Understanding and designing one-dimensional assemblies of ligand-protected metal nanoclusters
Hossain, Sakiat; Imai, Yukari; Motohashi, Yuichi; Chen, Zhaoheng; Suzuki, Daiki; Suzuki, Taiyo; Kataoka, Yuki; Hirata, Momoko; Ono, Tasuku; Kurashige, Wataru; Kawawaki, Tokuhisa; Yamamoto, Takahiro; Negishi, Yuichi; Materials Horizons 7 (2020) 796–803; doi:10.1039/C9MH01691K

data_1556726
_publ_section_title
;
 Understanding and designing one-dimensional assemblies of
 ligand-protected metal nanoclusters
;
_journal_issue                   3
_journal_name_full               'Materials Horizons'
_journal_page_first              796
_journal_page_last               803
_journal_paper_doi               10.1039/C9MH01691K
_journal_volume                  7
_journal_year                    2020
_chemical_formula_moiety         '0.25(C256 H288 Au16 Pt8 S32), 0.5(C7 H8)'
_chemical_formula_sum            'C67.5 H76 Au4 Pt2 S8'
_chemical_formula_weight         2321.80
_chemical_name_systematic        'Au4Pt2(SC2H4Ph)8 polymer'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2019-09-27 deposited with the CCDC.	2019-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.0367(17)
_cell_length_b                   30.034(3)
_cell_length_c                   24.600(2)
_cell_measurement_reflns_used    7623
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      24.863
_cell_measurement_theta_min      2.265
_cell_volume                     13283(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0702
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            64038
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.320
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.290
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1034 before and 0.0535 after correction. The Ratio of minimum to maximum transmission is 0.7477. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.322
_exptl_crystal_description       needle
_exptl_crystal_F_000             8648
_exptl_crystal_recrystallization_method
'EtOH vapor diffusion to the toluene solution of the sample'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.205
_refine_diff_density_min         -1.780
_refine_diff_density_rms         0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1469
_refine_ls_number_reflns         23360
_refine_ls_number_restraints     1713
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15798
_reflns_number_total             23360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9mh01691k2.cif
_cod_data_source_block           Au4Pt2(SC2H4Ph)8
_cod_depositor_comments
;Adding full bibliography for 1556724--1556728.cif.

 Adding full bibliography for 1556724--1556728.cif.
;
_cod_original_cell_volume        13284(2)
_cod_original_formula_sum        'C67.50 H76 Au4 Pt2 S8'
_cod_database_code               1556726
_shelx_shelxl_version_number     2016/6
_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. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111
\\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim C118
\\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125
\\sim C126 \\sim C127 \\sim C128 \\sim C129 \\sim C130 \\sim C131 \\sim C132
\\sim C133 \\sim C134 \\sim C135: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C64) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C88) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48,
 C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64,
  C65, C66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, C79,
 C80, C81, C82, C83, C84, C85, C86, C87, C88, C89, C90, C91, C92, C93, C94, C95,
  C96, C97, C98, C99, C100, C101, C102, C103, C104, C105, C106, C107, C108,
 C109, C110, C111, C112, C113, C114, C115, C116, C117, C118, C119, C120, C121,
 C122, C123, C124, C125, C126, C127, C128, C129, C130, C131, C132, C133, C134,
 C135
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C11(H11A,H11B), C16(H16A,H16B), C19(H19A,H19B), C24(H24A,H24B), C27(H27A,H27B),
  C29(H29A,H29B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,
 H39B), C48(H48A,H48B), C60(H60A,H60B), C61(H61A,H61B), C64(H64A,H64B),
 C66(H66A,H66B), C71(H71A,H71B), C75(H75A,H75B), C76(H76A,H76B), C84(H84A,H84B),
  C91(H91A,H91B), C100(H10A,H10B), C104(H10C,H10D), C106(H10E,H10F), C107(H10G,
 H10H), C115(H11C,H11D), C128(H12A,H12B)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C13(H13), C14(H14), C21(H21), C22(H22), C23(H23), C25(H25),
 C28(H28), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C51(H51), C53(H53),
 C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C62(H62), C63(H63),
  C68(H68), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74), C77(H77),
 C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C85(H85), C86(H86),
  C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93), C94(H94),
 C95(H95), C96(H96), C97(H97), C98(H98), C101(H101), C102(H102), C103(H103),
 C105(H105), C108(H108), C109(H109), C110(H110), C111(H111), C112(H112),
 C113(H113), C114(H114), C116(H116), C117(H117), C118(H118), C119(H119),
 C120(H120), C121(H121), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C127(H127), C129(H129), C130(H130), C131(H131), C132(H132),
 C134(H134)
4.c Idealised Me refined as rotating group:
 C135(H13A,H13B,H13C)
;
_shelx_res_checksum              46776
_olex2_submission_special_instructions 'No special instructions were received'