Effects of turn-structure on folding and entanglement in artificial molecular overhand knots.
Song, Yiwei; Schaufelberger, Fredrik; Ashbridge, Zoe; Pirvu, Lucian; Vitorica-Yrezabal, Iñigo J; Leigh, David A.; Chemical science 12 (2020) 1826–1833; doi:10.1039/d0sc05897a

data_1559742
_publ_section_title
;
 Effects of turn-structure on folding and entanglement in artificial
 molecular overhand knots.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1826
_journal_page_last               1833
_journal_paper_doi               10.1039/d0sc05897a
_journal_volume                  12
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C119 H125 Lu N9 O20, 3(C F3 O3 S), 0.792(C2 H3 N)'
_chemical_formula_sum            'C123.64 H127.46 F9 Lu N9.82 O29 S3'
_chemical_formula_weight         2657.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-07-27 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2976(2)
_cell_length_b                   25.7772(2)
_cell_length_c                   38.6074(7)
_cell_measurement_reflns_used    27278
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.9260
_cell_measurement_theta_min      1.5630
_cell_volume                     13233.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 179.00   1.00    0.10   0.00   0.00   0.00    --   179
  2  \w   -145.00  24.00   1.00    0.10    --   30.00   0.00   0.00  169
  3  \w   -145.00  24.00   1.00    0.10    --   30.00   0.00 120.00  169
  4  \w   -145.00  24.00   1.00    0.10    --   30.00   0.00 240.00  169
;
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0418254000
_diffrn_orient_matrix_UB_12      0.0143404000
_diffrn_orient_matrix_UB_13      0.0043679000
_diffrn_orient_matrix_UB_21      0.0032943000
_diffrn_orient_matrix_UB_22      0.0131330000
_diffrn_orient_matrix_UB_23      -0.0155126000
_diffrn_orient_matrix_UB_31      -0.0303900000
_diffrn_orient_matrix_UB_32      -0.0183295000
_diffrn_orient_matrix_UB_33      -0.0076652000
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            175761
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.503
_diffrn_reflns_theta_min         1.531
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             5480
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 5425 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.050(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     1957
_refine_ls_number_reflns         27068
_refine_ls_number_restraints     2940
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0780
_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^)+(0.1589P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2195
_refine_ls_wR_factor_ref         0.2503
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                15935
_reflns_number_total             27068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05897a2.cif
_cod_data_source_block           m_za218_2_c1_col1_
_cod_depositor_comments
;Adding full bibliography for 1559742.cif.

 Adding full bibliography for 1559742.cif.
;
_cod_database_code               1559742
