From Racemic Metal Nanoparticles to Optically Pure Enantiomers in One Pot.
Yang, Huayan; Yan, Juanzhu; Wang, Yu; Deng, Guocheng; Su, Haifeng; Zhao, Xiaojing; Xu, Chaofa; Teo, Boon K.; Zheng, Nanfeng; Journal of the American Chemical Society 139 (2017) 16113–16116; doi:10.1021/jacs.7b10448

data_4131760
_publ_section_title
;
 From Racemic Metal Nanoparticles to Optically Pure Enantiomers in One
 Pot.
;
_journal_issue                   45
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16113
_journal_page_last               16116
_journal_paper_doi               10.1021/jacs.7b10448
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'Ag78 C468 F126 P12 S42'
_chemical_formula_sum            'C468 Ag78 F126 P12 S42'
_chemical_formula_weight         18146.70
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_Hall           'I 2 2 3'
_space_group_name_H-M_alt        'I 2 3'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   52.0957(8)
_cell_length_b                   52.0957(8)
_cell_length_c                   52.0957(8)
_cell_measurement_reflns_used    10871
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      57.3050
_cell_measurement_theta_min      3.5780
_cell_volume                     141386(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41o (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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -117.00 -63.00   1.00   12.50    --  -38.11-142.00-129.00   54
  2  \w   -117.00 -59.00   1.00   12.50    --  -38.11-149.00 125.00   58
  3  \w      9.00 129.00   1.00   50.00    --   93.00 -77.00-150.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0108333000
_diffrn_orient_matrix_UB_12      0.0057721000
_diffrn_orient_matrix_UB_13      0.0268847000
_diffrn_orient_matrix_UB_21      -0.0186474000
_diffrn_orient_matrix_UB_22      -0.0196768000
_diffrn_orient_matrix_UB_23      0.0117751000
_diffrn_orient_matrix_UB_31      0.0202173000
_diffrn_orient_matrix_UB_32      -0.0213198000
_diffrn_orient_matrix_UB_33      -0.0036311000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0866
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            83379
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        61.160
_diffrn_reflns_theta_max         61.160
_diffrn_reflns_theta_min         3.174
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41o (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       block
_exptl_crystal_F_000             67680
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.700
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.188
_refine_ls_abs_structure_details
;
 Flack x determined using 5266 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.053(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         32355
_refine_ls_number_restraints     1349
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1594
_refine_ls_R_factor_gt           0.1029
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2785
_refine_ls_wR_factor_ref         0.3434
_reflns_Friedel_coverage         0.723
_reflns_Friedel_fraction_full    0.779
_reflns_Friedel_fraction_max     0.779
_reflns_number_gt                16369
_reflns_number_total             32355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10448_si_004.cif
_cod_data_source_block           yjz160606-10-b_2
