# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TripPh(NO2)2
_database_code_depnum_ccdc_archive 'CCDC 2182983'
loop_
_audit_author_name
_audit_author_address
'Wataru Setaka'
;Tokyo Metropolitan University
Japan
;
_audit_update_record             
;
2022-06-30 deposited with the CCDC.	2022-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        (dinitrophenyl)triptycene
_chemical_name_common            TripPh(NO2)2
_chemical_melting_point          '> 573 K'
_chemical_formula_moiety         'C26 H16 N2 O4'
_chemical_formula_sum            'C26 H16 N2 O4'
_chemical_formula_weight         420.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   17.026(3)
_cell_length_b                   13.546(2)
_cell_length_c                   8.1803(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1886.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9808
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      74.51

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_F_000             872
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.829
_shelx_estimated_absorpt_T_min   0.820
_shelx_estimated_absorpt_T_max   0.937
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_T_max  0.937

_exptl_special_details           
;
;


_diffrn_ambient_temperature      100(2)
_diffrn_source                   'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            15105
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         8.890
_diffrn_reflns_theta_max         74.521
_diffrn_reflns_theta_full        73.500
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measured_fraction_theta_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             1914
_reflns_number_gt                1909
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'Sir-2011 (IUCr, 2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2020)'
_computing_publication_material  'WinGX (Farrugia, 2020)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0376P)²+1.2073P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1914
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.0965
_refine_ls_wR_factor_gt          0.0964
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.46092(6) 0.06929(8) 0.65091(12) 0.0175(2) Uani 1 1 d . . . . .
O1 O 0.43033(5) -0.00709(6) 0.60169(11) 0.0207(2) Uani 1 1 d . . . . .
O2 O 0.51282(5) 0.07279(7) 0.75489(12) 0.0259(3) Uani 1 1 d . . . . .
C1 C 0.36253(9) 0.250000 0.37084(19) 0.0130(3) Uani 1 2 d S T P . .
C2 C 0.38537(6) 0.16142(8) 0.44445(14) 0.0139(3) Uani 1 1 d . . . . .
H2 H 0.367405 0.100158 0.402062 0.017 Uiso 1 1 calc R U . . .
C3 C 0.43451(6) 0.16352(9) 0.57997(14) 0.0149(3) Uani 1 1 d . . . . .
C4 C 0.46083(9) 0.250000 0.6507(2) 0.0156(3) Uani 1 2 d S T P . .
H4 H 0.494989 0.250002 0.742542 0.019 Uiso 1 2 calc R U P . .
C5 C 0.30248(9) 0.250000 0.23339(19) 0.0122(3) Uani 1 2 d S T P . .
C6 C 0.18509(9) 0.250000 0.0260(2) 0.0137(3) Uani 1 2 d S T P . .
H6 H 0.140624 0.249998 -0.053915 0.016 Uiso 1 2 calc R U P . .
C7 C 0.30412(7) 0.16175(8) 0.11263(14) 0.0126(3) Uani 1 1 d . . . . .
C8 C 0.36370(7) 0.09287(9) 0.09100(14) 0.0146(3) Uani 1 1 d . . . . .
H8 H 0.409065 0.094469 0.158562 0.018 Uiso 1 1 calc R U . . .
C9 C 0.35633(7) 0.02121(9) -0.03099(15) 0.0181(3) Uani 1 1 d . . . . .
H9 H 0.396332 -0.027037 -0.044147 0.022 Uiso 1 1 calc R U . . .
C10 C 0.29132(7) 0.01976(9) -0.13298(15) 0.0192(3) Uani 1 1 d . . . . .
H10 H 0.286708 -0.029792 -0.214601 0.023 Uiso 1 1 calc R U . . .
C11 C 0.23260(7) 0.09099(9) -0.11598(14) 0.0168(3) Uani 1 1 d . . . . .
H11 H 0.188393 0.090955 -0.186853 0.020 Uiso 1 1 calc R U . . .
C12 C 0.23957(6) 0.16157(8) 0.00527(14) 0.0134(3) Uani 1 1 d . . . . .
C13 C 0.21975(9) 0.250000 0.3134(2) 0.0125(3) Uani 1 2 d S T P . .
C14 C 0.20368(9) 0.250000 0.4798(2) 0.0143(3) Uani 1 2 d S T P . .
H14 H 0.245361 0.250000 0.556975 0.017 Uiso 1 2 calc R U P . .
C15 C 0.12586(10) 0.250000 0.5324(2) 0.0174(4) Uani 1 2 d S T P . .
H15 H 0.114819 0.250000 0.646272 0.021 Uiso 1 2 calc R U P . .
C16 C 0.06413(10) 0.250000 0.4214(2) 0.0182(4) Uani 1 2 d S T P . .
