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_4125392
_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(Ag63 C312 F72 P8 S36), 0.5(Ag63 C318 F72 P8 S36), 1(Br)'
_chemical_formula_sum            'C315 Ag63 Br F72 P8 S36'
_chemical_formula_weight         13428.79
_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_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                   25.2879(4)
_cell_length_b                   25.2879(4)
_cell_length_c                   114.758(2)
_cell_measurement_reflns_used    20509
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      61.0150
_cell_measurement_theta_min      4.0650
_cell_volume                     63553.5(18)
_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      100.01(10)
_diffrn_detector_area_resol_mean 10.3415
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -91.00   -1.40   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9924  125.0000  150.0000 128

  2 omega  -95.00  -67.70   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9924  125.0000 -150.0000 39

  3 omega  -47.00  -19.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9924  125.0000 -150.0000 40

  4 omega -113.00  -16.40   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9924  -38.0000  -60.0000 138

  5 omega -118.00   -7.40   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9924  -77.0000   90.0000 158

  6 omega  -48.00   -0.40   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   45.0000   90.0000 68

  7 omega   36.00  105.30   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -94.0000   60.0000 99

  8 omega   30.00   70.60   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000   30.0000 58

  9 omega   79.00  177.00   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940   30.0000  -30.0000 140

 10 omega   36.00   84.30   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000   60.0000 69

 11 omega   48.00  135.50   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -61.0000 -120.0000 125

 12 omega   78.00  150.10   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940   30.0000   60.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0077987000
_diffrn_orient_matrix_UB_12      -0.0492855000
_diffrn_orient_matrix_UB_13      -0.0063753000
_diffrn_orient_matrix_UB_21      -0.0303735000
_diffrn_orient_matrix_UB_22      0.0084811000
_diffrn_orient_matrix_UB_23      -0.0109313000
_diffrn_orient_matrix_UB_31      0.0629616000
_diffrn_orient_matrix_UB_32      0.0494715000
_diffrn_orient_matrix_UB_33      -0.0044784000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       130
_diffrn_reflns_limit_l_min       -130
_diffrn_reflns_number            87736
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        61.150
_diffrn_reflns_theta_max         61.150
_diffrn_reflns_theta_min         3.368
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.420
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36499
_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    2.105
_exptl_crystal_description       block
_exptl_crystal_F_000             37380
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.142
_refine_diff_density_min         -3.086
_refine_diff_density_rms         0.422
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1399
_refine_ls_number_reflns         21696
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1520
_refine_ls_R_factor_gt           0.1246
_refine_ls_shift/su_max          0.081
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1549P)^2^+22635.4551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3893
_refine_ls_wR_factor_ref         0.4101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15656
_reflns_number_total             21696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10053_si_005.cif
_cod_data_source_block           '[Ag63(SPhF2)36(PnBu3)8]Br'
_cod_depositor_comments
'Adding full bibliography for 4125391--4125393.cif.'
_cod_original_cell_volume        63554(3)
_cod_database_code               4125392
_reflns_odcompleteness_completeness 85.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 C52-S7
 2.8 with sigma of 0.02
 C68-S7
 2.8 with sigma of 0.02
 S7-C55
 1.8 with sigma of 0.02
 C121-C0AA = C184-C121 = C184-C13 = C177-C13
 1.5 with sigma of 0.02
 C198-C141 = C141-C140 = C174-C140
 1.5 with sigma of 0.02
 C294-C113
 1.5 with sigma of 0.02
 C193-C125
 1.5 with sigma of 0.02
 C184-C0AA
 2.5 with sigma of 0.04
 C121-C13
 2.5 with sigma of 0.04
 C184-C177
 2.5 with sigma of 0.04
 C294-C154
 2.5 with sigma of 0.04
 C193-C82
 2.5 with sigma of 0.04
 C183-C125
 2.5 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
Uanis(C99) \\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C177) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C160) \\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: Br29(0.33333)
4.a Fitted hexagon refined as free rotating group:
 C3(C18,C58,C79,C78,C90), C6(C27,C66,C80,C104,C122), C16(C23,C31,C65,C115,
 C136), C43(C34,C63,C98,C95,C84), C52(C55,C68,C134,C160,C77), C149(C112,C57,C45,
 C110,C114), C179(C14,C47,C119,C129,C38)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'