Improved activity for the oxygen evolution reaction using a tiara-like thiolate-protected nickel nanocluster.
Funaki, Sota; Kawawaki, Tokuhisa; Okada, Tomoshige; Takemae, Kana; Hossain, Sakiat; Niihori, Yoshiki; Naito, Takumi; Takagi, Makito; Shimazaki, Tomomi; Kikkawa, Soichi; Yamazoe, Seiji; Tachikawa, Masanori; Negishi, Yuichi; Nanoscale 15 (2023) 5201–5208; doi:10.1039/d2nr06952k

data_1568460
_publ_section_title
;
 Improved activity for the oxygen evolution reaction using a tiara-like
 thiolate-protected nickel nanocluster.
;
_journal_issue                   11
_journal_name_full               Nanoscale
_journal_page_first              5201
_journal_page_last               5208
_journal_paper_doi               10.1039/d2nr06952k
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C80 H90 Ni5 S10, C Cl2'
_chemical_formula_sum            'C81 H90 Cl2 Ni5 S10'
_chemical_formula_weight         1748.57
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-13 deposited with the CCDC.	2023-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                61.5700(10)
_cell_angle_beta                 70.3550(10)
_cell_angle_gamma                68.3270(10)
_cell_formula_units_Z            2
_cell_length_a                   16.3158(3)
_cell_length_b                   17.0494(3)
_cell_length_c                   17.7725(4)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      3.42
_cell_volume                     3961.72(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.921
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37197
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.374
_diffrn_reflns_theta_min         2.741
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.540
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0389 before and 0.0294 after correction.
The Ratio of minimum to maximum transmission is 0.9376.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.876
_refine_diff_density_min         -2.047
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     880
_refine_ls_number_reflns         13420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0098P)^2^+8.8218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12411
_reflns_number_total             13420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr06952k2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 1568460.cif.'
_cod_original_cell_volume        3961.73(14)
_cod_database_code               1568460
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: C3(0.5) C1(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C00I(H00A,H00B), C00K(H00C,H00D), C00L(H00E,H00F), C00M(H00G,H00H), C00N(H00I,
 H00J), C00P(H00K,H00L), C00W(H00M,H00N), C00X(H00P,H00Q), C00Y(H00R,H00S),
 C00Z(H00U,H00V), C010(H01A,H01B), C012(H01C,H01D), C015(H01E,H01F), C019(H01G,
 H01H), C01D(H01L,H01M), C01E(H01N,H01O), C01L(H01V,H01W), C01U(H4,H),
 C021(H02A,H02B), C02L(H02Q,H02R)
3.b Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00T(H00T), C013(H013), C014(H014), C02E(H02E), C02N(H02N),
 C02P(H02P), C02O(H02O), C02I(H02I), C018(H018), C01A(H01I), C01B(H01J),
 C01C(H01K), C01F(H01P), C01G(H01Q), C01H(H01R), C01I(H01S), C01J(H01T),
 C01K(H01U), C01M(H01X), C01O(H01Y), C01P(H01Z), C01Q(H01), C01R(H1), C01S(H2),
 C01T(H3), C01V(H5), C01W(H6), C01X(H7), C01Y(H8), C01Z(H9), C020(H020),
 C022(H022), C023(H023), C024(H024), C025(H025), C026(H026), C027(H027),
 C028(H028), C029(H029), C02A(H02C), C02B(H02D), C02C(H02F), C02D(H02G),
 C02F(H02H), C02G(H02J), C02H(H02K), C02J(H02L), C02K(H02M), C02M(H02S)
3.c Fitted hexagon refined as free rotating group:
 C017(C02E,C02N,C02P,C02O,C02I)
;
_shelx_res_checksum              90164
_olex2_submission_special_instructions 'No special instructions were received'