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_4128329
_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            'C112.5 H199 Au23 Pd S17'
_chemical_formula_weight         6733.35
_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                92.2400(10)
_cell_angle_beta                 108.4480(10)
_cell_angle_gamma                96.7850(10)
_cell_formula_units_Z            4
_cell_length_a                   19.5656(3)
_cell_length_b                   26.9697(3)
_cell_length_c                   29.4945(4)
_cell_measurement_reflns_used    63829
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      72.940
_cell_measurement_theta_min      3.029
_cell_volume                     14612.0(4)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku AFC11 with Pilatus 200K'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            204497
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.253
_diffrn_reflns_theta_min         3.039
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    45.609
_exptl_absorpt_correction_T_max  0.431
_exptl_absorpt_correction_T_min  0.021
_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            Black
_exptl_crystal_density_diffrn    3.061
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             12036
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.023
_refine_diff_density_max         6.324
_refine_diff_density_min         -4.248
_refine_diff_density_rms         0.468
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2677
_refine_ls_number_reflns         52519
_refine_ls_number_restraints     619
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0673
_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^)+(0.0965P)^2^+456.0443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                42992
_reflns_number_total             52519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08055_si_005.cif
_cod_data_source_block           shelxs_sq
_cod_original_formula_sum        'C112.50 H199 Au23 Pd S17'
_cod_database_code               4128329
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.581
_oxdiff_exptl_absorpt_empirical_full_max 2.317
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              19920
_shelx_hkl_checksum              36792
_shelx_fab_checksum              91169