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_4133994
_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         'C260 H320 B6 F24 N24 O12 Pd12 S12'
_chemical_formula_sum            'C260 H320 B6 F24 N24 O12 Pd12 S12'
_chemical_formula_weight         6155.80
_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
_audit_creation_date             2019-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.462(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.852(3)
_cell_length_b                   31.236(4)
_cell_length_c                   25.397(4)
_cell_measurement_reflns_used    9664
_cell_measurement_temperature    167(2)
_cell_measurement_theta_max      66.65
_cell_measurement_theta_min      3.75
_cell_volume                     14266(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      166.94
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            288989
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.063
_diffrn_reflns_theta_max         67.063
_diffrn_reflns_theta_min         3.473
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.369
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4916
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             6268
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.867
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1646
_refine_ls_number_reflns         25216
_refine_ls_number_restraints     593
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+76.8863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1910
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23693
_reflns_number_total             25216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12309_si_004.cif
_cod_data_source_block           Complex_2c
_cod_original_cell_volume        14266(3)
_cod_database_code               4133994
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C24-C26
 2.55 with sigma of 0.01
 C25-C27
 2.55 with sigma of 0.01
 C27-C29
 2.55 with sigma of 0.01
 O6-C116
 2.55 with sigma of 0.01
 F4-B1 = F1-B1 = F3-B1 = F2-B1
 1.34 with sigma of 0.01
 O6-C115 = O5-C113 = O2-C24 = O3-C85 = O4-C87 = O1-C30
 1.47 with sigma of 0.01
 C90-C118
 1.5 with sigma of 0.01
 C118-C117 = C29-C28 = C35-C34
 1.52 with sigma of 0.01
 O4-C88
 2.52 with sigma of 0.01
 C90-C117
 2.55 with sigma of 0.01
 C90-C88
 2.55 with sigma of 0.01
 C25-C24 = C26-C25 = C27-C26 = C28-C27 = C114-C113 = C116-C115 = C88-C87 = C89-
 C88 = C90-C89 = C86-C85 = C31-C30 = C32-C31 = C33-C32 = C34-C33
 1.54 with sigma of 0.01
 C114-C113 = C121-C114 = C121-C119 = C124-C119 = C127-C124
 1.54 with sigma of 0.02
 C88-C87 = C89-C88 = C90-C89 = C90-C118 = C118-C117
 1.54 with sigma of 0.02
 C88-C87 = C89-C88
 1.54 with sigma of 0.02
 H88A-H89B_$1
 2.1 with sigma of 0.02
 C132-C116 = C125-C116 = C133-C132 = C126-C125 = C133-C135 = C131-C126 = C134-
 C135
 1.54 with sigma of 0.02
 C134-C131 = C135-C134
 1.54 with sigma of 0.02
 C86-C120 = C86-C130 = C130-C129 = C123-C120 = C123-C122 = C129-C128
 1.54 with sigma of 0.02
 C136-C137
 1.54 with sigma of 0.02
 C86-C130 = C136-C129 = C128-C122
 1.54 with sigma of 0.02
 C86-C85 = C86-C120 = C123-C120 = C130-C129 = C123-C122 = C137-C136 = C128-C122
 1.54 with sigma of 0.02
 C87-C89
 2.5 with sigma of 0.04
 C88-C90
 2.5 with sigma of 0.04
 C89-C118
 2.5 with sigma of 0.04
 C90-C117
 2.5 with sigma of 0.04
 C113-C121 = C114-C119 = C121-C124 = C119-C127
 2.5 with sigma of 0.04
 C87-C89 = C88-C90 = C89-C118 = C90-C117
 2.5 with sigma of 0.04
 C116-C133 = C116-C126 = C132-C135 = C133-C134 = C125-C131
 2.5 with sigma of 0.04
 C129-C137
 2.5 with sigma of 0.04
 C86-C129 = C130-C128 = C86-C123 = C120-C122
 2.5 with sigma of 0.04
 C130-C136 = C123-C128
 2.5 with sigma of 0.04
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F3-F4
 with sigma of 0.001
 C116-C132 \\sim C116-C125
 with sigma of 0.02
 C116-C133 \\sim C116-C126
 with sigma of 0.04
 C116-C135 \\sim C116-C131
 with sigma of 0.04
 C86-C130 \\sim C86-C120
 with sigma of 0.02
 C86-C129 \\sim C86-C123
 with sigma of 0.02
 C135-C134 \\sim C134-C131
 with sigma of 0.02
 C134-C126 \\sim C134-C133
 with sigma of 0.04
 C86-C128 \\sim C86-C122
