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_1570364
_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         'C132 H110 Ni11 S22, 2(C H2 Cl2)'
_chemical_formula_sum            'C134 H114 Cl4 Ni11 S22'
_chemical_formula_weight         3217.18
_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   mixed
_audit_creation_date             2022-08-11
_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                90
_cell_angle_beta                 99.45(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.984(4)
_cell_length_b                   28.994(6)
_cell_length_c                   28.216(6)
_cell_measurement_reflns_used    11717
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      70.311
_cell_measurement_theta_min      4.404
_cell_volume                     15320(6)
_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      273.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45301
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.311
_diffrn_reflns_theta_min         4.404
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.190
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       needle
_exptl_crystal_F_000             6584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.526
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         13994
_refine_ls_number_restraints     1166
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0681
_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^)+(0.1438P)^2^+53.3916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2096
_refine_ls_wR_factor_ref         0.2183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11717
_reflns_number_total             13994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr05328h2.cif
_cod_data_source_block           Ni11
_cod_depositor_comments
'Adding full bibliography for 1570364--1570367.cif.'
_cod_database_code               1570364
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.625
_shelx_estimated_absorpt_t_min   0.305
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1-Cl1
 1.63 with sigma of 0.02
 C1-Cl00
 1.63 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C00K \\sim C2 \\sim C00L \\sim C3 \\sim C00M \\sim C4 \\sim C00O \\sim C5 \\sim
C00P \\sim C6 \\sim C016 \\sim C7 \\sim C028 \\sim C8 \\sim C02G \\sim C01R
\\sim C00Q \\sim 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 C018 \\sim C019 \\sim C01A \\sim C01B \\sim C01D \\sim C01E \\sim C01F
\\sim C01G \\sim C01H \\sim C01I \\sim C01K \\sim C01L \\sim C01M \\sim C01O
\\sim C01P \\sim C01Q \\sim C01S \\sim C01T \\sim C01U \\sim C01V \\sim C01W
\\sim C01Y \\sim C01Z \\sim C020 \\sim C023 \\sim C024 \\sim C025 \\sim C026
\\sim C029 \\sim C02A \\sim C02B \\sim C02C \\sim C02D \\sim C02E \\sim C02H
\\sim C02I \\sim C1 \\sim C02K: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
4. Others
 Fixed Sof: Cl1(0.5) Cl00(0.5) C1(0.5) H1A(0.5) H1B(0.5) H02F(0.5) H02J(0.5)
5.a Riding coordinates:
 C02K(H02F,H02J)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C00O(H00O), C5(H5), C6(H6), C016(H016), C7(H7), C028(H028),
 C8(H8), C02G(H02G), C01R(H01R), C00Q(H00Q), C00S(H00S), C00T(H00T), C00W(H00W),
  C00Y(H00Y), C010(H010), C013(H013), C014(H014), C018(H018), C019(H019),
 C01A(H01A), C01B(H01B), C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01G),
 C01H(H01H), C01I(H01I), C01K(H01K), C01L(H01L), C01M(H01M), C01O(H01O),
 C01P(H01P), C01Q(H01Q), C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V),
 C01W(H01W), C01Y(H01Y), C01Z(H01Z), C020(H020), C023(H023), C024(H024),
 C025(H025), C026(H026), C029(H029), C02A(H02A), C02B(H02B), C02C(H02C),
 C02D(H02D), C02E(H02E), C02H(H02H), C02I(H02I)
;
_shelx_res_checksum              40570
_shelx_fab_checksum              17860
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'