Heterogeneous metal alloy engineering: embryonic growth of M<sub>13</sub> icosahedra in Ag-based alloy superatomic nanoclusters.
Liu, Ying; Wang, Shuxin; Kang, Xi; Yin, Bing; Jin, Shan; Chen, Shuang; Zhu, Manzhou; Chemical communications (Cambridge, England) 56 (2020) 14203–14206; doi:10.1039/d0cc05575a

data_7127762
_publ_section_title
;
 Heterogeneous metal alloy engineering: embryonic growth of M<sub>13</sub>
 icosahedra in Ag-based alloy superatomic nanoclusters.
;
_journal_issue                   91
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14203
_journal_page_last               14206
_journal_paper_doi               10.1039/d0cc05575a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C280 H406 Ag48 Au3 Cl7 S28, 2(F6 Sb)'
_chemical_formula_sum            'C280 H406 Ag48 Au3 Cl7 F12 S28 Sb2'
_chemical_formula_weight         11158.01
_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             2019-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-09 deposited with the CCDC.	2020-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.9609(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.6940(5)
_cell_length_b                   29.9362(4)
_cell_length_c                   62.1774(9)
_cell_measurement_reflns_used    9673
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.66
_cell_measurement_theta_min      2.26
_cell_volume                     73396.4(17)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_unetI/netI     0.1114
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       78
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_number            440232
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.469
_exptl_absorpt_coefficient_mu    4.087
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0988 before and 0.0658 after correction.
The Ratio of minimum to maximum transmission is 0.8690.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_description       block
_exptl_crystal_F_000             42848
_refine_diff_density_max         11.817
_refine_diff_density_min         -6.544
_refine_diff_density_rms         0.421
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3746
_refine_ls_number_reflns         76000
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      3.235
_refine_ls_R_factor_all          0.1983
_refine_ls_R_factor_gt           0.1218
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3289
_refine_ls_wR_factor_ref         0.3725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                41310
_reflns_number_total             76000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05575a2.cif
_cod_data_source_block           20171119d_0ma_sq
_cod_database_code               7127762
