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_1556725
_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         'C88 H120 Au4 Pt2 S8, C7 H8, 0.5(C7)'
_chemical_formula_sum            'C98.5 H128 Au4 Pt2 S8'
_chemical_formula_weight         2746.53
_chemical_name_systematic        Au4Pt2(SCH2PhtBu)8
_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
_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                 98.553(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.070(6)
_cell_length_b                   14.7091(19)
_cell_length_c                   31.214(4)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.944
_cell_measurement_theta_min      2.516
_cell_volume                     20009(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_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
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            59805
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.155
_diffrn_reflns_theta_min         1.319
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.839
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0602 before and 0.0376 after correction. The Ratio of minimum to maximum transmission is 0.8682. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_description       block
_exptl_crystal_F_000             10552
_exptl_crystal_recrystallization_method
'Vapor diffusion of EtOH to the toluene solution of cluster'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.448
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         24716
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+81.5085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17923
_reflns_number_total             24716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9mh01691k2.cif
_cod_data_source_block           Au4Pt2(SCH2PhtBu)8
_cod_depositor_comments
;Adding full bibliography for 1556724--1556728.cif.

 Adding full bibliography for 1556724--1556728.cif.
;
_cod_original_cell_volume        20009(4)
_cod_original_formula_sum        'C98.50 H128 Au4 Pt2 S8'
_cod_database_code               1556725
_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. Restrained distances
 C1A-C1B
 1.51 with sigma of 0.02
 C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F \\sim C1F-C1G \\sim C1G-C1B
 with sigma of 0.02
 C1B-C1F \\sim C1B-C1D \\sim C1G-C1E \\sim C1C-C1G \\sim C1D-C1F \\sim C1C-C1E
 with sigma of 0.04
 C1A-C1G \\sim C1A-C1C
 with sigma of 0.04
3. Restrained planarity
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F \\sim C1G: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C94) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C89)
\\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C91) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C91) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C90)
\\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C93) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C89) = Uanis(C93)
Uanis(C90) = Uanis(C94)
Uanis(C95) = Uanis(C94) = Uanis(C95) = Uanis(C92)
5. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C1A(0.5) C1B(0.5) C1C(0.5) C1D(0.5) C1E(0.5) C1F(0.5) C1G(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C32(H32A,H32B), C38(H38A,H38B), C41(H41A,H41B), C43(H43A,
 H43B), C65(H65A,H65B), C71(H71A,H71B), C72(H72A,H72B)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C11(H11), C13(H13), C17(H17), C18(H18),
 C22(H22), C24(H24), C25(H25), C27(H27), C29(H29), C30(H30), C31(H31), C35(H35),
  C36(H36), C39(H39), C42(H42), C44(H44), C45(H45), C47(H47), C49(H49),
 C50(H50), C52(H52), C53(H53), C55(H55), C61(H61), C64(H64), C67(H67), C68(H68),
  C69(H69), C90(H90), C92(H92), C93(H93), C94(H94), C95(H95)
7.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C48(H48A,H48B,H48C), C51(H51A,H51B,
 H51C), C54(H54A,H54B,H54C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C62(H62A,
 H62B,H62C), C66(H66A,H66B,H66C), C70(H70A,H70B,H70C), C73(H73A,H73B,H73C),
 C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C78(H78A,H78B,
 H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C82(H82A,
 H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C),
 C86(H86A,H86B,H86C), C88(H88A,H88B,H88C), C91(H91A,H91B,H91C)
;
_shelx_res_checksum              93193
_olex2_submission_special_instructions 'No special instructions were received'