H16 H 0.011330 0.250000 0.458938 0.022 Uiso 1 2 calc R U P . .
C17 C 0.08035(10) 0.250000 0.2544(2) 0.0164(4) Uani 1 2 d S T P . .
H17 H 0.038663 0.250000 0.177195 0.020 Uiso 1 2 calc R U P . .
C18 C 0.15774(9) 0.250000 0.2017(2) 0.0133(3) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 O1 1.2264(14) . ?
N1 O2 1.2273(14) . ?
N1 C3 1.4726(15) . ?
C1 C2 1.3977(14) 8_565 ?
C1 C2 1.3977(14) . ?
C1 C5 1.520(2) . ?
C2 C3 1.3891(17) . ?
C2 H2 0.9500 . ?
C3 C4 1.3813(15) . ?
C4 H4 0.9500 . ?
C5 C7 1.5510(15) 8_565 ?
C5 C7 1.5511(15) . ?
C5 C13 1.553(2) . ?
C6 C18 1.511(2) . ?
C6 C12 1.5245(15) 8_565 ?
C6 C12 1.5245(15) . ?
C6 H6 1.0000 . ?
C7 C8 1.3895(16) . ?
C7 C12 1.4068(16) . ?
C8 C9 1.3978(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.3863(18) . ?
C9 H9 0.9500 . ?
C10 C11 1.3964(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.3828(17) . ?
C11 H11 0.9500 . ?
C13 C14 1.388(2) . ?
C13 C18 1.396(2) . ?
C14 C15 1.393(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.394(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.386(2) . ?
C17 H17 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 N1 O2 124.46(10) . . ?
O1 N1 C3 118.18(10) . . ?
O2 N1 C3 117.36(10) . . ?
C2 C1 C2 118.30(15) 8_565 . ?
C2 C1 C5 120.39(7) 8_565 . ?
C2 C1 C5 120.39(7) . . ?
C3 C2 C1 119.58(11) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 123.17(11) . . ?
C4 C3 N1 118.09(11) . . ?
C2 C3 N1 118.73(10) . . ?
C3 C4 C3 116.00(15) 8_565 . ?
C3 C4 H4 122.0 8_565 . ?
C3 C4 H4 122.0 . . ?
C1 C5 C7 117.33(8) . 8_565 ?
C1 C5 C7 117.33(8) . . ?
C7 C5 C7 100.84(12) 8_565 . ?
C1 C5 C13 107.36(13) . . ?
C7 C5 C13 106.54(9) 8_565 . ?
C7 C5 C13 106.54(9) . . ?
C18 C6 C12 107.04(9) . 8_565 ?
C18 C6 C12 107.04(9) . . ?
C12 C6 C12 103.59(12) 8_565 . ?
C18 C6 H6 112.8 . . ?
C12 C6 H6 112.8 8_565 . ?
C12 C6 H6 112.8 . . ?
C8 C7 C12 119.31(10) . . ?
C8 C7 C5 127.72(11) . . ?
C12 C7 C5 112.63(10) . . ?
C7 C8 C9 119.46(11) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C10 C9 C8 120.74(11) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 120.13(11) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C12 C11 C10 119.19(11) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C11 C12 C7 121.07(11) . . ?
C11 C12 C6 124.79(11) . . ?
C7 C12 C6 113.87(10) . . ?
C14 C13 C18 119.51(14) . . ?
C14 C13 C5 126.28(14) . . ?
C18 C13 C5 114.21(14) . . ?
C13 C14 C15 119.38(15) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C16 C15 C14 121.15(16) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C17 119.41(15) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C18 C17 C16 119.55(15) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C13 121.00(15) . . ?
C17 C18 C6 126.08(15) . . ?
C13 C18 C6 112.92(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C3 -4.8(2) 8_565 . . . ?
C5 C1 C2 C3 -173.87(12) . . . . ?
C1 C2 C3 C4 2.01(19) . . . . ?
C1 C2 C3 N1 -177.11(11) . . . . ?
O1 N1 C3 C4 171.20(12) . . . . ?
O2 N1 C3 C4 -9.37(16) . . . . ?
O1 N1 C3 C2 -9.62(16) . . . . ?
O2 N1 C3 C2 169.80(10) . . . . ?
C2 C3 C4 C3 0.9(2) . . . 8_565 ?
N1 C3 C4 C3 179.99(8) . . . 8_565 ?
C2 C1 C5 C7 35.41(19) 8_565 . . 8_565 ?
C2 C1 C5 C7 -155.76(12) . . . 8_565 ?
C2 C1 C5 C7 155.76(12) 8_565 . . . ?
C2 C1 C5 C7 -35.41(19) . . . . ?
