From π-conjugated macrocycles to heterocycloarenes based on benzo[2,1-<i>b</i>:3,4-<i>b</i>']dithiophene (BDTh): size- and geometry-dependent host-guest properties.
An, Dongyue; Zhang, Rong; Zhu, Jiangyu; Wang, Teng; Zhao, Yan; Lu, Xuefeng; Liu, Yunqi; Chemical science 15 (2024) 4590–4601; doi:10.1039/d3sc05074b

data_1571056
_publ_section_title
;
 From &#x3c0;-conjugated macrocycles to heterocycloarenes based on
 benzo[2,1-<i>b</i>:3,4-<i>b</i>']dithiophene (BDTh): size- and
 geometry-dependent host-guest properties.
;
_journal_issue                   12
_journal_name_full               'Chemical science'
_journal_page_first              4590
_journal_page_last               4601
_journal_paper_doi               10.1039/d3sc05074b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(C120 H132 O12 S6), 0.167(C420)'
_chemical_formula_sum            'C310 H264 O24 S12'
_chemical_formula_weight         4757.93
_chemical_name_systematic        MS6T@C70
_space_group_crystal_system      cubic
_space_group_IT_number           206
_space_group_name_Hall           '-I 2b 2c 3'
_space_group_name_H-M_alt        'I a -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-01-15
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-22 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.5768(8)
_cell_length_b                   36.5768(8)
_cell_length_c                   36.5768(8)
_cell_measurement_reflns_used    3093
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      59.58
_cell_measurement_theta_min      2.96
_cell_volume                     48934.7(19)
_computing_cell_refinement       'SAINT V8.40B (bruker, 2016)'
_computing_data_collection       'SAINT V8.40B (bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            21400
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        63.722
_diffrn_reflns_theta_max         63.722
_diffrn_reflns_theta_min         2.959
_exptl_absorpt_coefficient_mu    1.553
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.5875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0480 before and 0.0393 after correction.
The Ratio of minimum to maximum transmission is 0.7808.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             20064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene, methanol, CS2'
_exptl_crystal_size_max          0.828
_exptl_crystal_size_mid          0.724
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.00010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.586
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         6435
_refine_ls_number_restraints     7176
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.2527
_refine_ls_R_factor_gt           0.1824
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4436
_refine_ls_wR_factor_ref         0.5144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2690
_reflns_number_total             6435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05074b2.cif
_cod_data_source_block           d3c70_0m
