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_4127016
_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(C8 H26 Ag4 B20 N2 S4)'
_chemical_formula_sum            'C4 H13 Ag2 B10 N S2'
_chemical_formula_weight         463.11
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.73310(10)
_cell_length_b                   26.9421(4)
_cell_length_c                   7.57270(10)
_cell_measurement_reflns_used    2366
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.3410
_cell_measurement_theta_min      3.2880
_cell_volume                     1373.72(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      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.980
_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      0.00  58.00   0.50    1.00    --   45.70  38.00 -90.00  116
  2  \w     62.00 134.00   0.50    1.00    --   45.70  38.00 -90.00  144
  3  \w     91.00 134.00   0.50    1.00    --   45.70  82.00 -30.00   86
  4  \w     90.00 127.00   0.50    1.00    --   45.70  77.00  30.00   74
  5  \w    118.00 180.00   0.50    5.00    --  100.10  82.00   0.00  124
  6  \w     85.00 139.00   0.50    5.00    --  100.10  45.00-150.00  108
  7  \w     59.00 169.00   0.50    5.00    --  100.10  45.00  90.00  220
  8  \w     49.00 137.00   0.50    5.00    --  100.10 -77.00 150.00  176
  9  \w     15.00  40.00   0.50    5.00    --  100.10 -77.00 150.00   50
;
_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      0.1105543000
_diffrn_orient_matrix_UB_12      -0.0274336000
_diffrn_orient_matrix_UB_13      0.1488535000
_diffrn_orient_matrix_UB_21      -0.0110844000
_diffrn_orient_matrix_UB_22      0.0469081000
_diffrn_orient_matrix_UB_23      0.1158525000
_diffrn_orient_matrix_UB_31      -0.2000793000
_diffrn_orient_matrix_UB_32      -0.0177694000
_diffrn_orient_matrix_UB_33      0.0761462000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4208
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.781
_diffrn_reflns_theta_min         3.281
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.419
_exptl_absorpt_correction_T_max  0.520
_exptl_absorpt_correction_T_min  0.319
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.239
_exptl_crystal_description       irregular
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+1.6467P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1231
_reflns_number_total             1352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11338_si_005.cif
_cod_data_source_block           hy
_cod_database_code               4127016
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C4 H13 Ag2 B10 N S2'
_chemical_oxdiff_usercomment     st
_shelx_estimated_absorpt_t_max   0.394
_shelx_estimated_absorpt_t_min   0.192
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Ag2B)=0.5*(1-FVAR(2))
 Sof(Ag2A)=0.5*FVAR(2)
 Fixed Sof: H3A(0.5) H3B(0.5) H3C(0.5)
3.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
3.b Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4), B5(H5)
;
_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 3.135
_oxdiff_exptl_absorpt_empirical_full_min 0.557