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         LuSFONCH
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.910
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C127-C126
 1.35 with sigma of 0.02
 O37-C46
 1.45 with sigma of 0.02
 C46-C36
 2.5 with sigma of 0.02
 C174-C175
 1.35 with sigma of 0.02
 C35-C33
 2.5 with sigma of 0.02
 C173-C175
 2.5 with sigma of 0.02
 O37-C35
 2.5 with sigma of 0.02
 C159-C161
 2.5 with sigma of 0.02
 C160-O158
 2.5 with sigma of 0.02
 C161-C159
 2.45 with sigma of 0.02
 C128-C126
 2.5 with sigma of 0.02
 C127-C128
 1.35 with sigma of 0.02
 C77-C78
 1.5 with sigma of 0.02
 C167-O172
 1.45 with sigma of 0.02
 O172-C173
 1.45 with sigma of 0.02
 O172-C166 = C173-C167
 2.5 with sigma of 0.02
 O34-C32
 2.5 with sigma of 0.02
 C17-C23 = O22-C24
 2.5 with sigma of 0.02
 S21A-F22A
 2.6 with sigma of 0.02
 O31-C33
 2.5 with sigma of 0.02
 O25-C27 = C30-C32
 2.5 with sigma of 0.02
 C174-C173
 1.54 with sigma of 0.02
 O25-C23
 2.5 with sigma of 0.02
 C24-C23
 1.54 with sigma of 0.02
 C29-C30
 1.54 with sigma of 0.02
 C24-C26
 2.5 with sigma of 0.02
 O28-C26 = C27-C29
 2.5 with sigma of 0.02
 O139-C140
 1.45 with sigma of 0.02
 C140-C142
 2.45 with sigma of 0.02
 C142-C140
 2.45 with sigma of 0.02
 O28-C30
 2.5 with sigma of 0.02
 O34-C36
 2.5 with sigma of 0.02
 F21A-F22A
 2.35 with sigma of 0.02
 F23A-F21A
 2.35 with sigma of 0.02
 C175-C174 \\sim C161-C160
 with sigma of 0.02
 C47-O37 \\sim O37-C45
 with sigma of 0.02
 C173-C175 \\sim C159-C161
 with sigma of 0.04
 C45-C44 \\sim C45A-C44A
 with sigma of 0.02
 C44-C43 \\sim C44A-C43A
 with sigma of 0.02
 O37-C36 \\sim O22-C23 \\sim O25-C24 \\sim O25-C26 \\sim O28-C27 \\sim O28-C29
\\sim O31-C30 \\sim O31-C32
 \\sim O34-C33 \\sim O34-C35
 with sigma of 0.02
 C47-C46 \\sim C47A-C46A
 with sigma of 0.02
 C46-C44 \\sim C46A-C44A
 with sigma of 0.04
 C46-C45 \\sim C46A-C45A
 with sigma of 0.02
 C24-C23 \\sim C27-C26 \\sim C30-C29 \\sim C32-C33 \\sim C36-C35
 with sigma of 0.02
 C44-C39 \\sim C44A-C39A
 with sigma of 0.02
 C40-C48 \\sim C40A-C48
 with sigma of 0.04
 C42-C41 \\sim C42A-C41A
 with sigma of 0.02
 C41-C40 \\sim C41A-C40A
 with sigma of 0.02
 O37-C46 \\sim O37A-C46A
 with sigma of 0.02
 O76-C77 \\sim O76-C75 \\sim O73-C74 \\sim O79-C78 \\sim O79-C80 \\sim O82-C81
\\sim O82-C83 \\sim O85-C84
 \\sim O85-C86 \\sim O88-C87
 with sigma of 0.01
 C41-C48 \\sim C41A-C48
 with sigma of 0.02
 C40-C39 \\sim C40A-C39A
 with sigma of 0.02
 C45-C43 \\sim C45A-C43A
 with sigma of 0.04
 C44-C40 \\sim C44A-C40A
 with sigma of 0.04
 C43-C41 \\sim C43A-C41A
 with sigma of 0.04
 C42-C48 \\sim C42A-C48
 with sigma of 0.04
 C38-C47 \\sim C38A-C47A
 with sigma of 0.02
 C38-C43 \\sim C38A-C43A
 with sigma of 0.02
 C43-C42 \\sim C43A-C42A
 with sigma of 0.02
 C167-C173 \\sim C153-C159
 with sigma of 0.04
 C45-C39 \\sim C45A-C39A
 with sigma of 0.04
 C44-C42 \\sim C44A-C42A
 with sigma of 0.04
 C126-C127 \\sim C140-C141
 with sigma of 0.02
 O37-C47 \\sim O37A-C47A
 with sigma of 0.04
 C43-C39 \\sim C43A-C39A
 with sigma of 0.04
 O37-C45 \\sim O37A-C45A
