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_4128336
_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
'C116 H116 Ir4 N12, 4(C F3 O3 S), 0.5(C4 H10 O), 1.5(C2 H3 N)'
_chemical_formula_sum            'C130 H141 F12 Ir4 N16 O16.5 S4'
_chemical_formula_weight         3316.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-03-03
_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                 106.495(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   49.616(2)
_cell_length_b                   15.5826(7)
_cell_length_c                   37.8111(16)
_cell_measurement_reflns_used    9439
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.91
_cell_measurement_theta_min      3.23
_cell_volume                     28030(2)
_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      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0735
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            156300
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.908
_diffrn_reflns_theta_min         3.204
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.793
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.3815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1641 before and 0.0830 after correction. 
The Ratio of minimum to maximum transmission is 0.5081. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       block
_exptl_crystal_F_000             13160
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         2.940
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details
; 
 Refined as a perfect inversion twin. 
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3196
_refine_ls_number_reflns         49817
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0784P)^2^+46.4785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                48477
_reflns_number_total             49817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08254_si_003.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C130 H141 F12 Ir4 N16 O16.50 S4'
_cod_database_code               4128336
_shelx_estimated_absorpt_t_max   0.259
_shelx_estimated_absorpt_t_min   0.081
_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 
 S7-C239 = S7'-C339 
 1.8 with sigma of 0.02 
 S8-O22 
 1.43 with sigma of 0.01 
 S7-O19 = S7-O20 = S7-O21 = S8-O23 = S8-O24 
 1.43 with sigma of 0.02 
 C240-F22 = C240-F23 = C240-F24 
 1.35 with sigma of 0.02 
 C339-F19' = C339-F20' = C339-F21' 
 1.35 with sigma of 0.02 
 C237-F15 = C239-F19 = C239-F20 = C239-F21 
 1.35 with sigma of 0.02 
 C241-C242 = C243-C244 
 1.52 with sigma of 0.03 
 C242-O25 = C243-O25 
 1.42 with sigma of 0.02 
 C249-N27 
 1.15 with sigma of 0.03 
 C249-C250 
 1.45 with sigma of 0.03 
3. Uiso/Uaniso restraints and constraints 
S7 \\sim S7': within 2A with sigma of 0.02 and sigma for terminal atoms of 0.05 
Uanis(C185) \\sim Ueq, Uanis(C186) \\sim Ueq: with sigma of 0.01 and sigma for 
terminal atoms of 0.02 
Uanis(O13) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) 
\\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(C45) \\sim Ueq, 
Uanis(C46) \\sim Ueq, Uanis(C155) \\sim Ueq, Uanis(C156) \\sim Ueq: with sigma 
of 0.02 and sigma for terminal atoms of 0.04 
Uanis(S7) \\sim Ueq, Uanis(C239) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20) 
\\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(S7') \\sim Ueq, Uanis(C339) \\sim Ueq, 
Uanis(F19') \\sim Ueq, Uanis(F20') \\sim Ueq, Uanis(F21') \\sim Ueq: with sigma 
of 0.02 and sigma for terminal atoms of 0.04 
Uanis(C241) \\sim Ueq, Uanis(C242) \\sim Ueq, Uanis(C243) \\sim Ueq, 
Uanis(C244) \\sim Ueq, Uanis(C247) \\sim Ueq, Uanis(C249) \\sim Ueq, 
Uanis(C250) \\sim Ueq, Uanis(N26) \\sim Ueq, Uanis(N27) \\sim Ueq: with sigma 
of 0.02 and sigma for terminal atoms of 0.04 
Uanis(O16) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(C39) 
\\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(F22) \\sim Ueq, 
Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq: with sigma of 0.02 and sigma for 
terminal atoms of 0.04 
4. Others 
 Sof(S7')=Sof(O19')=Sof(O20')=Sof(O21')=Sof(C339)=Sof(F19')=Sof(F20')= 
 Sof(F21')=1-FVAR(1) 
 Sof(S7)=Sof(O19)=Sof(O20)=Sof(O21)=Sof(C239)=Sof(F19)=Sof(F20)=Sof(F21)=FVAR(1) 
5.a Secondary CH2 refined with riding coordinates: 
 C34(H34A,H34B), C47(H47A,H47B), C58(H58A,H58B), C71(H71A,H71B), C150(H15A, 
 H15B), C163(H16A,H16B), C174(H17A,H17B), C187(H18A,H18B), C242(H24D,H24E), 
 C243(H24F,H24G) 
5.b Me refined with riding coordinates: 
 C222(H22G,H22H,H22I) 
5.c 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), 
  C29(H29), C30(H30), C32(H32), C33(H33), C36(H36), C37(H37), C39(H39), 
 C40(H40), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48), C49(H49), C51(H51), 
  C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C60(H60), C61(H61), 
 C63(H63), C64(H64), C66(H66), C67(H67), C69(H69), C70(H70), C72(H72), C73(H73), 
  C75(H75), C76(H76), C120(H120), C121(H121), C122(H122), C123(H123), 
 C126(H126), C127(H127), C128(H128), C129(H129), C134(H134), C135(H135), 
 C136(H136), C137(H137), C140(H140), C141(H141), C142(H142), C143(H143), 
 C145(H145), C146(H146), C148(H148), C149(H149), C152(H152), C153(H153), 
 C155(H155), C156(H156), C158(H158), C159(H159), C161(H161), C162(H162), 
 C164(H164), C165(H165), C167(H167), C168(H168), C169(H169), C170(H170), 
 C172(H172), C173(H173), C176(H176), C177(H177), C179(H179), C180(H180), 
 C182(H182), C183(H183), C185(H185), C186(H186), C188(H188), C189(H189), 
 C191(H191), C192(H192) 
5.d Idealised Me refined as rotating group: 
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B, 
 H85C), C86(H86A,H86B,H86C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C94(H94A, 
 H94B,H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C102(H10A,H10B,H10C), 
 C103(H10D,H10E,H10F), C104(H10G,H10H,H10I), C105(H10J,H10K,H10L), C106(H10M, 
 H10N,H10O), C112(H11A,H11B,H11C), C113(H11D,H11E,H11F), C114(H11G,H11H,H11I), 
 C115(H11J,H11K,H11L), C116(H11M,H11N,H11O), C198(H19A,H19B,H19C), C199(H19D, 
 H19E,H19F), C200(H20A,H20B,H20C), C201(H20D,H20E,H20F), C202(H20G,H20H,H20I), 
 C208(H20J,H20K,H20L), C209(H20M,H20N,H20O), C210(H21A,H21B,H21C), C211(H21D, 
 H21E,H21F), C212(H21G,H21H,H21I), C218(H21J,H21K,H21L), C219(H21M,H21N,H21O), 
 C220(H22A,H22B,H22C), C221(H22D,H22E,H22F), C228(H22J,H22K,H22L), C229(H22M, 
 H22N,H22O), C230(H23A,H23B,H23C), C231(H23D,H23E,H23F), C232(H23G,H23H,H23I), 
 C241(H24A,H24B,H24C), C244(H24H,H24I,H24J), C246(H24K,H24L,H24M), C248(H24N, 
 H24O,H24P), C250(H25A,H25B,H25C) 
;
_shelx_res_checksum              97932
_shelx_hkl_checksum              98740
_shelx_fab_checksum              2272
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'