C2 C1 C5 C13 -84.42(12) 8_565 . . . ?
C2 C1 C5 C13 84.41(12) . . . . ?
C1 C5 C7 C8 -15.32(18) . . . . ?
C7 C5 C7 C8 113.37(12) 8_565 . . . ?
C13 C5 C7 C8 -135.58(12) . . . . ?
C1 C5 C7 C12 171.41(10) . . . . ?
C7 C5 C7 C12 -59.90(13) 8_565 . . . ?
C13 C5 C7 C12 51.15(13) . . . . ?
C12 C7 C8 C9 -3.61(16) . . . . ?
C5 C7 C8 C9 -176.49(11) . . . . ?
C7 C8 C9 C10 1.66(17) . . . . ?
C8 C9 C10 C11 0.73(18) . . . . ?
C9 C10 C11 C12 -1.10(18) . . . . ?
C10 C11 C12 C7 -0.90(17) . . . . ?
C10 C11 C12 C6 172.86(11) . . . . ?
C8 C7 C12 C11 3.28(16) . . . . ?
C5 C7 C12 C11 177.18(10) . . . . ?
C8 C7 C12 C6 -171.13(10) . . . . ?
C5 C7 C12 C6 2.78(14) . . . . ?
C18 C6 C12 C11 128.49(12) . . . . ?
C12 C6 C12 C11 -118.59(11) 8_565 . . . ?
C18 C6 C12 C7 -57.35(13) . . . . ?
C12 C6 C12 C7 55.58(15) 8_565 . . . ?
C1 C5 C13 C14 0.000(0) . . . . ?
C7 C5 C13 C14 -126.48(8) 8_565 . . . ?
C7 C5 C13 C14 126.48(8) . . . . ?
C1 C5 C13 C18 180.000(0) . . . . ?
C7 C5 C13 C18 53.52(8) 8_565 . . . ?
C7 C5 C13 C18 -53.52(8) . . . . ?
C18 C13 C14 C15 0.000(0) . . . . ?
C5 C13 C14 C15 180.000(0) . . . . ?
C13 C14 C15 C16 0.000(0) . . . . ?
C14 C15 C16 C17 0.000(0) . . . . ?
C15 C16 C17 C18 0.000(0) . . . . ?
C16 C17 C18 C13 0.000(0) . . . . ?
C16 C17 C18 C6 180.000(0) . . . . ?
C14 C13 C18 C17 0.000(0) . . . . ?
C5 C13 C18 C17 180.000(0) . . . . ?
C14 C13 C18 C6 180.000(0) . . . . ?
C5 C13 C18 C6 0.000(0) . . . . ?
C12 C6 C18 C17 124.72(8) 8_565 . . . ?
C12 C6 C18 C17 -124.73(8) . . . . ?
C12 C6 C18 C13 -55.28(8) 8_565 . . . ?
C12 C6 C18 C13 55.27(8) . . . . ?

_refine_diff_density_max         0.316
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.045


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloroethane'
_chemical_compound_source        no
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_(OMe)2PhTripCl3
_database_code_depnum_ccdc_archive 'CCDC 2182985'
loop_
_audit_author_name
_audit_author_address
'Wataru Setaka'
;Tokyo Metropolitan University
Japan
;
_audit_update_record             
;
2022-06-30 deposited with the CCDC.	2022-08-19 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        PhenylTriptyceneDeriv.
_chemical_name_common            (OMe)2PhTripCl3
_chemical_melting_point          '458-459 K'
_chemical_formula_moiety         'C28 H19 Cl3 O2'
_chemical_formula_sum            'C28 H19 Cl3 O2'
_chemical_formula_weight         493.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   15.5816(4)
_cell_length_b                   9.3605(2)
_cell_length_c                   31.6875(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4621.67(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9837
_cell_measurement_theta_min      3.98
_cell_measurement_theta_max      74.45

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    3.784
_shelx_estimated_absorpt_T_min   0.335
_shelx_estimated_absorpt_T_max   0.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_T_max  0.556
_exptl_absorpt_process_details   'SADABS Bruker'

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'shield tube'
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            38013
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.789
_diffrn_reflns_theta_max         74.596
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8907
_reflns_number_gt                8341
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR-2019 (IUCr)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0673P)²+7.4745P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8907
_refine_ls_number_parameters     625
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0600
_refine_ls_wR_factor_ref         0.1590
_refine_ls_wR_factor_gt          0.1566
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.3119(3) 0.5519(8) 0.21899(15) 0.0499(14) Uani 1 1 d . . . . .
O2 O 0.0476(3) 0.6303(6) 0.29836(18) 0.0467(13) Uani 1 1 d . . . . .
Cl1 Cl 0.22299(14) 0.53464(19) 0.40020(6) 0.0481(5) Uani 1 1 d . . . . .
