Spontaneous Resolution of Chiral Multi-Thiolate-Protected Ag30 Nanoclusters
Huang, Jia-Hong; Wang, Zhao-Yang; Zang, Shuang-Quan; Mak, Thomas C. W.; ACS Central Science  (2020) –; doi:10.1021/acscentsci.0c01045

data_4518096
_publ_section_title
;
 Spontaneous Resolution of Chiral Multi-Thiolate-Protected Ag30
 Nanoclusters
;
_journal_name_full               'ACS Central Science'
_journal_paper_doi               10.1021/acscentsci.0c01045
_journal_year                    2020
_chemical_formula_moiety         'C166 H204 Ag30 B80 P12 S24, 4(C4 H9 N O)'
_chemical_formula_sum            'C182 H240 Ag30 B80 N4 O4 P12 S24'
_chemical_formula_weight         7789.75
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   34.9242(3)
_cell_length_b                   34.9242(3)
_cell_length_c                   24.1417(2)
_cell_measurement_reflns_used    34515
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      70.6490
_cell_measurement_theta_min      2.9450
_cell_volume                     25500.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(13)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -31.00   1.00   0.50    0.50    --    0.00 -19.00 120.00   64
  2  \w    -86.00 -60.00   0.50    0.50    --    0.00 -19.00 120.00   52
  3  \w    -19.00  87.00   0.50    0.50    --    0.00  38.00 150.00  212
  4  \w     76.00 161.00   0.50    3.69    --   95.20  45.00 -90.00  170
  5  \w     47.00 128.00   0.50    3.69    --   95.20 -82.00  60.00  162
  6  \w     36.00 112.00   0.50    3.69    --   95.20 -61.00  60.00  152
  7  \w    102.00 182.00   0.50    3.69    --   95.20  45.00-120.00  160
;
_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      -0.0359419000
_diffrn_orient_matrix_UB_12      -0.0421462000
_diffrn_orient_matrix_UB_13      -0.0286933000
_diffrn_orient_matrix_UB_21      0.0322187000
_diffrn_orient_matrix_UB_22      -0.0179609000
_diffrn_orient_matrix_UB_23      -0.0032150000
_diffrn_orient_matrix_UB_31      -0.0163324000
_diffrn_orient_matrix_UB_32      -0.0222919000
_diffrn_orient_matrix_UB_33      0.0568973000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            81938
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        64.998
_diffrn_reflns_theta_max         64.998
_diffrn_reflns_theta_min         2.342
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.689
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       needle
_exptl_crystal_F_000             11298
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 8277 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1487
_refine_ls_number_reflns         28183
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0869P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                22155
_reflns_number_total             28183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oc0c01045_si_003.cif
_cod_data_source_block           exp_1131_sq
_cod_original_cell_volume        25500.7(5)
_cod_database_code               4518096
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.453
_shelx_estimated_absorpt_t_min   0.089
_reflns_odcompleteness_completeness 99.96
_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 C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C55-C54 = C56-C57
 1.39 with sigma of 0.02
 C84-N1
 2.5 with sigma of 0.02
 H84b-H87b
 2.2 with sigma of 0.04
 H88b-H91c
 2.2 with sigma of 0.04
 H5-H90a
 2.2 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C18 \\sim C19: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C7 \\sim C8 \\sim B36 \\sim B39: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(B17) \\sim Ueq, Uanis(B14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C78) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C76) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(B15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C81) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C56) \\sim Ueq, Uanis(B39) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C51) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C85) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C78) \\sim Ueq,
Uanis(C80) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(B18) \\sim Ueq, Uanis(B16) \\sim Ueq,
Uanis(B19) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(B30) \\sim Ueq, Uanis(C74)
\\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C75) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C67) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: Ag16(0.5)
5.a Riding coordinates:
 C91(H91a,H91b,H91c)
5.b Secondary CH2 refined with riding coordinates:
 C21(H21a,H21b), C46(H46a,H46b), C71(H71a,H71b)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45),
  C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C55(H55),
 C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64),
  C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C72(H72), C73(H73),
 C74(H74), C75(H75), C76(H76), C79(H79), C78(H78), C82(H82), C81(H81), C80(H80)
5.d Fitted hexagon refined as free rotating group:
 C16(C17,C18,C19,C20,C15), C77(C72,C73,C74,C75,C76), C79(C78,C83,C82,C81,C80)
5.e Idealised Me refined as rotating group:
 C84(H84a,H84b,H84c), C86(H86a,H86b,H86c), C87(H87a,H87b,H87c), C88(H88a,H88b,
 H88c), C90(H90a,H90b,H90c)
5.f Boron cage BH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), B4(H4a),
 B5(H5a), B6(H6a), B7(H7a), B8(H8a), B9(H9), B10(H10a), B14(H14a), B15(H15),
 B16(H16a), B17(H17a), B18(H18a), B19(H19a), B20(H20a), B22(H22a), B23(H23),
 B25(H25a), B27(H27a), B28(H28a), B29(H29), B30(H30a), B33(H33a), B35(H35a),
 B36(H36a), B37(H37a), B38(H38a), B39(H39a), B40(H40a)
;
_shelx_res_checksum              53838
_shelx_hkl_checksum              84384
_shelx_fab_checksum              36498
_platon_squeeze_void_probe_radius 1.20
_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 7.346
_oxdiff_exptl_absorpt_empirical_full_min 0.354