Diphosphine-protected ultrasmall gold nanoclusters: opened icosahedral Au<sub>13</sub> and heart-shaped Au<sub>8</sub> clusters.
Zhang, Shan-Shan; Feng, Lei; Senanayake, Ravithree D.; Aikens, Christine M.; Wang, Xing-Po; Zhao, Quan-Qin; Tung, Chen-Ho; Sun, Di; Chemical science 9 (2018) 1251–1258; doi:10.1039/c7sc03566g

data_1553988
_publ_section_title
;
 Diphosphine-protected ultrasmall gold nanoclusters: opened icosahedral
 Au<sub>13</sub> and heart-shaped Au<sub>8</sub> clusters.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1251
_journal_page_last               1258
_journal_paper_doi               10.1039/c7sc03566g
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C150 H132 Au13 P12, Cl, 4(F6 P), C6 H6'
_chemical_formula_sum            'C156 H138 Au13 Cl F24 P16'
_chemical_formula_weight         5560.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-10-02 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                86.3850(10)
_cell_angle_beta                 84.3990(10)
_cell_angle_gamma                84.4130(10)
_cell_formula_units_Z            2
_cell_length_a                   17.4438(3)
_cell_length_b                   19.0667(4)
_cell_length_c                   24.5099(4)
_cell_measurement_reflns_used    51282
_cell_measurement_temperature    93.00(10)
_cell_measurement_theta_max      30.6090
_cell_measurement_theta_min      3.2770
_cell_volume                     8062.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_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      93.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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     -1.00  68.00   0.50   30.00    --   -4.48  57.00 -60.00  138
  2  \w      7.00  35.00   0.50   30.00    --   -4.48  37.00-120.00   56
  3  \w    -36.00   0.00   0.50   30.00    --    5.65 -77.00-120.00   72
  4  \w    -24.00  38.00   0.50   30.00    --    5.65 -99.00 -60.00  124
  5  \w    -25.00  39.00   0.50   30.00    --    5.65 -99.00-150.00  128
  6  \w     -6.00  21.00   0.50   30.00    --    5.65  37.00  60.00   54
  7  \w     23.00  60.00   0.50   30.00    --    5.65  37.00  60.00   74
  8  \w     25.00  70.00   0.50   30.00    --   -4.48  19.00 120.00   90
  9  \w      0.00  25.00   0.50   30.00    --    5.65-112.00 172.00   50
 10  \w    -17.00  23.00   0.50   30.00    --   -4.48  19.00 120.00   80
 11  \w    -25.00  29.00   0.50   30.00    --   -4.48 -99.00 150.00  108
 12  \w    -25.00  37.00   0.50   30.00    --    5.65 -99.00  90.00  124
 13  \w    -63.00   7.00   0.50   30.00    --   -4.48 -37.00-180.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0269896000
_diffrn_orient_matrix_UB_12      -0.0087910000
_diffrn_orient_matrix_UB_13      0.0223432000
_diffrn_orient_matrix_UB_21      0.0300092000
_diffrn_orient_matrix_UB_22      -0.0037001000
_diffrn_orient_matrix_UB_23      0.0178109000
_diffrn_orient_matrix_UB_31      -0.0073831000
_diffrn_orient_matrix_UB_32      0.0361977000
_diffrn_orient_matrix_UB_33      0.0056190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            148622
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.331
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.027
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.290
_exptl_crystal_description       block
_exptl_crystal_F_000             5148
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.958
_refine_diff_density_min         -2.401
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1820
_refine_ls_number_reflns         32833
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+195.3347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25427
_reflns_number_total             32833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03566g2.cif
_cod_data_source_block           SD_Au3
_cod_database_code               1553988
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         AuCHPCl
_diffrn_oxdiff_ac3_digest_frames
;
0197e3a5f2eeabe51fe04cdc5432bc35ff0123883dd
;
_diffrn_oxdiff_ac3_digest_hkl
;
01a93112096161de4be8024f6f0bb12c930e32
;
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F17-F16
 2.3 with sigma of 0.01
 P15-F17
 1.55 with sigma of 0.01
 F15-P15
 1.55 with sigma of 0.01
 P16-F24 = F18-P15
 1.55 with sigma of 0.01
 F13-P15
 1.55 with sigma of 0.01
 F13-F15
 2.3 with sigma of 0.01
 F21-F20
 2.3 with sigma of 0.01
 F21-F23
 2.3 with sigma of 0.02
 F21-P16
 1.55 with sigma of 0.01
 F22-F21
 2.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
P15 \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17 \\sim F18: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.08
C151 \\sim C152 \\sim C153 \\sim C154 \\sim C155 \\sim C156: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.08
C27 \\sim C26 \\sim C31 \\sim C30 \\sim C29 \\sim C28: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C26 \\sim C27 \\sim C28 \\sim C30 \\sim C31 \\sim C29: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C32 \\sim C37 \\sim C36 \\sim C35 \\sim C34 \\sim C33: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
4. Others
 Fixed Sof: Cl1(0.65) Cl1A(0.35)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C50(H50A,H50B), C63(H63A,H63B), C88(H88A,H88B), C113(H11A,
 H11B), C144(H14A,H14B)
5.b 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), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40),
  C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59),
  C60(H60), C61(H61), C62(H62), C65(H65), C66(H66), C67(H67), C68(H68),
 C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C77(H77), C78(H78),
  C79(H79), C80(H80), C81(H81), C83(H83), C84(H84), C85(H85), C86(H86),
 C87(H87), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96), C97(H97),
  C98(H98), C99(H99), C100(H100), C102(H102), C103(H103), C104(H104),
 C105(H105), C106(H106), C108(H108), C109(H109), C110(H110), C111(H111),
 C112(H112), C115(H115), C116(H116), C117(H117), C118(H118), C119(H119),
 C121(H121), C122(H122), C123(H123), C124(H124), C125(H125), C127(H127),
 C128(H128), C129(H129), C130(H130), C131(H131), C133(H133), C134(H134),
 C135(H135), C136(H136), C137(H137), C139(H139), C140(H140), C141(H141),
 C142(H142), C143(H143), C146(H146), C147(H147), C148(H148), C149(H149),
 C150(H150), C151(H151), C152(H152), C153(H153), C154(H154), C155(H155),
 C156(H156)
;
_shelx_res_checksum              58385
_shelx_fab_checksum              21340
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.684
_oxdiff_exptl_absorpt_empirical_full_min 0.691