Self-Assembly, Structural Transformation and Guest-Binding Properties of Supramolecular Assemblies with Triangular Metal-Metal Bonded Units.
Wang, Li-Juan; Li, Xin; Bai, Sha; Wang, Yaoyu; Han, Ying-Feng; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b12309

data_4133995
_publ_section_title
;
 Self-Assembly, Structural Transformation and Guest-Binding Properties of
 Supramolecular Assemblies with Triangular Metal-Metal Bonded Units.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12309
_journal_year                    2020
_chemical_formula_moiety         'C126 H154 B4 F16 N14 O7 Pt6 S6'
_chemical_formula_sum            'C126 H154 B4 F16 N14 O7 Pt6 S6'
_chemical_formula_weight         3686.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                91.662(2)
_cell_angle_beta                 93.669(3)
_cell_angle_gamma                106.756(2)
_cell_formula_units_Z            2
_cell_length_a                   16.6090(13)
_cell_length_b                   18.7796(15)
_cell_length_c                   23.567(2)
_cell_measurement_reflns_used    9029
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.39
_cell_volume                     7015.6(10)
_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      185.01
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77975
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.410
_diffrn_reflns_theta_min         2.118
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.126
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4259
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       block
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.506
_refine_diff_density_min         -2.251
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1735
_refine_ls_number_reflns         25514
_refine_ls_number_restraints     406
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0003P)^2^+62.7313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20685
_reflns_number_total             25514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12309_si_006.cif
_cod_data_source_block           Complex_3b
_cod_original_cell_volume        7015.7(10)
_cod_database_code               4133995
_shelx_shelxl_version_number     2018/3
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C113-C127 = C115-C113 = C120-C115 = C131-C127 = C130-C131 = C121-C120
 1.54 with sigma of 0.02
 C84-C132 = C101-C84 = C109-C101 = C133-C132 = C126-C109 = C134-C133
 1.54 with sigma of 0.02
 C135-C137 = C118-C117 = C137-C94 = C117-C94
 1.54 with sigma of 0.02
 C138-C82 = C108-C82 = C136-C138 = C114-C108
 1.54 with sigma of 0.02
 C113-C131 = C113-C120 = C127-C130 = C115-C121
 2.5 with sigma of 0.04
 C84-C109 = C84-C133 = C101-C126 = C132-C134
 2.5 with sigma of 0.04
 C94-C135 = C94-C118
 2.5 with sigma of 0.04
 C82-C136 = C82-C114
 2.5 with sigma of 0.04
 C102-C129 \\sim C110-C102
 with sigma of 0.02
 C102-C116 \\sim C102-C128
 with sigma of 0.04
 C116-C110 \\sim C128-C129
 with sigma of 0.02
3. Rigid bond restraints
 C31, C24, C42, C78, C56, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C102 \\sim C110 \\sim C116: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C129 \\sim C116 \\sim C110 \\sim C128: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C120 \\sim C115 \\sim C121: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O3 \\sim C113 \\sim C115 \\sim C120 \\sim C121: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C127 \\sim C115 \\sim C120 \\sim C131 \\sim C130 \\sim C121: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C84 \\sim C101 \\sim C109 \\sim C126: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C132 \\sim C101 \\sim C109 \\sim C133 \\sim C134 \\sim C126: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C94 \\sim C117 \\sim C118: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C118 \\sim C135 \\sim C137 \\sim C117: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C138 \\sim C108 \\sim C114 \\sim C136: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C113) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(F1)
