Controlled Assembly Synthesis of Atomically Precise Ultrastable Silver Nanoclusters with Polyoxometalates.
Yonesato, Kentaro; Ito, Hiroyasu; Itakura, Hiroyuki; Yokogawa, Daisuke; Kikuchi, Takashi; Mizuno, Noritaka; Yamaguchi, Kazuya; Suzuki, Kosuke; Journal of the American Chemical Society 141 (2019) 19550–19554; doi:10.1021/jacs.9b10569

data_4133897
_publ_section_title
;
 Controlled Assembly Synthesis of Atomically Precise Ultrastable Silver
 Nanoclusters with Polyoxometalates.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19550
_journal_page_last               19554
_journal_paper_doi               10.1021/jacs.9b10569
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C120 H268 Ag6 Cl8 N7 O68 Si2 W18'
_chemical_formula_weight         7193.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 100.2067(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.0068(6)
_cell_length_b                   16.6856(2)
_cell_length_c                   29.7859(5)
_cell_measurement_reflns_used    39506
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.2600
_cell_measurement_theta_min      2.0270
_cell_volume                     19568.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            83705
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.283
_diffrn_reflns_theta_min         2.069
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.310
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.442
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13436
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.486
_refine_diff_density_min         -2.028
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1033
_refine_ls_number_reflns         24139
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+539.6310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19144
_reflns_number_total             24139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10569_si_002.cif
_cod_data_source_block           Ag6
_cod_original_cell_volume        19568.5(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4133897
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.602
_shelx_estimated_absorpt_t_max   0.602
_shelx_res_checksum              90797
_shelx_hkl_checksum              6867
_shelx_fab_checksum              36711