Cd<sub>12</sub>Ag<sub>32</sub>(SePh)<sub>36</sub>: Non-Noble Metal Doped Silver Nanoclusters.
Bootharaju, Megalamane S.; Chang, Hogeun; Deng, Guocheng; Malola, Sami; Baek, Woonhyuk; Häkkinen, Hannu; Zheng, Nanfeng; Hyeon, Taeghwan; Journal of the American Chemical Society 141 (2019) 8422–8425; doi:10.1021/jacs.9b03257

data_4127271
_publ_section_title
;
 Cd<sub>12</sub>Ag<sub>32</sub>(SePh)<sub>36</sub>: Non-Noble Metal Doped
 Silver Nanoclusters.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8422
_journal_page_last               8425
_journal_paper_doi               10.1021/jacs.9b03257
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C216 H180 Ag32 Cd12 Se36'
_chemical_formula_sum            'C216 H180 Ag32 Cd12 Se36'
_chemical_formula_weight         10418.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                88.3916(13)
_cell_angle_beta                 86.2435(13)
_cell_angle_gamma                85.6543(15)
_cell_formula_units_Z            2
_cell_length_a                   19.2821(4)
_cell_length_b                   19.3677(4)
_cell_length_c                   34.7903(5)
_cell_measurement_reflns_used    34009
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      64.5660
_cell_measurement_theta_min      3.4830
_cell_volume                     12923.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.847
_diffrn_measured_fraction_theta_max 0.999
_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    -59.00  33.00   1.00   12.50    --  -40.57  57.00   0.00   92
  2  \w    -62.00  28.00   1.00   12.50    --  -40.57  37.00 -90.00   90
  3  \w    -54.00  33.00   1.00   12.50    --  -40.57  57.00 120.00   87
  4  \w     65.00 167.00   1.00   36.00    --   89.29  30.00  60.00  102
  5  \w     42.00 118.00   1.00   36.00    --   89.29-125.00  90.00   76
  6  \w     95.00 124.00   1.00   36.00    --   89.29 125.00 150.00   29
  7  \w     58.00 112.00   1.00   36.00    --   89.29-125.00 -30.00   54
  8  \w     32.00 103.00   1.00   36.00    --   89.29 -30.00-120.00   71
  9  \w     73.00 116.00   1.00   36.00    --   89.29  30.00 150.00   43
 10  \w    120.00 167.00   1.00   36.00    --   89.29  30.00 150.00   47
 11  \w    111.00 163.00   1.00   36.00    --   89.29 125.00   0.00   52
 12  \w     15.00  41.00   1.00   36.00    --   89.29 -61.00 -90.00   26
 13  \w     59.00 108.00   1.00   36.00    --   89.29 -61.00 -90.00   49
 14  \w     63.00 103.00   1.00   36.00    --   89.29-125.00-120.00   40
 15  \w     34.00 119.00   1.00   36.00    --   89.29 -30.00  90.00   85
 16  \w     11.00 116.00   1.00   36.00    --   89.29 -77.00  90.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0475436000
_diffrn_orient_matrix_UB_12      0.0510958000
_diffrn_orient_matrix_UB_13      0.0161877000
_diffrn_orient_matrix_UB_21      -0.0642600000
_diffrn_orient_matrix_UB_22      0.0494336000
_diffrn_orient_matrix_UB_23      0.0108361000
_diffrn_orient_matrix_UB_31      -0.0075203000
_diffrn_orient_matrix_UB_32      -0.0362291000
_diffrn_orient_matrix_UB_33      0.0398859000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.847
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            81562
_diffrn_reflns_point_group_measured_fraction_full 0.847
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         61.169
_diffrn_reflns_theta_min         3.366
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    32.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear blackish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.677
_exptl_crystal_description       block
_exptl_crystal_F_000             9560
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.175
_refine_diff_density_min         -2.080
_refine_diff_density_rms         0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2617
_refine_ls_number_reflns         39636
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+320.3164P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33741
_reflns_number_total             39636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03257_si_002.cif
_cod_data_source_block           Ag32Cd12
_cod_depositor_comments          'Adding full bibliography for 4127271.cif.'
_cod_database_code               4127271
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C118) \\sim Ueq,
Uanis(C117) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C111) \\sim Ueq,
Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C141) \\sim Ueq, Uanis(C140) \\sim Ueq, Uanis(C143) \\sim Ueq,
Uanis(C144) \\sim Ueq, Uanis(C142) \\sim Ueq, Uanis(C139) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C82) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C76) \\sim Ueq,
Uanis(C75) \\sim Ueq, Uanis(C193) \\sim Ueq, Uanis(C198) \\sim Ueq, Uanis(C196)
\\sim Ueq, Uanis(C197) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C146) \\sim Ueq,
Uanis(C147) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C71)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C148) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C212) \\sim Ueq, Uanis(C211) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C195) \\sim Ueq, Uanis(C69) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C77) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C78) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C78(H78), C74(H74),
  C75(H75), C76(H76), C77(H77), C80(H80), C81(H81), C82(H82), C83(H83),
 C84(H84), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93),
  C94(H94), C95(H95), C96(H96), C98(H98), C99(H99), C100(H100), C101(H101),
 C102(H102), C104(H104), C105(H105), C106(H106), C107(H107), C108(H108),
 C110(H110), C111(H111), C112(H112), C113(H113), C114(H114), C116(H116),
 C117(H117), C118(H118), C119(H119), C120(H120), C122(H122), C123(H123),
 C124(H124), C125(H125), C126(H126), C128(H128), C129(H129), C130(H130),
 C131(H131), C132(H132), C134(H134), C135(H135), C136(H136), C137(H137),
 C138(H138), C140(H140), C144(H144), C143(H143), C142(H142), C141(H141),
 C146(H146), C147(H147), C148(H148), C149(H149), C150(H150), C152(H152),
 C153(H153), C154(H154), C155(H155), C156(H156), C158(H158), C159(H159),
 C160(H160), C161(H161), C162(H162), C164(H164), C165(H165), C166(H166),
 C167(H167), C168(H168), C170(H170), C171(H171), C172(H172), C173(H173),
 C174(H174), C176(H176), C177(H177), C178(H178), C179(H179), C180(H180),
 C182(H182), C183(H183), C184(H184), C185(H185), C186(H186), C187(H187),
 C188(H188), C189(H189), C190(H190), C191(H191), C198(H198), C197(H197),
 C196(H196), C195(H195), C194(H194), C200(H200), C201(H201), C202(H202),
 C203(H203), C204(H204), C206(H206), C207(H207), C208(H208), C209(H209),
 C210(H210), C212(H212), C213(H213), C214(H214), C215(H215), C216(H216)
3.b Fitted hexagon refined as free rotating group:
 C78(C73,C74,C75,C76,C77), C79(C80,C81,C82,C83,C84), C140(C139,C144,C143,C142,
 C141), C193(C198,C197,C196,C195,C194)
;
_shelx_res_checksum              73041
_shelx_hkl_checksum              51190
_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 2.287
_oxdiff_exptl_absorpt_empirical_full_min 0.521