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_4127018
_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         'C60 H116 Ag14 B60 N8 S12, 3(C H2 Cl2)'
_chemical_formula_sum            'C63 H122 Ag14 B60 Cl6 N8 S12'
_chemical_formula_weight         3747.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            4
_cell_length_a                   18.37789(16)
_cell_length_b                   25.1011(2)
_cell_length_c                   28.6642(3)
_cell_measurement_reflns_used    30736
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.5000
_cell_measurement_theta_min      3.8500
_cell_volume                     13222.9(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_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    -37.00  44.00   0.50    0.50    --   45.20 -77.00   0.00  162
  2  \w     29.00  55.00   0.50    1.00    --  100.10 -82.00-120.00   52
  3  \w     76.00 119.00   0.50    1.00    --  100.10 -82.00-120.00   86
  4  \w     77.00 103.00   0.50    1.00    --  100.10 -82.00-150.00   52
  5  \w     11.00 144.00   0.50    1.00    --  100.10 -82.00 -90.00  266
  6  \w    146.00 186.00   0.50    1.00    --  100.10  45.00 -60.00   80
  7  \w     92.00 128.00   0.50    0.50    --   45.20  82.00   0.00   72
  8  \w    -33.00  60.00   0.50    0.50    --   45.20 -82.00 -60.00  186
  9  \w     98.00 132.00   0.50    1.00    --  100.10  45.00 -60.00   68
 10  \w     59.00 189.00   0.50    1.00    --  100.10  45.00-150.00  260
;
_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      0.0148884000
_diffrn_orient_matrix_UB_12      -0.0035655000
_diffrn_orient_matrix_UB_13      -0.0528099000
_diffrn_orient_matrix_UB_21      0.0824307000
_diffrn_orient_matrix_UB_22      0.0014273000
_diffrn_orient_matrix_UB_23      0.0095018000
_diffrn_orient_matrix_UB_31      0.0010990000
_diffrn_orient_matrix_UB_32      -0.0612761000
_diffrn_orient_matrix_UB_33      0.0033331000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            49208
_diffrn_reflns_point_group_measured_fraction_full 0.992
_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         3.083
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.406
_exptl_absorpt_correction_T_max  0.264
_exptl_absorpt_correction_T_min  0.038
_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    1.883
_exptl_crystal_description       block
_exptl_crystal_F_000             7232
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.111
_refine_diff_density_max         1.631
_refine_diff_density_min         -1.778
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         11871
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0472P)^2^+67.0051P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11259
_reflns_number_total             11871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11338_si_004.cif
_cod_data_source_block           hy
_cod_database_code               4127018
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C63 H122 N8 Ag14 S12 B60 Cl6'
_chemical_oxdiff_usercomment     st
_reflns_odcompleteness_completeness 95.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl3-C32 \\sim Cl4-C32 \\sim Cl2-C31 \\sim Cl1-C31
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C32) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(Cl2)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cl3(0.5) Cl4(0.5) C32(0.5) H32A(0.5) H32B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14), C16(H16), C17(H17),
 C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C), C30(H30A,H30B,
 H30C)
5.d Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7A), B8(H8A), B9(H9),
 B10(H10A), B11(H11A), B12(H12), B13(H13A), B14(H14A), B15(H15), B16(H16A),
 B17(H17A), B18(H18), B19(H19A), B20(H20A), B21(H21), B22(H22A), B23(H23A),
 B24(H24), B25(H25A), B26(H26A), B27(H27), B28(H28A), B29(H29A), B30(H30)
;
_olex2_submission_original_sample_id NC-3
_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 1.514
_oxdiff_exptl_absorpt_empirical_full_min 0.601