Cl2 Cl 0.33388(14) 1.0880(2) 0.49350(7) 0.0570(5) Uani 1 1 d . . . . .
Cl3 Cl 0.57771(13) 1.0737(2) 0.41626(7) 0.0371(6) Uani 0.781(6) 1 d . . P A 1
Cl4 Cl 0.3797(6) 1.3420(7) 0.3662(3) 0.042(2) Uani 0.219(6) 1 d . . P A 2
C1 C 0.2695(4) 0.7219(7) 0.3196(2) 0.0318(14) Uani 1 1 d . . . . .
C2 C 0.3102(4) 0.6729(9) 0.2841(2) 0.0383(16) Uani 1 1 d . . . . .
H2 H 0.370287 0.685944 0.280961 0.046 Uiso 1 1 calc R U . . .
C3 C 0.2635(4) 0.6035(8) 0.2523(2) 0.0364(15) Uani 1 1 d . . . . .
C4 C 0.1760(4) 0.5849(8) 0.2559(2) 0.0390(16) Uani 1 1 d . . . . .
H4 H 0.144704 0.535883 0.234676 0.047 Uiso 1 1 calc R U . . .
C5 C 0.1341(4) 0.6397(8) 0.2916(2) 0.0337(14) Uani 1 1 d . . . . .
C6 C 0.1805(4) 0.7086(7) 0.3234(2) 0.0320(14) Uani 1 1 d . . . . .
H6 H 0.151790 0.745978 0.347436 0.038 Uiso 1 1 calc R U . . .
C7 C 0.3149(4) 0.8210(7) 0.3509(2) 0.0307(14) Uani 1 1 d . . . . .
C8 C 0.3811(5) 1.0218(7) 0.3978(3) 0.0378(17) Uani 1 1 d . . . . .
H8 H 0.407278 1.097420 0.416014 0.045 Uiso 1 1 calc R U . . .
C9 C 0.2868(4) 0.8122(6) 0.3984(2) 0.0296(13) Uani 1 1 d . . . . .
C10 C 0.2452(4) 0.7021(7) 0.4210(2) 0.0359(14) Uani 1 1 d . . . . .
C11 C 0.2259(5) 0.7196(8) 0.4634(2) 0.0401(16) Uani 1 1 d . . . . .
H11 H 0.195410 0.646213 0.477719 0.048 Uiso 1 1 calc R U . . .
C12 C 0.2493(5) 0.8379(8) 0.4850(2) 0.0423(16) Uani 1 1 d . . . . .
H12 H 0.232769 0.850359 0.513655 0.051 Uiso 1 1 calc R U . . .
C13 C 0.2975(4) 0.9402(7) 0.4646(2) 0.0370(15) Uani 1 1 d . . . . .
C14 C 0.3174(4) 0.9272(6) 0.4222(2) 0.0298(13) Uani 1 1 d . . . . .
C15 C 0.4132(4) 0.8074(7) 0.3568(2) 0.0297(13) Uani 1 1 d . . . . .
C16 C 0.4655(4) 0.6946(7) 0.3452(2) 0.0330(14) Uani 1 1 d . . . . .
H16 H 0.441729 0.612538 0.332007 0.040 Uiso 1 1 calc R U . . .
C17 C 0.5541(4) 0.7025(8) 0.3531(2) 0.0371(15) Uani 1 1 d . . . . .
H17 H 0.590408 0.626576 0.344359 0.044 Uiso 1 1 calc R U . . .
C18 C 0.5893(4) 0.8206(8) 0.3736(2) 0.0350(15) Uani 1 1 d . . . . .
H18 H 0.649392 0.827117 0.378108 0.042 Uiso 1 1 calc R U . . .
C19 C 0.5351(4) 0.9278(7) 0.3871(2) 0.0315(14) Uani 1 1 d . . . . .
H19 H 0.558464 1.007602 0.401648 0.038 Uiso 0.219(6) 1 calc R U P A 1
C20 C 0.4469(4) 0.9217(7) 0.3799(2) 0.0298(13) Uani 1 1 d . . . . .
C21 C 0.2971(4) 0.9775(8) 0.3357(3) 0.0337(16) Uani 1 1 d . . . . .
C22 C 0.2524(5) 1.0139(10) 0.2990(3) 0.052(2) Uani 1 1 d . . . . .
H22 H 0.228647 0.943210 0.280980 0.062 Uiso 1 1 calc R U . . .
C23 C 0.2445(6) 1.1595(12) 0.2903(4) 0.070(3) Uani 1 1 d . . . . .
H23 H 0.211983 1.187173 0.266269 0.084 Uiso 1 1 calc R U . . .
