New atomically precise M1Ag21 (M = Au/Ag) nanoclusters as excellent oxygen reduction reaction catalysts
Zou, Xuejuan; He, Shuping; Kang, Xi; Chen, Shuang; Yu, Haizhu; Jin, Shan; Astruc, Didier; Zhu, Manzhou; Chemical Science 12 (2021) 3660–3667; doi:10.1039/D0SC05923D

data_1559983
_publ_section_title
;
 New atomically precise M1Ag21 (M = Au/Ag) nanoclusters as excellent
 oxygen reduction reaction catalysts
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3660
_journal_page_last               3667
_journal_paper_doi               10.1039/D0SC05923D
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety
'C222 H264 Ag22 Fe3 P6 S12, 2(C24 H20 B), 3(C7 H8), C7 H5'
_chemical_formula_sum            'C298 H333 Ag22 B2 Fe3 P6 S12'
_chemical_formula_weight         7047.47
_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             2019-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-14 deposited with the CCDC.	2021-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                79.1230(10)
_cell_angle_beta                 70.4930(10)
_cell_angle_gamma                66.9560(10)
_cell_formula_units_Z            2
_cell_length_a                   21.4120(2)
_cell_length_b                   27.2727(3)
_cell_length_c                   29.7612(3)
_cell_measurement_reflns_used    185704
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.39
_cell_measurement_theta_min      3.49
_cell_volume                     15040.9(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            155377
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         67.000
_diffrn_reflns_theta_min         3.476
_exptl_absorpt_coefficient_mu    13.755
_exptl_absorpt_correction_T_max  0.2646
_exptl_absorpt_correction_T_min  0.0448
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       block
_exptl_crystal_F_000             7050
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.376
_refine_diff_density_min         -2.145
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3031
_refine_ls_number_reflns         52178
_refine_ls_number_restraints     7192
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0741
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+198.1240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1974
_refine_ls_wR_factor_ref         0.2054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                43400
_reflns_number_total             52178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05923d2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1559982--1559983.cif.'
_cod_original_cell_volume        15041.0(3)
_cod_database_code               1559983
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.546
_shelx_estimated_absorpt_t_min   0.340
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C53-C08R = C53-C0AA = C22-C0AA = C49-C0AA = C56-C49 = C56-C24 = C59-C56 = C59-
 C08R
 1.45 with sigma of 0.01
 C22-C07C = C08Q-C07C = C24-C07C
 1.5 with sigma of 0.05
 C23-C08M
 1.45 with sigma of 0.01
 C26-C07W = C26-C08N = C08N-C089 = C23-C089
 1.45 with sigma of 0.01
 C23-C089
 1.45 with sigma of 0.01
3. Restrained planarity
 C56, C0AA, C59, C53
 with sigma of 0.1
 C085, C088, C08C, C08J, C08T, C08Y, C12
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C018 \\sim C019 \\sim C01A \\sim C01B \\sim C01C \\sim C01D \\sim C01E \\sim
C01F \\sim C01G \\sim C01H \\sim C01I \\sim C01J \\sim C01K \\sim C01L \\sim
C01M \\sim C01N \\sim C01O \\sim C01P \\sim C01Q \\sim C01R \\sim C01S \\sim
