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_4133991
_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         'C240 H278 B6 F24 N26 O12 Pd12 S12'
_chemical_formula_sum            'C240 H278 B6 F24 N26 O12 Pd12 S12'
_chemical_formula_weight         5901.28
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                112.829(3)
_cell_angle_beta                 103.394(3)
_cell_angle_gamma                101.148(4)
_cell_formula_units_Z            1
_cell_length_a                   15.8619(18)
_cell_length_b                   23.109(3)
_cell_length_c                   23.149(3)
_cell_measurement_reflns_used    9484
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.45
_cell_volume                     7218.4(16)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193.43
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0791
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            139364
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.475
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1210 before and 0.0822 after correction.
The Ratio of minimum to maximum transmission is 0.8468.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             2986
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.248
_refine_diff_density_min         -2.283
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1558
_refine_ls_number_reflns         25359
_refine_ls_number_restraints     622
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1620
_refine_ls_R_factor_gt           0.1450
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+432.5070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3419
_refine_ls_wR_factor_ref         0.3514
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20385
_reflns_number_total             25359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12309_si_003.cif
_cod_data_source_block           Complex_2b
_cod_original_cell_volume        7218.4(15)
_cod_database_code               4133991
_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
 F5-B2 = F8-B2 = F7-B2 = F6-B2
 1.34 with sigma of 0.01
 C98-C109
 1.32 with sigma of 0.01
 C97-C59 = C100-C97 = C93-C100
 1.54 with sigma of 0.02
 C108-C115
 1.54 with sigma of 0.02
 C87-C116 = C116-C115 = C115-C108
 1.49 with sigma of 0.01
 C87-C115
 2.46 with sigma of 0.01
 C116-C108
 2.46 with sigma of 0.01
 C87-C122 = C87-C116 = C116-C115 = C123-C122 = C121-C123 = C115-C108
 1.54 with sigma of 0.02
 C102-C99
 1.32 with sigma of 0.01
 C90-C102 = C90-C124
 1.54 with sigma of 0.02
 C125-C124 = C102-C99
 1.4 with sigma of 0.02
 N12-C114
 1.49 with sigma of 0.01
 C114-C119
 1.51 with sigma of 0.01
 C119-C120
 1.32 with sigma of 0.01
 C78-C91 = C114-C120
 2.55 with sigma of 0.01
 C119-C114 = C127-C126
 1.54 with sigma of 0.02
 C120-C119 = C127-C128
 1.4 with sigma of 0.02
 C103-C75
 1.54 with sigma of 0.02
 C86-C85
 1.54 with sigma of 0.02
 C111-C113
 1.54 with sigma of 0.02
 C103-C75 = C105-C103
 1.54 with sigma of 0.02
 C87-C116 = C87-C122 = C116-C115 = C123-C122 = C115-C108 = C121-C123
 1.54 with sigma of 0.02
 C122-C121 = C116-C108
 2.5 with sigma of 0.04
 C87-C115 = C87-C123
 2.5 with sigma of 0.04
 C126-C128
 2.5 with sigma of 0.04
 C75-C105
 2.5 with sigma of 0.04
 F5-F6 \\sim F5-F7 \\sim F5-F8 \\sim F6-F7 \\sim F6-F8 \\sim F7-F8
 with sigma of 0.001
 C90-C102 \\sim C90-C124
 with sigma of 0.02
 C90-C99 \\sim C90-C125
 with sigma of 0.04
 N12-C114 \\sim N12-C126
 with sigma of 0.02
 N12-C119 \\sim C119-C127
 with sigma of 0.04
3. Rigid bond restraints
 C60, C26, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C39, N8, N6, C71, C79
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C112 \\sim C113 \\sim C111 \\sim C107: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C74 \\sim C86 \\sim C85 \\sim C110: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
F6 \\sim F8 \\sim B2 \\sim F5 \\sim F7: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C11 \\sim C6 \\sim C51: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
