PtAg<sub>18</sub> superatoms costabilized by phosphines and halides: synthesis, structure, and catalysis.
Wang, Meng; Wang, Lin; Wu, Haoyuan; Sun, Jing; Xu, Xiaoxuan; Guo, Shuo; Jia, Yanyuan; Li, Simin; Guan, Zong-Jie; Shen, Hui; Nanoscale 15 (2023) 17818–17824; doi:10.1039/d3nr02196c

data_1569733
_publ_section_title
;
 PtAg<sub>18</sub> superatoms costabilized by phosphines and halides:
 synthesis, structure, and catalysis.
;
_journal_issue                   44
_journal_name_full               Nanoscale
_journal_page_first              17818
_journal_page_last               17824
_journal_paper_doi               10.1039/d3nr02196c
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C162 H158 Ag18 Cl8 P12 Pt, 2(F6 Sb)'
_chemical_formula_sum            'C162 H158 Ag18 Cl8 F12 P12 Pt Sb2'
_chemical_formula_weight         5368.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-14 deposited with the CCDC.	2023-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.714(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4557(4)
_cell_length_b                   30.7351(6)
_cell_length_c                   37.4768(10)
_cell_measurement_reflns_used    9063
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      64.9190
_cell_measurement_theta_min      3.7180
_cell_volume                     18783.0(8)
_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)'
_computing_structure_solution    'ShelXT (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 0.849
_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    -77.00  36.00   1.00    2.50    --  -42.73  19.00 150.00  113
  2  \w   -115.00 -30.00   1.00    2.50    --  -42.73 -37.00 -30.00   85
  3  \w    -83.00 -13.00   1.00    2.50    --  -42.73 125.00-180.00   70
  4  \w     80.00 160.00   1.00    5.00    --   88.62  45.00 -30.00   80
  5  \w    106.00 146.00   1.00    5.00    --   88.62  61.00-180.00   40
  6  \w    111.00 159.00   1.00    5.00    --   88.62 106.00-134.00   48
  7  \w    112.00 145.00   1.00    5.00    --   88.62 125.00 120.00   33
  8  \w     66.00 139.00   1.00    5.00    --   88.62  30.00 -60.00   73
  9  \w     31.00 120.00   1.00    5.00    --   88.62 -77.00 -90.00   89
 10  \w    115.00 158.00   1.00    5.00    --   88.62 125.00 -60.00   43
 11  \w     67.00 138.00   1.00    5.00    --   88.62  45.00  60.00   71
 12  \w     23.00  98.00   1.00    5.00    --   88.62-125.00-180.00   75
 13  \w     73.00 111.00   1.00    5.00    --   88.62-125.00 120.00   38
 14  \w    130.00 159.00   1.00    5.00    --   88.62 125.00-180.00   29
 15  \w     23.00 118.00   1.00    5.00    --   88.62-125.00 -90.00   95
;
_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      -0.0269472000
_diffrn_orient_matrix_UB_12      0.0104320000
_diffrn_orient_matrix_UB_13      -0.0400563000
_diffrn_orient_matrix_UB_21      0.0605443000
_diffrn_orient_matrix_UB_22      0.0384209000
_diffrn_orient_matrix_UB_23      0.0025659000
_diffrn_orient_matrix_UB_31      0.0673387000
_diffrn_orient_matrix_UB_32      -0.0304314000
_diffrn_orient_matrix_UB_33      -0.0105127000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_Laue_measured_fraction_full 0.849
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            58253
_diffrn_reflns_point_group_measured_fraction_full 0.849
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         61.168
_diffrn_reflns_theta_min         3.420
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.723
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35813
_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_density_diffrn    1.898
_exptl_crystal_description       block
_exptl_crystal_F_000             10320
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.503
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.303
_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     933
_refine_ls_number_reflns         14428
_refine_ls_number_restraints     657
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0826
_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^)+(0.1431P)^2^+796.4240P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2206
_refine_ls_wR_factor_ref         0.2627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9531
_reflns_number_total             14428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr02196c2.cif
_cod_data_source_block           xl-2-2200925-f-cord
_cod_depositor_comments          'Adding full bibliography for 1569733.cif.'