 with sigma of 0.04
 C168-C167 \\sim C154-C153
 with sigma of 0.02
 C42-C40 \\sim C42A-C40A
 with sigma of 0.04
 C173-O172 \\sim C159-O158
 with sigma of 0.02
 O172-C174 \\sim O158-C160
 with sigma of 0.04
 C41-C39 \\sim C41A-C39A
 with sigma of 0.04
 C47-C43 \\sim C47A-C43A
 with sigma of 0.04
 C167-O172 \\sim C153-O158
 with sigma of 0.02
 C36-C46 \\sim C36A-C46A
 with sigma of 0.04
 C173-C174 \\sim C159-C160
 with sigma of 0.02
 C126-C128 \\sim C140-C142
 with sigma of 0.04
 C38-C46 \\sim C38A-C46A
 with sigma of 0.04
 C38-C44 \\sim C38A-C44A
 with sigma of 0.04
 C38-C42 \\sim C38A-C42A
 with sigma of 0.04
 C47-C45 \\sim C47A-C45A
 with sigma of 0.04
 C128-C127 \\sim C142-C141
 with sigma of 0.02
 C169-C167 \\sim C155-C153
 with sigma of 0.04
 C120-C127 \\sim C134-C141
 with sigma of 0.04
 C165-C167 \\sim C151-C153
 with sigma of 0.04
 C167-C166 \\sim C153-C152
 with sigma of 0.02
 C127-O125 \\sim C141-O139
 with sigma of 0.04
 C124-C123 \\sim C130-C131
 with sigma of 0.02
 C128-O125 \\sim C142-O139
 with sigma of 0.04
 C120-C126 \\sim C134-C140
 with sigma of 0.04
 C126-O125 \\sim C140-O139
 with sigma of 0.04
 C124-C129 \\sim C130-C129
 with sigma of 0.02
 C124-C118 \\sim C130-C136
 with sigma of 0.04
 C124-C122 \\sim C130-C132
 with sigma of 0.04
 C168-O172 \\sim C154-O158
 with sigma of 0.04
 C169-C168 \\sim C155-C154
 with sigma of 0.02
 C166-O172 \\sim C152-O158
 with sigma of 0.04
 C170-C168 \\sim C156-C154
 with sigma of 0.04
 C116-C113 \\sim C113-C124
 with sigma of 0.02
 C168-C166 \\sim C154-C152
 with sigma of 0.04
 S21A-O23A \\sim S21A-O22A \\sim S21A-O21A \\sim S11A_$1-O11A_$1 \\sim
S11A_$1-O13A_$1 ~
 S11A_$1-O12A_$1
 with sigma of 0.02
 F12A-C11A \\sim F13A-C11A \\sim F11A-C11A \\sim F22A_$2-C21A_$2 \\sim
F23A_$2-C21A_$2 ~
 F21A_$2-C21A_$2
 with sigma of 0.02
 S11A-C11A \\sim S21A_$2-C21A_$2
 with sigma of 0.02
 C129-C116 \\sim C129-C138
 with sigma of 0.02
 C116-C117 \\sim C138-C137
 with sigma of 0.02
 C119-O125 \\sim C135-O139
 with sigma of 0.04
 C117-C118 \\sim C137-C136
 with sigma of 0.02
 C118-C123 \\sim C136-C131
 with sigma of 0.02
 C118-C119 \\sim C136-C135
 with sigma of 0.02
 C123-C119 \\sim C131-C135
 with sigma of 0.04
 C123-C122 \\sim C131-C132
 with sigma of 0.02
 C121-C119 \\sim C133-C135
 with sigma of 0.04
 C117-C119 \\sim C137-C135
 with sigma of 0.04
 C118-C120 \\sim C136-C134
 with sigma of 0.04
 C117-C123 \\sim C137-C131
 with sigma of 0.04
 C121-C120 \\sim C133-C134
 with sigma of 0.02
 C118-C122 \\sim C136-C132
 with sigma of 0.04
 C120-C119 \\sim C134-C135
 with sigma of 0.02
 C120-O125 \\sim C134-O139
 with sigma of 0.02
 C123-C121 \\sim C131-C133
 with sigma of 0.04
 C122-C120 \\sim C132-C134
 with sigma of 0.04
 C121-O125 \\sim C133-O139
 with sigma of 0.04
 C129-C117 \\sim C129-C137
 with sigma of 0.04
 C129-C123 \\sim C129-C131
 with sigma of 0.04
 C122-C121 \\sim C132-C133
 with sigma of 0.02
 C116-C118 \\sim C138-C136
 with sigma of 0.04
 S1A-F1A \\sim S1A-F3A \\sim S1A-F2A
 with sigma of 0.04
 C1A-F1A \\sim C1A-F3A \\sim C1A-F2A
 with sigma of 0.02
