[Ag<sub>67</sub>(SPhMe<sub>2</sub>)<sub>32</sub>(PPh<sub>3</sub>)<sub>8</sub>]<sup>3+</sup>: Synthesis, Total Structure, and Optical Properties of a Large Box-Shaped Silver Nanocluster.
Alhilaly, Mohammad J.; Bootharaju, Megalamane S.; Joshi, Chakra P.; Besong, Tabot M.; Emwas, Abdul-Hamid; Juarez-Mosqueda, Rosalba; Kaappa, Sami; Malola, Sami; Adil, Karim; Shkurenko, Aleksander; Häkkinen, Hannu; Eddaoudi, Mohamed; Bakr, Osman M.; Journal of the American Chemical Society 138 (2016) 14727–14732; doi:10.1021/jacs.6b09007

data_4131056
_publ_section_title
;
 [Ag<sub>67</sub>(SPhMe<sub>2</sub>)<sub>32</sub>(PPh<sub>3</sub>)<sub>8</sub>]<sup>3+</sup>:
 Synthesis, Total Structure, and Optical Properties of a Large Box-Shaped
 Silver Nanocluster.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14727
_journal_page_last               14732
_journal_paper_doi               10.1021/jacs.6b09007
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C400 H406 Ag67 P8 S32 3+,   3(C6 H5)4 B 1-)'
_chemical_formula_sum            'C472 H466 Ag67 B3 P8 S32'
_chemical_formula_weight         14671.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           37
_space_group_name_Hall           'C 2 -2c'
_space_group_name_H-M_alt        'C c c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   46.195(1)
_cell_length_b                   48.069(1)
_cell_length_c                   25.6424(8)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      68.41
_cell_measurement_theta_min      3.83
_cell_volume                     56940(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            105002
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        65.080
_diffrn_reflns_theta_max         65.080
_diffrn_reflns_theta_min         3.694
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    19.616
_exptl_absorpt_correction_T_max  0.2735
_exptl_absorpt_correction_T_min  0.1448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0818 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.5294.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_description       prism
_exptl_crystal_F_000             28376
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.35(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2126
_refine_ls_number_reflns         43399
_refine_ls_number_restraints     581
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+804.5305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1518
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                39625
_reflns_number_total             43399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09007_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        56941(3)
_cod_database_code               4131056
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.202
_shelx_estimated_absorpt_t_max   0.271
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              72033
_shelx_hkl_checksum              93955
_shelx_fab_checksum              57657