_cod_depositor_comments
'Adding full bibliography for 1571054--1571057.cif.'
_cod_original_cell_volume        48935(3)
_cod_database_code               1571056
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.360
_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
 C69-C014
 1.54 with sigma of 0.005
 C68-C63
 1.54 with sigma of 0.005
 C8-C23 = C10-C11 = C15-C16 = C18-C19 = C29-C49 = C33-C53 = C39-C58 = C43-C44 =
  C1B-C1C = C1G-C1H
 1.4 with sigma of 0.02
 C2-C3 = C3-C4 = C5-C6 = C6-C7 = C12-C13 = C13-C14 = C20-C21 = C21-C22 = C30-
 C31 = C31-C32 = C40-C41 = C41-C42 = C50-C51 = C51-C52 = C59-C60 = C60-C61 =
 C1A-C71 = C1D-C1E = C1E-C1F = C1I-C71
 1.43 with sigma of 0.02
 C3-C13 = C6-C21 = C31-C51 = C41-C60 = C1E-C71
 1.47 with sigma of 0.02
 C65-C67
 1.54 with sigma of 0.005
 C9-C26 = C17-C36 = C24-C25 = C27-C28 = C34-C35 = C37-C38 = C45-C46 = C47-C48 =
  C54-C55 = C56-C57
 1.41 with sigma of 0.02
 C01A-C70
 1.54 with sigma of 0.005
 O005-C65
 1.42 with sigma of 0.005
 C25-C26 = C25-C46 = C26-C27 = C27-C47 = C35-C36 = C35-C55 = C36-C37 = C37-C56
 = C46-C47 = C55-C56
 1.46 with sigma of 0.02
 C014-C00Y
 1.54 with sigma of 0.005
 C010-C01A
 1.54 with sigma of 0.005
 C64-C66
 1.54 with sigma of 0.005
 C1-C62
 1.54 with sigma of 0.02
 C2-C7 = C4-C5 = C12-C30 = C14-C32 = C20-C40 = C22-C42 = C50-C1D = C52-C1F =
 C59-C1I = C61-C1A
 1.44 with sigma of 0.02
 C62-C63
 1.54 with sigma of 0.02
 C67-C64
 1.54 with sigma of 0.02
 O00C-C1
 1.42 with sigma of 0.005
 C00Y-C00S
 1.54 with sigma of 0.005
 C00X-C010
 1.54 with sigma of 0.005
 C2-C10 = C4-C16 = C5-C18 = C7-C8 = C8-C9 = C9-C10 = C11-C12 = C11-C28 = C14-
 C15 = C15-C34 = C16-C17 = C17-C18 = C19-C20 = C19-C38 = C22-C23 = C23-C24 =
 C24-C43 = C28-C29 = C29-C30 = C32-C33 = C33-C34 = C38-C39 = C39-C40 = C42-C43 =
  C44-C45 = C44-C61 = C45-C1B = C48-C49 = C48-C1C = C49-C50 = C52-C53 = C53-C54
 = C54-C1G = C57-C58 = C57-C1H = C58-C59 = C1A-C1B = C1C-C1D = C1F-C1G = C1H-C1I
 1.45 with sigma of 0.02
 C73-C74
 1.54 with sigma of 0.005
 C74-C75
 1.54 with sigma of 0.005
 C73-C72
 1.54 with sigma of 0.005
 O003-C72
 1.42 with sigma of 0.005
 C2-C13 = C2-C6 = C3-C5 = C3-C12 = C3-C14 = C4-C6 = C5-C21 = C6-C20 = C6-C22 =
 C12-C31 = C13-C32 = C14-C31 = C20-C41 = C21-C42 = C22-C41 = C30-C51 = C31-C50 =
  C31-C52 = C40-C60 = C41-C59 = C41-C61 = C50-C1E = C51-C1F = C52-C1E = C59-C71
 = C60-C1A = C61-C71 = C1A-C1E = C1D-C71 = C1E-C1I
 2.5 with sigma of 0.04
 C3-C16 = C6-C8 = C11-C13 = C13-C15 = C19-C21 = C21-C23 = C29-C31 = C31-C33 =
 C39-C41 = C41-C43 = C44-C60 = C49-C51 = C51-C53 = C58-C60 = C1C-C1E = C1E-C1G =
  C1H-C71
 2.51 with sigma of 0.04
 C2-C4 = C5-C7 = C12-C14 = C20-C22 = C30-C32 = C40-C42 = C50-C52 = C59-C61 =
 C1A-C1I = C1D-C1F
 2.43 with sigma of 0.04
 C2-C8 = C4-C18 = C8-C10 = C11-C30 = C11-C29 = C12-C29 = C14-C33 = C15-C33 =
 C16-C18 = C19-C40 = C19-C39 = C20-C39 = C22-C43 = C23-C43 = C44-C1B = C44-C1A =
  C49-C1D = C50-C1C = C52-C1G = C53-C1G = C58-C1I = C59-C1H = C61-C1B
