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_1570365
_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         'C140 H140 Ni10 S20, 0.25(C8 O4)'
_chemical_formula_sum            'C142 H140 Ni10 O S20'
_chemical_formula_weight         3090.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-09-16
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.4478(13)
_cell_length_b                   30.2351(16)
_cell_length_c                   48.070(3)
_cell_measurement_reflns_used    5669
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      69.925
_cell_measurement_theta_min      3.647
_cell_volume                     34079(3)
_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      273.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_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  0.0778
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            60663
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.925
_diffrn_reflns_theta_min         3.647
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.760
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_correction_T_min  0.466
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             12800
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7980
_refine_ls_number_restraints     1044
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0940P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5669
_reflns_number_total             7980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr05328h2.cif
_cod_data_source_block           Ni10
_cod_depositor_comments
'Adding full bibliography for 1570364--1570367.cif.'
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               1570365
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.398
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C3
 1.42 with sigma of 0.02
 C3-C2
 1.51 with sigma of 0.02
 O2-C2
 2.37 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O2 \\sim C3 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 3.8A
4. Rigid body (RIGU) restrains
 O2, C3, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O2(0.25) C3(0.25) C2(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C009(H009), C00D(H00D), C00F(H00F), C00I(H00I), C00J(H00J), C00K(H00K),
 C00L(H00L), C00M(H00M), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R),
 C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00Z(H00Z), C010(H010),
 C011(H011), C012(H012)
6.b Idealised Me refined as rotating group:
 C00Y(H00A,H00B,H00C), C014(H01A,H01B,H01C), C015(H01D,H01E,H01F), C016(H01G,
 H01H,H01I), C018(H01J,H01K,H01L)
;
_shelx_res_checksum              86812
_shelx_fab_checksum              5594
_olex2_submission_special_instructions 'No special instructions were received'