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_1570367
_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         'C108 H90 Pd9 S18, 2(C H2 Cl2)'
_chemical_formula_sum            'C110 H94 Cl4 Pd9 S18'
_chemical_formula_weight         3092.33
_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                73.147(4)
_cell_angle_beta                 85.831(5)
_cell_angle_gamma                88.799(5)
_cell_formula_units_Z            2
_cell_length_a                   15.4893(15)
_cell_length_b                   17.1391(16)
_cell_length_c                   27.979(3)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      53.61
_cell_measurement_theta_min      2.34
_cell_volume                     7089.8(12)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.979
_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  0.0819
_diffrn_reflns_av_unetI/netI     0.0983
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            67310
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.503
_diffrn_reflns_theta_min         1.241
_diffrn_source_current           2.86
_diffrn_source_power             0.1993706
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.491
_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    1.449
_exptl_crystal_description       needle
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.200
_refine_diff_density_min         -1.799
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.00041(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1223
_refine_ls_number_reflns         25851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1555
_refine_ls_R_factor_gt           0.0987
_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^)+(0.1539P)^2^+79.0054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2794
_refine_ls_wR_factor_ref         0.3172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15040
_reflns_number_total             25851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr05328h2.cif
_cod_data_source_block           yy_sq
_cod_depositor_comments
'Adding full bibliography for 1570364--1570367.cif.'
_cod_database_code               1570367
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.663
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C01J) = Uanis(C02D) = Uanis(C041) = Uanis(C04F) = Uanis(C04B) =
Uanis(C043) = Uanis(C04G)
3.a Secondary CH2 refined with riding coordinates:
 C02B(H02B,H02D), C03V(H03B,H03H)
3.b Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C011(H011), C013(H013), C017(H017), C018(H018), C019(H019),
 C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F), C01H(H01H), C01I(H01I),
 C01J(H01J), C01K(H01K), C01M(H01M), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C01U(H01U), C01V(H01V), C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020),
 C021(H021), C022(H022), C023(H023), C024(H024), C026(H026), C028(H028),
 C029(H029), C02A(H02A), C02C(H02C), C02F(H02F), C02G(H02G), C02H(H02H),
 C02J(H02J), C02K(H02K), C02L(H02L), C02N(H02N), C02O(H02O), C02P(H02P),
 C02Q(H02Q), C02R(H02R), C02S(H02S), C02T(H02T), C02U(H02U), C02W(H02W),
 C02X(H02X), C02Z(H02Z), C030(H030), C031(H031), C032(H032), C033(H033),
 C035(H035), C036(H036), C038(H038), C039(H039), C03A(H03A), C03C(H03C),
 C03D(H03D), C03E(H03E), C03F(H03F), C03G(H03G), C03I(H03I), C03J(H03J),
 C03K(H03K), C03M(H03M), C03O(H03O), C03P(H03P), C03Q(H03Q), C03R(H03R),
 C03S(H03S), C03T(H03T), C03U(H03U), C03W(H03W), C03Y(H03Y), C03Z(H03Z),
 C040(H040), C042(H042), C044(H044), C045(H045), C048(H048), C04A(H04A),
 C04C(H04C), C043(H043), C04G(H04G), C041(H041), C04F(H04F), C04B(H04B)
3.c Fitted hexagon refined as free rotating group:
 C043(C04G,C02D,C041,C04F,C04B)
;
_shelx_res_checksum              11172
_shelx_fab_checksum              63970
_olex2_submission_special_instructions 'No special instructions were received'