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C9QA-C1SA
 1.55 with sigma of 0.02
 C9QA-C3RA
 1.55 with sigma of 0.02
 C9QA-C2RA
 1.55 with sigma of 0.02
 C1SA-C5UA
 1.55 with sigma of 0.02
 C0VA-C9UA
 1.55 with sigma of 0.02
 C9UA-C5UA
 1.55 with sigma of 0.02
 C5UA-C8UA
 1.55 with sigma of 0.02
 C8UA-C7UA
 1.55 with sigma of 0.02
 C7UA-C217
 1.55 with sigma of 0.02
 C217-C0VA
 1.55 with sigma of 0.02
 C2RA-C0VA
 1.55 with sigma of 0.02
 C3RA-C7UA
 1.55 with sigma of 0.02
 C3RA-C9QA
 1.55 with sigma of 0.02
 C2RA-C9QA
 1.55 with sigma of 0.02
 C1SA-C9QA
 1.55 with sigma of 0.02
 C2RA-C1SA
 2.55 with sigma of 0.02
 C2RA-C3RA
 2.55 with sigma of 0.02
 C3RA-C1SA
 2.55 with sigma of 0.02
 C217-C5UA
 3 with sigma of 0.02
 C0VA-C8UA
 3 with sigma of 0.02
 C9UA-C7UA
 3 with sigma of 0.02
 Sb2-F75
 1.815 with sigma of 0.01
 F21-F75
 2.63 with sigma of 0.01
 F75-F22
 2.345 with sigma of 0.01
 F9-F75
 2.602 with sigma of 0.01
 F7-F75
 2.563 with sigma of 0.01
 C3NA-C254
 1.5 with sigma of 0.01
 C7NA-C254
 1.5 with sigma of 0.01
 C9NA-C254
 1.5 with sigma of 0.01
 C68-C74
 1.55 with sigma of 0.01
 C1UA-C0UA
 1.55 with sigma of 0.01
 C3UA-C0UA
 1.55 with sigma of 0.01
 C5RA-C2SA
 1.55 with sigma of 0.01
 C9JA-C9TA
 1.55 with sigma of 0.01
 C9JA-C3VA
 1.55 with sigma of 0.01
 C9JA-C8TA
 1.55 with sigma of 0.01
 C9TA-C0UA
 1.55 with sigma of 0.01
 C0UA-C1UA
 1.55 with sigma of 0.01
 C1UA-C2UA
 1.55 with sigma of 0.01
 C2UA-C74
 1.55 with sigma of 0.01
 C74-C68
 1.55 with sigma of 0.01
 C68-C3UA
 1.55 with sigma of 0.01
 C3VA-C68
 1.55 with sigma of 0.01
 C3UA-C2UA
 3 with sigma of 0.01
 C1UA-C68
 3 with sigma of 0.01
 C74-C0UA
 3 with sigma of 0.01
 C3VA-C9TA
 2.52 with sigma of 0.01
 C9TA-C8TA
 2.52 with sigma of 0.01
 C8TA-C3VA
 2.52 with sigma of 0.01
 Sb4-F2
 1.85 with sigma of 0.02
 Sb4-F1AA
 1.85 with sigma of 0.02
 F2-F69
 2.5 with sigma of 0.02
 F2-F58
 2.5 with sigma of 0.02
 F1AA-F2
 2.5 with sigma of 0.02
 F2-F61
 2.5 with sigma of 0.02
 Sb3-F0AA
 1.81 with sigma of 0.02
 C0SA-C2SA
 2.447 with sigma of 0.01
 C2SA-C3SA
 2.636 with sigma of 0.01
3. Restrained planarity
 F13, F69, Sb4, F2, F58
 with sigma of 0.1
 F61, F13, Sb4, F2, F1AA
 with sigma of 0.1
 F0AA, Sb3, F78, F32, F95
 with sigma of 0.1
 C3SA, C4UA, C99, C2SA
 with sigma of 0.1
 C4UA, C3SA, C6UA, C0SA
 with sigma of 0.1
 C6UA, C0SA, C2SA, C99
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
S16 \\sim C9JA \\sim C3VA \\sim C9TA \\sim C8TA \\sim C2UA \\sim C74 \\sim C68
\\sim C3UA \\sim C0UA \\sim C1UA: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.0005
S28 \\sim C5RA \\sim C2SA \\sim C0SA \\sim C3SA \\sim C4UA \\sim C4NA \\sim
C6UA \\sim C75 \\sim C241 \\sim C99: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.0005
