Stepwise construction of Ag<sub>29</sub> nanocluster-based hydrogen evolution electrocatalysts.
Shen, Honglei; Zhu, Qingtao; Xu, Jiawei; Ni, Kun; Wei, Xiao; Du, Yuanxin; Gao, Shan; Kang, Xi; Zhu, Manzhou; Nanoscale 15 (2023) 14941–14948; doi:10.1039/d3nr03537a

data_1569762
_publ_section_title
;
 Stepwise construction of Ag<sub>29</sub> nanocluster-based hydrogen
 evolution electrocatalysts.
;
_journal_issue                   36
_journal_name_full               Nanoscale
_journal_page_first              14941
_journal_page_last               14948
_journal_paper_doi               10.1039/d3nr03537a
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C108 H78 Ag28 P2 Pt S36, 4(C24 H20 P)'
_chemical_formula_sum            'C204 H158 Ag28 P6 Pt S36'
_chemical_formula_weight         7164.72
_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   geom
_audit_creation_date             2022-05-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-12-15 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.3153(2)
_cell_length_b                   21.4400(2)
_cell_length_c                   37.3504(3)
_cell_measurement_reflns_used    134152
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.41
_cell_measurement_theta_min      4.29
_cell_volume                     24838.1(3)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
 2242 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            80478
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        62.499
_diffrn_reflns_theta_max         62.499
_diffrn_reflns_theta_min         4.749
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    21.799
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13768
_refine_diff_density_max         4.210
_refine_diff_density_min         -3.582
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1125
_refine_ls_number_reflns         19213
_refine_ls_number_restraints     2028
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0838
_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^)+(0.1765P)^2^+469.4580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2300
_refine_ls_wR_factor_ref         0.2420
_reflns_d_resolution_high        0.821
_reflns_d_resolution_low         9.313
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              13
_reflns_limit_h_min              -36
_reflns_limit_k_max              24
_reflns_limit_k_min              -25
_reflns_limit_l_max              45
_reflns_limit_l_min              -42
_reflns_number_gt                57417
_reflns_number_total             90277
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d3nr03537a2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments          'Adding full bibliography for 1569762.cif.'
_cod_database_code               1569762
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 P1-C49
 1.8 with sigma of 0.01
 P1-C17
 1.8 with sigma of 0.01
 P1-C49 = P1-C2AA = P1-C17 = P1-C4
 1.81 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
C026 \\sim C48 \\sim C105 \\sim C76 \\sim C0AA \\sim C02U: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C028 \\sim C02R \\sim C78 \\sim C95 \\sim C98 \\sim C02W: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C024 \\sim C027 \\sim C02B \\sim C02S \\sim C02Z \\sim C20 \\sim C02P \\sim
C02N \\sim C02V \\sim C031 \\sim C033 \\sim C8: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 3.8A
C036 \\sim C035 \\sim C01Z \\sim C012 \\sim C01F \\sim C02Q: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C01T \\sim C029 \\sim C01W \\sim C01X \\sim C016 \\sim C01A: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C02C \\sim C01D \\sim C01Q \\sim C02G \\sim C021 \\sim C02J: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C022 \\sim C02K \\sim C02X \\sim C02A \\sim C020 \\sim C02D: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C01R \\sim C01Y \\sim C025 \\sim C02F \\sim C02I \\sim C02O: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C01N \\sim C01J \\sim C018 \\sim C011 \\sim C014 \\sim C01B: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
