Atomically Precise Site-Specific Tailoring and Directional Assembly of Superatomic Silver Nanoclusters.
Wang, Zhao-Yang; Wang, Meng-Qi; Li, Yan-Ling; Luo, Peng; Jia, Tong-Tong; Huang, Ren-Wu; Zang, Shuang-Quan; Mak, Thomas C. W.; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b11338

data_4127017
_publ_section_title
;
 Atomically Precise Site-Specific Tailoring and Directional Assembly of
 Superatomic Silver Nanoclusters.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11338
_journal_year                    2018
_chemical_formula_moiety         '0.5(C152 H216 Ag28 B120 N16 S24)'
_chemical_formula_sum            'C76 H108 Ag14 B60 N8 S12'
_chemical_formula_weight         3677.20
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1757(3)
_cell_length_b                   27.1757(3)
_cell_length_c                   26.6358(5)
_cell_measurement_reflns_used    8311
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.3520
_cell_measurement_theta_min      2.3260
_cell_volume                     19671.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w      9.00 129.00   0.50    5.00    --   45.50  57.00  30.00  240
  2  \w     93.00 176.00   0.50   30.00    --  100.10  82.00  90.00  166
  3  \w     88.00 189.00   0.50   30.00    --  100.10  82.00   0.00  202
  4  \w     47.00 137.00   0.50   30.00    --  100.10 -61.00 -60.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0236613000
_diffrn_orient_matrix_UB_12      0.0126564000
_diffrn_orient_matrix_UB_13      0.0509127000
_diffrn_orient_matrix_UB_21      -0.0059871000
_diffrn_orient_matrix_UB_22      -0.0538779000
_diffrn_orient_matrix_UB_23      0.0168953000
_diffrn_orient_matrix_UB_31      0.0511791000
_diffrn_orient_matrix_UB_32      -0.0122778000
_diffrn_orient_matrix_UB_33      -0.0216177000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23428
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.489
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.307
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             7080
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.04
_platon_squeeze_details          'TITL hy_pl I 41/a R = 0.08'
_refine_diff_density_max         1.977
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         8780
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0644
_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^)+(0.1511P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1984
_refine_ls_wR_factor_ref         0.2099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6029
_reflns_number_total             8780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11338_si_009.cif
_cod_data_source_block           hy
_cod_original_cell_volume        19671.0(6)
_cod_database_code               4127017
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C76 H108 N8 S12 Ag14 B60'
_shelx_estimated_absorpt_t_max   0.639
_shelx_estimated_absorpt_t_min   0.388
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All B(H,H) groups, All C(H) groups
2. Shared sites
{B16A, C20B}
{B15B, C20A}
{B15A, C19B}
{B16B, C19A}
{B5, C17}
{B6, C18}
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(B15A) \\sim Ueq, Uanis(B15B) \\sim Ueq, Uanis(B13) \\sim Ueq, Uanis(B9)
\\sim Ueq, Uanis(B7) \\sim Ueq, Uanis(B11) \\sim Ueq, Uanis(B16B) \\sim Ueq,
Uanis(B16A) \\sim Ueq, Uanis(B14) \\sim Ueq, Uanis(B10) \\sim Ueq, Uanis(B8)
\\sim Ueq, Uanis(B12) \\sim Ueq, Uanis(B5) \\sim Ueq, Uanis(B6) \\sim Ueq,
Uanis(B4) \\sim Ueq, Uanis(B3) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(B2) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(B16A) = Uanis(C20B)
Uanis(B15B) = Uanis(C20A)
Uanis(B15A) = Uanis(C19B)
Uanis(B16B) = Uanis(C19A)
Uanis(C17) = Uanis(B5)
Uanis(C18) = Uanis(B6)
4. Others
 Fixed Sof: S1(0.5) S2(0.5) S3B(0.5) S3A(0.5) S4B(0.5) S4A(0.5) C17(0.5)
 C18(0.5) C19B(0.5) C19A(0.5) C20A(0.5) C20B(0.5) H3B(0.5) H3A(0.5) H4B(0.5)
 H4A(0.5) B5(0.5) H5A(0.5) B6(0.5) H6(0.5) H7A(0.5) H7B(0.5) H9A(0.5) H9B(0.5)
 H13B(0.5) H13A(0.5) H14B(0.5) H14A(0.5) B15B(0.5) H15B(0.5) B15A(0.5)
 H15A(0.5) B16B(0.5) H16B(0.5) B16A(0.5) H16A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16)
5.b Boron cage BH refined with riding coordinates:
 B1(H1A), B2(H2A), B3(H3B), B3(H3A), B4(H4B), B4(H4A), B5(H5A), B6(H6),
 B7(H7A), B7(H7B), B8(H8A), B9(H9A), B9(H9B), B10(H10A), B11(H11A), B12(H12),
 B13(H13B), B13(H13A), B14(H14B), B14(H14A), B15B(H15B), B15A(H15A), B16B(H16B),
  B16A(H16A)
;
_olex2_submission_original_sample_id SCAM-4
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.433
_oxdiff_exptl_absorpt_empirical_full_min 0.788