5. Others
 Sof(Ag)=1-FVAR(1)
 Sof(Ag55)=FVAR(1)
 Fixed Sof: Ag3(0.5) Ag0A(0.5) Ag1(0.5) S5(0.5) Ag66(0.5) S3(0.5) S2(0.5)
 S4(0.5) Sb1(0.5) Sb2(0.5) Sb3(0.5) Sb4(0.5) F11(0.5) F16(0.5) F35(0.5)
 F15(0.5) F20(0.5) F32(0.5) C9OA(0.5) F58(0.5) F61(0.5) F64(0.5) F66(0.5)
 F69(0.5) F71(0.5) F78(0.5) F95(0.5) C97(0.5) H97A(0.5) H97B(0.5) H0TA(0.5)
 H0TB(0.5) F7(0.5) F9(0.5) C7SA(0.5) H7SA(0.5) F14(0.5) C6SA(0.5) F21(0.5)
 F22(0.5) C6TA(0.5) H6TA(0.5) H6TB(0.5) C7TA(0.5) H7TA(0.5) C1TA(0.5) H1TA(0.5)
 C3TA(0.5) H3TA(0.5) H3TB(0.5) C4TA(0.5) H4TA(0.5) C5TA(0.5) H5TA(0.5)
 H5TB(0.5) C2TA(0.5) H2TA(0.5) C9SA(0.5) H9SA(0.5) H9SB(0.5) C8SA(0.5)
 H8SA(0.5) H8SB(0.5) C61(0.5) H61(0.5) C69(0.5) H69A(0.5) H69B(0.5) C72(0.5)
 H72A(0.5) H72B(0.5) F75(0.5) F13(0.5) Ag40(0.5) Ag41(0.5) S91(0.5) H3RC(0.5)
 H3RD(0.5) H3RA(0.5) H3RB(0.5) C9QA(0.5) C2RA(0.5) H2RA(0.5) H2RB(0.5)
 C1SA(0.5) H1SA(0.5) H1SB(0.5) C0VA(0.5) H0VA(0.5) H9UB(0.5) H9UC(0.5)
 H9UA(0.5) C8UA(0.5) H8UA(0.5) H8UB(0.5) C5UA(0.5) H5UA(0.5) C217(0.5)
 H21C(0.5) H21D(0.5) C2VA(0.5) C4VA(0.5) H4VA(0.5) H4VB(0.5) C5VA(0.5)
 H5VA(0.5) C6VA(0.5) H6VA(0.5) H6VB(0.5) C7VA(0.5) C1VA(0.5) S76(0.5) C98(0.5)
 F2(0.5) F1AA(0.5) F0AA(0.5)
6.a Ternary CH refined with riding coordinates:
 C6(H6), C10(H10), C23(H23), C34(H34), C36(H36), C43(H43), C47(H47), C50(H50),
 C54(H54), C7BA(H7BA), C0EA(H0EA), C8(H8), C7CA(H7CA), C3BA(H3BA), C9CA(H9CA),
 C7AA(H7AA), C6AA(H6AA), C8AA(H8AA), C2DA(H2DA), C2BA(H2BA), C5BA(H5BA),
 C5CA(H5CA), C1IA(H1IA), C3EA(H3EA), C7GA(H7GA), C6GA(H6GA), C9EA(H9EA),
 C9HA(H9HA), C2FA(H2FA), C6IA(H6IA), C7FA(H7FA), C4HA(H4HA), C4IA(H4IA),
 C8IA(H8IA), C6HA(H6HA), C3GA(H3GA), C2JA(H2JA), C6FA(H6FA), C4FA(H4FA),
 C9FA(H9FA), C5EA(H5EA), C6EA(H6EA), C9KA(H9KA), C7JA(H7JA), C5KA(H5KA),
 C0KA(H0KA), C9MA(H9MA), C37(H37), C6JA(H6JA), C1LA(H1LA), C2LA(H2LA),
 C5LA(H5LA), C5NA(H5NA), C1MA(H1MA), C1PA(H1PA), C4PA(H4PA), C6RA(H6RA),
 C9PA(H9PA), C6PA(H6PA), C4QA(H4QA), C0QA(H0QA), C0OA(H0OA), C77(H77),
 C0TA(H0TB), C9RA(H9RA), C7SA(H7SA), C2UA(H2UA), C0UA(H0UA), C7TA(H7TA),
 C1TA(H1TA), C4TA(H4TA), C2TA(H2TA), C5MA(H5MA), C5QA(H5QA), C1RA(H1RA),
 C6UA(H6UA), C4UA(H4UA), C254(H254), C99(H99), C1JA(H1JA), C4OA(H4OA),
 C3OA(H3OA), C2OA(H2OA), C7UA(H7UA), C0VA(H0VA), C9UA(H9UA), C5UA(H5UA),
 C5VA(H5VA)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C11(H11A,H11B), C13(H13A,H13B), C16(H16A,H16B),
 C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B), C24(H24A,H24B), C26(H26A,H26B),
  C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C45(H45A,H45B),
 C46(H46A,H46B), C48(H48A,H48B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
  C58(H58A,H58B), C60(H60A,H60B), C9BA(H9BA,H9BB), C8CA(H8CA,H8CB), C6CA(H6CA,
