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_4131762
_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_absolute_configuration rm
_chemical_formula_moiety         'C468 H348 Ag78 F126 P12 S42'
_chemical_formula_sum            'C468 H348 Ag78 F126 P12 S42'
_chemical_formula_weight         18497.46
_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_hydrogens   geom
_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                   51.7906(4)
_cell_length_b                   51.7906(4)
_cell_length_c                   51.7906(4)
_cell_measurement_reflns_used    27664
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      58.2140
_cell_measurement_theta_min      3.5950
_cell_volume                     138916.2(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_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    -45.00  35.00   1.00   12.50    --  -38.29  37.00-180.00   80
  2  \w     15.00  41.00   1.00   12.50    --  -38.29  37.00-120.00   26
  3  \w   -108.00  -7.00   1.00   12.50    --  -38.29 -57.00  30.00  101
  4  \w      8.00 127.00   1.00   45.00    --   92.37 -77.00   0.00  119
  5  \w     52.00  94.00   1.00   45.00    --   92.37 -45.00  60.00   42
  6  \w     95.00 140.00   1.00   45.00    --   92.37 125.00  30.00   45
  7  \w     19.00  49.00   1.00   45.00    --   92.37 -45.00  60.00   30
  8  \w    106.00 171.00   1.00   45.00    --   92.37 125.00  60.00   65
  9  \w     62.00 172.00   1.00   45.00    --   92.37 -15.00 -30.00  110
 10  \w      9.00  35.00   1.00   45.00    --   92.37 -15.00 -30.00   26
;
_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      0.0104264000
_diffrn_orient_matrix_UB_12      0.0157684000
_diffrn_orient_matrix_UB_13      -0.0229801000
_diffrn_orient_matrix_UB_21      0.0265837000
_diffrn_orient_matrix_UB_22      -0.0129887000
_diffrn_orient_matrix_UB_23      0.0031485000
_diffrn_orient_matrix_UB_31      -0.0083380000
_diffrn_orient_matrix_UB_32      -0.0215948000
_diffrn_orient_matrix_UB_33      -0.0186483000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            256952
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        65.854
_diffrn_reflns_theta_max         65.854
_diffrn_reflns_theta_min         3.193
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.234
_exptl_absorpt_correction_T_max  0.245
_exptl_absorpt_correction_T_min  0.043
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_description       block
_exptl_crystal_F_000             70464
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 6674 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1936
_refine_ls_number_reflns         39828
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.169
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1147P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1749
_refine_ls_wR_factor_ref         0.2142
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                19358
_reflns_number_total             39828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10448_si_003.cif
_cod_data_source_block           yjz160606-7-a_2face
_cod_original_cell_volume        138916(3)
_cod_database_code               4131762
_chemical_oxdiff_formula         Ag78(SC6H4CF3)42P13(CH2)3(C6H5)16
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     65.57
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C93-C92
 1.5 with sigma of 0.02
 C100-C99
 1.5 with sigma of 0.02
 C114-C113
 1.5 with sigma of 0.02
 C127-C128
 1.5 with sigma of 0.02
 C156-C157
 1.5 with sigma of 0.02
 C29-C30
 1.5 with sigma of 0.02
 C121-C120
 1.5 with sigma of 0.02
 C49-C50
 1.5 with sigma of 0.02
 F14-C86
 1.4 with sigma of 0.02
 F13-C86
 1.4 with sigma of 0.02
 C86-F15