 2.34 with sigma of 0.04
 C2-C9 = C4-C17 = C5-C17 = C7-C9 = C14-C34 = C22-C24 = C24-C42 = C25-C27 = C25-
 C47 = C26-C47 = C27-C46 = C28-C30 = C32-C34 = C35-C37 = C35-C56 = C36-C56 =
 C37-C55 = C38-C40 = C45-C1A = C48-C50 = C48-C1D = C52-C54 = C54-C1F = C57-C59 =
  C57-C1I
 2.36 with sigma of 0.04
 C2-C11 = C4-C15 = C5-C19 = C7-C23 = C8-C22 = C8-C24 = C9-C11 = C10-C12 = C10-
 C28 = C14-C16 = C15-C17 = C17-C19 = C18-C20 = C18-C38 = C24-C44 = C28-C49 =
 C29-C48 = C29-C50 = C32-C53 = C33-C52 = C33-C54 = C38-C58 = C39-C57 = C39-C59 =
  C42-C44 = C43-C45 = C43-C61 = C45-C1C = C48-C1B = C54-C1H = C57-C1G = C1A-C1C
 = C1B-C1D = C1F-C1H = C1G-C1I
 2.47 with sigma of 0.04
 C8-C26 = C9-C25 = C9-C27 = C11-C27 = C15-C35 = C16-C36 = C17-C35 = C17-C37 =
 C19-C37 = C23-C25 = C24-C26 = C24-C46 = C25-C45 = C26-C28 = C27-C29 = C27-C48 =
  C33-C35 = C34-C36 = C34-C55 = C35-C54 = C36-C38 = C37-C39 = C37-C57 = C44-C46
 = C45-C47 = C46-C48 = C47-C49 = C47-C1C = C53-C55 = C54-C56 = C55-C57 = C56-
 C58 = C56-C1H
 2.48 with sigma of 0.04
 C41-C60 \\sim C71-C1E \\sim C31-C51 \\sim C13-C3 \\sim C21-C6
 with sigma of 0.02
 C22-C21 \\sim C32-C31 \\sim C31-C30 \\sim C14-C13 \\sim C12-C13 \\sim C1I-C71
\\sim C1A-C71 \\sim C59-C60
 \\sim C60-C61 \\sim C21-C20 \\sim C6-C7 \\sim C6-C5 \\sim C51-C52 \\sim
C51-C50 \\sim C1D-C1E \\sim C1E-C1F ~
 C42-C41 \\sim C41-C40 \\sim C2-C3 \\sim C3-C4
 with sigma of 0.02
 C3-C12 \\sim C3-C14 \\sim C30-C51 \\sim C31-C52 \\sim C31-C50 \\sim C32-C51
\\sim C1D-C71 \\sim C1E-C1I ~
 C1E-C1A \\sim C1F-C71 \\sim C61-C41 \\sim C59-C41 \\sim C22-C6 \\sim C20-C6
\\sim C2-C13 \\sim C4-C13 ~
 C60-C40 \\sim C60-C42 \\sim C21-C7 \\sim C21-C5 \\sim C2-C6 \\sim C4-C6 \\sim
C31-C14 \\sim C31-C12 \\sim C1D-
 C51 \\sim C1F-C51 \\sim C21-C40 \\sim C21-C42 \\sim C3-C7 \\sim C3-C5 \\sim
C30-C13 \\sim C32-C13 \\sim C1E-
 C50 \\sim C1E-C52 \\sim C61-C71 \\sim C60-C1I \\sim C60-C1A \\sim C59-C71
\\sim C22-C41 \\sim C20-C41
 with sigma of 0.04
 C11-C13 \\sim C10-C3 \\sim C3-C16 \\sim C49-C51 \\sim C29-C31 \\sim C31-C33
\\sim C13-C15 \\sim C1B-C71 ~
 C1C-C1E \\sim C1E-C1G \\sim C51-C53 \\sim C43-C41 \\sim C44-C60 \\sim C60-C58
\\sim C71-C1H \\sim C8-C6 ~
 C23-C21 \\sim C21-C19 \\sim C41-C39 \\sim C6-C18
 with sigma of 0.04
 C1B-C1C \\sim C1H-C1G \\sim C29-C49 \\sim C8-C23 \\sim C44-C43 \\sim C58-C39
\\sim C18-C19 \\sim C33-C53
 \\sim C11-C10 \\sim C16-C15 \\sim C55-C54 \\sim C35-C34 \\sim C37-C38 \\sim
C45-C46 \\sim C56-C57 \\sim C26-C9
 \\sim C17-C36 \\sim C28-C27 \\sim C47-C48 \\sim C25-C24
 with sigma of 0.02
 C55-C56 \\sim C55-C35 \\sim C46-C47 \\sim C27-C47 \\sim C35-C36 \\sim C37-C36
\\sim C37-C56 \\sim C46-C25
 \\sim C26-C27 \\sim C26-C25
 with sigma of 0.02
 C29-C28 \\sim C45-C44 \\sim C8-C9 \\sim C58-C57 \\sim C34-C15 \\sim C34-C33
\\sim C18-C17 \\sim C39-C38 ~
 C28-C11 \\sim C43-C24 \\sim C1H-C57 \\sim C45-C1B \\sim C1G-C54 \\sim C54-C53
\\sim C9-C10 \\sim C17-C16 ~
 C23-C24 \\sim C19-C38 \\sim C49-C48 \\sim C48-C1C
 with sigma of 0.02