C24 C 0.2805(5) 1.2630(11) 0.3141(4) 0.071(4) Uani 1 1 d . . . . .
H24 H 0.274528 1.360637 0.306487 0.085 Uiso 1 1 calc R U . . .
C25 C 0.3261(5) 1.2246(10) 0.3498(4) 0.059(3) Uani 1 1 d . . . . .
H25 H 0.352623 1.295801 0.366716 0.071 Uiso 0.781(6) 1 calc R U P . .
C26 C 0.3328(4) 1.0837(8) 0.3605(3) 0.0381(16) Uani 1 1 d . . . . .
C27 C 0.2686(6) 0.4850(9) 0.1861(3) 0.046(2) Uani 1 1 d . . . . .
H27A H 0.309912 0.453616 0.164763 0.069 Uiso 1 1 calc R U . . .
H27B H 0.237355 0.402001 0.197093 0.069 Uiso 1 1 calc R U . . .
H27C H 0.227871 0.552202 0.173424 0.069 Uiso 1 1 calc R U . . .
C28 C -0.0041(5) 0.5786(9) 0.2660(3) 0.0473(19) Uani 1 1 d . . . . .
H28A H -0.064110 0.577875 0.275231 0.071 Uiso 1 1 calc R U . . .
H28B H 0.001771 0.640162 0.241134 0.071 Uiso 1 1 calc R U . . .
H28C H 0.013654 0.481146 0.258740 0.071 Uiso 1 1 calc R U . . .
O3 O 0.4376(3) 0.9391(6) 0.73771(16) 0.0389(11) Uani 1 1 d . . . . .
O4 O 0.6993(3) 0.8922(5) 0.66030(17) 0.0382(11) Uani 1 1 d . . . . .
Cl11 Cl 0.52438(12) 0.97591(16) 0.55690(6) 0.0405(4) Uani 1 1 d . . . . .
Cl12 Cl 0.42349(14) 0.4226(2) 0.46022(6) 0.0511(5) Uani 1 1 d . . . . .
Cl13 Cl 0.17779(10) 0.42124(18) 0.53735(6) 0.0323(5) Uani 0.878(6) 1 d . . P B
3
Cl14 Cl 0.3593(10) 0.1604(14) 0.5856(6) 0.053(5) Uani 0.122(6) 1 d . . P B 4
C51 C 0.4795(4) 0.7806(6) 0.6356(2) 0.0243(12) Uani 1 1 d . . . . .
C52 C 0.4386(4) 0.8283(6) 0.67217(19) 0.0261(12) Uani 1 1 d . . . . .
H52 H 0.378899 0.811796 0.675769 0.031 Uiso 1 1 calc R U . . .
C53 C 0.4841(4) 0.8996(6) 0.7033(2) 0.0281(12) Uani 1 1 d . . . . .
C54 C 0.5723(4) 0.9225(6) 0.6998(2) 0.0283(13) Uani 1 1 d . . . . .
H54 H 0.603436 0.971624 0.721112 0.034 Uiso 1 1 calc R U . . .
C55 C 0.6130(4) 0.8698(7) 0.6636(2) 0.0286(13) Uani 1 1 d . . . . .
C56 C 0.5687(4) 0.7992(7) 0.63221(19) 0.0274(12) Uani 1 1 d . . . . .
H56 H 0.598501 0.763062 0.608321 0.033 Uiso 1 1 calc R U . . .
C57 C 0.4357(4) 0.6851(6) 0.60318(19) 0.0236(12) Uani 1 1 d . . . . .
C58 C 0.3736(4) 0.4817(6) 0.5550(2) 0.0263(13) Uani 1 1 d . . . . .
H58 H 0.349675 0.405379 0.536320 0.032 Uiso 1 1 calc R U . . .
C59 C 0.4636(4) 0.6959(6) 0.5567(2) 0.0264(12) Uani 1 1 d . . . . .
C60 C 0.5032(4) 0.8073(6) 0.5356(2) 0.0293(12) Uani 1 1 d . . . . .
C61 C 0.5249(5) 0.7957(7) 0.4927(2) 0.0363(15) Uani 1 1 d . . . . .
H61 H 0.555104 0.870792 0.478988 0.044 Uiso 1 1 calc R U . . .
C62 C 0.5021(5) 0.6747(8) 0.4705(2) 0.0404(16) Uani 1 1 d . . . . .
H62 H 0.518506 0.664903 0.441804 0.048 Uiso 1 1 calc R U . . .
C63 C 0.4561(4) 0.5688(7) 0.4897(2) 0.0355(14) Uani 1 1 d . . . . .
C64 C 0.4343(4) 0.5799(6) 0.5319(2) 0.0294(12) Uani 1 1 d . . . . .
