Same knot, longer rope: altering ligand geometry provides control over nuclearity in self-assembled trefoil knots.
Wang, Qi-Li-Sha; Lin, Yue-Jian; Jin, Guo-Xin; Chemical communications (Cambridge, England) 57 (2021) 9772–9775; doi:10.1039/d1cc03699h

data_7128914
_publ_section_title
;
 Same knot, longer rope: altering ligand geometry provides control over
 nuclearity in self-assembled trefoil knots.
;
_journal_issue                   76
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9772
_journal_page_last               9775
_journal_paper_doi               10.1039/d1cc03699h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C120 H112 N12 O12 Rh4, 2(C F3 O3 S), C H4 O, H2 O, O'
_chemical_formula_sum            'C138 H172 F12 N14 O41 Rh4 S4'
_chemical_formula_weight         3450.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-08-11
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) 
;
_audit_update_record
;
2021-05-31 deposited with the CCDC.	2021-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                111.167(4)
_cell_angle_beta                 104.102(4)
_cell_angle_gamma                94.488(4)
_cell_formula_units_Z            2
_cell_length_a                   18.7640(13)
_cell_length_b                   20.0235(12)
_cell_length_c                   23.0409(15)
_cell_measurement_reflns_used    6715
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      56.58
_cell_measurement_theta_min      2.47
_cell_volume                     7696.2(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1710
_diffrn_reflns_av_unetI/netI     0.2305
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            93371
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.499
_diffrn_reflns_theta_max         67.499
_diffrn_reflns_theta_min         2.150
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.742
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1210 before and 0.0836 after correction. 
The Ratio of minimum to maximum transmission is 0.6756. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             3556
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.300
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.00114(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1539
_refine_ls_number_reflns         27676
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1772
_refine_ls_R_factor_gt           0.1095
_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^)+(0.1469P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2902
_refine_ls_wR_factor_ref         0.3584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12260
_reflns_number_total             27676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03699h2.cif
_cod_data_source_block           platon_sq_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7128912--7128915.cif.'
_cod_database_code               7128914
_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, All O(H) groups, All O(H,H) groups 
2. Restrained distances 
 C67-C68 = C72-C73 
 1.41 with sigma of 0.02 
 C122-F5 
 1.32 with sigma of 0.02 
 S2-O17 
 1.43 with sigma of 0.02 
 C104-C105 = C105-C101 = C112-C113 = C113-C114 
 1.4 with sigma of 0.02 
 C63-C64 
 1.5 with sigma of 0.02 
 H25A-O26 = H26A-O13 = H26B-O1 
 2 with sigma of 0.05 
3. Rigid bond restraints 
 C64, C73, C65, C66, C67, C68 
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02 
 C111, C112 
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02 
 S2, O17 
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02 
4. Uiso/Uaniso restraints and constraints 
Uanis(C105) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(O17) 
\\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, 
Uanis(C111) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq, 
Uanis(C115) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C117) \\sim Ueq, 
Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq: with sigma of 0.02 and sigma for 
terminal atoms of 0.04 
Uanis(O18) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(C118) \\sim Ueq: with sigma of 
0.01 and sigma for terminal atoms of 0.02 
5.a Free rotating group: 
 O26(H26A,H26B) 
5.b Secondary CH2 refined with riding coordinates: 
 C39(H39A,H39B), C50(H50A,H50B), C63(H63A,H63B), C74(H74A,H74B) 
5.c Aromatic/amide H refined with riding coordinates: 
 C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16), 
 C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32), 
  C33(H33), C34(H34), C36(H36), C37(H37), C41(H41), C43(H43), C44(H44), 
 C46(H46), C48(H48), C49(H49), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), 
  C58(H58), C60(H60), C61(H61), C65(H65), C66(H66), C68(H68), C70(H70), 
 C71(H71), C73(H73), C76(H76), C77(H77), C79(H79), C80(H80) 
5.d Idealised Me refined as rotating group: 
 C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C89(H89A,H89B, 
 H89C), C90(H90A,H90B,H90C), C96(H96A,H96B,H96C), C97(H97A,H97B,H97C), C98(H98A, 
 H98B,H98C), C99(H99A,H99B,H99C), C100(H10A,H10B,H10C), C106(H10D,H10E,H10F), 
 C107(H10G,H10H,H10I), C108(H10J,H10K,H10L), C109(H10M,H10N,H10O), C110(H11A, 
 H11B,H11C), C116(H11D,H11E,H11F), C117(H11G,H11H,H11I), C118(H11J,H11K,H11L), 
 C119(H11M,H11N,H11O), C120(H12A,H12B,H12C), C125(H12D,H12E,H12F) 
5.e Idealised tetrahedral OH refined as rotating group: 
 O25(H25A) 
;
_shelx_res_checksum              35380
_shelx_hkl_checksum              8003
_shelx_fab_checksum              95549
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'