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_4133990
_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         'C136 H169 B4 F16 N15 O6 Pt6 S6'
_chemical_formula_sum            'C136 H169 B4 F16 N15 O6 Pt6 S6'
_chemical_formula_weight         3819.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3945(17)
_cell_length_b                   36.360(2)
_cell_length_c                   16.2541(10)
_cell_measurement_reflns_used    9623
_cell_measurement_temperature    174(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.49
_cell_volume                     16781.1(17)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      174.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0861
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            525531
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.371
_diffrn_reflns_theta_min         1.985
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.125
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.1362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1147 before and 0.0728 after correction.
The Ratio of minimum to maximum transmission is 0.5259.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       block
_exptl_crystal_F_000             7464
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.778
_refine_diff_density_min         -1.898
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1104
_refine_ls_number_reflns         15634
_refine_ls_number_restraints     1288
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0566P)^2^+120.0126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11180
_reflns_number_total             15634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12309_si_007.cif
_cod_data_source_block           Complex_3c
_cod_original_cell_volume        16780.9(18)
_cod_database_code               4133990
_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
 C40-C1 = C76-C1 = C75-C76 = C40-C32 = C56-C32 = C75-C77
 1.54 with sigma of 0.02
 C68-C33 = C93-C33
 1.54 with sigma of 0.02
 C61-C52 = C52-C96
 1.54 with sigma of 0.02
 C61-C44 = C95-C96
 1.4 with sigma of 0.02
 C98-C46 = C97-C98 = C97-C100 = C101-C100 = C101-C99
 1.54 with sigma of 0.02
 C43-C39 = C72-C39 = C62-C39 = C62-C41 = C70-C72 = C70-C71 = C69-C41
 1.54 with sigma of 0.02
 C68-C92 = C93-C94
 1.4 with sigma of 0.02
 C59-C46 = C60-C23 = C63-C60 = C63-C34
 1.54 with sigma of 0.02
 C59-C23 = C59-C46 = C60-C23 = C63-C60 = C63-C34
 1.54 with sigma of 0.02
 C43-C72 = C43-C62
 2.5 with sigma of 0.04
 C1-C32 = C1-C75
 2.5 with sigma of 0.04
 C40-C56 = C77-C76
 2.5 with sigma of 0.04
 C23-C63
 2.5 with sigma of 0.04
 O1-C59
 2.5 with sigma of 0.04
 C46-C97 = C98-C100
 2.5 with sigma of 0.04
 C101-C97
 2.5 with sigma of 0.04
 C72-C71 = C62-C69
 2.5 with sigma of 0.04
 C39-C70 = C39-C41
 2.5 with sigma of 0.04
 C46-C23 = C60-C34 = C59-C63
 2.5 with sigma of 0.04
 C62-C39 \\sim C72-C39
 with sigma of 0.02
 C40-C1 \\sim C76-C1
 with sigma of 0.02
 C68-C33 \\sim C93-C33
 with sigma of 0.02
 C52-C96 \\sim C61-C52
 with sigma of 0.02
 C93-C94 \\sim C68-C92
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C73 \\sim N8 \\sim C74: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C1 \\sim C40 \\sim C76 \\sim C75 \\sim C32 \\sim C77 \\sim C56: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C29 \\sim C38 \\sim C42: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N6 \\sim C26 \\sim C27: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C78 \\sim C57 \\sim C79 \\sim C58 \\sim C80 \\sim C31 \\sim C81 \\sim C28 \\sim
C82 \\sim C50 \\sim C83 \\sim C37 \\sim C84 \\sim C51: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C52 \\sim C61 \\sim C96 \\sim C95 \\sim C44: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C39 \\sim C62 \\sim C72 \\sim C70 \\sim C41 \\sim C71 \\sim C69: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C92 \\sim C94 \\sim C93 \\sim C68 \\sim C33: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O1 \\sim C46 \\sim C59 \\sim C23 \\sim C60 \\sim C63 \\sim C34: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C98 \\sim C59 \\sim C23 \\sim C97 \\sim C60 \\sim C100 \\sim C101 \\sim C63
\\sim C34 \\sim C99: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
C65 \\sim C91 \\sim C15 \\sim C90 \\sim C49 \\sim C89 \\sim C64 \\sim C88 \\sim
