Carboxylic acid stimulated silver shell isomerism in a triple core–shell Ag <sub>84</sub> nanocluster
Wang, Zhi; Sun, Hao-Tian; Kurmoo, Mohamedally; Liu, Qing-Yun; Zhuang, Gui-Lin; Zhao, Quan-Qin; Wang, Xing-Po; Tung, Chen-Ho; Sun, Di; Chemical Science 10 (2019) 4862–4867; doi:10.1039/C8SC05666H

data_1550818
_publ_section_title
;
 Carboxylic acid stimulated silver shell isomerism in a triple core--shell
 Ag <sub>84</sub> nanocluster
;
_journal_issue                   18
_journal_name_full               'Chemical Science'
_journal_page_first              4862
_journal_page_last               4867
_journal_paper_doi               10.1039/C8SC05666H
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C246 H370 Ag84 O88 S42 W14'
_chemical_formula_sum            'C246 H370 Ag84 O88 S42 W14'
_chemical_formula_weight         17716.90
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-14 deposited with the CCDC.    2019-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                74.1307(13)
_cell_angle_beta                 70.9758(13)
_cell_angle_gamma                68.5642(17)
_cell_formula_units_Z            1
_cell_length_a                   21.5617(11)
_cell_length_b                   22.2473(10)
_cell_length_c                   24.5285(13)
_cell_measurement_reflns_used    9336
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.766
_cell_measurement_theta_min      2.402
_cell_volume                     10193.5(9)
_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      100.15
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'SSRF beamline BL17B'
_diffrn_radiation_wavelength     0.68877
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.916
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            126316
_diffrn_reflns_point_group_measured_fraction_full 0.916
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        23.048
_diffrn_reflns_theta_max         22.854
_diffrn_reflns_theta_min         1.117
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    6.444
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.5185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1846 before and 0.0821 after correction.
The Ratio of minimum to maximum transmission is 0.6960.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    2.886
_exptl_crystal_description       block
_exptl_crystal_F_000             8206
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         5.487
_refine_diff_density_min         -3.248
_refine_diff_density_rms         0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1944
_refine_ls_number_reflns         33781
_refine_ls_number_restraints     643
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+598.7421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27037
_reflns_number_total             33781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05666h2.cif
_cod_data_source_block           SD_Ag84b
_cod_database_code               1550818
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.830
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C6-C4A
 1.55 with sigma of 0.01
 S19-C4A
 2.75 with sigma of 0.01
 C7A-C9
 1.55 with sigma of 0.01
 C7-C9
 1.55 with sigma of 0.01
 C8-C9
 1.55 with sigma of 0.01
 C8A-C9
 1.55 with sigma of 0.01
 C7-S4
 2.75 with sigma of 0.01
 C7A-S4
 2.75 with sigma of 0.01
 C8-S4
 2.75 with sigma of 0.01
 C8A-S4
 2.75 with sigma of 0.01
 C49-C50
 1.55 with sigma of 0.01
 C50-C51
 1.55 with sigma of 0.01
 C49-C51
 2.35 with sigma of 0.01
 C49-S12
 2.75 with sigma of 0.01
 C51-S12
 2.75 with sigma of 0.01
 S12-C50
 1.85 with sigma of 0.01
 O32-C117