C01T \\sim C01U \\sim C01V \\sim C01W \\sim C01X \\sim C01Y \\sim C01Z \\sim
C020 \\sim C021 \\sim C022 \\sim C023 \\sim C024 \\sim C025 \\sim C026 \\sim
C027 \\sim C028 \\sim C029 \\sim C02A \\sim C02B \\sim C02C \\sim C02D \\sim
C02E \\sim C02F \\sim C02G \\sim C02H \\sim C02I \\sim C02J \\sim C02K \\sim
C02L \\sim C02M \\sim C02N \\sim C02O \\sim C02P \\sim C02Q \\sim C02R \\sim
C02S \\sim C02T \\sim C02U \\sim C02V \\sim C02W \\sim C02X \\sim C02Y \\sim
C02Z \\sim C030 \\sim C031 \\sim C032 \\sim C033 \\sim C034 \\sim C035 \\sim
C036 \\sim C037 \\sim C038 \\sim C039 \\sim C03A \\sim C03B \\sim C03C \\sim
C03D \\sim C03E \\sim C03F \\sim C03G \\sim C03H \\sim C03I \\sim C03J \\sim
C03K \\sim C03L \\sim C03M \\sim C03N \\sim C03O \\sim C03P \\sim C03Q \\sim
C03R \\sim C03S \\sim C03T \\sim C03U \\sim C03V \\sim C03W \\sim C03X \\sim
C03Y \\sim C03Z \\sim C040 \\sim C041 \\sim C042 \\sim C043 \\sim C044 \\sim
C045 \\sim C046 \\sim C047 \\sim C048 \\sim C049 \\sim C04A \\sim C04B \\sim
C04C \\sim C04D \\sim C04E \\sim C04F \\sim C04G \\sim C04H \\sim C04I \\sim
C04J \\sim C04K \\sim C04L \\sim C04M \\sim C04N \\sim C04O \\sim C04P \\sim
C04Q \\sim C04R \\sim C04S \\sim C04T \\sim C04U \\sim C04V \\sim C04W \\sim
C04X \\sim C04Y \\sim C04Z \\sim C050 \\sim C051 \\sim C052 \\sim C053 \\sim
C054 \\sim C055 \\sim C056 \\sim C057 \\sim C058 \\sim C059 \\sim C05A \\sim
C05B \\sim C05C \\sim C05D \\sim C05E \\sim C05F \\sim C05G \\sim C05H \\sim
C05I \\sim C05J \\sim C05K \\sim C05L \\sim C05M \\sim C05N \\sim C05O \\sim
C05P \\sim C05Q \\sim C05R \\sim C05S \\sim C05T \\sim C05U \\sim C05V \\sim
C05W \\sim C05X \\sim C05Y \\sim C05Z \\sim C060 \\sim C061 \\sim C062 \\sim
C063 \\sim C064 \\sim C065 \\sim C066 \\sim C067 \\sim C068 \\sim C069 \\sim
C06A \\sim C06B \\sim C06C \\sim C06D \\sim C06E \\sim C06F \\sim C06G \\sim
C06H \\sim C06I \\sim C06J \\sim C06K \\sim C06L \\sim C06M \\sim C06N \\sim
C06O \\sim C06P \\sim C06Q \\sim C06R \\sim C06S \\sim C06T \\sim C06U \\sim
C06V \\sim C06W \\sim C06X \\sim C06Y \\sim C070 \\sim C071 \\sim C072 \\sim
C073 \\sim C074 \\sim C075 \\sim C076 \\sim C077 \\sim C078 \\sim C079 \\sim
C07A \\sim C07B \\sim C07C \\sim C07D \\sim C07E \\sim C07F \\sim C07G \\sim
C07H \\sim C07I \\sim C07J \\sim C07K \\sim C07L \\sim C07M \\sim C07N \\sim
C07O \\sim C07P \\sim C07R \\sim C07S \\sim C07T \\sim C07U \\sim C07V \\sim
C07W \\sim C07X \\sim C07Y \\sim C07Z \\sim C080 \\sim C081 \\sim C083 \\sim
C084 \\sim C085 \\sim C086 \\sim C087 \\sim C088 \\sim C089 \\sim C08A \\sim
C08B \\sim C08C \\sim C08D \\sim C08E \\sim C08F \\sim C08G \\sim C08J \\sim
C08K \\sim C08M \\sim C08N \\sim C08O \\sim C08Q \\sim C08R \\sim C08T \\sim
C08U \\sim C08W \\sim C08Y \\sim C08Z \\sim C090 \\sim C6 \\sim C7 \\sim C2
\\sim C0AA \\sim C11 \\sim C13 \\sim C19 \\sim C18 \\sim C5 \\sim C15 \\sim C12
\\sim C16 \\sim C46 \\sim C68 \\sim C72 \\sim C57 \\sim C69 \\sim C22 \\sim C23
\\sim C24 \\sim C26 \\sim C27 \\sim C49 \\sim C53 \\sim C56 \\sim C59 \\sim
C70: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C01H(H01J), C01X(H01X), C02I(H02Q), C02K(H02S), C032(H032), C039(H039),
 C03L(H03L), C03M(H03M), C03T(H03T), C03V(H03V), C046(H046), C04K(H04N),
 C04P(H04T), C052(H052), C056(H056), C05F(H05P), C05L(H05T), C05O(H05V),
 C05Y(H05Z), C060(H060), C061(H061), C06C(H06G), C071(H071), C072(H072),
 C073(H073), C078(H078), C07D(H07F), C07I(H07J), C07T(H07T), C07V(H07V),
 C07W(H07W), C080(H080), C08N(H08N), C08R(H08R), C0AA(H0AB), C23(H23), C56(H56)
