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_4127022
_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(C80 H176 Ag28 B120 N24 S24)'
_chemical_formula_sum            'C40 H88 Ag14 B60 N12 S12'
_chemical_formula_weight         3280.72
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 111.905(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.3664(4)
_cell_length_b                   19.6548(3)
_cell_length_c                   19.5374(3)
_cell_measurement_reflns_used    17185
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.1650
_cell_measurement_theta_min      3.4090
_cell_volume                     7968.7(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.997
_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     85.00 133.00   0.50    0.58    --   45.50  57.00 120.00   96
  2  \w      8.00  84.00   0.50    0.58    --   45.50 -77.00  90.00  152
  3  \w     21.00  46.00   0.50    0.58    --   45.50  57.00  60.00   50
  4  \w     24.00 133.00   0.50    0.58    --   45.50  57.00-120.00  218
  5  \w     27.00  57.00   0.50    0.58    --   45.50  57.00 120.00   60
  6  \w     93.00 118.00   0.50    0.58    --   45.50  57.00  60.00   50
  7  \w     69.00 189.00   0.50    2.30    --  100.10  61.00-150.00  240
  8  \w     71.00  96.00   0.50    2.30    --  100.10  77.00  90.00   50
  9  \w     11.00 136.00   0.50    2.30    --  100.10 -82.00  30.00  250
 10  \w    101.00 189.00   0.50    2.30    --  100.10  30.00 -60.00  176
 11  \w    152.00 189.00   0.50    2.30    --  100.10  82.00 -90.00   74
 12  \w    150.00 181.00   0.50    2.30    --  100.10  77.00  90.00   62
 13  \w     17.00  53.00   0.50    2.30    --  100.10 -45.00  90.00   72
 14  \w     59.00  95.00   0.50    2.30    --  100.10  82.00 -90.00   72
 15  \w     65.00  91.00   0.50    2.30    --  100.10  30.00 -60.00   52
 16  \w    110.00 135.00   0.50    2.30    --  100.10 -45.00  90.00   50
 17  \w     56.00 175.00   0.50    2.30    --  100.10  30.00 -30.00  238
;
_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      0.0649321000
_diffrn_orient_matrix_UB_12      -0.0327974000
_diffrn_orient_matrix_UB_13      0.0085615000
_diffrn_orient_matrix_UB_21      0.0351393000
_diffrn_orient_matrix_UB_22      0.0499199000
_diffrn_orient_matrix_UB_23      0.0630111000
_diffrn_orient_matrix_UB_31      -0.0074523000
_diffrn_orient_matrix_UB_32      -0.0507809000
_diffrn_orient_matrix_UB_33      0.0563862000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22094
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.498
_diffrn_reflns_theta_min         2.437
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.126
_exptl_absorpt_correction_T_max  0.287
_exptl_absorpt_correction_T_min  0.123
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             3124
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.151
_refine_diff_density_max         1.732
_refine_diff_density_min         -1.605
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7399
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0693
_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^)+(0.1031P)^2^+135.7707P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.1930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6924
_reflns_number_total             7399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11338_si_007.cif
_cod_data_source_block           hy_sq
_cod_database_code               4127022
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C48 H96 N12 S12 B64 Ag14'
_reflns_odcompleteness_completeness 99.69
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C13, B14}
{C12, B15}
{C11, B16}
{B22, C14}
{C15, B20}
{C8, B6}
{C9, B7}
{C10, B8}
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(B7) \\sim Ueq, Uanis(B11) \\sim Ueq, Uanis(B8) \\sim Ueq, Uanis(B6) \\sim
Ueq, Uanis(B2) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(B4) \\sim Ueq, Uanis(B3)
\\sim Ueq, Uanis(B5) \\sim Ueq, Uanis(B15) \\sim Ueq, Uanis(B13) \\sim Ueq,
Uanis(B16) \\sim Ueq, Uanis(B14) \\sim Ueq, Uanis(B12) \\sim Ueq, Uanis(B10)
\\sim Ueq, Uanis(B9) \\sim Ueq, Uanis(B20) \\sim Ueq, Uanis(B22) \\sim Ueq,
Uanis(B17) \\sim Ueq, Uanis(B21) \\sim Ueq, Uanis(B19) \\sim Ueq, Uanis(B18)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) = Uanis(B20)
Uanis(B22) = Uanis(C14)
Uanis(C9) = Uanis(B7)
Uanis(B6) = Uanis(C8)
Uanis(B8) = Uanis(C10)
Uanis(C12) = Uanis(B15)
Uanis(C11) = Uanis(B16)
Uanis(C13) = Uanis(B14)
4. Others
 Fixed Sof: S1(0.2) S2(0.2) S3(0.6) S4(0.3) S5(0.4) S6(0.3) S7(0.6) S8(0.4)
 C8(0.3) C9(0.4) C10(0.3) C11(0.2) C12(0.6) C13(0.2) C14(0.4) C15(0.6) H1A(0.5)
 H1B(0.5) H4B(0.5) H4A(0.5) B6(0.2) H6(0.2) B7(0.6) H7(0.6) B8(0.2) H8(0.2)
 H12A(0.5) H12(0.5) H13(0.5) H13A(0.5) B14(0.3) H14(0.3) B15(0.4) H15(0.4)
 B16(0.3) H16(0.3) H17(0.5) H17A(0.5) B20(0.4) H20(0.4) H21(0.5) H21A(0.5)
 B22(0.6) H22(0.6)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
5.c Boron cage BH refined with riding coordinates:
 B1(H1A), B1(H1B), B2(H2A), B3(H3), B4(H4B), B4(H4A), B5(H5A), B6(H6), B7(H7),
 B8(H8), B9(H9), B10(H10), B11(H11), B12(H12A), B12(H12), B13(H13), B13(H13A),
 B14(H14), B15(H15), B16(H16), B17(H17), B17(H17A), B18(H18), B19(H19),
 B20(H20), B21(H21), B21(H21A), B22(H22)
;
_olex2_submission_original_sample_id SCAM-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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.599
_oxdiff_exptl_absorpt_empirical_full_min 0.381