Efficient and Selective Conversion of Phosphine-Protected (MAu<sub>8</sub>)<sup>2+</sup> (M = Pd, Pt) Superatoms to Thiolate-Protected (MAu<sub>12</sub>)<sup>6+</sup> or Alkynyl-Protected (MAu<sub>12</sub>)<sup>4+</sup> Superatoms via Hydride Doping.
Takano, Shinjiro; Ito, Shun; Tsukuda, Tatsuya; Journal of the American Chemical Society 141 (2019) 15994–16002; doi:10.1021/jacs.9b08055

data_4128333
_publ_section_title
;
 Efficient and Selective Conversion of Phosphine-Protected
 (MAu<sub>8</sub>)<sup>2+</sup> (M = Pd, Pt) Superatoms to
 Thiolate-Protected (MAu<sub>12</sub>)<sup>6+</sup> or Alkynyl-Protected
 (MAu<sub>12</sub>)<sup>4+</sup> Superatoms via Hydride Doping.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15994
_journal_page_last               16002
_journal_paper_doi               10.1021/jacs.9b08055
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C72 H198 Au24 Pd S18 Si18'
_chemical_formula_weight         6980.59
_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   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                103.768(2)
_cell_angle_beta                 112.008(2)
_cell_angle_gamma                107.269(2)
_cell_formula_units_Z            1
_cell_length_a                   16.8731(4)
_cell_length_b                   16.9117(4)
_cell_length_c                   17.0006(4)
_cell_measurement_reflns_used    27976
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.2770
_cell_measurement_theta_min      2.7490
_cell_volume                     3946.7(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC11 with Pilatus200K'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48541
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         2.664
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    22.715
_exptl_absorpt_correction_T_max  0.085
_exptl_absorpt_correction_T_min  0.019
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
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            Green
_exptl_crystal_density_diffrn    2.937
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.082
_refine_diff_density_max         3.860
_refine_diff_density_min         -2.541
_refine_diff_density_rms         0.355
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         14396
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0543P)^2^+92.3727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12946
_reflns_number_total             14396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08055_si_003.cif
_cod_data_source_block           shelxs_sq
_cod_original_cell_volume        3946.65(18)
_cod_database_code               4128333
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.577
_oxdiff_exptl_absorpt_empirical_full_max 2.133
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              74739
_shelx_hkl_checksum              20462
_shelx_fab_checksum              61954