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_4133997
_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         'C436 H398 B12 F48 N77 Pd24 S24'
_chemical_formula_sum            'C436 H398 B12 F48 N77 Pd24 S24'
_chemical_formula_weight         11081.10
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   42.8160(19)
_cell_length_b                   42.8160(19)
_cell_length_c                   76.435(3)
_cell_measurement_reflns_used    9385
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.23
_cell_measurement_theta_min      2.30
_cell_volume                     121349(9)
_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      150.01
_diffrn_measured_fraction_theta_full 0.998
_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  0.0658
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       90
_diffrn_reflns_limit_l_min       -90
_diffrn_reflns_number            229254
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.064
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2195
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             49797
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.508
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1471
_refine_ls_number_reflns         23763
_refine_ls_number_restraints     351
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0733
_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^)+(0.1363P)^2^+1666.5083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2000
_refine_ls_wR_factor_ref         0.2603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14505
_reflns_number_total             23763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12309_si_008.cif
_cod_data_source_block           Complex_4a
_cod_original_cell_volume        121349(12)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4133997
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C67-C66
 1.32 with sigma of 0.01
 C94-C93
 1.32 with sigma of 0.01
 C66-C65 = C105-C104 = C93-C92 = C31-C30 = C54-C53
 1.5 with sigma of 0.01
 C55-C54
 1.32 with sigma of 0.01
 N19-C107
 1.15 with sigma of 0.01
 C106-C104
 2.54 with sigma of 0.01
 C68-C69
 1.32 with sigma of 0.01
 C69-C70
 1.5 with sigma of 0.01
 C68-C70
 2.54 with sigma of 0.001
 C29-C30
 1.32 with sigma of 0.01
 C108-N19
 2.78 with sigma of 0.01
 C108-C107
 1.5 with sigma of 0.01
 F7-B2 = F5-B2 = F6-B2 = F8-B2
 1.34 with sigma of 0.01
 C70-C69 \\sim C70-C0AA
 with sigma of 0.02
 C70-C68 \\sim C70-C1AA
 with sigma of 0.04
 C30-C29 \\sim C30-C2AA
 with sigma of 0.02
 C31-C2AA \\sim C31-C29
 with sigma of 0.04
 F17-B2 \\sim F1AA-B2 \\sim F27-B2 \\sim F0AA-B2
 with sigma of 0.02
 F17-F1AA \\sim F1AA-F0AA \\sim F0AA-F27 \\sim F27-F17
 with sigma of 0.04
 F7-F5 \\sim F7-F6 \\sim F7-F8 \\sim F5-F6 \\sim F5-F8 \\sim F6-F8
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C70 \\sim C69 \\sim C0AA \\sim C1AA \\sim C68: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C30 \\sim C2AA \\sim C29: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
F7 \\sim F17 \\sim F5 \\sim F27 \\sim F8 \\sim F0AA \\sim F6 \\sim F1AA: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(B2) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C106) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C8) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C21)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C16) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.005
Uanis(C108) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(N19) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.005
Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(F7) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
Uanis(F5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F17) \\sim Ueq, Uanis(F27) \\sim Ueq, Uanis(F0AA) \\sim Ueq, Uanis(F6)
\\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F1AA) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(F5) = Uanis(F8)
4. Others
 Sof(H70C)=Sof(H70D)=Sof(C0AA)=Sof(H0AA)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=1-FVAR(1)
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(H69)=Sof(H70A)=Sof(H70B)=FVAR(1)
 Sof(H30A)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=1-FVAR(2)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H30)=FVAR(2)
 Sof(F0AA)=Sof(F1AA)=Sof(F17)=Sof(F27)=1-FVAR(3)
 Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=FVAR(3)
 Fixed Sof: N19(0.25) C107(0.5) C108(0.5) H10E(0.5) H10F(0.5) H10G(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14A), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C53(H53A,H53B), C65(H65A,H65B), C70(H70A,H70B), C70(H70C,
 H70D), C92(H92A,H92B), C104(H10A,H10B)
5.c Me refined with riding coordinates:
 C108(H10E,H10F,H10G)
5.d Aromatic/amide H refined with riding coordinates:
 N14(H14), C30(H30), C30(H30A), C33(H33), C34(H34), C36(H36), C37(H37),
 C39(H39), C40(H40), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51),
  C54(H54), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63),
 C66(H66), C69(H69), C71(H71), C72(H72), C75(H75), C76(H76), C78(H78), C79(H79),
  C84(H84), C85(H85), C87(H87), C88(H88), C89(H89), C90(H90), C93(H93),
 C96(H96), C97(H97), C99(H99), C100(H100), C101(H101), C102(H102), C105(H105),
 C0AA(H0AA)
5.e X=CH2 refined with riding coordinates:
 C29(H29A,H29B), C55(H55A,H55B), C67(H67A,H67B), C68(H68A,H68B), C94(H94A,
 H94B), C106(H10C,H10D), C2AA(H2AA,H2AB), C1AA(H1AA,H1AB)
5.f Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C)
;
_shelx_res_checksum              11457
_shelx_hkl_checksum              99075
_shelx_fab_checksum              35094
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'