Diphosphine-protected ultrasmall gold nanoclusters: opened icosahedral Au<sub>13</sub> and heart-shaped Au<sub>8</sub> clusters.
Zhang, Shan-Shan; Feng, Lei; Senanayake, Ravithree D.; Aikens, Christine M.; Wang, Xing-Po; Zhao, Quan-Qin; Tung, Chen-Ho; Sun, Di; Chemical science 9 (2018) 1251–1258; doi:10.1039/c7sc03566g

data_1553986
_publ_section_title
;
 Diphosphine-protected ultrasmall gold nanoclusters: opened icosahedral
 Au<sub>13</sub> and heart-shaped Au<sub>8</sub> clusters.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1251
_journal_page_last               1258
_journal_paper_doi               10.1039/c7sc03566g
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C150 H132 Au13 P12, 5(Cl)'
_chemical_formula_sum            'C150 H132 Au13 Cl5 P12'
_chemical_formula_weight         5044.00
_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-10-02 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   19.878(2)
_cell_length_b                   19.878(2)
_cell_length_c                   27.361(3)
_cell_measurement_reflns_used    3414
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.837
_cell_measurement_theta_min      2.366
_cell_volume                     9362.8(17)
_computing_cell_refinement       'SAINT V8.30C (?, 2016)'
_computing_data_reduction        'SAINT V8.30C (?, 2016)'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_number            7211
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.532
_diffrn_reflns_theta_min         1.901
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    10.352
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0596 before and 0.0478 after correction.
The Ratio of minimum to maximum transmission is 0.8821.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       block
_exptl_crystal_F_000             4648
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.204
_refine_diff_density_min         -1.500
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         7211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0406P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4680
_reflns_number_total             7211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03566g2.cif
_cod_data_source_block           SD_Au1
_cod_original_cell_volume        9362(2)
_cod_database_code               1553986
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              69546
_shelx_fab_checksum              52742