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_4133996
_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         'C236 H300 B7 F28 N28 O16 Pd12 S12'
_chemical_formula_sum            'C236 H300 B7 F28 N28 O16 Pd12 S12'
_chemical_formula_weight         6054.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.525(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   50.785(3)
_cell_length_b                   23.3504(15)
_cell_length_c                   25.3445(17)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.24
_cell_volume                     29640(3)
_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      153.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0412
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            197515
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.212
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             12284
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.999
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1567
_refine_ls_number_reflns         26102
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1218P)^2^+415.6122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2382
_refine_ls_wR_factor_ref         0.2576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20232
_reflns_number_total             26102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12309_si_002.cif
_cod_data_source_block           Complex_2a
_cod_database_code               4133996
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.813
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C107-C108
 1.54 with sigma of 0.02
 F4-B1 = F1-B1 = F2-B1 = F3-B1
 1.34 with sigma of 0.001
 F5-B2 = F7-B2 = F8-B2 = F6-B2
 1.34 with sigma of 0.01
 C103-C104
 1.48 with sigma of 0.005
 C102-C103
 1.48 with sigma of 0.005
 C102-C101
 1.53 with sigma of 0.005
 C50-C49 = C51-C50
 1.48 with sigma of 0.01
 C80-C81
 1.48 with sigma of 0.005
 F10-B3 = F12-B3 = F9-B3
 1.34 with sigma of 0.01
 C74-C75
 1.45 with sigma of 0.001
 C74-C73
 1.53 with sigma of 0.005
 C48-C73
 3.96 with sigma of 0.01
 C75-C73
 2.5 with sigma of 0.005
 C51-C52
 1.53 with sigma of 0.01
 C75-C74
 1.54 with sigma of 0.02
 C75-C73
 2.5 with sigma of 0.04
 F3-F1 \\sim F3-F2 \\sim F3-F4 \\sim F1-F2 \\sim F1-F4 \\sim F2-F4
 with sigma of 0.001
 F5-F7 \\sim F5-F8 \\sim F5-F6 \\sim F7-F8 \\sim F7-F6 \\sim F8-F6
 with sigma of 0.001
 F12-F11 \\sim F12-F9 \\sim F12-F10 \\sim F11-F9 \\sim F11-F10 \\sim F9-F10
 with sigma of 0.001
3. Rigid bond restraints
 C29, N2, C30, C31, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C57, N5, C59, C58, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C104 \\sim C103 \\sim C102 \\sim C101: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C84 \\sim C83: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C110 \\sim C109 \\sim C108 \\sim C107: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
B1 \\sim F3 \\sim F1 \\sim F4 \\sim F2 \\sim F6 \\sim B2 \\sim F5 \\sim F7
\\sim F8: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C51 \\sim C50 \\sim C49: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C73 \\sim C74 \\sim C75 \\sim C76: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C49 \\sim C50 \\sim C51 \\sim C52: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C113) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C82) \\sim Ueq,
Uanis(C81) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(F9)
\\sim Ueq, Uanis(F12) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(F10) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F4AA) \\sim Ueq, Uanis(C115)
\\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C75) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(B3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(B2)
\\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq,
Uanis(F8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(B4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C74) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C48) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
5. Others
 Fixed Sof: F3(0.5) F1(0.5) B1(0.5) F4(0.5) F2(0.5) B2(0.5) F5(0.5) F6(0.5)
 F7(0.5) F8(0.5)
6.a Riding coordinates:
 C48(H48A,H48B,H48C), C73(H73A,H73B,H73C), C52(H52A,H52B,H52C)
6.b Ternary CH refined with riding coordinates:
 C26(H26), C25(H25), C14(H14), C27(H27), C24(H24), C11(H11), C8(H8), C6(H6),
 C17(H17), C16(H16), C15(H15), C5(H5), C18(H18), C3(H3), C19(H19), C28(H28),
 C13(H13), C20(H20), C7(H7), C21(H21), C4(H4), C12(H12), C23(H23), C9(H9),
 C1(H1), C10(H10), C2(H2), C22(H22)
6.c Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C49(H49A,H49B), C45(H45A,H45B), C50(H50A,H50B), C110(H11A,
 H11B), C111(H11C,H11D), C46(H46A,H46B), C105(H10A,H10B), C76(H76A,H76B),
 C104(H10C,H10D), C82(H82A,H82B), C53(H53A,H53B), C84(H84A,H84B), C81(H81A,
 H81B), C75(H75A,H75B), C47(H47A,H47B), C78(H78A,H78B), C80(H80A,H80B),
 C109(H10E,H10F), C103(H10J,H10K), C102(H10L,H10M), C108(H10Q,H10R), C51(H51A,
 H51B), C74(H74A,H74B)
6.d Aromatic/amide H refined with riding coordinates:
 C66(H66), C65(H65), C33(H33), C62(H62), C93(H93), C31(H31), C30(H30),
 C41(H41), C69(H69), C36(H36), C38(H38), C94(H94), C90(H90), C72(H72), C43(H43),
  C100(H100), C97(H97), C58(H58), C59(H59), C44(H44), C71(H71), C115(H115),
 C118(H118), C99(H99), C87(H87), C86(H86)
6.e Fitted pentagon refined as free rotating group:
 C29(N1,C31,C30,N2), C57(N6,C58,C59,N5)
6.f Idealised Me refined as rotating group:
 C117(H11H,H11I,H11J), C116(H11K,H11L,H11M), C56(H56A,H56B,H56C), C114(H11N,
 H11O,H11P), C54(H54A,H54B,H54C), C112(H11E,H11F,H11G), C77(H77A,H77B,H77C),
 C106(H10G,H10H,H10I), C107(H10N,H10O,H10P), C83(H83A,H83B,H83C), C79(H79A,H79B,
 H79C), C113(H11Q,H11R,H11S), C101(H10S,H10T,H10U)
;
_shelx_res_checksum              35366
_shelx_hkl_checksum              45881
_shelx_fab_checksum              13822
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'