C66 \\sim C87 \\sim C67 \\sim C86 \\sim C21 \\sim C85: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N8) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C76) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C38) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C78) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C83)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C51) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C61) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C44)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C98) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C101)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C99) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C69) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C72) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C71) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C41) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C93) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C94) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C92) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C46) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C49) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C21) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C87) \\sim Ueq,
Uanis(C66) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C89)
\\sim Ueq, Uanis(C90) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C41) = Uanis(C70)
4. Others
 Sof(H39C)=Sof(H39D)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=Sof(H71B)=
 Sof(H71C)=Sof(C72)=Sof(H72A)=Sof(H72B)=1-FVAR(1)
 Sof(H39A)=Sof(H39B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C62)=Sof(H62A)=Sof(H62B)=
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=1-FVAR(2)
 Sof(H1AA)=Sof(H1AB)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(2)
 Sof(C78)=Sof(H78)=Sof(C79)=Sof(H79)=Sof(C80)=Sof(H80)=Sof(C81)=Sof(H81)=
 Sof(C82)=Sof(H82)=Sof(C83)=Sof(H83)=Sof(C84)=Sof(H84)=1-FVAR(3)
 Sof(C28)=Sof(H28)=Sof(C31)=Sof(H31)=Sof(C37)=Sof(H37)=Sof(C50)=Sof(H50)=
 Sof(C51)=Sof(H51)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=FVAR(3)
 Sof(C85)=Sof(H85)=Sof(C86)=Sof(H86)=Sof(C87)=Sof(H87)=Sof(C88)=Sof(H88)=
 Sof(C89)=Sof(H89)=Sof(C90)=Sof(H90)=Sof(C91)=Sof(H91)=1-FVAR(4)
 Sof(C15)=Sof(H15)=Sof(C21)=Sof(H21)=Sof(C49)=Sof(H49)=Sof(C64)=Sof(H64)=
 Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=Sof(C67)=Sof(H67)=FVAR(4)
 Sof(H33C)=Sof(H33D)=Sof(C93)=Sof(H93)=Sof(C94)=Sof(H94A)=Sof(H94B)=1-FVAR(5)
 Sof(H33A)=Sof(H33B)=Sof(C68)=Sof(H68)=Sof(C92)=Sof(H92A)=Sof(H92B)=FVAR(5)
 Sof(H52C)=Sof(H52D)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96)=1-FVAR(6)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H52A)=Sof(H52B)=Sof(C61)=Sof(H61)=FVAR(6)
 Sof(H46C)=Sof(H46D)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(C98)=Sof(H98A)=Sof(H98B)=
 Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(C101)=
 Sof(H10C)=Sof(H10D)=1-FVAR(7)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(H46A)=
 Sof(H46B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C63)=
 Sof(H63A)=Sof(H63B)=FVAR(7)
 Fixed Sof: C8(0.5) C9(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
5.a Ternary CH refined with riding coordinates:
 C21(H21), C28(H28), C31(H31), C37(H37), C49(H49), C50(H50), C51(H51),
 C57(H57), C58(H58), C64(H64), C65(H65), C66(H66), C67(H67), C78(H78), C79(H79),
  C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86),
 C87(H87), C88(H88), C89(H89), C90(H90), C91(H91)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C14(H14A,H14B), C23(H23A,H23B), C29(H29A,H29B),
 C32(H32A,H32B), C33(H33A,H33B), C33(H33C,H33D), C35(H35A,H35B), C39(H39A,H39B),
  C39(H39C,H39D), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,
 H45B), C46(H46A,H46B), C46(H46C,H46D), C52(H52A,H52B), C52(H52C,H52D),
 C59(H59A,H59B), C60(H60A,H60B), C62(H62A,H62B), C63(H63A,H63B), C70(H70A,H70B),
  C72(H72A,H72B), C75(H75A,H75B), C76(H76A,H76B), C97(H97A,H97B), C98(H98A,
 H98B), C100(H10A,H10B), C101(H10C,H10D)
5.c Me refined with riding coordinates:
 C34(H34A,H34B,H34C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C36(H36), C38(H38), C53(H53), C54(H54), C55(H55), C61(H61), C68(H68),
  C93(H93), C96(H96)
5.e Fitted pentagon refined as free rotating group:
 C11(N1,C12,C13,N2), N4(C18,C19,N5,C20)
5.f Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C8,C9)
5.g X=CH2 refined with riding coordinates:
 C42(H42A,H42B), C44(H44A,H44B), C92(H92A,H92B), C94(H94A,H94B), C95(H95A,H95B)
5.h Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C56(H56A,H56B,H56C), C74(H74A,H74B,H74C), C77(H77A,H77B,
 H77C), C99(H99A,H99B,H99C)
;
_shelx_res_checksum              56012
_shelx_hkl_checksum              69268
_shelx_fab_checksum              7589
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'