with sigma of 0.02
 C22-C21
 1.2 with sigma of 0.02
 C23-C22
 1.54 with sigma of 0.02
 Au17-C22
 3.1 with sigma of 0.02
 C21-C23
 2.74 with sigma of 0.02
 C112-Au20
 3.1 with sigma of 0.02
 C113-C112
 1.54 with sigma of 0.02
 Au20-C111
 1.89 with sigma of 0.02
 C113-C111
 2.74 with sigma of 0.02
 C112-C111
 1.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Au24 \\sim Au7 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim
C126: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Au21 \\sim Au6 \\sim Au25 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75
\\sim C76: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Au13 \\sim Au14 \\sim C151 \\sim C152 \\sim C153 \\sim C154 \\sim C155 \\sim
C156: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Au11 \\sim Au16 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Au1 \\sim Au14 \\sim C141 \\sim C142 \\sim C143 \\sim C144 \\sim C145 \\sim
C146: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Au22 \\sim Au21 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Au15 \\sim Au16 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Au10 \\sim Au8 \\sim Au24 \\sim C131 \\sim C132 \\sim C133 \\sim C134 \\sim
C135 \\sim C136: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Au3 \\sim Au22 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Au23 \\sim Au18 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Au18 \\sim Au17 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Au2 \\sim Au9 \\sim Au6 \\sim Au25 \\sim C91 \\sim C92 \\sim C93 \\sim C94
\\sim C95 \\sim C96: within 2A with sigma of 0.001 and sigma for terminal atoms
of 0.002 within 2A
Au12 \\sim Au19 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim
C106: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Au4 \\sim Au18 \\sim Au17 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Au19 \\sim Au20 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim
C116: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
4. Others
 Fixed Sof: Au24(0.8) Au6(0.2) Au7(0.2) Au25(0.8)
5.a Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C74(H74A,
 H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C84(H84A,H84B,H84C),
 C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C94(H94A,H94B,H94C), C95(H95A,H95B,
 H95C), C96(H96A,H96B,H96C), C104(H10A,H10B,H10C), C105(H10D,H10E,H10F),
 C106(H10G,H10H,H10I), C114(H11A,H11B,H11C), C115(H11D,H11E,H11F), C116(H11G,
 H11H,H11I), C124(H12A,H12B,H12C), C125(H12D,H12E,H12F), C126(H12G,H12H,H12I),
 C134(H13A,H13B,H13C), C135(H13D,H13E,H13F), C136(H13G,H13H,H13I), C144(H14D,
 H14E,H14F), C145(H14G,H14H,H14I), C146(H14J,H14K,H14L), C154(H15D,H15E,H15F),
 C155(H15G,H15H,H15I), C156(H15J,H15K,H15L)
;
_shelx_res_checksum              20687
_shelx_hkl_checksum              1123
_olex2_submission_special_instructions 'No special instructions were received'