_cod_original_cell_volume        141386(6)
_cod_database_code               4131760
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Restrained distances
 P4-C99
 1.75 with sigma of 0.02
 C156-P3
 1.75 with sigma of 0.02
 C30-S5
 1.75 with sigma of 0.02
 C36-P1
 1.75 with sigma of 0.02
 P2-C140
 1.75 with sigma of 0.02
 C3-S1
 1.75 with sigma of 0.02
 P3-C116
 1.75 with sigma of 0.02
 C146-P2
 1.75 with sigma of 0.02
 C146-P2
 1.75 with sigma of 0.02
 C21-C20
 1.64 with sigma of 0.02
 C138-C137
 1.64 with sigma of 0.02
 C73-C72
 1.64 with sigma of 0.02
 C73-C72
 1.64 with sigma of 0.02
 C51-C52
 1.64 with sigma of 0.02
 C34-C33
 1.64 with sigma of 0.02
 C7-C6
 1.64 with sigma of 0.02
 C14-C13
 1.64 with sigma of 0.02
 C126-C125
 1.64 with sigma of 0.02
 C113-C112
 1.64 with sigma of 0.02
 C10-S6
 2.67 with sigma of 0.02
 C10-S6
 1.64 with sigma of 0.02
 C10-S6
 1.75 with sigma of 0.02
 C94-C93
 1.64 with sigma of 0.02
 C87-C86
 1.76 with sigma of 0.02
 F27-C66
 1.6 with sigma of 0.02
 F25-C66
 1.6 with sigma of 0.02
 F15-C14
 1.6 with sigma of 0.02
 C34-F7
 1.6 with sigma of 0.02
 C34-F8
 1.6 with sigma of 0.02
 F9-C34
 1.6 with sigma of 0.02
 F25-C66
 1.6 with sigma of 0.02
 F27-C66
 1.6 with sigma of 0.02
 F32-C73
 1.6 with sigma of 0.02
 F31-C73
 1.6 with sigma of 0.02
 F33-C73
 1.6 with sigma of 0.02
 F15-C14
 1.6 with sigma of 0.02
 F32-C73
 1.6 with sigma of 0.02
 F33-C73
 1.6 with sigma of 0.02
 F31-C73
 1.6 with sigma of 0.02
 F21-C52
 1.6 with sigma of 0.02
 C52-F19
 1.6 with sigma of 0.02
 C52-F20
 1.6 with sigma of 0.02
 F3-C126
 1.6 with sigma of 0.02
 F37-C94
 1.6 with sigma of 0.02
 C94-F38
 1.6 with sigma of 0.02
 C94-F39
 1.6 with sigma of 0.02
 C80-C79
 1.64 with sigma of 0.02
 F12-C7
 1.6 with sigma of 0.02
 C59-C58
 1.64 with sigma of 0.02
 C59-C58
 1.64 with sigma of 0.02
 C80-C79
 1.64 with sigma of 0.02
 C76-S4
 1.78 with sigma of 0.02
 F34-C80
 1.6 with sigma of 0.02
 F36-C80
 1.6 with sigma of 0.02
 F35-C80
 1.6 with sigma of 0.02
 F41-C87
 1.6 with sigma of 0.02
 C87-F42
 1.6 with sigma of 0.02
 C7-F11
 1.6 with sigma of 0.02
 F10-C7
 1.6 with sigma of 0.02
 C14-F14
 1.6 with sigma of 0.02
 C14-F15
 1.6 with sigma of 0.02
 C14-F13
 1.6 with sigma of 0.02
 C126-F1
 1.6 with sigma of 0.02
 C126-F2
 1.6 with sigma of 0.02
 C126-F3
 1.6 with sigma of 0.02
 F24-C59
 1.6 with sigma of 0.02
 F22-C59
 1.6 with sigma of 0.02
 F23-C59
 1.6 with sigma of 0.02
 F40-C87
 1.6 with sigma of 0.02
 C138-F4
 1.6 with sigma of 0.02
 F6-C138
 1.6 with sigma of 0.02
 F5-C138
 1.6 with sigma of 0.02
 C66-C65
 1.64 with sigma of 0.02
 C66-F26
 1.6 with sigma of 0.02
 F26-C66
 1.6 with sigma of 0.02
 P4-C98
 2.76 with sigma of 0.04
 P4-C100
 2.76 with sigma of 0.04
 P4-C97
 4.06 with sigma of 0.04
 P4-C95
 4.06 with sigma of 0.04
 P4-C96
 4.6 with sigma of 0.04
 C151-P3
 2.76 with sigma of 0.04
 C155-P3
 2.76 with sigma of 0.04
 C152-P3
 4.06 with sigma of 0.04
 C154-P3
 4.06 with sigma of 0.04
 C153-P3
 4.6 with sigma of 0.04
 C31-S5
 2.76 with sigma of 0.04
 C29-S5
 2.76 with sigma of 0.04
 C32-S5
 4.06 with sigma of 0.04
 C28-S5
 4.06 with sigma of 0.04
 C33-S5
 4.6 with sigma of 0.04
 C37-P1
 2.76 with sigma of 0.04
 C35-P1
 2.76 with sigma of 0.04
 C38-P1
 4.06 with sigma of 0.04
 C40-P1
 4.06 with sigma of 0.04
 C39-P1
