Selective synthesis and structural transformation between a molecular ring-in-ring architecture and an abnormal trefoil knot
Dang, Li-Long; Gao, Xiang; Lin, Yue-Jian; Jin, Guo-Xin; Chemical Science  (2020) –; doi:10.1039/D0SC02733B

data_1558592
_publ_section_title
;
 Selective synthesis and structural transformation between a molecular
 ring-in-ring architecture and an abnormal trefoil knot
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02733B
_journal_year                    2020
_chemical_formula_moiety
'C124 H112 Ir4 N16 O8, 2(C F3 O3 S), 2(C3 H7 N O), O'
_chemical_formula_sum            'C154 H182 F12 Ir4 N24 O33 S4'
_chemical_formula_weight         4022.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-26
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_audit_update_record
;
2020-06-17 deposited with the CCDC.	2020-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4001(8)
_cell_length_b                   56.956(2)
_cell_length_c                   13.5367(4)
_cell_measurement_reflns_used    5972
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.66
_cell_measurement_theta_min      3.43
_cell_volume                     16499.4(10)
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      172.98
_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           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       72
_diffrn_reflns_limit_k_min       -72
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            61156
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         58.000
_diffrn_reflns_theta_min         3.428
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.054
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.4410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1158 before and 0.0851 after correction. 
The Ratio of minimum to maximum transmission is 0.5867. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       block
_exptl_crystal_F_000             8072
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.142
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.109(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         17437
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0528
_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^)+(0.1035P)^2^+4.6692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1604
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                14355
_reflns_number_total             17437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02733b1.cif
_cod_data_source_block           platon_sq_CCDC2
_cod_original_cell_volume        16499.3(10)
_cod_database_code               1558592
_shelx_estimated_absorpt_t_max   0.377
_shelx_estimated_absorpt_t_min   0.231
_olex2_refinement_description
; 
1. Twinned data refinement 
 Scales: 0.891(17) 0.109(17) 
2. 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 
3. Restrained distances 
 C63-F1 = C63-F2 = C63-F3 
 1.35 with sigma of 0.02 
 S1-C63 
 1.8 with sigma of 0.02 
 C46-C51 = C57-C62 
 1.5 with sigma of 0.02 
 C44-C45 = C45-C46 = C53-C54 = C54-C55 
 1.4 with sigma of 0.02 
 H13-H51B 
 2.2 with sigma of 0.1 
4. Rigid bond restraints 
 C11, C12, C12, C13, C44, C49, C55, C60, C57, C62 
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02 
 C63, F1 
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02 
5. Uiso/Uaniso restraints and constraints 
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) 
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, 
Uanis(C54) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(C63) 
\\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq: with 
sigma of 0.02 and sigma for terminal atoms of 0.04 
6.a Secondary CH2 refined with riding coordinates: 
 C20(H20A,H20B), C37(H37A,H37B) 
6.b Me refined with riding coordinates: 
 C60(H60A,H60B,H60C) 
6.c Aromatic/amide H refined with riding coordinates: 
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), 
 C15(H15), C16(H16), C18(H18), C19(H19), C23(H23), C25(H25), C26(H26), C31(H31), 
  C33(H33), C34(H34), C38(H38), C39(H39), C41(H41), C42(H42), C65(H65) 
6.d Idealised Me refined as rotating group: 
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B, 
 H51C), C52(H52A,H52B,H52C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A, 
 H61B,H61C), C62(H62A,H62B,H62C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C) 
;
_shelx_res_checksum              67852
_shelx_fab_checksum              87694
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'