 1.25 with sigma of 0.01
 O31-C117
 1.25 with sigma of 0.01
 O31-O32
 2.3 with sigma of 0.01
 O32-C118
 2.35 with sigma of 0.01
 O31-C118
 2.35 with sigma of 0.01
 C117-C118
 1.55 with sigma of 0.01
 C1-C3
 1.55 with sigma of 0.01
 C3-C2
 2.35 with sigma of 0.01
 C1A-C3
 1.55 with sigma of 0.01
 C27-C28
 1.55 with sigma of 0.01
 C28-S10
 2.75 with sigma of 0.01
 C37-C36
 1.55 with sigma of 0.01
 C37-C38
 1.55 with sigma of 0.01
 C4-C6
 1.55 with sigma of 0.01
 S19-C4
 2.75 with sigma of 0.01
 C6-C5A
 1.55 with sigma of 0.01
 C5A-C4A
 2.35 with sigma of 0.01
 S19-C5A
 2.75 with sigma of 0.01
 C21-C22
 1.55 with sigma of 0.01
 C40-C39
 1.55 with sigma of 0.01
 C6-C5
 1.55 with sigma of 0.01
 C5-S19
 2.75 with sigma of 0.01
 C4-C5
 2.35 with sigma of 0.01
 C89-C90
 1.55 with sigma of 0.01
 C89-S14
 1.85 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: Ag1(0.2) Ag1A(0.8) Ag2(0.7) Ag2A(0.3) Ag3(0.5) Ag3A(0.5) Ag4(0.7)
 Ag4A(0.3) Ag5(0.5) Ag5A(0.5) Ag6(0.5) Ag6A(0.5) Ag7(0.65) Ag7A(0.35) S1(0.35)
 S1A(0.65) C1(0.5) H1(0.5) C1A(0.5) H1A(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5)
 H2BD(0.5) H2BE(0.5) H2BF(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) H3BD(0.5)
 H3BE(0.5) H3BF(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C4A(0.5) H4AA(0.5)
 H4AB(0.5) H4AC(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C5A(0.5) H5AA(0.5)
 H5AB(0.5) H5AC(0.5) H6B(0.5) H6A(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
 C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5)
 C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) H9B(0.5) H9A(0.5)
5.a Riding coordinates:
 C5(H5A,H5B,H5C)
5.b Ternary CH refined with riding coordinates:
 C1(H1), C1A(H1A), C6(H6B), C6(H6A), C9(H9B), C9(H9A), C18(H18), C22(H22),
 C24(H24), C27(H27), C37(H37), C47(H47), C50(H50), C53(H53), C63(H63), C73(H73),
  C76(H76), C86(H86), C89(H89), C92(H92), C102(H102), C112(H112), C115(H115)
5.c Me refined with riding coordinates:
 C2(H2AA,H2AB,H2AC), C2(H2BD,H2BE,H2BF), C3(H3AA,H3AB,H3AC), C3(H3BD,H3BE,
 H3BF), C4(H4A,H4B,H4C), C5A(H5AA,H5AB,H5AC), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C101(H10A,H10B,H10C)
5.d Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C14(H14), C13(H13), C12(H12), C35(H35), C34(H34),
 C33(H33), C32(H32), C31(H31), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45),
  C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C67(H67), C68(H68),
 C69(H69), C70(H70), C71(H71), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84),
  C96(H96), C97(H97), C98(H98), C99(H99), C100(H100), C106(H106), C107(H107),
 C108(H108), C109(H109), C110(H110), C119(H119), C120(H120), C121(H121),
 C122(H122), C123(H123)
5.e Fitted hexagon refined as free rotating group:
 C16(C15,C14,C13,C12,C11), C30(C35,C34,C33,C32,C31), C118(C119,C120,C121,C122,
 C123)
5.f Idealised Me refined as rotating group:
 C4A(H4AA,H4AB,H4AC), C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C8(H8A,H8B,H8C),
 C8A(H8AA,H8AB,H8AC), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C46(H46A,
 H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C62(H62A,H62B,H62C), C64(H64A,H64B,
 H64C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C77(H77A,
 H77B,H77C), C85(H85A,H85B,H85C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C),
 C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C93(H93A,H93B,H93C), C103(H10D,H10E,
 H10F), C111(H11A,H11B,H11C), C113(H11D,H11E,H11F), C114(H11G,H11H,H11I),
 C116(H11J,H11K,H11L)
;
_shelx_res_checksum              8238
_shelx_fab_checksum              31572
_olex2_submission_special_instructions 'No special instructions were received'