 H6CB), C4BA(H4BA,H4BB), C1AA(H1AA,H1AB), C0AA(H0AA,H0AB), C3DA(H3DA,H3DB),
 C4AA(H4AA,H4AB), C15(H15A,H15B), C3AA(H3AA,H3AB), C9AA(H9AA,H9AB), C4CA(H4CA,
 H4CB), C9DA(H9DA,H9DB), C27(H27A,H27B), C2CA(H2CA,H2CB), C8BA(H8BA,H8BB),
 C0DA(H0DA,H0DB), C4DA(H4DA,H4DB), C0BA(H0BA,H0BB), C1BA(H1BA,H1BB), C38(H38A,
 H38B), C7DA(H7DA,H7DB), C6BA(H6BA,H6BB), C5AA(H5AA,H5AB), C2AA(H2AA,H2AB),
 C5DA(H5DA,H5DB), C1DA(H1DA,H1DB), C6DA(H6DA,H6DB), C56(H56A,H56B), C57(H57A,
 H57B), C3CA(H3CA,H3CB), C2EA(H2EA,H2EB), C8GA(H8GA,H8GB), C8FA(H8FA,H8FB),
 C9IA(H9IA,H9IB), C7EA(H7EA,H7EB), C3IA(H3IA,H3IB), C4GA(H4GA,H4GB), C0IA(H0IA,
 H0IB), C2IA(H2IA,H2IB), C0JA(H0JA,H0JB), C8HA(H8HA,H8HB), C8EA(H8EA,H8EB),
 C2GA(H2GA,H2GB), C1GA(H1GA,H1GB), C7IA(H7IA,H7IB), C7HA(H7HA,H7HB), C0FA(H0FA,
 H0FB), C1HA(H1HA,H1HB), C3HA(H3HA,H3HB), C0HA(H0HA,H0HB), C5GA(H5GA,H5GB),
 C2HA(H2HA,H2HB), C5IA(H5IA,H5IB), C4EA(H4EA,H4EB), C3FA(H3FA,H3FB), C5HA(H5HA,
 H5HB), C0GA(H0GA,H0GB), C5FA(H5FA,H5FB), C1FA(H1FA,H1FB), C0LA(H0LA,H0LB),
 C4JA(H4JA,H4JB), C3MA(H3MA,H3MB), C8MA(H8MA,H8MB), C6LA(H6LA,H6LB), C1KA(H1KA,
 H1KB), C0NA(H0NA,H0NB), C3KA(H3KA,H3KB), C1NA(H1NA,H1NB), C25(H25A,H25B),
 C3LA(H3LA,H3LB), C6KA(H6KA,H6KB), C9LA(H9LA,H9LB), C7MA(H7MA,H7MB), C4LA(H4LA,
 H4LB), C6NA(H6NA,H6NB), C2KA(H2KA,H2KB), C0MA(H0MA,H0MB), C5JA(H5JA,H5JB),
 C2NA(H2NA,H2NB), C8KA(H8KA,H8KB), C8JA(H8JA,H8JB), C7NA(H7NA,H7NB), C2MA(H2MA,
 H2MB), C7KA(H7KA,H7KB), C4KA(H4KA,H4KB), C2PA(H2PA,H2PB), C0PA(H0PA,H0PB),
 C7RA(H7RA,H7RB), C1QA(H1QA,H1QB), C5PA(H5PA,H5PB), C4RA(H4RA,H4RB), C7PA(H7PA,
 H7PB), C0RA(H0RA,H0RB), C2QA(H2QA,H2QB), C9NA(H9NA,H9NB), C3QA(H3QA,H3QB),
 C8PA(H8PA,H8PB), C63(H63A,H63B), C65(H65A,H65B), C97(H97A,H97B), C4SA(H4SA,
 H4SB), C5SA(H5SA,H5SB), C8RA(H8RA,H8RB), C1UA(H1UA,H1UB), C6TA(H6TA,H6TB),
 C3TA(H3TA,H3TB), C5TA(H5TA,H5TB), C8TA(H8TA,H8TB), C9SA(H9SA,H9SB), C8SA(H8SA,
 H8SB), C69(H69A,H69B), C72(H72A,H72B), C9TA(H9TA,H9TB), C7OA(H7OA,H7OB),
 C8OA(H8OA,H8OB), C7QA(H7QA,H7QB), C6QA(H6QA,H6QB), C125(H12A,H12B), C8QA(H8QA,
 H8QB), C8NA(H8NA,H8NB), C148(H14A,H14B), C0SA(H0SA,H0SB), C2SA(H2SA,H2SB),
 C3SA(H3SA,H3SB), C4NA(H4NA,H4NB), C75(H75A,H75B), C241(H24C,H24D), C6MA(H6MA,
 H6MB), C5OA(H5OA,H5OB), C1OA(H1OA,H1OB), C6OA(H6OA,H6OB), C3PA(H3PA,H3PB),
 C8LA(H8LA,H8LB), C3RA(H3RC,H3RD), C3RA(H3RA,H3RB), C2RA(H2RA,H2RB), C1SA(H1SA,
 H1SB), C9UA(H9UB,H9UC), C8UA(H8UA,H8UB), C217(H21C,H21D), C4VA(H4VA,H4VB),
 C6VA(H6VA,H6VB)
6.c Aromatic/amide H refined with riding coordinates:
 C3NA(H3NA), C0TA(H0TA), C61(H61)
;
_shelx_res_checksum              70383
_shelx_hkl_checksum              73451
_shelx_fab_checksum              82116
_olex2_submission_special_instructions 'No special instructions were received'