C65 C 0.3368(4) 0.6894(6) 0.5985(2) 0.0265(12) Uani 1 1 d . . . . .
C66 C 0.2808(4) 0.7964(7) 0.6116(2) 0.0345(14) Uani 1 1 d . . . . .
H66 H 0.302107 0.877969 0.626061 0.041 Uiso 1 1 calc R U . . .
C67 C 0.1931(4) 0.7833(8) 0.6035(2) 0.0392(16) Uani 1 1 d . . . . .
H67 H 0.154965 0.855664 0.612902 0.047 Uiso 1 1 calc R U . . .
C68 C 0.1613(4) 0.6680(8) 0.5821(2) 0.0355(14) Uani 1 1 d . . . . .
H68 H 0.101271 0.658133 0.577872 0.043 Uiso 1 1 calc R U . . .
C69 C 0.2183(4) 0.5643(7) 0.5666(2) 0.0299(13) Uani 1 1 d . . . . .
H69 H 0.196874 0.484920 0.551157 0.036 Uiso 0.122(6) 1 calc R U P B 3
C70 C 0.3039(4) 0.5775(6) 0.57353(19) 0.0265(12) Uani 1 1 d . . . . .
C71 C 0.4550(4) 0.5280(6) 0.6180(2) 0.0257(13) Uani 1 1 d . . . . .
C72 C 0.4988(5) 0.4892(7) 0.6541(2) 0.0270(14) Uani 1 1 d . . . . .
H72 H 0.522397 0.560658 0.671981 0.032 Uiso 1 1 calc R U . . .
C73 C 0.5087(4) 0.3436(8) 0.6645(2) 0.0373(15) Uani 1 1 d . . . . .
H73 H 0.537722 0.317034 0.689695 0.045 Uiso 1 1 calc R U . . .
C74 C 0.4758(5) 0.2381(7) 0.6377(3) 0.0411(18) Uani 1 1 d . . . . .
H74 H 0.482745 0.139851 0.644308 0.049 Uiso 1 1 calc R U . . .
C75 C 0.4324(5) 0.2795(7) 0.6009(2) 0.0345(15) Uani 1 1 d . . . . .
H75 H 0.411319 0.208923 0.581965 0.041 Uiso 0.878(6) 1 calc R U P . .
C76 C 0.4204(4) 0.4222(6) 0.5920(2) 0.0286(13) Uani 1 1 d . . . . .
C77 C 0.4841(6) 0.9980(12) 0.7727(3) 0.058(3) Uani 1 1 d . . . . .
H77A H 0.443958 1.022211 0.795425 0.087 Uiso 1 1 calc R U . . .
H77B H 0.525738 0.927673 0.783033 0.087 Uiso 1 1 calc R U . . .
H77C H 0.514488 1.084422 0.763644 0.087 Uiso 1 1 calc R U . . .
C78 C 0.7461(6) 0.8446(12) 0.6262(4) 0.043(3) Uani 0.659(16) 1 d . . P C 5
H78A H 0.806451 0.871259 0.629836 0.065 Uiso 0.659(16) 1 calc R U P C 5
H78B H 0.741323 0.740466 0.624159 0.065 Uiso 0.659(16) 1 calc R U P C 5
H78C H 0.723735 0.888327 0.600326 0.065 Uiso 0.659(16) 1 calc R U P C 5
C178 C 0.7497(11) 0.953(2) 0.6913(6) 0.032(5) Uani 0.341(16) 1 d . U P C 6
H17A H 0.809313 0.957678 0.681587 0.047 Uiso 0.341(16) 1 calc R U P C 6
H17B H 0.728949 1.049714 0.697393 0.047 Uiso 0.341(16) 1 calc R U P C 6
H17C H 0.746522 0.894877 0.716986 0.047 Uiso 0.341(16) 1 calc R U P C 6


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C3 1.384(9) . ?
O1 C27 1.390(10) . ?
O2 C5 1.369(8) . ?
O2 C28 1.391(9) . ?
Cl1 C10 1.734(7) . ?
Cl2 C13 1.753(7) . ?
Cl3 C19 1.777(7) . ?
C1 C2 1.372(10) . ?
C1 C6 1.397(9) . ?
C1 C7 1.531(10) . ?
C2 C3 1.402(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(10) . ?
C4 C5 1.403(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.398(9) . ?
C6 H6 0.9500 . ?
C7 C15 1.549(9) . ?
C7 C21 1.567(9) . ?
C7 C9 1.570(9) . ?
C8 C20 1.501(10) . ?
C8 C26 1.515(11) . ?
C8 C14 1.538(9) . ?
C8 H8 1.0000 . ?
C9 C14 1.398(9) . ?
C9 C10 1.411(9) . ?
C10 C11 1.388(10) . ?