_cod_database_code               1569733
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C00S, C00T, C00U, C00V, C00W, C00X, C00Y, C00Z, C010, C011, C012, C013, C014,
 C015, C016, C017, C018, C01I, C02G, C8, C17, C02F, C019, C01A, C01B, C01C,
 C01D, C01E, C01F, C01G, C01H, C01J, C01K, C01L, C01M, C01N, C01O, C01P, C01Q,
 C01R, C01S, C01T, C01U, C01V, C01W, C01X, C01Y, C13, C1AA, C18, C24, C5, C01Z,
 C020, C021, C022, C023, C024, C02A, C7, C0AA, C19, C02J, C025, C026, C027,
 C028, C029, C02B, C02C, C02D, C02E, C02H, C02I, C02L, C02M, C4, C6, C9, C11,
 C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C00S \\sim C00T \\sim C00U \\sim C00V \\sim C00W \\sim C00X \\sim C00Y \\sim
C00Z \\sim C010 \\sim C011 \\sim C012 \\sim C013 \\sim C014 \\sim C015 \\sim
C016 \\sim C017 \\sim C018 \\sim C01I \\sim C02G \\sim C8 \\sim C17 \\sim C02F
\\sim C019 \\sim C01A \\sim C01B \\sim C01C \\sim C01D \\sim C01E \\sim C01F
\\sim C01G \\sim C01H \\sim C01J \\sim C01K \\sim C01L \\sim C01M \\sim C01N
\\sim C01O \\sim C01P \\sim C01Q \\sim C01R \\sim C01S \\sim C01T \\sim C01U
\\sim C01V \\sim C01W \\sim C01X \\sim C01Y \\sim C13 \\sim C1AA \\sim C18
\\sim C24 \\sim C5 \\sim C01Z \\sim C020 \\sim C021 \\sim C022 \\sim C023 \\sim
C024 \\sim C02A \\sim C7 \\sim C0AA \\sim C19 \\sim C02J \\sim C025 \\sim C026
\\sim C027 \\sim C028 \\sim C029 \\sim C02B \\sim C02C \\sim C02D \\sim C02E
\\sim C02H \\sim C02I \\sim C02L \\sim C02M \\sim C4 \\sim C6 \\sim C9 \\sim
C11 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C01I) \\sim Ueq, Uanis(C02G) \\sim Ueq, Uanis(C02F) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C024) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C00T(H00A,H00B), C00U(H00C,H00D), C00V(H00E,H00F), C011(H01A,H01B), C013(H01C,
 H01D), C016(H01E,H01F), C017(H01G,H01H), C01B(H01K,H01L), C01U(H01X,H01Y),
 C02I(H02I,H02K)
4.b Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C00X(H00X), C00Y(H00Y), C010(H010), C012(H012), C014(H014),
 C015(H015), C01I(H01I), C02G(H02G), C8(H8), C17(H17), C02F(H02F), C01A(H01J),
 C01C(H01M), C01D(H01N), C01F(H01O), C01G(H01P), C01H(H01Q), C01J(H01R),
 C01K(H01S), C01L(H01T), C01N(H01U), C01O(H01V), C01Q(H01W), C01V(H01Z),
 C01W(H01), C01X(H0AA), C13(H13), C1AA(H1AA), C18(H18), C24(H24), C5(H5),
 C01Z(H2AA), C020(H020), C021(H021), C022(H022), C023(H023), C02A(H02A), C7(H7),
  C0AA(H0AB), C19(H19), C02J(H02J), C025(H025), C026(H026), C027(H027),
 C028(H028), C029(H029), C02B(H02B), C02C(H02C), C02D(H02D), C02E(H02E),
 C02H(H02H), C02L(H02L), C02M(H02M), C4(H4), C6(H6), C9(H9), C11(H11), C16(H16)
4.c Fitted hexagon refined as free rotating group:
 C018(C01I,C02G,C8,C17,C02F), C01Y(C13,C1AA,C18,C24,C5), C024(C02A,C7,C0AA,C19,
 C02J)
;
_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 2.380
_oxdiff_exptl_absorpt_empirical_full_min 0.660