 4.6 with sigma of 0.04
 C141-P2
 2.75 with sigma of 0.04
 C139-P2
 2.75 with sigma of 0.04
 C144-P2
 4.06 with sigma of 0.04
 C142-P2
 4.06 with sigma of 0.04
 C143-P2
 4.6 with sigma of 0.04
 S1-C2
 2.75 with sigma of 0.04
 C4-S1
 2.75 with sigma of 0.04
 S1-C1
 4.06 with sigma of 0.04
 S1-C5
 4.06 with sigma of 0.04
 S1-C6
 4.6 with sigma of 0.04
 C117-P3
 2.75 with sigma of 0.04
 C115-P3
 2.75 with sigma of 0.04
 C114-P3
 4.06 with sigma of 0.04
 C118-P3
 4.06 with sigma of 0.04
 C119-P3
 4.6 with sigma of 0.04
 C147-P2
 2.75 with sigma of 0.04
 C145-P2
 2.75 with sigma of 0.04
 C150-P2
 4.06 with sigma of 0.04
 P2-C148
 4.06 with sigma of 0.04
 C149-P2
 4.6 with sigma of 0.04
 C21-C19
 2.68 with sigma of 0.04
 C21-C15
 2.68 with sigma of 0.04
 C138-C132
 2.68 with sigma of 0.04
 C138-C136
 2.68 with sigma of 0.04
 C73-C71
 2.68 with sigma of 0.04
 C73-C67
 2.68 with sigma of 0.04
 C73-C71
 2.68 with sigma of 0.04
 C73-C67
 2.68 with sigma of 0.04
 C52-C50
 2.68 with sigma of 0.04
 C52-C46
 2.68 with sigma of 0.04
 C28-C34
 2.68 with sigma of 0.04
 C34-C32
 2.68 with sigma of 0.04
 C7-C1
 2.68 with sigma of 0.04
 C5-C7
 2.68 with sigma of 0.04
 C8-C14
 2.68 with sigma of 0.04
 C14-C12
 2.68 with sigma of 0.04
 C124-C126
 2.68 with sigma of 0.04
 C126-C120
 2.68 with sigma of 0.04
 C113-C111
 2.68 with sigma of 0.04
 C113-C107
 2.68 with sigma of 0.04
 C9-S6
 2.76 with sigma of 0.04
 C11-S6
 2.76 with sigma of 0.04
 S6-C8
 4.06 with sigma of 0.04
 C12-S6
 4.06 with sigma of 0.04
 S6-C13
 4.6 with sigma of 0.04
 C11-S6
 2.76 with sigma of 0.04
 C9-S6
 2.76 with sigma of 0.04
 C12-S6
 4.06 with sigma of 0.04
 C8-S6
 4.06 with sigma of 0.04
 C13-S6
 4.6 with sigma of 0.04
 C94-C88
 2.68 with sigma of 0.04
 C94-C92
 2.68 with sigma of 0.04
 C87-C81
 2.76 with sigma of 0.04
 C85-C87
 2.76 with sigma of 0.04
 C87-C84
 4.06 with sigma of 0.04
 C87-C82
 4.06 with sigma of 0.04
 F27-F25
 2.3 with sigma of 0.04
 F9-F8
 2.3 with sigma of 0.04
 F8-F7
 2.3 with sigma of 0.04
 F7-F9
 2.3 with sigma of 0.04
 F25-F27
 2.3 with sigma of 0.04
 F32-F33
 2.3 with sigma of 0.04
 F31-F32
 2.3 with sigma of 0.04
 F33-F31
 2.3 with sigma of 0.04
 F32-F33
 2.3 with sigma of 0.04
 F33-F31
 2.3 with sigma of 0.04
 F31-F32
 2.3 with sigma of 0.04
 F21-F20
 2.3 with sigma of 0.04
 F20-F19
 2.3 with sigma of 0.04
 F21-F19
 2.3 with sigma of 0.04
 F39-F38
 2.3 with sigma of 0.04
 F37-F39
 2.3 with sigma of 0.04
 F38-F37
 2.3 with sigma of 0.04
 C80-C78
 2.68 with sigma of 0.04
 C80-C74
 2.68 with sigma of 0.04
 C59-C57
 2.68 with sigma of 0.04
 C59-C53
 2.68 with sigma of 0.04
 C59-C53
 2.68 with sigma of 0.04
 C59-C57
 2.68 with sigma of 0.04
 C80-C74
 2.68 with sigma of 0.04
 C80-C78
 2.68 with sigma of 0.04
 C75-S4
 2.76 with sigma of 0.04
 C77-S4
 2.76 with sigma of 0.04
 C78-S4
 4.06 with sigma of 0.04
 C74-S4
 4.06 with sigma of 0.04
 C79-S4
 4.6 with sigma of 0.04
 F34-F35
 2.3 with sigma of 0.04
 F36-F35
 2.3 with sigma of 0.04
 F34-F36
 2.3 with sigma of 0.04
 F41-F42
 2.3 with sigma of 0.04
 F11-F12
 2.3 with sigma of 0.04
 F10-F12
 2.3 with sigma of 0.04
 F10-F11
 2.3 with sigma of 0.04
 F13-F14
 2.3 with sigma of 0.04
 F13-F15
 2.3 with sigma of 0.04
 F14-F15
 2.3 with sigma of 0.04
 F2-F3
 2.3 with sigma of 0.04
 F2-F1
 2.3 with sigma of 0.04
 F1-F3
 2.3 with sigma of 0.04
