Selective Construction of Very Large Stacking-Interaction-Induced Molecular 818 Metalla-knots and Borromean Ring Using Curved Dipyridyl Ligands
Zhang, Hai-Ning; Lin, Yue-Jian; Jin, Guo-Xin; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11925

data_4135464
_publ_section_title
;
 Selective Construction of Very Large Stacking-Interaction-Induced
 Molecular 818 Metalla-knots and Borromean Ring Using Curved Dipyridyl
 Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11925
_journal_year                    2020
_chemical_formula_moiety
'0.167(C488 H432 N16 O32 Rh16), 1.333(C F3 O3 S)'
_chemical_formula_sum            'C82.7 H72 F4 N2.7 O9.3 Rh2.7 S1.3'
_chemical_formula_weight         1645.335
_chemical_name_systematic        202209d
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_symmetry_Int_Tables_number      85
_audit_creation_date             2020-11-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   35.295(3)
_cell_length_b                   35.295(3)
_cell_length_c                   26.356(3)
_cell_measurement_reflns_used    9261
_cell_measurement_temperature    141.68
_cell_measurement_theta_max      52.78
_cell_measurement_theta_min      3.41
_cell_volume                     32833(5)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      141.68
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_Laue_measured_fraction_full 0.9993
_diffrn_reflns_Laue_measured_fraction_max 0.9993
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            172322
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.9993
_diffrn_reflns_theta_full        53.5942
_diffrn_reflns_theta_max         54.49
_diffrn_reflns_theta_min         2.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.562
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_crystal_colour            'dull dark blue'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    0.999
_exptl_crystal_description       block
_exptl_crystal_F_000             10092.961
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.4120
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.1355
_refine_ls_d_res_high            0.8239
_refine_ls_d_res_low             13.5418
_refine_ls_goodness_of_fit_ref   1.2154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    175
_refine_ls_number_parameters     1354
_refine_ls_number_reflns         30760
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.2151
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.1051
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3156
_refine_ls_wR_factor_ref         0.3676
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              42
_reflns_limit_h_min              0
_reflns_limit_k_max              42
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                17462
_reflns_number_total             30760
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c11925_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4135464
_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
 C83-C87
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C97 \\sim C93 \\sim C102: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
4.a :
 C93(C94,C95,C96,C97,C98,C99,C100,C101,C102,C103,C104,C105,C106,C107,C108,C109,
 C110,C111,C112)
4.b Secondary CH2 refined with riding coordinates:
 C45(H45a,H45b), C68(H68a,H68b)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17),
 C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35),
  C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C47(H47), C49(H49),
 C50(H50), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60),
  C61(H61), C63(H63), C64(H64), C66(H66), C70(H70), C72(H72), C73(H73),
 C76(H76), C77(H77), C78(H78), C79(H79), C81(H81), C82(H82)
4.d Idealised Me refined as rotating group:
 C88(H88a,H88b,H88c), C89(H89a,H89b,H89c), C90(H90a,H90b,H90c), C91(H91a,H91b,
 H91c), C92(H92a,H92b,H92c), C98(H98a,H98b,H98c), C99(H99a,H99b,H99c),
 C100(H10a,H10b,H10c), C101(H10d,H10e,H10f), C102(H10g,H10h,H10i), C108(H10j,
 H10k,H10l), C109(H10m,H10n,H10o), C110(H11a,H11b,H11c), C111(H11d,H11e,H11f),
 C112(H11g,H11h,H11i), C118(H11j,H11k,H11l), C119(H11m,H11n,H11o), C120(H12a,
 H12b,H12c), C121(H12d,H12e,H12f), C122(H12g,H12h,H12i)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'