One-step preparation of Pt/Ag nanoclusters for CO<sub>2</sub> transformation.
Wang, Meng; Li, Simin; Tang, Xiongkai; Zuo, Dongjie; Jia, Yanyuan; Guo, Shuo; Guan, Zong-Jie; Shen, Hui; Physical chemistry chemical physics : PCCP 25 (2023) 30373–30380; doi:10.1039/d3cp02736h

data_7247522
_publ_section_title
;
 One-step preparation of Pt/Ag nanoclusters for CO<sub>2</sub>
 transformation.
;
_journal_issue                   44
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              30373
_journal_page_last               30380
_journal_paper_doi               10.1039/d3cp02736h
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C126 H84 Ag9 Br21 Cl3 P7 Pt1, C18 H12 Br3 P1'
_chemical_formula_sum            'C144 H96 Ag9 Br24 Cl3 P8 Pt'
_chemical_formula_weight         5264.07
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-28 deposited with the CCDC.	2023-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.1020(3)
_cell_length_b                   19.1020(3)
_cell_length_c                   90.1075(13)
_cell_measurement_reflns_used    11556
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      62.1640
_cell_measurement_theta_min      2.6960
_cell_volume                     28474.1(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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    -94.00  -8.00   0.50    1.00    --  -33.39 -66.00 137.00  172
  2  \w    -69.00  37.00   0.50    1.00    --  -33.39  66.00 -88.00  212
  3  \w    123.00 150.00   0.50    1.00    --   92.84  66.00 -88.00   54
  4  \w     28.00  73.00   0.50    1.00    --   92.84 -66.00 137.00   90
  5  \w     68.00 118.00   0.50    1.00    --   92.84  66.00 -88.00  100
  6  \w   -162.00 -93.00   0.50    1.00    --  -95.65 -66.00 137.00  138
  7  \w    -92.00 -66.00   0.50    1.00    --  -95.65 -66.00 137.00   52
  8  \w    -71.00 -46.00   0.50    1.00    --  -95.65  66.00 -88.00   50
  9  \w     74.00 113.00   0.50    1.00    --   30.58 178.00 120.00   78
 10  \w     53.00 113.00   0.50    1.00    --   30.58 178.00-180.00  120
 11  \w    -60.00  27.00   0.50    1.00    --   30.58 -19.00 150.00  174
 12  \w    -40.00 -14.00   0.50    1.00    --   30.58 -66.00 137.00   52
 13  \w      4.00  98.00   0.50    1.00    --   30.58  66.00 -88.00  188
 14  \w     43.00  69.00   0.50    1.00    --   30.58 -99.00   0.00   52
 15  \w      7.00  37.00   0.50    1.00    --   30.58 -99.00   0.00   60
 16  \w    -86.00 -43.00   0.50    1.00    --  -33.39-178.00 -60.00   86
 17  \w     -6.00  47.00   0.50    1.00    --  -33.39  19.00  60.00  106
 18  \w     25.00  72.00   0.50    1.00    --   92.84 -61.00   0.00   94
 19  \w      8.00  36.00   0.50    1.00    --   92.84 -30.00 120.00   56
 20  \w    110.00 143.00   0.50    1.00    --   92.84 178.00 150.00   66
 21  \w      4.00  37.00   0.50    1.00    --   92.84 -30.00 150.00   66
 22  \w      7.00  37.00   0.50    1.00    --   92.84 -30.00 -90.00   60
 23  \w     56.00  82.00   0.50    1.00    --   92.84 178.00 150.00   52
 24  \w      4.00  37.00   0.50    1.00    --   92.84 -30.00-180.00   66
 25  \w     11.00  37.00   0.50    1.00    --   92.84 -30.00 -30.00   52
 26  \w    136.00 171.00   0.50    1.00    --   92.84 111.00 120.00   70
 27  \w     93.00 133.00   0.50    1.00    --   92.84 111.00 120.00   80
 28  \w      4.00  37.00   0.50    1.00    --   92.84 -30.00   0.00   66
 29  \w     22.00  48.00   0.50    1.00    --   92.84 -61.00  30.00   52
 30  \w     10.00 105.00   0.50    1.00    --   92.84-111.00 -90.00  190
 31  \w      6.00  36.00   0.50    1.00    --   92.84 -30.00  30.00   60
 32  \w     16.00  73.00   0.50    1.00    --   92.84 -61.00 -60.00  114
 33  \w     39.00  67.00   0.50    1.00    --   92.84 -61.00 -90.00   56
