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_4128332
_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            'C229 H96 Au24 Cl2 F108 P2 Pd'
_chemical_formula_weight         9865.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 95.792(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.477(4)
_cell_length_b                   20.733(4)
_cell_length_c                   35.724(7)
_cell_measurement_reflns_used    28163
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      1.7
_cell_volume                     12879(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku AFC11 with Saturn724+'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            133572
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.303
_diffrn_reflns_theta_min         1.965
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    13.834
_exptl_absorpt_correction_T_max  0.207
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.544
_exptl_crystal_description       Block
_exptl_crystal_F_000             8896
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.170
_refine_diff_density_max         3.231
_refine_diff_density_min         -2.495
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1605
_refine_ls_number_reflns         23380
_refine_ls_number_restraints     902
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+125.9502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20691
_reflns_number_total             23380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08055_si_007.cif
_cod_data_source_block           shelxs_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4128332
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.123
_shelx_estimated_absorpt_t_max   0.202
_shelx_res_checksum              72959
_shelx_hkl_checksum              89687
_shelx_fab_checksum              46352