 S1A-O2A \\sim S1A-O1A \\sim S1A-O3A
 with sigma of 0.02
 O2A-O1A \\sim O1A-O3A \\sim O2A-O3A
 with sigma of 0.04
 F1A-F3A \\sim F3A-F2A \\sim F2A-F1A
 with sigma of 0.04
 C1A-O2A \\sim C1A-O1A \\sim C1A-O3A
 with sigma of 0.04
 C165-C169 \\sim C151-C155
 with sigma of 0.04
 C164-C170 \\sim C150-C156
 with sigma of 0.04
 C170-C166 \\sim C156-C152
 with sigma of 0.04
 C163-C164 \\sim C149-C150
 with sigma of 0.02
 C162-C163 \\sim C148-C149
 with sigma of 0.02
 C164-C165 \\sim C150-C151
 with sigma of 0.02
 C171-C162 \\sim C157-C148
 with sigma of 0.02
 C165-C170 \\sim C151-C156
 with sigma of 0.02
 C165-C166 \\sim C151-C152
 with sigma of 0.02
 C170-C169 \\sim C156-C155
 with sigma of 0.02
 C146-C162 \\sim C146-C148
 with sigma of 0.02
 C164-C166 \\sim C150-C152
 with sigma of 0.04
 C146-C171 \\sim C146-C157
 with sigma of 0.04
 C146-C163 \\sim C146-C149
 with sigma of 0.04
 C171-C163 \\sim C157-C149
 with sigma of 0.04
 C171-C165 \\sim C157-C151
 with sigma of 0.04
 C171-C169 \\sim C157-C155
 with sigma of 0.04
 C162-C164 \\sim C148-C150
 with sigma of 0.04
 C162-C170 \\sim C148-C156
 with sigma of 0.04
 C171-C170 \\sim C157-C156
 with sigma of 0.02
 C163-C165 \\sim C149-C151
 with sigma of 0.04
 C68-C67 \\sim C67-C66
 with sigma of 0.02
 C67-C66 \\sim C68-C67 \\sim C69-C68 \\sim C70-C69 \\sim C71-C70 \\sim C71-C66
 with sigma of 0.01
 O34-C35 \\sim O34A-C35A
 with sigma of 0.02
 C32-C33 \\sim C32A-C33A
 with sigma of 0.02
 O22-C24 \\sim O1-C24A
 with sigma of 0.04
 O22-C23 \\sim O1-C23A
 with sigma of 0.02
 O28-C29 \\sim O28A-C29A
 with sigma of 0.02
 O25-C26 \\sim O25A-C26A
 with sigma of 0.02
 O25-C27 \\sim O25A-C27A
 with sigma of 0.04
 O31-C32 \\sim O31A-C32A
 with sigma of 0.02
 O28-C26 \\sim O28A-C26A
 with sigma of 0.04
 O31-C29 \\sim O31A-C29A
 with sigma of 0.04
 C26-C27 \\sim C26A-C27A
 with sigma of 0.02
 O31-C33 \\sim O31A-C33A
 with sigma of 0.04
 O34-C32 \\sim O34A-C32A
 with sigma of 0.04
 O34-C36 \\sim O34A-C36A
 with sigma of 0.04
 O37-C35 \\sim O37A-C35A
 with sigma of 0.04
 C17-C23 \\sim C17-C23A
 with sigma of 0.04
 C24-C26 \\sim C24A-C26A
 with sigma of 0.04
 O25-C23 \\sim O25A-C23A
 with sigma of 0.04
 C27-C29 \\sim C27A-C29A
 with sigma of 0.04
 O22-C17 \\sim O1-C17
 with sigma of 0.02
 C30-C32 \\sim C30A-C32A
 with sigma of 0.04
 O25-C24 \\sim O25A-C24A
 with sigma of 0.02
 O28-C27 \\sim O28A-C27A
 with sigma of 0.02
 O31-C30 \\sim O31A-C30A
 with sigma of 0.02
 C33-C35 \\sim C33A-C35A
 with sigma of 0.04
 O34-C33 \\sim O34A-C33A
 with sigma of 0.02
 O28-C30 \\sim O28A-C30A
 with sigma of 0.04
 O37-C36 \\sim O37A-C36A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 O21A-C21A \\sim O23A-C21A \\sim O22A-C21A
 with sigma of 0.02
 S21A-F23A \\sim S21A-F22A \\sim S21A-F21A
 with sigma of 0.02
3. Restrained planarity
 O158, C148, C149, C150, C151, C152, C153, C154, C155, C156, C157
 with sigma of 0.1
 O172, C167, C168, C169, C170, C171, C162, C163, C164, C165, C166
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C11 \\sim C10: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C173 \\sim C174 \\sim C175 \\sim C159 \\sim C160 \\sim C161: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