 C11-C29 \\sim C10-C8 \\sim C18-C16 \\sim C1G-C53 \\sim C33-C15 \\sim C49-C1C
\\sim C1B-C44 \\sim C43-C23
 \\sim C19-C39 \\sim C58-C1H \\sim C11-C30 \\sim C10-C7 \\sim C2-C8 \\sim
C4-C18 \\sim C49-C1D \\sim C29-C12 ~
 C32-C15 \\sim C14-C33 \\sim C1B-C61 \\sim C1F-C53 \\sim C52-C1G \\sim C43-C22
\\sim C44-C1A \\sim C59-C1H
 \\sim C1I-C58 \\sim C23-C42 \\sim C20-C39 \\sim C40-C19 \\sim C5-C16 \\sim
C1C-C50
 with sigma of 0.04
 C2-C4 \\sim C30-C32 \\sim C12-C14 \\sim C1D-C1F \\sim C50-C52 \\sim C61-C59
\\sim C1A-C1I \\sim C22-C20 ~
 C42-C40 \\sim C7-C5
 with sigma of 0.04
 C1C-C1A \\sim C10-C12 \\sim C49-C30 \\sim C29-C50 \\sim C32-C53 \\sim C14-C16
\\sim C1B-C1D \\sim C1F-C1H
 \\sim C52-C33 \\sim C43-C61 \\sim C59-C39 \\sim C1I-C1G \\sim C23-C7 \\sim
C5-C19 \\sim C11-C2 \\sim C4-C15 ~
 C44-C42 \\sim C8-C22 \\sim C20-C18 \\sim C40-C58 \\sim C28-C10 \\sim C9-C23
\\sim C19-C17 \\sim C34-C16 ~
 C28-C49 \\sim C11-C9 \\sim C48-C29 \\sim C48-C1B \\sim C45-C1C \\sim C45-C43
\\sim C24-C8 \\sim C24-C44 ~
 C38-C58 \\sim C38-C18 \\sim C57-C39 \\sim C54-C1H \\sim C54-C33 \\sim C34-C53
\\sim C17-C15 \\sim C57-C1G
 \\sim C28-C47 \\sim C28-C26 \\sim C27-C48 \\sim C48-C46 \\sim C47-C45 \\sim
C45-C25 \\sim C46-C24 \\sim C24-
 C26 \\sim C25-C9 \\sim C38-C36 \\sim C38-C56 \\sim C37-C17 \\sim C37-C57 \\sim
C57-C55 \\sim C56-C54 \\sim C54-
 C35 \\sim C55-C34 \\sim C34-C36 \\sim C27-C9 \\sim C35-C17 \\sim C11-C27 \\sim
C27-C29 \\sim C10-C26 \\sim C49-
 C47 \\sim C1B-C46 \\sim C46-C44 \\sim C43-C25 \\sim C25-C23 \\sim C8-C26 \\sim
C19-C37 \\sim C18-C36 \\sim C37-
 C39 \\sim C58-C56 \\sim C56-C1H \\sim C55-C53 \\sim C33-C35 \\sim C35-C15
\\sim C16-C36 \\sim C47-C1C ~
 C1G-C55
 with sigma of 0.04
 C47-C26 \\sim C47-C25 \\sim C37-C55 \\sim C55-C36 \\sim C27-C46 \\sim C27-C25
\\sim C46-C26 \\sim C37-C35
 \\sim C56-C36 \\sim C56-C35 \\sim C9-C7 \\sim C5-C17 \\sim C28-C12 \\sim
C28-C30 \\sim C2-C9 \\sim C4-C17 ~
 C48-C50 \\sim C48-C1D \\sim C32-C34 \\sim C14-C34 \\sim C45-C1A \\sim C45-C61
\\sim C1F-C54 \\sim C52-C54
 \\sim C24-C22 \\sim C24-C42 \\sim C59-C57 \\sim C1I-C57 \\sim C20-C38 \\sim
C40-C38
 with sigma of 0.04
 C42-C22 \\sim C40-C20 \\sim C2-C7 \\sim C4-C5 \\sim C32-C14 \\sim C30-C12
\\sim C1I-C59 \\sim C1A-C61 ~
 C50-C1D \\sim C52-C1F
 with sigma of 0.02
 C1H-C1I \\sim C32-C33 \\sim C30-C29 \\sim C14-C15 \\sim C12-C11 \\sim C1B-C1A
\\sim C1G-C1F \\sim C8-C7 ~
 C59-C58 \\sim C61-C44 \\sim C18-C5 \\sim C53-C52 \\sim C49-C50 \\sim C42-C43
\\sim C22-C23 \\sim C40-C39 ~
 C20-C19 \\sim C10-C2 \\sim C4-C16 \\sim C1C-C1D
 with sigma of 0.02
3. Restrained planarity
 C12, C13, C14, C30
 with sigma of 0.1
 C49, C50, C1C, C1D
 with sigma of 0.1
 C45, C48, C1B, C1C
 with sigma of 0.1
 C57, C59, C1H, C1I
 with sigma of 0.1
 C14, C15, C33, C34
 with sigma of 0.1
 C16, C17, C18, C5
 with sigma of 0.1
 C44, C45, C61, C1A
 with sigma of 0.1
 C17, C18, C4, C5
 with sigma of 0.1
 C47, C48, C1B, C1C
 with sigma of 0.1
 C19, C36, C37, C38
 with sigma of 0.1
 C52, C53, C54, C1F