N13 \\sim C117 \\sim C118: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C87 \\sim C116 \\sim C115 \\sim C108: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C87 \\sim O3 \\sim C122 \\sim C116 \\sim C123 \\sim C115 \\sim C121 \\sim C108:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C90 \\sim C102 \\sim C124 \\sim C125 \\sim C99: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C114 \\sim C119 \\sim C120: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C126 \\sim C114 \\sim C119 \\sim C127 \\sim C128 \\sim C120 \\sim N12: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
B3 \\sim F4 \\sim F2 \\sim F3 \\sim F1: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C71) \\sim Ueq, Uanis(C100) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C98) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C75) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C123) \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C116)
\\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C108) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C124) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C125)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C126) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C127) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C128) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(B3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim
Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C94) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C109)
\\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C97) \\sim Ueq,
Uanis(C59) \\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C116)
\\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C106) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F9) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C105)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C60) = Uanis(C72)
Uanis(C80) = Uanis(C77)
Uanis(C48) = Uanis(C6)
5. Others
 Sof(H87C)=Sof(H87D)=Sof(C121)=Sof(H12C)=Sof(H12D)=Sof(H12E)=Sof(C122)=
 Sof(H12F)=Sof(H12G)=Sof(C123)=Sof(H12H)=Sof(H12I)=1-FVAR(1)
 Sof(H87A)=Sof(H87B)=Sof(C108)=Sof(H10R)=Sof(H10S)=Sof(H10T)=Sof(C115)=
 Sof(H11L)=Sof(H11M)=Sof(C116)=Sof(H11N)=Sof(H11O)=FVAR(1)
 Sof(H90C)=Sof(H90D)=Sof(C124)=Sof(H124)=Sof(C125)=Sof(H12J)=Sof(H12K)=1-FVAR(2)
 Sof(H90A)=Sof(H90B)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(C102)=Sof(H102)=FVAR(2)
 Sof(C126)=Sof(H12L)=Sof(H12M)=Sof(C127)=Sof(H127)=Sof(C128)=Sof(H12N)=
 Sof(H12O)=1-FVAR(3)
 Sof(C114)=Sof(H11J)=Sof(H11K)=Sof(C119)=Sof(H119)=Sof(C120)=Sof(H12A)=
 Sof(H12B)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C13(H13), C16(H16), C18(H18),
 C19(H19), C22(H22), C23(H23), C32(H32), C33(H33), C34(H34), C36(H36), C41(H41),
  C42(H42), C45(H45), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54),
 C58(H58), C64(H64), C84(H84), C89(H89)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C59(H59A,H59B), C65(H65A,H65B), C70(H70A,H70B), C74(H74A,H74B),
 C75(H75A,H75B), C78(H78A,H78B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B),
  C87(H87C,H87D), C90(H90A,H90B), C90(H90C,H90D), C92(H92A,H92B), C95(H95A,
 H95B), C96(H96A,H96B), C97(H97A,H97B), C100(H10A,H10B), C103(H10E,H10F),
 C104(H10G,H10H), C111(H11D,H11E), C112(H11F,H11G), C113(H11H,H11I), C114(H11J,
 H11K), C115(H11L,H11M), C116(H11N,H11O), C122(H12F,H12G), C123(H12H,H12I),
 C126(H12L,H12M)
6.c Me refined with riding coordinates:
 C105(H10I,H10J,H10K), C106(H10L,H10M,H10N)
6.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C15(H15), C20(H20), C27(H27), C28(H28), C35(H35), C38(H38), C43(H43),
 C47(H47), C48(H48), C56(H56), C57(H57), C60(H60), C61(H61), C66(H66), C67(H67),
  C69(H69), C71(H71), C72(H72), C73(H73), C76(H76), C77(H77), C79(H79),
 C82(H82), C83(H83), C88(H88), C94(H94), C102(H102), C109(H109), C119(H119),
 C124(H124), C127(H127)
6.e X=CH2 refined with riding coordinates:
 C81(H81A,H81B), C91(H91A,H91B), C98(H98A,H98B), C99(H99A,H99B), C101(H10C,
 H10D), C120(H12A,H12B), C125(H12J,H12K), C128(H12N,H12O)
6.f Idealised Me refined as rotating group:
 C93(H93A,H93B,H93C), C107(H10O,H10P,H10Q), C108(H10R,H10S,H10T), C110(H11A,
 H11B,H11C), C118(H11P,H11Q,H11R), C121(H12C,H12D,H12E)
;
_shelx_res_checksum              46980
_shelx_hkl_checksum              26133
_shelx_fab_checksum              85094
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'