 F2-F3
 2.3 with sigma of 0.04
 F24-F22
 2.3 with sigma of 0.04
 F22-F23
 2.3 with sigma of 0.04
 F24-F23
 2.3 with sigma of 0.04
 F41-F40
 2.3 with sigma of 0.04
 F40-F42
 2.3 with sigma of 0.04
 F6-F5
 2.3 with sigma of 0.04
 F5-F4
 2.3 with sigma of 0.04
 F4-F6
 2.3 with sigma of 0.04
 F34-C79
 2.4 with sigma of 0.04
 C79-F36
 2.4 with sigma of 0.04
 F35-C79
 2.4 with sigma of 0.04
 F32-C72
 2.4 with sigma of 0.04
 F31-C72
 2.4 with sigma of 0.04
 F33-C72
 2.4 with sigma of 0.04
 F36-C79
 2.4 with sigma of 0.04
 C66-C64
 2.68 with sigma of 0.04
 C66-C60
 2.68 with sigma of 0.04
 F26-F25
 2.3 with sigma of 0.04
 F26-F27
 2.3 with sigma of 0.04
 F26-F25
 2.3 with sigma of 0.04
 F26-F27
 2.3 with sigma of 0.04
 F11-C6
 2.4 with sigma of 0.04
 F26-C65
 2.4 with sigma of 0.04
 F26-F27
 2.3 with sigma of 0.04
 F26-F25
 2.3 with sigma of 0.04
 F25-F27
 2.3 with sigma of 0.04
 C13-F14
 2.3 with sigma of 0.04
 F15-C13
 2.3 with sigma of 0.04
 C13-F13
 2.4 with sigma of 0.04
2. Restrained planarity
 C12, C13, C8, S6
 with sigma of 0.1
 S9, C85, C84, C83, C82, C81, C86
 with sigma of 0.1
 C31, C30, C29, C28, C33, C32, S5
 with sigma of 0.1
 C122, C123, C124, C125, C120, C121, S14
 with sigma of 0.1
 C4, C3, C2, C1, C6, C5, S1
 with sigma of 0.1
 C118, C119, C114, C115, C116, C117, P3
 with sigma of 0.1
 C147, C146, C145, C150, C148, C149
 with sigma of 0.1
 C146, C145, C150, C148, C119, C147, P2
 with sigma of 0.1
 S2, C19, C18, C17, C16, C15, C20, C21
 with sigma of 0.1
 C38, C39, C40, C35, C36, C37, P1
 with sigma of 0.1
 C12, C13, C8, C9, C10, C11, C14, S6
 with sigma of 0.1
 C6, C7, C3, C2, C1, C5, C4, S1
 with sigma of 0.1
 C126, C125, C124, C123, C122, S14, C121, C120
 with sigma of 0.1
 C52, C47, C49, C50, C51, C46, C48, S3
 with sigma of 0.1
 C77, C76, C75, C74, C79, C78, C80
 with sigma of 0.1
 C34, C31, C30, C29, C28, C33, C32, S5
 with sigma of 0.1
 C73, C72, C68, C69, C70, C71, C67
 with sigma of 0.1
 C94, C90, C89, C88, C93, C92, C91
 with sigma of 0.1
 C87, C86, C85, C84, C83, C82, C81
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(P1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uiso(C132) = Uiso(C2) = Uiso(C1) = Uiso(C6) = Uiso(C4) = Uiso(C28) = Uiso(C33)
= Uiso(C143) = Uiso(C141) = Uiso(C148) = Uiso(C147) = Uiso(C11) = Uiso(C12) =
Uiso(C117) = Uiso(C152) = Uiso(C154) = Uiso(C139) = Uiso(C140) = Uiso(C8)
Uiso(C134) = Uiso(C132)
Uiso(C60) = Uiso(C66)
Uiso(F41) = Uiso(F40)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Fitted hexagon refined as free rotating group:
 C133(C132,C137,C136,C135,C134), C85(C84,C83,C82,C81,C86), C90(C89,C88,C93,C92,
 C91), C68(C69,C70,C71,C72,C67), C47(C48,C49,C50,C51,C46), C112(C111,C110,C109,
 C108,C107), C105(C104,C103,C102,C101,C106), C77(C76,C75,C74,C79,C78), C24(C23,
 C22,C27,C26,C25), C122(C123,C124,C125,C120,C121), C98(C99,C100,C95,C96,C97),
 C55(C56,C57,C58,C53,C54), C65(C64,C63,C62,C61,C60), C19(C18,C17,C16,C15,C20),
 C31(C30,C29,C28,C33,C32), C12(C13,C8,C9,C10,C11), C38(C39,C40,C35,C36,C37),
 C139(C144,C143,C142,C141,C140), C155(C154,C153,C152,C151,C156), C147(C146,C145,
 C150,C149,C148), C118(C119,C114,C115,C116,C117), C4(C3,C2,C1,C6,C5)
;
_shelx_shelxl_version_number     2014/7
_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 1.959
_oxdiff_exptl_absorpt_empirical_full_min 0.586