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_4127019
_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         'C52 H100 Ag14 B60 N8 S12'
_chemical_formula_sum            'C52 H100 Ag14 B60 N8 S12'
_chemical_formula_weight         3380.89
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-19
_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            2
_cell_length_a                   15.7244(2)
_cell_length_b                   15.7244(2)
_cell_length_c                   21.4690(4)
_cell_measurement_reflns_used    3660
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.9230
_cell_measurement_theta_min      3.9740
_cell_volume                     5308.36(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (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    'SIR2004 (Burla et al., 2007)'
_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 0.994
_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    -27.00  30.00   0.50    2.00    --   45.50 -82.00-180.00  114
  2  \w     46.00  78.00   0.50    2.00    --   45.50 -82.00-180.00   64
  3  \w     86.00 138.00   0.50   10.00    --  100.10 -61.00 120.00  104
  4  \w     64.00 183.00   0.50   10.00    --  100.10  61.00 -60.00  238
  5  \w     88.00 128.00   0.50    2.00    --   45.50  82.00  30.00   80
  6  \w     88.00 137.00   0.50   10.00    --  100.10  82.00 -30.00   98
  7  \w     16.00  79.00   0.50   10.00    --  100.10 -61.00 120.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0919960000
_diffrn_orient_matrix_UB_12      -0.0325814000
_diffrn_orient_matrix_UB_13      -0.0062565000
_diffrn_orient_matrix_UB_21      -0.0174828000
_diffrn_orient_matrix_UB_22      0.0252934000
_diffrn_orient_matrix_UB_23      0.0681528000
_diffrn_orient_matrix_UB_31      -0.0289648000
_diffrn_orient_matrix_UB_32      0.0888122000
_diffrn_orient_matrix_UB_33      -0.0216404000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6727
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.398
_diffrn_reflns_theta_min         3.484
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.721
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_description       block
_exptl_crystal_F_000             3236
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2456
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0614P)^2^+32.2110P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2134
_reflns_number_total             2456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11338_si_003.cif
_cod_data_source_block           hy
_cod_original_cell_volume        5308.35(17)
_cod_database_code               4127019
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C52 N8 H100 S12 B60 Ag14'
_chemical_oxdiff_usercomment     st
_reflns_odcompleteness_completeness 94.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.59
_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
{B11, C9}
{B6, C7}
{B7, C8}
{C6, B8}
3. Uiso/Uaniso restraints and constraints
Uanis(B11) \\sim Ueq, Uanis(B9) \\sim Ueq, Uanis(B10) \\sim Ueq, Uanis(B8)
\\sim Ueq, Uanis(B6) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(C8) \\sim Ueq,
Uanis(B2) \\sim Ueq, Uanis(B4) \\sim Ueq, Uanis(B5) \\sim Ueq, Uanis(B3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(B11) = Uanis(C9)
Uanis(B7) = Uanis(C8)
Uanis(B6) = Uanis(C7)
Uanis(C6) = Uanis(B8)
4. Others
 Fixed Sof: S1(0.25) S2(0.25) S3(0.5) S4(0.5) C6(0.25) C7(0.25) C8(0.5)
 C9(0.5) H4A(0.5) H4B(0.5) H5A(0.5) H5B(0.5) B6(0.25) H6(0.25) B7(0.5) H7(0.5)
 B8(0.25) H8(0.25) H9A(0.5) H9B(0.5) B11(0.5) H11(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5)
5.b Boron cage BH refined with riding coordinates:
 B1(H1A), B2(H2A), B3(H3A), B4(H4A), B4(H4B), B5(H5A), B5(H5B), B6(H6), B7(H7),
  B8(H8), B9(H9A), B9(H9B), B10(H10), B11(H11)
;
_olex2_submission_original_sample_id NC-2
_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 1.421
_oxdiff_exptl_absorpt_empirical_full_min 0.655