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_4125393
_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         'C252 H286 Ag38 F52 P8 S26, 4(C H2 Cl2)'
_chemical_formula_sum            'C256 H294 Ag38 Cl8 F52 P8 S26'
_chemical_formula_weight         9822.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.9564(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.5229(2)
_cell_length_b                   22.1084(2)
_cell_length_c                   30.7227(3)
_cell_measurement_reflns_used    42937
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.1480
_cell_measurement_theta_min      3.5310
_cell_volume                     15630.8(3)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -71.00   21.25   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9299   57.0000  120.0000 123

  2 omega  -47.00   28.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9299   38.0000  -90.0000 100

  3 omega -116.00   -8.75   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9299  -77.0000  -30.0000 143

  4 omega   22.00   92.50   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9299 -124.0000 -116.0000 94

  5 omega -102.00  -36.00   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   15.0000  120.0000 88

  6 omega   31.00   87.25   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000   30.0000 75

  7 omega   37.00   93.25   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -45.0000  -90.0000 75

  8 omega   29.00  140.00   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -77.0000    0.0000 148

  9 omega   34.00   90.25   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000  -30.0000 75

 10 omega   34.00  105.25   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -94.0000  -60.0000 95

 11 omega   72.00  109.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940 -125.0000 -150.0000 50

 12 omega   53.00  177.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940   15.0000  -30.0000 166

 13 omega   57.00   84.00   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000    0.0000 36

 14 omega   38.00   85.25   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -45.0000   90.0000 63

 15 omega   95.00  120.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940 -125.0000   90.0000 34

 16 omega   34.00   93.25   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -45.0000 -180.0000 79
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0157459000
_diffrn_orient_matrix_UB_12      0.0646918000
_diffrn_orient_matrix_UB_13      -0.0119557000
_diffrn_orient_matrix_UB_21      0.0125334000
_diffrn_orient_matrix_UB_22      0.0172701000
_diffrn_orient_matrix_UB_23      0.0496324000
_diffrn_orient_matrix_UB_31      0.0638626000
_diffrn_orient_matrix_UB_32      -0.0193198000
_diffrn_orient_matrix_UB_33      0.0043010000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            84044
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        61.169
_diffrn_reflns_theta_max         61.169
_diffrn_reflns_theta_min         3.319
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.891
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12613
_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            'metallic blackish'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_density_diffrn    2.087
_exptl_crystal_description       block
_exptl_crystal_F_000             9512
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.492
_refine_diff_density_min         -3.611
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1686
_refine_ls_number_reflns         23785
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+294.1549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20245
_reflns_number_total             23785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10053_si_002.cif
_cod_data_source_block           '[Ag38(SPhF2)26(PnBu3)8]'
_cod_depositor_comments
'Adding full bibliography for 4125391--4125393.cif.'
_cod_original_cell_volume        15630.9(3)
_cod_database_code               4125393
_reflns_odcompleteness_completeness 98.59
_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
 P3-C107
 1.8 with sigma of 0.02
 C108-P3
 2.6 with sigma of 0.02
 C108-C107
 1.5 with sigma of 0.02
 C108-C109
 1.5 with sigma of 0.02
 C110-C109
 1.5 with sigma of 0.02
 C109-C107
 2.5 with sigma of 0.02
 C108-C110
 2.5 with sigma of 0.02
 Cl3-C128
 1.8 with sigma of 0.02
 Cl4-C128
 1.8 with sigma of 0.02
 Cl4-Cl3
 2.9 with sigma of 0.02
 C88-C87 = C89-C88 = C90-C89
 1.5 with sigma of 0.02
 C87-C89
 2.5 with sigma of 0.02
 C90-C88
 2.5 with sigma of 0.02
 C98-C97
 1.5 with sigma of 0.02
 C94-C93
 1.5 with sigma of 0.02
 C122-C121
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C89, C90
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C89, C88
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C109, C110
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C97 \\sim C96 \\sim C98: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C9) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C94) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C97)
\\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C89) \\sim Ueq,
Uanis(C90) \\sim Ueq, Uanis(C126) \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(C109)
\\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C108) \\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(C9) = Uanis(C94) = Uanis(C93) = Uanis(C126) = Uanis(C109) = Uanis(C110)
5. Others
 Sof(F7A)=1-FVAR(1)
 Sof(F7)=FVAR(1)
 Sof(F4A)=1-FVAR(2)
 Sof(F4)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C119(H11A,H11B), C123(H12A,H12B), C115(H11C,H11D), C111(H11E,H11F), C112(H11G,
 H11H), C80(H80A,H80B), C103(H10A,H10B), C79(H79A,H79B), C113(H11I,H11J),
 C91(H91A,H91B), C120(H12C,H12D), C104(H10C,H10D), C84(H84A,H84B), C124(H12E,
 H12F), C92(H92A,H92B), C117(H11N,H11O), C83(H83A,H83B), C99(H99A,H99B),
 C81(H81A,H81B), C87(H87A,H87B), C116(H11S,H11T), C100(H10E,H10F), C101(H10G,
 H10H), C121(H12G,H12H), C125(H12I,H12J), C105(H10L,H10M), C85(H85A,H85B),
 C88(H88A,H88B), C97(H97A,H97B), C93(H93A,H93B), C89(H89A,H89B), C127(H12Q,
 H12R), C107(H10Q,H10R), C108(H10S,H10T), C109(H10U,H10V), C128(H12S,H12T)
6.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C20(H20), C78(H78), C44(H44), C36(H36), C38(H38), C74(H74),
 C42(H42), C45(H45), C39(H39), C26(H26), C6(H6), C14(H14), C32(H32), C77(H77),
 C30(H30), C18(H18), C5(H5), C33(H33), C54(H54), C53(H53), C50(H50), C2(H2),
 C56(H56), C24(H24), C60(H60), C17(H17), C29(H29), C57(H57), C95(H95), C65(H65),
  C66(H66), C62(H62), C69(H69), C68(H68), C72(H72), C96(H96), C8(H8), C12(H12)
6.c Fitted hexagon refined as free rotating group:
 C49(C54,C53,C52,C51,C50), C63(C64,C65,C66,C61,C62), C70(C69,C68,C67,C72,C71),
 C11(C10,C9,C8,C7,C12)
6.d Idealised Me refined as rotating group:
 C114(H11K,H11L,H11M), C118(H11P,H11Q,H11R), C82(H82A,H82B,H82C), C106(H10I,
 H10J,H10K), C86(H86A,H86B,H86C), C122(H12K,H12L,H12M), C90(H90A,H90B,H90C),
 C102(H10N,H10O,H10P), C94(H94A,H94B,H94C), C126(H12N,H12O,H12P), C98(H98A,H98B,
 H98C), C110(H11U,H11V,H11W)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'