C11 C12 1.353(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.378(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(10) . ?
C15 C16 1.383(10) . ?
C15 C20 1.397(9) . ?
C16 C17 1.404(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.394(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.379(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.396(9) . ?
C19 H19 0.9500 . ?
C21 C26 1.385(11) . ?
C21 C22 1.396(12) . ?
C22 C23 1.396(13) . ?
C22 H22 0.9500 . ?
C23 C24 1.351(17) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(15) . ?
C24 H24 0.9500 . ?
C25 C26 1.367(11) . ?
C25 H25 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
O3 C53 1.361(8) . ?
O3 C77 1.435(10) . ?
O4 C55 1.365(7) . ?
O4 C78 1.377(12) . ?
O4 C178 1.381(18) . ?
Cl11 C60 1.749(6) . ?
Cl12 C63 1.733(7) . ?
Cl13 C69 1.746(7) . ?
C51 C52 1.395(9) . ?
C51 C56 1.405(9) . ?
C51 C57 1.523(8) . ?
C52 C53 1.386(9) . ?
C52 H52 0.9500 . ?
C53 C54 1.395(9) . ?
C54 C55 1.401(9) . ?
C54 H54 0.9500 . ?
C55 C56 1.379(9) . ?
C56 H56 0.9500 . ?
C57 C59 1.540(9) . ?
C57 C65 1.549(8) . ?
C57 C71 1.573(8) . ?
C58 C76 1.490(9) . ?
C58 C64 1.508(9) . ?
C58 C70 1.526(9) . ?
C58 H58 1.0000 . ?
C59 C60 1.384(8) . ?
C59 C64 1.416(8) . ?
C60 C61 1.405(10) . ?
C61 C62 1.379(10) . ?
C61 H61 0.9500 . ?
C62 C63 1.366(10) . ?
C62 H62 0.9500 . ?
C63 C64 1.383(10) . ?
C65 C66 1.393(9) . ?
C65 C70 1.408(8) . ?
C66 C67 1.395(9) . ?
C66 H66 0.9500 . ?
C67 C68 1.366(10) . ?
C67 H67 0.9500 . ?
C68 C69 1.405(10) . ?
C68 H68 0.9500 . ?
C69 C70 1.358(9) . ?
C69 H69 0.9500 . ?
C71 C72 1.381(10) . ?
C71 C76 1.396(9) . ?
C72 C73 1.411(9) . ?
C72 H72 0.9500 . ?
C73 C74 1.400(11) . ?
C73 H73 0.9500 . ?
C74 C75 1.403(11) . ?
C74 H74 0.9500 . ?
C75 C76 1.378(8) . ?
C75 H75 0.9500 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C178 H17A 0.9800 . ?
C178 H17B 0.9800 . ?
C178 H17C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 O1 C27 117.6(6) . . ?
C5 O2 C28 118.5(6) . . ?
C2 C1 C6 119.9(6) . . ?
C2 C1 C7 121.5(6) . . ?
C6 C1 C7 117.2(6) . . ?
C1 C2 C3 120.4(6) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C4 C3 O1 124.0(6) . . ?
C4 C3 C2 120.7(7) . . ?
O1 C3 C2 115.2(6) . . ?
C3 C4 C5 118.8(6) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
O2 C5 C6 115.3(6) . . ?
O2 C5 C4 124.1(6) . . ?
C6 C5 C4 120.6(6) . . ?
C1 C6 C5 119.5(6) . . ?
C1 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C1 C7 C15 119.0(6) . . ?
C1 C7 C21 106.6(5) . . ?
C15 C7 C21 106.8(5) . . ?
C1 C7 C9 117.4(5) . . ?
C15 C7 C9 99.0(5) . . ?
C21 C7 C9 107.2(6) . . ?
C20 C8 C26 106.3(7) . . ?
C20 C8 C14 105.7(5) . . ?
C26 C8 C14 107.0(5) . . ?
C20 C8 H8 112.4 . . ?
C26 C8 H8 112.4 . . ?
C14 C8 H8 112.4 . . ?
C14 C9 C10 116.5(6) . . ?
C14 C9 C7 112.4(5) . . ?
C10 C9 C7 130.7(6) . . ?
C11 C10 C9 120.2(6) . . ?
C11 C10 Cl1 115.5(5) . . ?
C9 C10 Cl1 124.0(5) . . ?
C12 C11 C10 121.9(7) . . ?
C12 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
C11 C12 C13 118.6(7) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C12 C13 C14 121.1(6) . . ?
C12 C13 Cl2 118.6(6) . . ?
C14 C13 Cl2 120.3(5) . . ?
C13 C14 C9 121.0(6) . . ?
C13 C14 C8 125.6(6) . . ?