O172 \\sim C173 \\sim C174 \\sim C175 \\sim O158 \\sim C159 \\sim C160 \\sim
C161: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within
2A
O22 \\sim O25 \\sim O28 \\sim O31 \\sim O34 \\sim O37 \\sim C23 \\sim C24 \\sim
C26 \\sim C27 \\sim C29 \\sim C30 \\sim C32 \\sim C33 \\sim C35 \\sim C36:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C167 \\sim C168 \\sim C169 \\sim C170 \\sim C171 \\sim C162 \\sim C163 \\sim
C164 \\sim C165 \\sim C166 \\sim O172 \\sim C173 \\sim C174 \\sim C175: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O73 \\sim O76 \\sim O79 \\sim O82 \\sim O85 \\sim O88 \\sim C74 \\sim C75 \\sim
C77 \\sim C78 \\sim C80 \\sim C81 \\sim C83 \\sim C84 \\sim C86 \\sim C87:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C38 \\sim C47 \\sim C45 \\sim C44 \\sim C43 \\sim C42 \\sim C41 \\sim C40 \\sim
C39 \\sim C41A \\sim C40A \\sim C39A \\sim C44A \\sim C45A \\sim C47A \\sim
C38A \\sim C43A \\sim C42A \\sim C46 \\sim C46A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O125 \\sim C126 \\sim C127 \\sim C128 \\sim O139 \\sim C140 \\sim C141 \\sim
C142: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
C41 \\sim C41A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C42A \\sim C41A \\sim C40A \\sim C39A \\sim C44A \\sim C43A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C116 \\sim C130: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O172 \\sim O158: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
S1A \\sim F1A \\sim F2A \\sim F3A \\sim O1A \\sim O2A \\sim O3A \\sim C1A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C153 \\sim C154 \\sim C155 \\sim C156 \\sim C157 \\sim C148 \\sim C149 \\sim
C150 \\sim C151 \\sim C152: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
C124 \\sim C138: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C148 \\sim C162 \\sim C163 \\sim C149 \\sim C165 \\sim C164 \\sim C150 \\sim
C171 \\sim C170 \\sim C157 \\sim C156 \\sim C151 \\sim C169 \\sim C155 \\sim
C154 \\sim C153 \\sim C168 \\sim C152 \\sim C167 \\sim C166: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O31 \\sim O34 \\sim O37 \\sim C29 \\sim C30 \\sim C32 \\sim C33 \\sim C35 \\sim
C36 \\sim O37A \\sim C36A \\sim C35A \\sim O34A \\sim C33A \\sim C32A \\sim
O31A \\sim C30A \\sim C29A \\sim O22 \\sim O25 \\sim O28 \\sim C23 \\sim C24
\\sim C26 \\sim C27 \\sim O28A \\sim C27A \\sim C26A \\sim O25A \\sim C24A
\\sim C23A \\sim O1 \\sim C17: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 O22, O25, O28, O31, O34, O37, C12, C13, C14, C15, C16, C17, C18, C19, C20,
 C21, C23, C24, C26, C27, C29, C30, C32, C33, C35, C36, C38, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C40, C39, C44, C45, C46, C47, C38, C43, C42, O37, C36, C35, O34, C33,
 C32, C30, O31, C29, O28, C27, C26, O25, C24, C23, O22, C17, C18, C19, C20, C15,
  C16, C21, C12, C13, C14
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C162, C163, C164, C165, C166, C167, C168, C169, C170, C171, O172, C173, C174,