\\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq,
Uanis(F7) \\sim Ueq, Uanis(F10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C113) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C123) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C116) \\sim Ueq, Uanis(C109) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C109) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C120) \\sim Ueq,
Uanis(C115) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C118) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C126) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C114) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) = Uanis(C24)
5. Others
 Sof(H10E)=Sof(H10F)=Sof(C128)=Sof(H12K)=Sof(H12L)=Sof(H12M)=Sof(C129)=
 Sof(H12N)=Sof(H12O)=1-FVAR(1)
 Sof(H10C)=Sof(H10D)=Sof(C110)=Sof(H11A)=Sof(H11B)=Sof(C116)=Sof(H11R)=
 Sof(H11S)=Sof(H11T)=FVAR(1)
 Sof(H11K)=Sof(H11L)=Sof(C127)=Sof(H12I)=Sof(H12J)=Sof(C130)=Sof(H13A)=
 Sof(H13B)=Sof(H13C)=Sof(C131)=Sof(H13D)=Sof(H13E)=1-FVAR(2)
 Sof(H11I)=Sof(H11J)=Sof(C115)=Sof(H11P)=Sof(H11Q)=Sof(C120)=Sof(H12A)=
 Sof(H12B)=Sof(C121)=Sof(H12C)=Sof(H12D)=Sof(H12E)=FVAR(2)
 Sof(H84C)=Sof(H84D)=Sof(C132)=Sof(H13F)=Sof(H13G)=Sof(C133)=Sof(H13H)=
 Sof(H13I)=Sof(C134)=Sof(H13J)=Sof(H13K)=Sof(H13L)=1-FVAR(3)
 Sof(H84A)=Sof(H84B)=Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(C109)=Sof(H10O)=
 Sof(H10P)=Sof(C126)=Sof(H12F)=Sof(H12G)=Sof(H12H)=FVAR(3)
 Sof(H82C)=Sof(H82D)=Sof(C136)=Sof(H13P)=Sof(H13Q)=Sof(H13R)=Sof(C138)=
 Sof(H13U)=Sof(H13V)=1-FVAR(4)
 Sof(H82A)=Sof(H82B)=Sof(C108)=Sof(H10M)=Sof(H10N)=Sof(C114)=Sof(H11M)=
 Sof(H11N)=Sof(H11O)=FVAR(4)
 Sof(H94C)=Sof(H94D)=Sof(C135)=Sof(H13M)=Sof(H13N)=Sof(H13O)=Sof(C137)=
 Sof(H13S)=Sof(H13T)=1-FVAR(5)
 Sof(H94A)=Sof(H94B)=Sof(C117)=Sof(H11U)=Sof(H11V)=Sof(C118)=Sof(H11W)=
 Sof(H11X)=Sof(H11Y)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10),
 C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20),
  C22(H22), C28(H28), C32(H32), C33(H33), C34(H34), C36(H36), C41(H41),
 C65(H65), C74(H74)
6.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C50(H50A,H50B), C54(H54A,H54B), C60(H60A,H60B), C68(H68A,
 H68B), C69(H69A,H69B), C72(H72A,H72B), C82(H82A,H82B), C82(H82C,H82D),
 C84(H84A,H84B), C84(H84C,H84D), C87(H87A,H87B), C88(H88A,H88B), C90(H90A,H90B),
  C93(H93A,H93B), C94(H94A,H94B), C94(H94C,H94D), C95(H95A,H95B), C101(H10A,
 H10B), C102(H10C,H10D), C102(H10E,H10F), C104(H10G,H10H), C105(H10I,H10J),
 C107(H10Q,H10R), C108(H10M,H10N), C109(H10O,H10P), C110(H11A,H11B), C113(H11I,
 H11J), C113(H11K,H11L), C115(H11P,H11Q), C117(H11U,H11V), C120(H12A,H12B),
 C127(H12I,H12J), C129(H12N,H12O), C131(H13D,H13E), C132(H13F,H13G), C133(H13H,
 H13I), C137(H13S,H13T), C138(H13U,H13V)
6.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C16(H16), C23(H23), C29(H29), C35(H35), C39(H39), C42(H42), C49(H49),
 C51(H51), C55(H55), C56(H56), C58(H58), C59(H59), C61(H61), C62(H62), C66(H66),
  C67(H67), C70(H70), C71(H71), C73(H73), C76(H76), C78(H78), C79(H79),
 C80(H80), C83(H83), C86(H86), C89(H89), C92(H92), C99(H99), C100(H100),
 C103(H103)
6.d X=CH2 refined with riding coordinates:
 C75(H75A,H75B), C91(H91A,H91B), C96(H96A,H96B), C98(H98A,H98B), C106(H10K,H10L)
6.e Idealised Me refined as rotating group:
 C97(H97A,H97B,H97C), C111(H11C,H11D,H11E), C112(H11F,H11G,H11H), C114(H11M,
 H11N,H11O), C116(H11R,H11S,H11T), C118(H11W,H11X,H11Y), C119(H11Z,H,HA),
 C121(H12C,H12D,H12E), C123(H12P,H12Q,H12R), C125(H12S,H12T,H12U), C126(H12F,
 H12G,H12H), C128(H12K,H12L,H12M), C130(H13A,H13B,H13C), C134(H13J,H13K,H13L),
 C135(H13M,H13N,H13O), C136(H13P,H13Q,H13R)
;
_shelx_res_checksum              54588
_shelx_hkl_checksum              73963
_shelx_fab_checksum              4482
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'