P1 \\sim C4 \\sim C7 \\sim C32 \\sim C33 \\sim C47 \\sim C92 \\sim C96 \\sim
C17 \\sim C132 \\sim C131 \\sim C140 \\sim C31 \\sim C29 \\sim C49 \\sim C75
\\sim C93 \\sim C16 \\sim C141 \\sim C11 \\sim C2AA \\sim C119 \\sim C3AA \\sim
C61 \\sim C1AA: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
Uanis(C026) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C76)
\\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C02U) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C028) \\sim Ueq, Uanis(C02R) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C95)
\\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C02W) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C024) \\sim Ueq, Uanis(C027) \\sim Ueq, Uanis(C02B) \\sim Ueq,
Uanis(C02S) \\sim Ueq, Uanis(C02Z) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C02P)
\\sim Ueq, Uanis(C02N) \\sim Ueq, Uanis(C02V) \\sim Ueq, Uanis(C031) \\sim Ueq,
Uanis(C033) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C035) \\sim Ueq, Uanis(C01Z) \\sim Ueq, Uanis(C012) \\sim Ueq,
Uanis(C01F) \\sim Ueq, Uanis(C02Q) \\sim Ueq, Uanis(C036) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01A) \\sim Ueq, Uanis(C016) \\sim Ueq, Uanis(C01X) \\sim Ueq,
Uanis(C01W) \\sim Ueq, Uanis(C029) \\sim Ueq, Uanis(C01T) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C02C) \\sim Ueq, Uanis(C01D) \\sim Ueq, Uanis(C01Q) \\sim Ueq,
Uanis(C02G) \\sim Ueq, Uanis(C021) \\sim Ueq, Uanis(C02J) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C022) \\sim Ueq, Uanis(C02K) \\sim Ueq, Uanis(C02X) \\sim Ueq,
Uanis(C02A) \\sim Ueq, Uanis(C020) \\sim Ueq, Uanis(C02D) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01R) \\sim Ueq, Uanis(C01Y) \\sim Ueq, Uanis(C025) \\sim Ueq,
Uanis(C02F) \\sim Ueq, Uanis(C02I) \\sim Ueq, Uanis(C02O) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01B) \\sim Ueq, Uanis(C014) \\sim Ueq, Uanis(C011) \\sim Ueq,
Uanis(C018) \\sim Ueq, Uanis(C01J) \\sim Ueq, Uanis(C01N) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(P1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C1AA)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C92) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C132)
\\sim Ueq, Uanis(C131) \\sim Ueq, Uanis(C140) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C29) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C93)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C141) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C2AA) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C61)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C011(H011), C01J(H01J), C01B(H01B), C013(H013), C016(H016), C017(H017),
 C019(H019), C01E(H01E), C01I(H01I), C01K(H01K), C01O(H01O), C01Q(H01Q),
 C01T(H01T), C01V(H01V), C01W(H01W), C01Y(H01Y), C021(H021), C02K(H02K),
 C02X(H02X), C02A(H02A), C020(H020), C02D(H02D), C023(H023), C025(H025),
 C48(H48), C105(H105), C76(H76), C0AA(H0AA), C02U(H02U), C027(H027), C02S(H02S),
  C02Z(H02Z), C20(H20), C02P(H02P), C028(H028), C78(H78), C95(H95), C98(H98),
 C02W(H02W), C02C(H02C), C02F(H02F), C02G(H02G), C02I(H02I), C02J(H02J),
 C02N(H02N), C02O(H02O), C02V(H02V), C031(H031), C033(H033), C035(H035),
 C012(H012), C02Q(H02Q), C7(H7), C1AA(H1AA), C32(H32), C33(H33), C47(H47),
 C92(H92), C96(H96), C132(H132), C131(H131), C140(H140), C8(H8), C31(H31),
 C29(H29), C75(H75), C93(H93), C16(H16), C141(H141), C11(H11), C119(H119),
 C3AA(H3AA), C61(H61)
3.b Fitted hexagon refined as free rotating group:
 C011(C018,C01J,C01N,C01B,C014), C022(C02K,C02X,C02A,C020,C02D), C026(C48,C105,
 C76,C0AA,C02U), C027(C02B,C02S,C02Z,C20,C02P), C028(C02R,C78,C95,C98,C02W),
 C036(C035,C01Z,C012,C01F,C02Q), C4(C7,C1AA,C32,C33,C47), C92(C96,C17,C132,C131,
 C140), C31(C29,C49,C75,C93,C16), C141(C11,C2AA,C119,C3AA,C61)
3.c Idealised tetrahedral OH refined as rotating group:
 S00U(H00U), S00V(H00V), S00W(H00W), S00X(H00X), S00Y(H00Y), S010(H010)
;
_olex2_submission_special_instructions 'No special instructions were received'