 with sigma of 0.1
 C22, C23, C42, C43
 with sigma of 0.1
 C1A, C1B, C1C, C71
 with sigma of 0.1
 C25, C27, C46, C47
 with sigma of 0.1
 C25, C26, C8, C9
 with sigma of 0.1
 C29, C30, C31, C51
 with sigma of 0.1
 C37, C38, C56, C57
 with sigma of 0.1
 C14, C15, C32, C34
 with sigma of 0.1
 C41, C42, C43, C44
 with sigma of 0.1
 C15, C16, C17, C34
 with sigma of 0.1
 C16, C17, C35, C36
 with sigma of 0.1
 C17, C18, C19, C38
 with sigma of 0.1
 C20, C21, C40, C41
 with sigma of 0.1
 C23, C24, C25, C26
 with sigma of 0.1
 C25, C26, C46, C47
 with sigma of 0.1
 C29, C30, C31, C49
 with sigma of 0.1
 C30, C31, C50, C51
 with sigma of 0.1
 C33, C34, C35, C55
 with sigma of 0.1
 C41, C42, C43, C60
 with sigma of 0.1
 C42, C43, C44, C61
 with sigma of 0.1
 C44, C61, C1A, C1B
 with sigma of 0.1
 C46, C47, C48, C1C
 with sigma of 0.1
 C48, C50, C1C, C1D
 with sigma of 0.1
 C50, C51, C52, C1D
 with sigma of 0.1
 C52, C53, C54, C1G
 with sigma of 0.1
 C58, C59, C1H, C1I
 with sigma of 0.1
 C1C, C1D, C1E, C71
 with sigma of 0.1
 C2, C12, C13, C3
 with sigma of 0.1
 C2, C8, C9, C10
 with sigma of 0.1
 C33, C34, C53, C54
 with sigma of 0.1
 C7, C8, C9, C10
 with sigma of 0.1
 C11, C12, C28, C29
 with sigma of 0.1
 C11, C28, C29, C30
 with sigma of 0.1
4. Rigid bond restraints
 C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18,
 C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34,
  C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48, C49,
 C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C1A, C1B, C1C, C1D,
  C1E, C1F, C1G, C1H, C1I, C71
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O005, C65, C67, C64, C66
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O004, C00X, C010, C01A, C70
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C65, O005
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10
\\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18
\\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26
\\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34
\\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42
\\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50
\\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58
\\sim C59 \\sim C60 \\sim C61 \\sim C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E
\\sim C1F \\sim C1G \\sim C1H \\sim C1I \\sim C71: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O004 \\sim C00X: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C65 \\sim O005: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C61) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C42) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C31)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C68)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C1) = Uanis(C63) = Uanis(C68) = Uanis(C62)
Uanis(C66) = Uanis(C67) = Uanis(C65) = Uanis(C64)
Uanis(C00X) = Uanis(C01A) = Uanis(C70) = Uanis(C010)
Uanis(C69) = Uanis(C014) = Uanis(C00Y) = Uanis(C00S)
Uanis(C74) = Uanis(C72) = Uanis(C75) = Uanis(C73)