 1.4 with sigma of 0.02
 F33-C50
 1.4 with sigma of 0.02
 C50-F33
 1.4 with sigma of 0.02
 F33-C50
 1.4 with sigma of 0.02
 C50-F31
 1.4 with sigma of 0.02
 F32-C50
 1.4 with sigma of 0.02
 C85-C86
 1.4 with sigma of 0.02
 F7-C121 = F9-C121
 1.4 with sigma of 0.02
 F40-C135 = F42-C135 = F41-C135
 1.4 with sigma of 0.02
 F3-C157 = F2-C157 = F1-C157
 1.4 with sigma of 0.02
 C30-F26
 1.4 with sigma of 0.02
 C23-C22
 1.5 with sigma of 0.02
 F18-C7
 1.3 with sigma of 0.02
 F16-C7 = F17-C7
 1.3 with sigma of 0.02
 C7-C6 = C7-F16 = C7-F17 = C7-F18
 1.3 with sigma of 0.02
 F25-C30
 1.3 with sigma of 0.02
 F27-C30 = F26-C30
 1.3 with sigma of 0.02
 F27-C29
 2.5 with sigma of 0.04
 F26-C29
 2.5 with sigma of 0.04
 C29-F25
 2.5 with sigma of 0.04
 F13-F15
 2.4 with sigma of 0.04
 F13-F14
 2.4 with sigma of 0.04
 F14-F15
 2.4 with sigma of 0.04
 F33-C49
 2.4 with sigma of 0.04
 F31-C49
 2.4 with sigma of 0.04
 C49-F32
 2.4 with sigma of 0.04
 F41-F42
 2.4 with sigma of 0.04
 F42-F40
 2.4 with sigma of 0.04
 F40-F41
 2.4 with sigma of 0.04
 F1-F3
 2.4 with sigma of 0.04
 F1-F2
 2.4 with sigma of 0.04
 F2-F3
 2.4 with sigma of 0.04
 C17-C23
 2.5 with sigma of 0.04
 C23-C21
 2.5 with sigma of 0.04
 F16-F18
 2.4 with sigma of 0.04
 F18-F17
 2.4 with sigma of 0.04
 F17-F16
 2.4 with sigma of 0.04
 F28-F29
 2.4 with sigma of 0.04
 F29-F30
 2.4 with sigma of 0.04
 F30-F28
 2.4 with sigma of 0.04
 F25-F27
 2.4 with sigma of 0.04
 F25-F26
 2.4 with sigma of 0.04
 F26-F27
 2.4 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C128) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C135) = Uanis(C128)
4. Rigid body (RIGU) restrains
 C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C143(H143), C64(H64), C66(H66), C9(H9)
5.b Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C144(H14A,H14B)
5.c Aromatic/amide H refined with riding coordinates:
 C94(H94), C95(H95), C97(H97), C98(H98), C40(H40), C37(H37), C25(H25),
 C27(H27), C28(H28), C24(H24), C112(H112), C108(H108), C109(H109), C111(H111),
 C123(H123), C125(H125), C126(H126), C122(H122), C41(H41), C47(H47), C115(H115),
  C116(H116), C118(H118), C119(H119), C4(H4), C2(H2), C1(H1), C5(H5), C44(H44),
 C132(H132), C133(H133), C129(H129), C130(H130), C105(H105), C81(H81), C83(H83),
  C84(H84), C80(H80), C69(H69), C73(H73), C72(H72), C71(H71), C70(H70),
 C104(H104), C45(H45), C18(H18), C17(H17), C21(H21), C20(H20), C101(H101),
 C38(H38), C102(H102), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C61(H61), C60(H60), C59(H59), C58(H58), C57(H57), C76(H76), C77(H77), C78(H78),
  C79(H79), C74(H74), C33(H33), C32(H32), C31(H31), C36(H36), C35(H35),
 C48(H48), C154(H154), C55(H55), C56(H56), C51(H51), C52(H52), C53(H53),
 C91(H91), C90(H90), C88(H88), C87(H87), C147(H147), C148(H148), C149(H149),
 C150(H150), C145(H145), C140(H140), C136(H136), C137(H137), C138(H138),
 C139(H139), C152(H152), C151(H151), C155(H155)
5.d Fitted hexagon refined as free rotating group:
 C99(C94,C95,C96,C97,C98), C25(C26,C27,C28,C29,C24), C112(C113,C108,C109,C110,
 C111), C123(C124,C125,C126,C127,C122), C115(C116,C117,C118,C119,C120), C4(C3,
 C2,C1,C6,C5), C131(C132,C133,C134,C129,C130), C81(C82,C83,C84,C85,C80),
 C69(C68,C73,C72,C71,C70), C19(C18,C17,C22,C21,C20), C11(C12,C13,C14,C15,C16),
 C62(C61,C60,C59,C58,C57), C75(C76,C77,C78,C79,C74), C34(C33,C32,C31,C36,C35),
 C54(C55,C56,C51,C52,C53), C91(C90,C89,C88,C87,C92), C146(C147,C148,C149,C150,
 C145), C140(C141,C136,C137,C138,C139)
5.e Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C63(H63A,H63B,H63C), C8(H8A,H8B,H8C), C142(H14C,H14D,H14E)
;
_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 1.694
_oxdiff_exptl_absorpt_empirical_full_min 0.613
_platon_squeeze_void_probe_radius 1.20