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C85 \\sim C86: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C116: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C113 \\sim C114: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C87 \\sim C88 \\sim C89 \\sim C90 \\sim C118 \\sim C117: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.01
O4 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C118 \\sim C117: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.02
C114 \\sim C121 \\sim C119 \\sim C124 \\sim C127: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C116 \\sim C125 \\sim C132 \\sim C133 \\sim C126 \\sim C135 \\sim C134 \\sim
C131: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C120 \\sim C130 \\sim C86 \\sim C129 \\sim C123 \\sim C128 \\sim C122: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C136 \\sim C128 \\sim C122 \\sim C129: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F8) \\sim
Ueq, Uanis(F10) \\sim Ueq, Uanis(F12) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.005
Uanis(C32) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(B1) \\sim
Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(C112) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C121) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C124) \\sim Ueq,
Uanis(C127) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C132) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C133) \\sim Ueq,
Uanis(C126) \\sim Ueq, Uanis(C135) \\sim Ueq, Uanis(C134) \\sim Ueq,
Uanis(C131) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C137) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C128) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C120) \\sim Ueq, Uanis(C130) \\sim Ueq, Uanis(C123) \\sim Ueq,
Uanis(C129) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C122) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C136) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(H86C)=Sof(H86D)=Sof(C129)=Sof(H12U)=Sof(H12V)=Sof(C130)=Sof(H13A)=
 Sof(H13B)=Sof(C136)=Sof(H13Q)=Sof(H13R)=Sof(C137)=Sof(H13S)=Sof(H13T)=
 Sof(H13U)=1-FVAR(1)
 Sof(H86A)=Sof(H86B)=Sof(C120)=Sof(H12A)=Sof(H12B)=Sof(C122)=Sof(H12E)=
 Sof(H12F)=Sof(C123)=Sof(H12G)=Sof(H12H)=Sof(C128)=Sof(H12R)=Sof(H12S)=
 Sof(H12T)=FVAR(1)
 Sof(H11M)=Sof(H11N)=Sof(C132)=Sof(H13E)=Sof(H13F)=Sof(C133)=Sof(H13G)=
 Sof(H13H)=Sof(H13L)=Sof(H13M)=Sof(H13N)=Sof(C135)=Sof(H13O)=Sof(H13P)=1-FVAR(2)
 Sof(H11K)=Sof(H11L)=Sof(C125)=Sof(H12K)=Sof(H12L)=Sof(C126)=Sof(H12M)=
 Sof(H12N)=Sof(C131)=Sof(H13C)=Sof(H13D)=Sof(H13I)=Sof(H13J)=Sof(H13K)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
  C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
 C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C21(H21A,H21B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
  C33(H33A,H33B), C34(H34A,H34B), C66(H66A,H66B), C82(H82A,H82B), C85(H85A,
 H85B), C86(H86A,H86B), C86(H86C,H86D), C87(H87A,H87B), C88(H88A,H88B),
 C89(H89A,H89B), C90(H90A,H90B), C93(H93A,H93B), C110(H11A,H11B), C113(H11E,
 H11F), C114(H11G,H11H), C115(H11I,H11J), C116(H11K,H11L), C116(H11M,H11N),
 C118(H11R,H11S), C119(H11T,H11U), C120(H12A,H12B), C121(H12C,H12D), C122(H12E,
 H12F), C123(H12G,H12H), C124(H12I,H12J), C125(H12K,H12L), C126(H12M,H12N),
 C129(H12U,H12V), C130(H13A,H13B), C131(H13C,H13D), C132(H13E,H13F), C133(H13G,
 H13H), C135(H13O,H13P), C136(H13Q,H13R)
5.c Me refined with riding coordinates:
 C134(H13I,H13J,H13K), C134(H13L,H13M,H13N), C137(H13S,H13T,H13U)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C10(H10), C12(H12), C15(H15), C17(H17), C19(H19),
 C20(H20), C22(H22), C65(H65), C68(H68), C69(H69), C72(H72), C74(H74), C76(H76),
  C78(H78), C79(H79), C80(H80), C83(H83), C92(H92), C95(H95), C96(H96),
 C99(H99), C101(H101), C104(H104), C106(H106), C108(H108), C109(H109),
 C111(H111)
5.e X=CH2 refined with riding coordinates:
 C1(H1A,H1B), C23(H23A,H23B), C64(H64A,H64B), C84(H84A,H84B), C91(H91A,H91B),
 C112(H11C,H11D)
5.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C117(H11O,H11P,H11Q), C127(H12O,
 H12P,H12Q), C128(H12R,H12S,H12T)
;
_shelx_res_checksum              52851
_shelx_hkl_checksum              8737
_shelx_fab_checksum              38525
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'