5.b Secondary CH2 refined with riding coordinates:
 C018(H01A,H01B), C01B(H01C,H01D), C01C(H01E,H01F), C01G(H01H,H01I), C01M(H01N,
 H01O), C01N(H01P,H01Q), C01W(H01S,H01V), C022(H02A,H02B), C028(H02C,H02D),
 C02D(H02H,H02I), C02E(H02J,H02K), C02F(H02L,H02M), C02H(H02O,H02P), C02N(H02V,
 H02W), C02U(H02,H), C02W(H1AA,HA), C02Y(H2AA,HB), C030(H03A,H03B), C03A(H03C,
 H03D), C03G(H03F,H03G), C03R(H03J,H03P), C03W(H03Q,H03R), C049(H04A,H04B),
 C04C(H04D,H04E), C04D(H04F,H04G), C04J(H04L,H04M), C04M(H04P,H04Q), C04N(H04R,
 H04S), C04Q(H04U,H04V), C04T(H04Y,HC), C04U(H04Z,HD), C04X(H4AA,HE), C04Y(H5AA,
 HF), C050(H05A,H05B), C053(H05C,H05D), C054(H05E,H05F), C055(H05G,H05H),
 C059(H05I,H05J), C05A(H05K,H05L), C05E(H05N,H05O), C05X(H05Y,HG), C062(H06A,
 H06B), C069(H06C,H06D), C06J(H06K,H06L), C06K(H06M,H06N), C06M(H06P,H06Q),
 C06O(H06R,H06S), C06R(H06T,H06U), C06S(H06V,H06W), C06U(H06Y,HH), C06Y(H06Z,
 HI), C070(H07A,H07B), C076(H07C,H07D), C07G(H07G,H07H), C07J(H07K,H07L),
 C07K(H07M,H07N), C07S(H07R,H07S), C07X(H07U,H07X), C07Z(H07Y,HJ), C081(H08A,
 H08B), C089(H08C,H08D), C08F(H08E,H08F), C08K(H08G,H08H), C08M(H08I,H08J),
 C08O(H08K,H08L), C08Q(H08M,H08O), C22(H22A,H22B), C24(H24A,H24B), C26(H26A,
 H26B), C49(H49A,H49B), C53(H53A,H53B), C59(H59A,H59B)
5.c Aromatic/amide H refined with riding coordinates:
 C019(H019), C01D(H01G), C01I(H01K), C01K(H01L), C01L(H01M), C01R(H01R),
 C01T(H01T), C01U(H01U), C01V(H01W), C01Y(H01Y), C023(H023), C027(H027),
 C02A(H02E), C02B(H02F), C02C(H02G), C02G(H02N), C02J(H02R), C02L(H02T),
 C02M(H02U), C02O(H02X), C02P(H7AA), C02Q(H02Y), C02S(H02Z), C02V(H0AA),
 C02Z(H3AA), C035(H035), C037(H037), C038(H038), C03E(H03E), C03F(H03W),
 C03H(H03H), C03I(H03I), C03J(H03Y), C03K(H03K), C03N(H03N), C03O(H03O),
 C03S(H03S), C03U(H03U), C03X(H03X), C03Z(H03Z), C040(H040), C041(H041),
 C042(H042), C044(H044), C045(H045), C047(H047), C048(H048), C04A(H04C),
 C04E(H04H), C04F(H8BA), C04G(H04I), C04H(H04J), C04I(H04K), C04L(H04O),
 C04R(H04W), C04S(H04X), C04V(H9BA), C04W(H04), C04Z(H6AA), C051(H051),
 C057(H057), C058(H058), C05B(H05M), C05C(H0CA), C05G(H8AA), C05H(H05Q),
 C05I(H05R), C05J(H05S), C05M(H05U), C05P(H9AA), C05Q(H1CA), C05R(H05W),
 C05S(H0BA), C05T(H05X), C05U(H1BA), C05V(H2BA), C05W(H3BA), C063(H063),
 C064(H064), C066(H066), C067(H067), C068(H068), C06A(H06E), C06B(H06F),
 C06D(H06H), C06E(H06I), C06F(H06), C06G(H2CA), C06H(H06J), C06L(H06O),
 C06N(H4BA), C06P(H3CA), C06Q(H4CA), C06T(H06X), C06V(H5BA), C06W(H5CA),
 C06X(H6BA), C074(H074), C075(H075), C077(H077), C079(H079), C08E(H08T),
 C08W(H08W), C6(H6), C08B(H08U), C07A(H07E), C07B(H07Z), C07E(H07), C07F(H6CA),
 C07H(H07I), C07L(H7BA), C07M(H07O), C07N(H7CA), C07O(H07P), C07P(H07Q),
 C07R(H8CA), C086(H086), C087(H087), C08A(H08P), C08D(H08Q), C08G(H08S),
 C088(H088), C085(H085), C08C(H08), C08J(H9CA), C08Y(H0DA), C08Z(H08Z), C7(H7),
 C083(H083), C05N(H05), C084(H084), C090(H090), C11(H11), C13(H13), C5(H5),
 C15(H15), C46(H46), C68(H68), C72(H72), C57(H57), C69(H69), C27(H27), C70(H70)
5.d Fitted hexagon refined as free rotating group:
 C079(C08E,C08W,C6,C08B,C07Y), C08T(C088,C085,C08C,C08J,C08Y), C7(C083,C05D,
 C05N,C084,C090), C11(C13,C19,C18,C5,C15), C16(C46,C68,C72,C57,C69)
5.e Idealised Me refined as rotating group:
 C08U(H08V,H08X,H08Y), C2(H2A,H2B,H2C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              36625
_shelx_fab_checksum              53184
_olex2_submission_special_instructions 'No special instructions were received'