Photochemical synthesis of group 10 metal nanoclusters for electrocatalysis.
Fan, Ji-Qiang; Cen, Kehui; Xu, Hua-Jun; Wang, Hai-Yang; Yang, Ying; Zhu, Ze-Min; Liu, Hao; Chen, Dengyu; Fan, Weigang; Li, Man-Bo; Nanoscale 15 (2023) 19079–19084; doi:10.1039/d3nr05328h

data_1570366
_publ_section_title
;
 Photochemical synthesis of group 10 metal nanoclusters for
 electrocatalysis.
;
_journal_issue                   47
_journal_name_full               Nanoscale
_journal_page_first              19079
_journal_page_last               19084
_journal_paper_doi               10.1039/d3nr05328h
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C120 H100 Pd10 S20, C Cl2'
_chemical_formula_sum            'C121 H100 Cl2 Pd10 S20'
_chemical_formula_weight         3330.10
_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             2022-09-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-09-05 deposited with the CCDC.	2023-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                64.679(4)
_cell_angle_beta                 77.271(4)
_cell_angle_gamma                69.706(5)
_cell_formula_units_Z            1
_cell_length_a                   15.8258(18)
_cell_length_b                   16.279(2)
_cell_length_c                   16.292(2)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.36
_cell_volume                     3545.7(8)
_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)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33637
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.602
_diffrn_reflns_theta_min         2.263
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.609
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       needle
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.508
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         16254
_refine_ls_number_restraints     1430
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0397P)^2^+7.7897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12714
_reflns_number_total             16254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr05328h2.cif
_cod_data_source_block           yy_sq_sq
_cod_depositor_comments
'Adding full bibliography for 1570364--1570367.cif.'
_cod_original_cell_volume        3545.6(8)
_cod_database_code               1570366
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.644
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-C1 = C5-C6 = C6-C7
 1.37 with sigma of 0.02
 C2-C7
 1.38 with sigma of 0.02
 C1-C4 = C4-C5
 1.36 with sigma of 0.02
 C2-C6
 2.38 with sigma of 0.04
 C1-C5
 2.36 with sigma of 0.04
 C2-C4 = C4-C6 = C5-C7
 2.37 with sigma of 0.04
 C2-C1 \\sim C1-C4 \\sim C4-C5 \\sim C5-C6 \\sim C6-C7 \\sim C7-C2
 with sigma of 0.02
 C2-C6 \\sim C2-C4 \\sim C6-C4 \\sim C5-C1 \\sim C5-C7 \\sim C7-C1
 with sigma of 0.04
3. Restrained planarity
 C2, C1, C4, C5, C6, C7
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C2 \\sim C1 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C00L \\sim C00N \\sim C00O \\sim C00P \\sim C00R \\sim C00S \\sim C00T \\sim
C00U \\sim C00V \\sim C00Y \\sim C00Z \\sim C010 \\sim C011 \\sim C012 \\sim
C014 \\sim C015 \\sim C016 \\sim C017 \\sim C019 \\sim C01A \\sim C01B \\sim
C01C \\sim C01D \\sim C01E \\sim C01F \\sim C01G \\sim C01H \\sim C01I \\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 C01Z \\sim C020 \\sim C021 \\sim C029 \\sim C024 \\sim C02B \\sim
C025 \\sim C013 \\sim C022 \\sim C023 \\sim C3 \\sim C7 \\sim C6 \\sim C5 \\sim
C4 \\sim C1 \\sim C2 \\sim C6A \\sim C7A \\sim C2A \\sim C1A \\sim C4A \\sim
C5A \\sim C9: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
Uanis(C6) = Uanis(C7) = Uanis(C5A) = Uanis(C7A)
Uanis(C013) = Uanis(C025) = Uanis(C02B)
Uanis(C00Z) = Uanis(C9)
5. Rigid body (RIGU) restrains
 C2, C1, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C7(0.5) C6(0.5) H6(0.5) C5(0.5) H5(0.5) C4(0.5) H4(0.5) C1(0.5)
 H1(0.5) C2(0.5) H2(0.5) C6A(0.5) H6A(0.5) C7A(0.5) C2A(0.5) H2A(0.5) C1A(0.5)
 H1A(0.5) C4A(0.5) H4A(0.5) C5A(0.5) H5A(0.5) C9(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00N(H00N), C00V(H00V), C00Z(H00Z), C010(H010), C011(H011),
 C012(H012), C014(H014), C015(H015), C016(H016), C017(H017), C019(H019),
 C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F),
 C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X),
 C01Z(H01Z), C020(H020), C021(H021), C029(H029), C024(H024), C02B(H02B),
 C025(H025), C022(H022), C023(H023), C6(H6), C5(H5), C4(H4), C1(H1), C2(H2),
 C6A(H6A), C2A(H2A), C1A(H1A), C4A(H4A), C5A(H5A)
7.b Fitted hexagon refined as free rotating group:
 C021(C029,C024,C02B,C025,C013), C7(C6,C5,C4,C1,C2), C6A(C7A,C2A,C1A,C4A,C5A)
;
_shelx_res_checksum              91961
_shelx_fab_checksum              1935
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'