Anisotropic Assembly of Ag52 and Ag76 Nanoclusters.
Liu, Jia-Wei; Feng, Lei; Su, Hai-Feng; Wang, Zhi; Zhao, Quan-Qin; Wang, Xing-Po; Tung, Chen-Ho; Sun, Di; Zheng, Lan-Sun; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b12777

data_4127078
_publ_section_title
;
 Anisotropic Assembly of Ag52 and Ag76 Nanoclusters.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b12777
_journal_year                    2018
_chemical_formula_moiety         'C450 H480 Ag52 Mo15 O60 P20 S26'
_chemical_formula_sum            'C450 H480 Ag52 Mo15 O60 P20 S26'
_chemical_formula_weight         15349.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 126.8950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   37.277(3)
_cell_length_b                   38.673(3)
_cell_length_c                   27.0826(19)
_cell_measurement_reflns_used    9544
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.211
_cell_measurement_theta_min      2.280
_cell_volume                     31224(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1174
_diffrn_reflns_av_unetI/netI     0.1066
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            94157
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.655
_exptl_absorpt_coefficient_mu    2.062
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1001 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.7311.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       block
_exptl_crystal_F_000             14900
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.815
_refine_diff_density_min         -2.457
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1080
_refine_ls_number_reflns         27919
_refine_ls_number_restraints     490
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1845
_refine_ls_R_factor_gt           0.1286
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1423P)^2^+2373.0688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3274
_refine_ls_wR_factor_ref         0.3690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17015
_reflns_number_total             27919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12777_si_002.cif
_cod_data_source_block           SD-Ag23
_cod_original_cell_volume        31223(4)
_cod_database_code               4127078
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.852
_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
 C101-C104
 1.55 with sigma of 0.01
 C101-C102
 1.55 with sigma of 0.01
 C101-C103
 1.55 with sigma of 0.01
 C105-C101
 2.35 with sigma of 0.01
 C101-C109
 2.35 with sigma of 0.01
 C104-C102
 2.35 with sigma of 0.01
 C104-C103
 2.35 with sigma of 0.01
 C103-C102
 2.35 with sigma of 0.01
 C14-C14_$1
 2.35 with sigma of 0.01
 C110-C115
 1.35 with sigma of 0.01
 C115-C111
 2.35 with sigma of 0.01
 C115-C113
 2.35 with sigma of 0.01
 C83-C86
 1.55 with sigma of 0.01
 C86-C88
 1.55 with sigma of 0.01
 C86-C87
 1.55 with sigma of 0.01
 C88-C87
 2.35 with sigma of 0.01
 C83-C88
 2.35 with sigma of 0.01
 C86-C84
 2.35 with sigma of 0.01
 C82-C86
 2.35 with sigma of 0.01
 C96-C97
 1.55 with sigma of 0.01
 C15_$1-C13
 1.55 with sigma of 0.01
 C13-C16
 2.35 with sigma of 0.01
 C14-C16
 2.35 with sigma of 0.01
 C15-C16
 1.55 with sigma of 0.01
 C10-C8
 2.35 with sigma of 0.01
 C8-C9
 2.35 with sigma of 0.01
 C100-C101
 1.55 with sigma of 0.01
 C104-C100
 2.35 with sigma of 0.01
 C103-C100
 2.35 with sigma of 0.01
 C102-C100
 2.35 with sigma of 0.01
 C96-C98
 2.35 with sigma of 0.01
 C98-C97
 1.55 with sigma of 0.01
 C113-C112
 1.35 with sigma of 0.01
 C114-C113
 1.35 with sigma of 0.01
 C115-C114
 1.35 with sigma of 0.01
 C114-C112
 2.35 with sigma of 0.01
 C96-C99
 2.35 with sigma of 0.01
 C97-C99
 1.55 with sigma of 0.01
 C98-C99
 2.35 with sigma of 0.01
 C86-C89
 1.55 with sigma of 0.01
 C88-C89
 2.35 with sigma of 0.01
 C87-C89
 2.35 with sigma of 0.01
 C119-C117
 1.55 with sigma of 0.01
 C118-C119
 1.55 with sigma of 0.01
 C119-C116
 1.55 with sigma of 0.01
 H11C-H11F
 2 with sigma of 0.1
3. Restrained planarity
 C101, C109, C104, C105
 with sigma of 0.01
 C84, C83, C82, C86
 with sigma of 0.01
 C94, C93, C92, C97