 C175
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C162, C163, C164, C165, C166, C167, C168, C169, C170, C171, C146, O172, C173,
 C174, C175
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O73, O76, O79, O82, O85, O88, C63, C64, C65, C66, C67, C68, C69, C70, C67,
 C72, C63, C64, C65, C66, C71, C72, C74, C75, C78, C80, C81, C83, C84, C86, C87
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C74, C75, O76, C77, C78, O79, C80, C81, O82, C83, C84, O85
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C152, O139, C157, O158, C130, C131, C132, C153, C133, C159, C134, C135, N19,
 C136, C150, C137, C151, H137, H152, C138, C154, H138, C155, C140, C156, C141,
 C160, C161, C142, C50, C148, C52, C149
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C148, C149, C150, C151, C152, C153, C154, C155, C156, C157, O158, C159, C160,
 C161
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1A, F1A, F2A, F3A, O1A, O2A, O3A, C1A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S21A, F21A, F22A, F23A, O21A, O22A, O23A, C21A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C129, C124, C123, C122, C121, C120, C119, C118, C117, C116, O125, C126, C127,
 C128
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C129, C124, C123, C122, C121, C120, C119, C118, C117, C116, O125
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C129, C138, C137, C136, C135, C134, C133, C132, C131, C130
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C94, C95, C96, C97, C98, C89, C90, C91, C92, C93, O88
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(O139)=Sof(C130)=Sof(H130)=Sof(C131)=Sof(C132)=Sof(H132)=Sof(C133)=
 Sof(H133)=Sof(C134)=Sof(C135)=Sof(H135)=Sof(C136)=Sof(C137)=Sof(H137)=
 Sof(C138)=Sof(H138)=Sof(C140)=Sof(H14E)=Sof(H14F)=Sof(C141)=Sof(H141)=
 Sof(C142)=Sof(H14G)=Sof(H14H)=1-FVAR(1)
 Sof(O125)=Sof(C124)=Sof(H124)=Sof(C116)=Sof(H116)=Sof(C117)=Sof(H117)=
 Sof(C118)=Sof(C123)=Sof(C122)=Sof(H122)=Sof(C121)=Sof(H121)=Sof(C120)=
 Sof(C119)=Sof(H119)=Sof(C126)=Sof(H12A)=Sof(H12B)=Sof(C127)=Sof(H127)=
 Sof(C128)=Sof(H12C)=Sof(H12D)=FVAR(1)
 Sof(H14A)=Sof(O158)=Sof(C148)=Sof(C149)=Sof(H149)=Sof(C150)=Sof(H150)=
 Sof(C151)=Sof(C152)=Sof(H152)=Sof(C153)=Sof(C154)=Sof(H154)=Sof(C155)=
 Sof(H155)=Sof(C156)=Sof(C157)=Sof(H157)=Sof(C159)=Sof(H15A)=Sof(H15B)=
 Sof(C160)=Sof(H160)=Sof(C161)=Sof(H16A)=Sof(H16B)=Sof(N19)=Sof(C50)=Sof(H50A)=
 Sof(H50B)=Sof(H50C)=Sof(C52)=1-FVAR(2)
 Sof(H146)=Sof(O172)=Sof(C171)=Sof(H171)=Sof(C162)=Sof(C163)=Sof(H163)=
 Sof(C164)=Sof(H164)=Sof(C165)=Sof(C170)=Sof(C169)=Sof(H169)=Sof(C168)=
 Sof(H168)=Sof(C167)=Sof(C166)=Sof(H166)=Sof(C173)=Sof(H17A)=Sof(H17B)=
 Sof(C174)=Sof(H174)=Sof(C175)=Sof(H17C)=Sof(H17D)=FVAR(2)
 Sof(H48A)=Sof(C41A)=Sof(C40A)=Sof(H40A)=Sof(C39A)=Sof(H39A)=Sof(C44A)=
 Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(C47A)=Sof(H47A)=Sof(C38A)=Sof(H38A)=
 Sof(C43A)=Sof(C42A)=Sof(H42A)=Sof(O37A)=Sof(C36A)=Sof(H36C)=Sof(H36D)=
 Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(O34A)=Sof(C33A)=Sof(H33C)=Sof(H33D)=
 Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(O31A)=Sof(C30A)=Sof(H30C)=Sof(H30D)=
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(O28A)=Sof(C27A)=Sof(H27C)=Sof(H27D)=
 Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(O25A)=Sof(C24A)=Sof(H24C)=Sof(H24D)=
 Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(O1)=1-FVAR(3)
 Sof(O22)=Sof(O25)=Sof(O28)=Sof(O31)=Sof(O34)=Sof(O37)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=
 Sof(H27A)=Sof(H27B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C38)=Sof(H38)=Sof(C47)=Sof(H47)=
 Sof(C46)=Sof(C45)=Sof(H45)=Sof(C44)=Sof(C43)=Sof(C42)=Sof(H42)=Sof(C41)=
 Sof(C40)=Sof(H40)=Sof(C39)=Sof(H39)=Sof(H48)=FVAR(3)
7.a Riding coordinates:
 C128(H12C,H12D), C175(H17C,H17D), C142(H14G,H14H), C161(H16A,H16B)
7.b Free rotating group:
 C1A(S1A,F1A,F2A,F3A,O1A,O2A,O3A)
7.c Ternary CH refined with riding coordinates:
 C10(H10), C48(H48), C48(H48A), C61(H61), C99(H99), C113(H113), C146(H146),
 C146(H14A)
7.d Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,
 H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B),
 C36(H36A,H36B), C74(H74A,H74B), C75(H75A,H75B), C77(H77A,H77B), C78(H78A,H78B),
  C80(H80A,H80B), C81(H81A,H81B), C83(H83A,H83B), C84(H84A,H84B), C86(H86A,
 H86B), C87(H87A,H87B), C126(H12A,H12B), C173(H17A,H17B), C140(H14E,H14F),
 C159(H15A,H15B), C36A(H36C,H36D), C35A(H35C,H35D), C33A(H33C,H33D), C32A(H32C,
 H32D), C30A(H30C,H30D), C29A(H29C,H29D), C27A(H27C,H27D), C26A(H26C,H26D),
 C24A(H24C,H24D), C23A(H23C,H23D)
7.e Me refined with riding coordinates:
 C50(H50A,H50B,H50C)
7.f Aromatic/amide H refined with riding coordinates:
 N9(H9), N50(H50), N60(H60), N101(H101), N112(H112), N145(H145), C3(H3),
 C4(H4), C5(H5), C13(H13), C14(H14), C16(H16), C18(H18), C19(H19), C21(H21),
 C38(H38), C47(H47), C45(H45), C42(H42), C40(H40), C39(H39), C56(H56), C57(H57),
  C58(H58), C69(H69), C70(H70), C67(H67), C72(H72), C64(H64), C65(H65),
 C90(H90), C91(H91), C93(H93), C95(H95), C96(H96), C98(H98), C105(H105),
 C106(H106), C107(H107), C124(H124), C116(H116), C117(H117), C122(H122),
 C121(H121), C119(H119), C127(H127), C171(H171), C163(H163), C164(H164),
 C169(H169), C168(H168), C166(H166), C174(H174), C130(H130), C132(H132),
 C133(H133), C135(H135), C137(H137), C138(H138), C141(H141), C149(H149),
 C150(H150), C152(H152), C154(H154), C155(H155), C157(H157), C160(H160),
 C40A(H40A), C39A(H39A), C45A(H45A), C47A(H47A), C38A(H38A), C42A(H42A)
7.g Fitted hexagon refined as free rotating group:
 C15(C16,C17,C18,C19,C20), C72(C63,C64,C65,C66,C71)
7.h Naphthalene refined as free rotating group:
 C38(C47,C46,C45,C44,C43,C42,C41,C40,C39), C124(C129,C116,C117,C118,C123,C122,
 C121,C120,C119), C171(C162,C163,C164,C165,C170,C169,C168,C167,C166)
7.i Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C49(H49A,H49B,H49C), C62(H62A,H62B,H62C), C100(H10A,H10B,
 H10C), C114(H11D,H11E,H11F), C147(H14B,H14C,H14D)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94951
_shelx_fab_checksum              32694
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.657
_oxdiff_exptl_absorpt_empirical_full_min 0.365