Embryonic Growth of Face-Center-Cubic Silver Nanoclusters Shaped in Nearly Perfect Half-Cubes and Cubes.
Yang, Huayan; Yan, Juanzhu; Wang, Yu; Su, Haifeng; Gell, Lars; Zhao, Xiaojing; Xu, Chaofa; Teo, Boon K.; Häkkinen, Hannu; Zheng, Nanfeng; Journal of the American Chemical Society 139 (2017) 31–34; doi:10.1021/jacs.6b10053

data_4125391
_publ_section_title
;
 Embryonic Growth of Face-Center-Cubic Silver Nanoclusters Shaped in
 Nearly Perfect Half-Cubes and Cubes.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              31
_journal_page_last               34
_journal_paper_doi               10.1021/jacs.6b10053
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'0.5(C318 H324 Ag63 F70.81 P8 S36), 0.5(C312 H324 Ag63 F72 P8 S36), C61 H15 B1'
_chemical_formula_sum            'C379 H345 Ag63 B Cl6 F71.41 P8 S36'
_chemical_formula_weight         14677.59
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-09-23
_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                120
_cell_formula_units_Z            6
_cell_length_a                   25.3369(5)
_cell_length_b                   25.3369(5)
_cell_length_c                   114.6628(17)
_cell_measurement_reflns_used    14015
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.0190
_cell_measurement_theta_min      4.0020
_cell_volume                     63747(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3415
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
  1 omega  -46.00   29.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9299   38.0000    0.0000 150

  2 omega -116.00  -17.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9299  -38.0000    0.0000 198

  3 omega   35.00   60.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9299 -147.0000  -85.0000 50

  4 omega -106.00  -78.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -125.0000  120.0000 56

  5 omega   54.00   94.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -94.0000  150.0000 80

  6 omega   56.00  110.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -61.0000   30.0000 108

  7 omega   34.00   90.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000  120.0000 112

  8 omega   78.00  178.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940   30.0000  -90.0000 200

  9 omega   35.00   90.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000   60.0000 110

 10 omega   99.00  160.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  124.0000  158.0000 122

 11 omega   31.00   90.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000    0.0000 118
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0134704000
_diffrn_orient_matrix_UB_12      0.0216127000
_diffrn_orient_matrix_UB_13      0.0115971000
_diffrn_orient_matrix_UB_21      0.0660286000
_diffrn_orient_matrix_UB_22      0.0537136000
_diffrn_orient_matrix_UB_23      0.0003491000
_diffrn_orient_matrix_UB_31      -0.0197268000
_diffrn_orient_matrix_UB_32      0.0397664000
_diffrn_orient_matrix_UB_33      -0.0067721000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       131
_diffrn_reflns_limit_l_min       -142
_diffrn_reflns_number            81299
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.178
_diffrn_reflns_theta_min         3.469
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.294
_exptl_crystal_description       block
_exptl_crystal_F_000             42154
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.844
_refine_diff_density_min         -2.379
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1562
_refine_ls_number_reflns         28186
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          3.328
_refine_ls_shift/su_mean         0.094
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+3976.2529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19573
_reflns_number_total             28186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10053_si_004.cif
_cod_data_source_block           '[Ag63(SPhF2)36(PBu3)8]BPPh4'
_cod_depositor_comments
'Adding full bibliography for 4125391--4125393.cif.'
_cod_original_cell_volume        63747(3)
_cod_database_code               4125391
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C101-C100 = C100-C99
 1.5 with sigma of 0.02
 C99-C101
 2.5 with sigma of 0.02
 C98-C100
 2.5 with sigma of 0.02
 C122-C118 = C119-C118 = C119-C120 = C121-C120
 1.35 with sigma of 0.02
 C122-C119
 2.4 with sigma of 0.02
 C120-C118
 2.4 with sigma of 0.02
 C119-C121
 2.4 with sigma of 0.02
 C123-C126 = C123-C124 = C125-C124
 1.35 with sigma of 0.02
 C126-C124
 2.4 with sigma of 0.02
 C123-C125
 2.4 with sigma of 0.02
 P16-C45
 1.75 with sigma of 0.02
 C45-C46 = C47-C46 = C47-C48
 1.5 with sigma of 0.02
 C48-C46
 2.5 with sigma of 0.04
 C47-C45
 2.5 with sigma of 0.04
 C46-P16
 2.6 with sigma of 0.04
3. Restrained planarity
 B1, C111, C110, C109, C108, C107, C106
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Sof(F22A)=1-FVAR(1)
 Sof(F22)=Sof(F21)=FVAR(1)
 Sof(F14A)=1-FVAR(2)
 Sof(F14)=FVAR(2)
 Fixed Sof: B1(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C94(H94A,H94B), C95(H95A,H95B), C93(H93A,H93B), C97(H97A,H97B), C37(H37A,
 H37B), C98(H98A,H98B), C89(H89A,H89B), C90(H90A,H90B), C102(H10A,H10B),
 C38(H38A,H38B), C42(H42A,H42B), C103(H10C,H10D), C104(H10E,H10F), C91(H91A,
 H91B), C39(H39A,H39B), C41(H41A,H41B), C99(H99A,H99B), C43(H43A,H43B),
 C100(H10G,H10H), C50(H50A,H50B), C45(H45A,H45B), C49(H49A,H49B), C51(H51A,
 H51B), C47(H47A,H47B), C46(H46A,H46B)
6.b Aromatic/amide H refined with riding coordinates:
 C70(H70), C82(H82), C58(H58), C67(H67), C6(H6), C66(H66), C54(H54), C72(H72),
 C64(H64), C23(H23), C12(H12), C76(H76), C60(H60), C84(H84), C2(H2), C61(H61),
 C26(H26), C88(H88), C87(H87), C78(H78), C18(H18), C19(H19), C14(H14), C8(H8),
 C32(H32), C36(H36), C33(H33), C27(H27), C73(H73), C9(H9), C5(H5), C20(H20),
 C30(H30), C15(H15), C117(H117), C113(H113), C114(H114), C115(H115), C116(H116)
6.c Fitted hexagon refined as free rotating group:
 C32(C31,C36,C35,C34,C33), C117(C112,C113,C114,C115,C116), C111(C106,C107,C108,
 C109,C110)
6.d Idealised Me refined as rotating group:
 C96(H96A,H96B,H96C), C92(H92A,H92B,H92C), C40(H40A,H40B,H40C), C105(H10I,H10J,
 H10K), C44(H44A,H44B,H44C), C52(H52A,H52B,H52C), C48(H48A,H48B,H48C),
 C101(H10L,H10M,H10N)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'