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C73 \\sim C72 \\sim C71 \\sim C70 \\sim C69 \\sim C68: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
Ag5 \\sim Ag5A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
C24 \\sim C29 \\sim C28 \\sim C27 \\sim C26 \\sim C25: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C36 \\sim C41 \\sim C40 \\sim C39 \\sim C38 \\sim C37: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C107 \\sim C108 \\sim C109 \\sim C104 \\sim C105 \\sim C106 \\sim S4: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
C33 \\sim C34 \\sim C35 \\sim C30 \\sim C31 \\sim C32 \\sim C36 \\sim C41 \\sim
C40 \\sim C39 \\sim C38 \\sim C37 \\sim C42 \\sim C48 \\sim C47 \\sim C46 \\sim
C45 \\sim C44 \\sim C43 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim
C54: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
S2: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.08
C11 \\sim C11 \\sim C12 \\sim C12 \\sim C13 \\sim C14 \\sim C14 \\sim C15 \\sim
C15 \\sim C16 \\sim C120: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.08
C4 \\sim C5 \\sim C6 \\sim C1 \\sim C2 \\sim C3 \\sim C7 \\sim C8 \\sim C9
\\sim C10: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C100 \\sim C101 \\sim C102 \\sim C103 \\sim C107 \\sim C108 \\sim C109 \\sim
C104 \\sim C105 \\sim C106 \\sim S4: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.08
C60 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C66 \\sim C65 \\sim
C64 \\sim C63 \\sim C62 \\sim C61: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.08
C90 \\sim C95 \\sim C94 \\sim C93 \\sim C92 \\sim C91 \\sim C96 \\sim C97 \\sim
C98 \\sim C99 \\sim S2: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
C81 \\sim C80 \\sim C85 \\sim C84 \\sim C83 \\sim C82 \\sim C86 \\sim C87 \\sim
C88 \\sim C89 \\sim S1: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
C110 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim
C116 \\sim C117 \\sim C118 \\sim C119 \\sim S3: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
5. Others
 Fixed Sof: Ag2(0.5) Ag4(0.5) Ag4A(0.5) Ag5(0.8) Ag5A(0.2) Ag6(0.2) Ag6A(0.8)
 Ag8(0.5) Ag8A(0.5) Ag9(0.35) Ag9A(0.65) H16A(0.5) H16B(0.5) H16C(0.5)
 C116(0.5) H11C(0.5) H11D(0.5) H11E(0.5) H11G(0.5) H11H(0.5) H11J(0.5)
 H11K(0.5) Mo1(0.25) Mo2(0.5) Mo2A(0.5) S8(0.6) S8A(0.4)
6.a Riding coordinates:
 C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C58(H58), C89(H89A,
 H89B,H89C), C98(H98A,H98B,H98C), C100(H10D,H10E,H10F), C112(H112), C114(H114),
 C116(H11C,H11D,H11E)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C17(H17A,H17B), C42(H42A,H42B), C67(H67A,H67B)
6.c Me refined with riding coordinates:
 C99(H99A,H99B,H99C), C117(H11F,H11G,H11H), C118(H11I,H11J,H11K)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C2(H2), C3(H3), C12(H12), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C29(H29), C28(H28), C27(H27), C26(H26), C25(H25), C33(H33),
  C34(H34), C30(H30), C31(H31), C32(H32), C41(H41), C40(H40), C39(H39),
 C38(H38), C37(H37), C47(H47), C46(H46), C45(H45), C44(H44), C43(H43), C50(H50),
  C51(H51), C52(H52), C53(H53), C54(H54), C60(H60), C56(H56), C57(H57),
 C59(H59), C65(H65), C64(H64), C63(H63), C62(H62), C61(H61), C72(H72), C71(H71),
  C70(H70), C69(H69), C68(H68), C74(H74), C76(H76), C77(H77), C78(H78),
 C79(H79), C81(H81), C85(H85), C84(H84), C82(H82), C95(H95), C92(H92), C91(H91),
  C108(H108), C109(H109), C105(H105), C106(H106), C111(H111), C115(H115)
6.e Fitted hexagon refined as free rotating group:
 C4(C5,C6,C1,C2,C3), C18(C19,C20,C21,C22,C23), C24(C29,C28,C27,C26,C25),
 C33(C34,C35,C30,C31,C32), C36(C41,C40,C39,C38,C37), C48(C47,C46,C45,C44,C43),
 C60(C55,C56,C57,C58,C59), C66(C65,C64,C63,C62,C61), C73(C72,C71,C70,C69,C68),
 C74(C75,C76,C77,C78,C79), C81(C80,C85,C84,C83,C82), C90(C95,C94,C93,C92,C91),
 C107(C108,C109,C104,C105,C106)
6.f Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C87(H87A,H87B,H87C), C88(H88A,H88B,
 H88C), C96(H96A,H96B,H96C), C102(H10G,H10H,H10I), C103(H10J,H10K,H10L)
;
_shelx_res_checksum              93582
_shelx_hkl_checksum              29871
_shelx_fab_checksum              32797
_olex2_submission_special_instructions 'No special instructions were received'