Assembly of Atomically Precise Silver Nanoclusters into Nanocluster-Based Frameworks.
Alhilaly, Mohammad J.; Huang, Ren-Wu; Naphade, Rounak; Alamer, Badriah; Hedhili, Mohamed Nejib; Emwas, Abdul-Hamid; Maity, Partha; Yin, Jun; Shkurenko, Aleksander; Mohammed, Omar F.; Eddaoudi, Mohamed; Bakr, Osman M.; Journal of the American Chemical Society 141 (2019) 9585–9592; doi:10.1021/jacs.9b02486

data_4127433
_publ_section_title
;
 Assembly of Atomically Precise Silver Nanoclusters into Nanocluster-Based
 Frameworks.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9585
_journal_page_last               9592
_journal_paper_doi               10.1021/jacs.9b02486
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
'C69.33 H102 Ag15 Cl F17 N6.33 O14.33 S8, 4.3(C3 H7 N O), 1(H2 O)'
_chemical_formula_sum            'C82.24 H134.13 Ag15 Cl F17 N10.64 O19.64 S8'
_chemical_formula_weight         3819.17
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                96.761(4)
_cell_angle_beta                 101.558(4)
_cell_angle_gamma                98.432(4)
_cell_formula_units_Z            2
_cell_length_a                   15.009(2)
_cell_length_b                   19.593(3)
_cell_length_c                   22.379(3)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      38.48
_cell_measurement_theta_min      2.83
_cell_volume                     6304.0(15)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON-II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            306927
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.906
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.509
_exptl_absorpt_correction_T_max  0.0317
_exptl_absorpt_correction_T_min  0.0317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1141 before and 0.0712 after correction.
The Ratio of minimum to maximum transmission is 0.3192.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_description       prism
_exptl_crystal_F_000             3724
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         4.236
_refine_diff_density_min         -3.008
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1791
_refine_ls_number_reflns         26478
_refine_ls_number_restraints     842
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0688
_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^)+(0.0616P)^2^+91.5774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24381
_reflns_number_total             26478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02486_si_002.cif
_cod_data_source_block           Ag15_1D
_cod_original_cell_volume        6304(2)
_cod_database_code               4127433
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.434
_shelx_estimated_absorpt_t_max   0.885
_shelx_res_checksum              19483
_shelx_hkl_checksum              60916