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_4133988
_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         'C228 H206 B7 F28 N26 Pd12 S12'
_chemical_formula_sum            'C228 H206 B7 F28 N26 Pd12 S12'
_chemical_formula_weight         5579.39
_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             2019-11-13
_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            18
_cell_length_a                   43.2323(18)
_cell_length_b                   43.2323(18)
_cell_length_c                   76.187(3)
_cell_measurement_reflns_used    9039
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.29
_cell_volume                     123318(9)
_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      149.96
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       91
_diffrn_reflns_limit_l_min       -91
_diffrn_reflns_number            232964
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.366
_diffrn_reflns_theta_min         2.207
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2155
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             88494
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.222
_refine_diff_density_min         -2.351
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1507
_refine_ls_number_reflns         25111
_refine_ls_number_restraints     510
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+1461.7935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.1941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18960
_reflns_number_total             25111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12309_si_009.cif
_cod_data_source_block           Complex_4b
_cod_original_cell_volume        123318(12)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4133988
_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
 F8-B4 = F1-B4 = F2-B4 = F3-B4
 1.35 with sigma of 0.01
 C100-C105 = C101-C104 = C108-C106 = C76-C87 = C33-C91 = C56-C97
 1.47 with sigma of 0.01
 C109-C108 = C97-C90 = C111-C100 = C99-C76 = C91-C70
 1.32 with sigma of 0.01
 C81-C75
 1.4 with sigma of 0.02
 C80-C75
 1.4 with sigma of 0.02
 F14-B3 = F15-B3
 1.35 with sigma of 0.02
 F15-B3 = F13-B3 = F16-B3 = F14-B3
 1.35 with sigma of 0.01
 F13-B3
 1.35 with sigma of 0.02
 B5-F19
 1.35 with sigma of 0.02
 B5-F17 = B5-F20 = B5-F19 = B5-F18
 1.35 with sigma of 0.02
 C44-C79 \\sim C79-C78 \\sim C67-C78 \\sim C67-C77 \\sim C89-C77 \\sim C89-C54
\\sim C54-C44
 with sigma of 0.001
 C97-C90 \\sim C115-C97
 with sigma of 0.02
 C108-C106 \\sim C114-C106
 with sigma of 0.02
 C106-C116 \\sim C106-C109
 with sigma of 0.04
 F3-B4 \\sim F8-B4 \\sim F2-B4 \\sim F1-B4
 with sigma of 0.02
 F8-F2 \\sim F8-F3 \\sim F8-F1 \\sim F2-F3 \\sim F2-F1 \\sim F1-F8
 with sigma of 0.04
 F14-F16 \\sim F14-F15 \\sim F14-F13 \\sim F15-F16 \\sim F15-F13 \\sim F16-F13
 with sigma of 0.04
 F18-B5 \\sim F17-B5 \\sim F20-B5 \\sim F14-B5
 with sigma of 0.02
 F18-F17 \\sim F18-F20 \\sim F18-F14 \\sim F17-F20 \\sim F17-F14 \\sim F20-F14
 with sigma of 0.04
 F20-F19 \\sim F20-F17 \\sim F20-F18 \\sim F19-F18 \\sim F19-F17 \\sim F18-F17
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C105 \\sim C100 \\sim C111 \\sim N11: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C48 \\sim C72 \\sim C95 \\sim C94 \\sim C103 \\sim C84 \\sim C96: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01
C80 \\sim C75 \\sim C81 \\sim C53 \\sim C13 \\sim C47 \\sim C69: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
C90 \\sim C97 \\sim C115: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C108 \\sim C109 \\sim C114 \\sim C116 \\sim C106: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
B4 \\sim F3 \\sim F8 \\sim F2 \\sim F1: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C87 \\sim C76 \\sim C99: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C101 \\sim C117: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
B3 \\sim F16 \\sim F14 \\sim F13 \\sim F15: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
F13 \\sim B3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
B5 \\sim F17 \\sim F19 \\sim F18 \\sim F20: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C115) \\sim Ueq, Uanis(C90) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C108) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C116) \\sim Ueq,
Uanis(C109) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(B4) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F2) \\sim
Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C99) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C87) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C117) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F13) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(B3) \\sim Ueq, Uanis(F14)
\\sim Ueq, Uanis(F16) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(F13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(B5) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19)
\\sim Ueq, Uanis(F20) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(H97A)=Sof(C115)=Sof(H11C)=Sof(H11D)=1-FVAR(1)
 Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H97)=FVAR(1)
 Sof(H10G)=Sof(H10H)=Sof(C114)=Sof(H114)=Sof(C116)=Sof(H11E)=Sof(H11F)=1-FVAR(2)
 Sof(H10E)=Sof(H10F)=Sof(C108)=Sof(H108)=Sof(C109)=Sof(H10I)=Sof(H10J)=FVAR(2)
 Fixed Sof: B3(0.3) F13(0.3) F14(0.3) F15(0.3) F16(0.3) B5(0.2) F17(0.2)
 F18(0.2) F19(0.2) F20(0.2)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C44(H44), C47(H47), C48(H48), C53(H53), C54(H54), C61(H61),
 C67(H67), C69(H69), C72(H72), C73(H73), C75(H75), C77(H77), C78(H78), C79(H79),
  C80(H80), C81(H81), C83(H83), C84(H84), C86(H86), C88(H88), C89(H89),
 C93(H93), C94(H94), C95(H95), C96(H96), C98(H98), C103(H103)
5.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C56(H56A,H56B), C87(H87A,H87B), C104(H10A,H10B), C105(H10C,
 H10D), C106(H10E,H10F), C106(H10G,H10H)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C7(H7), C10(H10), C15(H15), C16(H16), C18(H18), C19(H19),
 C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30),
  C32(H32), C36(H36), C39(H39), C42(H42), C43(H43), C45(H45), C46(H46),
 C50(H50), C52(H52), C55(H55), C57(H57), C58(H58), C60(H60), C62(H62), C63(H63),
  C64(H64), C65(H65), C66(H66), C68(H68), C71(H71), C74(H74), C76(H76),
 C82(H82), C85(H85), C91(H91), C92(H92), C97(H97), C97(H97A), C100(H100),
 C101(H101), C102(H102), C107(H107), C108(H108), C114(H114)
5.d X=CH2 refined with riding coordinates:
 C70(H70A,H70B), C90(H90A,H90B), C99(H99A,H99B), C109(H10I,H10J), C111(H11A,
 H11B), C115(H11C,H11D), C116(H11E,H11F), C117(H11G,H11H)
5.e Idealised Me refined as rotating group:
 C113(H11I,H11J,H11K)
;
_shelx_res_checksum              88336
_shelx_hkl_checksum              43330
_shelx_fab_checksum              1279
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'