 34  \w     12.00 102.00   0.50    1.00    --   92.84 -95.00 120.00  180
 35  \w     97.00 171.00   0.50    1.00    --   92.84 111.00-150.00  148
 36  \w      7.00 105.00   0.50    1.00    --   92.84 -95.00 -90.00  196
 37  \w      9.00  34.00   0.50    1.00    --   92.84 -45.00   0.00   50
 38  \w     67.00 101.00   0.50    1.00    --   92.84 -77.00 120.00   68
 39  \w      4.00  37.00   0.50    1.00    --   92.84 -30.00 -60.00   66
 40  \w     91.00 170.00   0.50    1.00    --   92.84 111.00 -90.00  158
 41  \w    -47.00 -21.00   0.50    1.00    --  -95.65  45.00  90.00   52
 42  \w   -108.00 -59.00   0.50    1.00    --  -95.65 111.00  60.00   98
 43  \w    -49.00 -24.00   0.50    1.00    --  -95.65  45.00-120.00   50
 44  \w    -43.00 -18.00   0.50    1.00    --  -95.65  45.00  60.00   50
 45  \w   -169.00-100.00   0.50    1.00    --  -95.65-111.00  60.00  138
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0594515000
_diffrn_orient_matrix_UB_12      0.0025660000
_diffrn_orient_matrix_UB_13      0.0118475000
_diffrn_orient_matrix_UB_21      0.0135628000
_diffrn_orient_matrix_UB_22      0.0821996000
_diffrn_orient_matrix_UB_23      0.0054882000
_diffrn_orient_matrix_UB_31      -0.0704649000
_diffrn_orient_matrix_UB_32      -0.0435884000
_diffrn_orient_matrix_UB_33      0.0110385000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       104
_diffrn_reflns_limit_l_min       -90
_diffrn_reflns_number            88547
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        64.563
_diffrn_reflns_theta_max         64.563
_diffrn_reflns_theta_min         2.716
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.871
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light red'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_description       block
_exptl_crystal_F_000             14832
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.979
_refine_diff_density_min         -1.249
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         10537
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+23.5852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7779
_reflns_number_total             10537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp02736h2.cif
_cod_data_source_block           w1-20230303-ptag-p28_auto
_cod_depositor_comments          'Adding full bibliography for 7247522.cif.'
_cod_original_cell_volume        28474.0(10)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7247522
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pt Ag P C'
_shelx_estimated_absorpt_t_max   0.742
_shelx_estimated_absorpt_t_min   0.647
_reflns_odcompleteness_completeness 99.99
_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. Rigid bond restraints
 C01H, C01K, Br00, C01E, C019, C01U, C01Q, C01T, Br2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Br00 \\sim Br2: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
Uanis(C01H) \\sim Ueq, Uanis(C01K) \\sim Ueq, Uanis(Br00) \\sim Ueq,
Uanis(C01E) \\sim Ueq, Uanis(C019) \\sim Ueq, Uanis(C01U) \\sim Ueq,
Uanis(C01Q) \\sim Ueq, Uanis(C01T) \\sim Ueq, Uanis(Br2) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 Br00, C01K, C01H, C01E, C019, C013
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00L(H00L), C00N(H00N), C00O(H00O), C00Q(H00Q), C00R(H00R),
 C00S(H00S), C00T(H00T), C00V(H00V), C00X(H00X), C00Y(H00Y), C00Z(H00Z),
 C011(H011), C013(H013), C015(H015), C016(H016), C018(H018), C019(H019),
 C01C(H01C), C01D(H01D), C01E(H01E), C01G(H01G), C01H(H01H), C01I(H01I),
 C01J(H01J), C01L(H01L), C01M(H01M), C01N(H01N), C01P(H01P), C01S(H01S),
 C01T(H01T), C01U(H01U)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.410
_oxdiff_exptl_absorpt_empirical_full_min 0.727