Reversible Structural Transformation between a Molecular Solomon Link and an Unusual Unsymmetrical Trefoil Knot.
Zhang, Hai-Ning; Gao, Wen-Xi; Lin, Yue-Jian; Jin, Guo-Xin; Journal of the American Chemical Society 141 (2019) 16057–16063; doi:10.1021/jacs.9b08254

data_4128335
_publ_section_title
;
 Reversible Structural Transformation between a Molecular Solomon Link and
 an Unusual Unsymmetrical Trefoil Knot.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16057
_journal_page_last               16063
_journal_paper_doi               10.1021/jacs.9b08254
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C52 H52 Ag2 Ir2 N10, 2(C F3 O3 S)'
_chemical_formula_sum            'C66 H70 Ag2 F6 Ir2 N16 O6 S2'
_chemical_formula_weight         1961.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-14
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                83.111(2)
_cell_angle_beta                 82.152(2)
_cell_angle_gamma                77.693(2)
_cell_formula_units_Z            1
_cell_length_a                   9.1921(5)
_cell_length_b                   13.8664(7)
_cell_length_c                   15.1426(7)
_cell_measurement_reflns_used    1674
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.62
_cell_measurement_theta_min      4.02
_cell_volume                     1859.83(16)
_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      173.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0607
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20228
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.960
_diffrn_reflns_theta_min         2.850
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.238
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1434 before and 0.0789 after correction. 
The Ratio of minimum to maximum transmission is 0.5804. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.864
_refine_diff_density_min         -1.958
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7055
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0640P)^2^+0.3298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6126
_reflns_number_total             7055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08254_si_004.cif
_cod_data_source_block           4
_cod_database_code               4128335
_shelx_estimated_absorpt_t_max   0.290
_shelx_estimated_absorpt_t_min   0.233
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Uiso/Uaniso restraints and constraints 
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 
3.a Aromatic/amide H refined with riding coordinates: 
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13) 
3.b Idealised Me refined as rotating group: 
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B, 
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C) 
;
_shelx_res_checksum              88410
_shelx_hkl_checksum              61000
_shelx_fab_checksum              90452
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'