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_4128338
_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         'C188 H182 Ag2 Ir6 N22, 3.5(C F3 O3 S)'
_chemical_formula_sum            'C210 H228 Ag2 F18 Ir6 N24 O26 S6'
_chemical_formula_weight         5407.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-23
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                90
_cell_angle_beta                 101.089(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.2902(19)
_cell_length_b                   21.3553(16)
_cell_length_c                   36.871(3)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.33
_cell_measurement_theta_min      3.30
_cell_volume                     21860(3)
_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      172.99
_diffrn_measured_fraction_theta_full 0.999
_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           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            146245
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.579
_diffrn_reflns_theta_min         3.288
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.531
_exptl_absorpt_correction_T_max  0.4568
_exptl_absorpt_correction_T_min  0.3381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1305 before and 0.0698 after correction. 
The Ratio of minimum to maximum transmission is 0.7401. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       block
_exptl_crystal_F_000             10712
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.056
_refine_diff_density_min         -3.174
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2349
_refine_ls_number_reflns         42453
_refine_ls_number_restraints     447
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+50.4112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.1794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30962
_reflns_number_total             42453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08254_si_005.cif
_cod_data_source_block           5
_cod_original_cell_volume        21859(3)
_cod_database_code               4128338
_shelx_estimated_absorpt_t_max   0.561
_shelx_estimated_absorpt_t_min   0.441
_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 
 C161-C162 = C162-C163 = C179-C180 = C180-C181 
 1.4 with sigma of 0.02 
 C179-C184 
 1.5 with sigma of 0.02 
 S3-C191 
 1.8 with sigma of 0.02 
 S1-O3 = S2-O4 = S2-O5 = S2-O6 = S3-O7 = S3-O8 = S3-O9 
 1.42 with sigma of 0.02 
 O7-O8 = O7-O9 = O8-O9 
 2.4 with sigma of 0.03 
 C190-F4 = C190-F5 = C190-F6 = C191-F7 = C191-F8 = C191-F9 
 1.35 with sigma of 0.02 
 S4-O11 
 1.35 with sigma of 0.02 
3. Rigid bond restraints 
 C190, F4, C163, C168, S4, C192, C192, F11 
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02 
4. Uiso/Uaniso restraints and constraints 
O12 \\sim O12': within 2A with sigma of 0.02 and sigma for terminal atoms of 
0.05 
S3 \\sim O7 \\sim O8 \\sim O9 \\sim C191 \\sim F7 \\sim F8 \\sim F9: within 2A 
with sigma of 0.02 and sigma for terminal atoms of 0.05 
Uanis(C162) \\sim Ueq, Uanis(C179) \\sim Ueq, Uanis(C180) \\sim Ueq, Uanis(S3) 
\\sim Ueq, Uanis(C191) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, 
Uanis(O9) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim 
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(S4) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) 
\\sim Ueq, Uanis(C192) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, 
Uanis(F12) \\sim Ueq, Uanis(S4') \\sim Ueq: with sigma of 0.02 and sigma for 
terminal atoms of 0.04 
Uanis(O10') \\sim Ueq, Uanis(O11') \\sim Ueq, Uanis(O12') \\sim Ueq, 
Uanis(C292) \\sim Ueq, Uanis(F10') \\sim Ueq, Uanis(F11') \\sim Ueq, 
Uanis(F12') \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F5) \\sim 
Ueq, Uanis(F6) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, 
Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) 
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C130) \\sim Ueq, Uanis(C131) \\sim Ueq, Uanis(C132) \\sim Ueq, 
Uanis(C135) \\sim Ueq, Uanis(C136) \\sim Ueq, Uanis(C137) \\sim Ueq, 
Uanis(C138) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C161) \\sim Ueq, Uanis(C162) \\sim Ueq, Uanis(C163) \\sim Ueq, 
Uanis(C164) \\sim Ueq, Uanis(C165) \\sim Ueq, Uanis(C166) \\sim Ueq, 
Uanis(C167) \\sim Ueq, Uanis(C168) \\sim Ueq: with sigma of 0.02 and sigma for 
terminal atoms of 0.04 
Uanis(C179) \\sim Ueq, Uanis(C180) \\sim Ueq, Uanis(C181) \\sim Ueq, 
Uanis(C182) \\sim Ueq, Uanis(C183) \\sim Ueq, Uanis(C184) \\sim Ueq, 
Uanis(C185) \\sim Ueq, Uanis(C186) \\sim Ueq, Uanis(C187) \\sim Ueq, 
Uanis(C188) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 
Uanis(S2) \\sim Ueq, Uanis(C190) \\sim Ueq: with sigma of 0.01 and sigma for 
terminal atoms of 0.02 
5. Others 
 Sof(S4')=Sof(O10')=Sof(O11')=Sof(O12')=Sof(C292)=Sof(F10')=Sof(F11')= 
 Sof(F12')=1-FVAR(1) 
 Sof(S4)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(C192)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1) 
 Fixed Sof: O7(0.5) O8(0.5) O9(0.5) S3(0.5) F7(0.5) F8(0.5) F9(0.5) C191(0.5) 
6.a Secondary CH2 refined with riding coordinates: 
 C62(H62A,H62B), C75(H75A,H75B), C86(H86A,H86B), C99(H99A,H99B), C110(H11A, 
 H11B), C123(H12A,H12B) 
6.b Aromatic/amide H refined with riding coordinates: 
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), 
 C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), 
  C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), 
 C41(H41), C46(H46), C47(H47), C48(H48), C49(H49), C52(H52), C53(H53), C54(H54), 
  C55(H55), C57(H57), C58(H58), C60(H60), C61(H61), C64(H64), C65(H65), 
 C67(H67), C68(H68), C70(H70), C71(H71), C73(H73), C74(H74), C76(H76), C77(H77), 
  C79(H79), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C88(H88), 
 C89(H89), C91(H91), C92(H92), C94(H94), C95(H95), C97(H97), C98(H98), 
 C100(H100), C101(H101), C103(H103), C104(H104), C105(H105), C106(H106), 
 C108(H108), C109(H109), C112(H112), C113(H113), C115(H115), C116(H116), 
 C118(H118), C119(H119), C121(H121), C122(H122), C124(H124), C125(H125), 
 C127(H127), C128(H128) 
6.c Idealised Me refined as rotating group: 
 C134(H13A,H13B,H13C), C135(H13D,H13E,H13F), C136(H13G,H13H,H13I), C137(H13J, 
 H13K,H13L), C138(H13M,H13N,H13O), C144(H14A,H14B,H14C), C145(H14D,H14E,H14F), 
 C146(H14G,H14H,H14I), C147(H14J,H14K,H14L), C148(H14M,H14N,H14O), C154(H15A, 
 H15B,H15C), C155(H15D,H15E,H15F), C156(H15G,H15H,H15I), C157(H15J,H15K,H15L), 
 C158(H15M,H15N,H15O), C164(H16A,H16B,H16C), C165(H16D,H16E,H16F), C166(H16G, 
 H16H,H16I), C167(H16J,H16K,H16L), C168(H16M,H16N,H16O), C174(H17A,H17B,H17C), 
 C175(H17D,H17E,H17F), C176(H17G,H17H,H17I), C177(H17J,H17K,H17L), C178(H17M, 
 H17N,H17O), C184(H18A,H18B,H18C), C185(H18D,H18E,H18F), C186(H18G,H18H,H18I), 
 C187(H18J,H18K,H18L), C188(H18M,H18N,H18O) 
;
_shelx_res_checksum              73473
_shelx_hkl_checksum              75415
_shelx_fab_checksum              52513
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'