Uanis(C41) = Uanis(C42) = Uanis(C40) = Uanis(C60)
Uanis(C45) = Uanis(C1B) = Uanis(C1A) = Uanis(C61) = Uanis(C44)
Uanis(C14) = Uanis(C13) = Uanis(C32) = Uanis(C15)
Uanis(O00C) = Uanis(C1) = Uanis(C62) = Uanis(C63) = Uanis(C68)
6. Rigid body (RIGU) restrains
 C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18,
 C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34,
  C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48, C49,
 C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C1A, C1B, C1C, C1D,
  C1E, C1F, C1G, C1H, C1I, C71
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O005, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00X, O004
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: C00S(0.5) H00A(0.5) H00B(0.5) C00Y(0.5) H00F(0.5) H00G(0.5)
 C014(0.5) H01C(0.5) H01D(0.5) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5)
 C2(0.16667) C3(0.16667) C4(0.16667) C5(0.16667) C6(0.16667) C7(0.16667)
 C8(0.16667) C9(0.16667) C10(0.16667) C11(0.16667) C12(0.16667) C13(0.16667)
 C14(0.16667) C15(0.16667) C16(0.16667) C17(0.16667) C18(0.16667) C19(0.16667)
 C20(0.16667) C21(0.16667) C22(0.16667) C23(0.16667) C24(0.16667) C25(0.16667)
 C26(0.16667) C27(0.16667) C28(0.16667) C29(0.16667) C30(0.16667) C31(0.16667)
 C32(0.16667) C33(0.16667) C34(0.16667) C35(0.16667) C36(0.16667) C37(0.16667)
 C38(0.16667) C39(0.16667) C40(0.16667) C41(0.16667) C42(0.16667) C43(0.16667)
 C44(0.16667) C45(0.16667) C46(0.16667) C47(0.16667) C48(0.16667) C49(0.16667)
 C50(0.16667) C51(0.16667) C52(0.16667) C53(0.16667) C54(0.16667) C55(0.16667)
 C56(0.16667) C57(0.16667) C58(0.16667) C59(0.16667) C60(0.16667) C61(0.16667)
 C1A(0.16667) C1B(0.16667) C1C(0.16667) C1D(0.16667) C1E(0.16667) C1F(0.16667)
 C1G(0.16667) C1H(0.16667) C1I(0.16667) C71(0.16667) C74(0.5) H74A(0.5)
 H74B(0.5) C73(0.5) H73A(0.5) H73B(0.5) C72(0.5) H72A(0.5) H72B(0.5) C75(0.5)
 H75A(0.5) H75B(0.5) H75C(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C00S(H00A,H00B), C00X(H00C,H00E), C00Y(H00F,H00G), C010(H01A,H01B), C014(H01C,
 H01D), C01A(H01E,H01F), C67(H67A,H67B), C63(H63A,H63B), C62(H62A,H62B), C1(H1A,
 H1B), C64(H64A,H64B), C65(H65A,H65B), C74(H74A,H74B), C73(H73A,H73B), C72(H72A,
 H72B)
8.b Me refined with riding coordinates:
 C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C)
8.c Aromatic/amide H refined with riding coordinates:
 C006(H006), C007(H007), C00D(H00D), C00M(H00M), C00N(H00N), C00O(H00O),
 C00T(H00T), C00V(H00V)
8.d Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C75(H75A,H75B,H75C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1216 electrons were 
found in a volume of 5264\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
6[C7H8], 6[C7H8] per Asymmetric Unit 
which account for 4800 electrons 
per unit cell.
;
_shelx_res_checksum              44513
_shelx_hkl_checksum              39149
_shelx_fab_checksum              69458
_olex2_submission_special_instructions 'No special instructions were received'