[Au<sub>9</sub>Ag<sub>6</sub>(CCR)<sub>10</sub>(DPPM)<sub>2</sub>Cl<sub>2</sub>](PPh<sub>4</sub>): a four-electron cluster with a bi-decahedral twisted metal core.
Deng, Guocheng; Ki, Taeyoung; Yoo, Seungwoo; Liu, Xiaolin; Lee, Kangjae; Bootharaju, Megalamane S.; Hyeon, Taeghwan; Nanoscale 16 (2024) 11090–11095; doi:10.1039/d4nr01471e

data_1571586
_publ_section_title
;
 [Au<sub>9</sub>Ag<sub>6</sub>(C&#xe002;CR)<sub>10</sub>(DPPM)<sub>2</sub>Cl<sub>2</sub>](PPh<sub>4</sub>):
 a four-electron cluster with a bi-decahedral twisted metal core.
;
_journal_issue                   23
_journal_name_full               Nanoscale
_journal_page_first              11090
_journal_page_last               11095
_journal_paper_doi               10.1039/d4nr01471e
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C150 H74 Ag6 Au9 Cl2 F60 P4, C24 H20 P'
_chemical_formula_sum            'C174 H94 Ag6 Au9 Cl2 F60 P5'
_chemical_formula_weight         5970.15
_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             2022-11-10
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.09.11 svn.r3730fd0d for OlexSys, GUI svn.r6159)
;
_audit_update_record
;
2024-03-28 deposited with the CCDC.	2024-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                91.2230(10)
_cell_angle_beta                 94.2580(10)
_cell_angle_gamma                114.0090(10)
_cell_formula_units_Z            2
_cell_length_a                   19.1458(2)
_cell_length_b                   22.7805(4)
_cell_length_c                   23.8161(2)
_cell_measurement_reflns_used    44196
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.4450
_cell_measurement_theta_min      4.1970
_cell_volume                     9447.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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     -5.00  62.00   0.50   18.00    --   38.00  82.00  60.00  134
  2  \w     79.00 105.00   0.50   18.00    --   38.00  57.00 120.00   52
  3  \w    -51.00 127.00   0.50   18.00    --   38.00  38.00-180.00  356
  4  \w     12.00 119.00   0.50   18.00    --   38.00  77.00-180.00  214
  5  \w     -6.00  43.00   0.50   18.00    --   38.00  57.00 120.00   98
  6  \w     -9.00  34.00   0.50   18.00    --   38.00 -57.00-150.00   86
  7  \w     47.00  74.00   0.50   18.00    --   38.00  57.00 120.00   54
  8  \w    -17.00   8.00   0.50   18.00    --   38.00 -38.00-180.00   50
  9  \w    -20.00  71.00   0.50   18.00    --   38.00 -77.00 -90.00  182
 10  \w     37.00  87.00   0.50   18.00    --   38.00 -82.00 120.00  100
 11  \w    -48.00  69.00   0.50   18.00    --   38.00 -57.00 -90.00  234
 12  \w     -4.00  32.00   0.50   18.00    --   38.00  57.00-180.00   72
 13  \w     80.00 106.00   0.50   42.50    --  103.80 -82.00-180.00   52
 14  \w     21.00  56.00   0.50   42.50    --  103.80 -82.00   0.00   70
 15  \w     91.00 117.00   0.50   42.50    --  103.80 -82.00 120.00   52
 16  \w     47.00 135.00   0.50   42.50    --  103.80 -50.00  60.00  176
 17  \w     15.00 148.00   0.50   42.50    --  103.80 -63.00  60.00  266
 18  \w     58.00  84.00   0.50   42.50    --  103.80 -82.00 120.00   52
 19  \w     29.00  98.00   0.50   42.50    --  103.80 -82.00  30.00  138
 20  \w     14.00 112.00   0.50   42.50    --  103.80 -63.00-150.00  196
 21  \w     79.00 146.00   0.50   42.50    --  103.80 -82.00  90.00  134
 22  \w     20.00  46.00   0.50   42.50    --  103.80 -82.00 -30.00   52
 23  \w    117.00 145.00   0.50   42.50    --  103.80 -63.00-150.00   56
 24  \w    143.00 193.00   0.50   42.50    --  103.80 -12.00-150.00  100
 25  \w     81.00 107.00   0.50   42.50    --  103.80 -82.00 -60.00   52
 26  \w     14.00 152.00   0.50   42.50    --  103.80 -82.00-120.00  276
 27  \w    101.00 192.00   0.50   42.50    --  103.80 -12.00 -60.00  182
 28  \w     66.00  98.00   0.50   42.50    --  103.80 -82.00   0.00   64
 29  \w     29.00 122.00   0.50   42.50    --  103.80 -82.00  60.00  186
 30  \w     74.00 100.00   0.50   42.50    --  103.80 -82.00 150.00   52
 31  \w     83.00 109.00   0.50   42.50    --  103.80 -12.00-150.00   52
 32  \w     15.00  96.00   0.50   42.50    --  103.80 -12.00 -60.00  162
 33  \w     73.00 115.00   0.50   42.50    --  103.80  63.00 -90.00   84
 34  \w    127.00 152.00   0.50   42.50    --  103.80 -82.00-180.00   50
 35  \w     14.00  67.00   0.50   42.50    --  103.80 -12.00-150.00  106
 36  \w     31.00  56.00   0.50   42.50    --  103.80 -82.00 -60.00   50
 37  \w    100.00 139.00   0.50   42.50    --  103.80 -82.00-150.00   78
 38  \w     24.00 142.00   0.50   42.50    --  103.80 -82.00 -90.00  236
 39  \w    158.00 183.00   0.50   42.50    --  103.80  12.00-150.00   50
 40  \w     32.00 133.00   0.50   42.50    --  103.80  12.00-150.00  202
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0558486000
_diffrn_orient_matrix_UB_12      -0.0638860000
_diffrn_orient_matrix_UB_13      -0.0308767000
_diffrn_orient_matrix_UB_21      0.0458319000
_diffrn_orient_matrix_UB_22      0.0177419000
_diffrn_orient_matrix_UB_23      -0.0521936000
_diffrn_orient_matrix_UB_31      0.0510292000
_diffrn_orient_matrix_UB_32      -0.0331978000
_diffrn_orient_matrix_UB_33      0.0233116000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            92935
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.923
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.238
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.099
_exptl_crystal_description       block
_exptl_crystal_F_000             5560
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.486
_refine_diff_density_min         -2.753
_refine_diff_density_rms         0.289
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2293
_refine_ls_number_reflns         32753
_refine_ls_number_restraints     1593
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+206.7358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27041
_reflns_number_total             32753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr01471e2.cif
_cod_data_source_block           Au9Ag6
_cod_depositor_comments          'Adding full bibliography for 1571586.cif.'
_cod_database_code               1571586
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.700
_reflns_odcompleteness_completeness 98.33
_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
2. Restrained distances
 F36-C153
 1.28 with sigma of 0.01
 F57-C173
 1.3 with sigma of 0.01
 F60-C153
 1.28 with sigma of 0.01
 F4-C153
 1.28 with sigma of 0.01
 F32-C174
 1.3 with sigma of 0.01
 C174-C151
 1.5 with sigma of 0.01
 F2-C147
 1.3 with sigma of 0.01
 F55-C173
 1.3 with sigma of 0.01
 F47-C173
 1.3 with sigma of 0.01
 C173-C166
 1.48 with sigma of 0.01
 F36-F60
 2.15 with sigma of 0.01
 F58-F33
 2.15 with sigma of 0.01
 F57-F55
 2.1 with sigma of 0.01
 F47-F55
 2.15 with sigma of 0.01
 F47-F57
 2.15 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(F57) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C173) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F55) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C19(H19), C23(H23), C24(H24), C25(H25), C27(H27),
 C28(H28), C32(H32), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C53(H53),
 C56(H56), C57(H57), C60(H60), C62(H62), C64(H64), C67(H67), C68(H68), C69(H69),
  C71(H71), C72(H72), C73(H73), C74(H74), C76(H76), C78(H78), C79(H79),
 C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C87(H87), C88(H88),
  C89(H89), C90(H90), C91(H91), C92(H92), C93(H93), C97(H97), C99(H99),
 C100(H100), C101(H101), C102(H102), C103(H103), C105(H105), C106(H106),
 C108(H108), C110(H110), C111(H111), C114(H114), C117(H117), C118(H118),
 C119(H119), C120(H120), C121(H121), C122(H122), C124(H124), C125(H125),
 C126(H126), C127(H127), C128(H128), C131(H131), C132(H132), C137(H137),
 C139(H139), C145(H145), C148(H148), C154(H154), C155(H155), C156(H156),
 C157(H157), C158(H158), C159(H159), C165(H165), C168(H168), C169(H169),
 C170(H170), C171(H171)
4.c Fitted hexagon refined as free rotating group:
 C155(C156,C157,C158,C159,C160)
;
_platon_squeeze_void_probe_radius 1.20
_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 5.798
_oxdiff_exptl_absorpt_empirical_full_min 0.387