C9 C14 C8 113.1(6) . . ?
C16 C15 C20 120.2(6) . . ?
C16 C15 C7 127.9(6) . . ?
C20 C15 C7 111.7(6) . . ?
C15 C16 C17 119.4(6) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C18 C17 C16 120.7(6) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C19 C18 C17 118.8(6) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 C20 121.4(6) . . ?
C18 C19 Cl3 119.5(5) . . ?
C20 C19 Cl3 119.0(6) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
Cl3 C19 H19 2.3 . . ?
C19 C20 C15 119.1(6) . . ?
C19 C20 C8 125.8(6) . . ?
C15 C20 C8 114.9(6) . . ?
C26 C21 C22 119.9(7) . . ?
C26 C21 C7 115.1(6) . . ?
C22 C21 C7 124.9(7) . . ?
C23 C22 C21 116.6(9) . . ?
C23 C22 H22 121.7 . . ?
C21 C22 H22 121.7 . . ?
C24 C23 C22 123.5(9) . . ?
C24 C23 H23 118.2 . . ?
C22 C23 H23 118.2 . . ?
C23 C24 C25 119.0(8) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
C26 C25 C24 119.6(10) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C21 121.3(8) . . ?
C25 C26 C8 127.0(8) . . ?
C21 C26 C8 111.6(6) . . ?
O1 C27 H27A 109.5 . . ?
O1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O2 C28 H28A 109.5 . . ?
O2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C53 O3 C77 117.1(6) . . ?
C55 O4 C78 122.1(6) . . ?
C55 O4 C178 124.7(9) . . ?
C52 C51 C56 118.4(6) . . ?
C52 C51 C57 122.9(5) . . ?
C56 C51 C57 117.6(6) . . ?
C53 C52 C51 120.7(5) . . ?
C53 C52 H52 119.6 . . ?
C51 C52 H52 119.6 . . ?
O3 C53 C52 115.4(5) . . ?
O3 C53 C54 123.1(6) . . ?
C52 C53 C54 121.5(6) . . ?
C53 C54 C55 117.2(5) . . ?
C53 C54 H54 121.4 . . ?
C55 C54 H54 121.4 . . ?
O4 C55 C56 120.8(6) . . ?
O4 C55 C54 117.0(6) . . ?
C56 C55 C54 122.2(5) . . ?
C55 C56 C51 119.9(6) . . ?
C55 C56 H56 120.0 . . ?
C51 C56 H56 120.0 . . ?
C51 C57 C59 118.8(5) . . ?
C51 C57 C65 119.7(5) . . ?
C59 C57 C65 100.8(5) . . ?
C51 C57 C71 105.1(5) . . ?
C59 C57 C71 107.1(5) . . ?
C65 C57 C71 104.1(5) . . ?
C76 C58 C64 107.7(5) . . ?
C76 C58 C70 105.4(6) . . ?
C64 C58 C70 106.0(5) . . ?
C76 C58 H58 112.5 . . ?
C64 C58 H58 112.5 . . ?
C70 C58 H58 112.5 . . ?
C60 C59 C64 116.9(6) . . ?
C60 C59 C57 129.6(6) . . ?
C64 C59 C57 112.9(5) . . ?
C59 C60 C61 121.2(6) . . ?
C59 C60 Cl11 125.2(5) . . ?
C61 C60 Cl11 113.5(5) . . ?
C62 C61 C60 119.5(6) . . ?
C62 C61 H61 120.2 . . ?
C60 C61 H61 120.2 . . ?
C63 C62 C61 120.4(7) . . ?
C63 C62 H62 119.8 . . ?
C61 C62 H62 119.8 . . ?
C62 C63 C64 120.3(6) . . ?
C62 C63 Cl12 119.2(6) . . ?
C64 C63 Cl12 120.5(5) . . ?
C63 C64 C59 121.0(6) . . ?
C63 C64 C58 125.3(6) . . ?
C59 C64 C58 113.6(6) . . ?
C66 C65 C70 118.4(5) . . ?
C66 C65 C57 127.8(6) . . ?
C70 C65 C57 113.4(5) . . ?
C65 C66 C67 119.6(6) . . ?
C65 C66 H66 120.2 . . ?
C67 C66 H66 120.2 . . ?
C68 C67 C66 121.1(6) . . ?
C68 C67 H67 119.4 . . ?
C66 C67 H67 119.4 . . ?
C67 C68 C69 119.3(6) . . ?
C67 C68 H68 120.3 . . ?
C69 C68 H68 120.3 . . ?
C70 C69 C68 120.1(6) . . ?
C70 C69 Cl13 120.7(5) . . ?
C68 C69 Cl13 119.2(5) . . ?
C70 C69 H69 120.0 . . ?
C68 C69 H69 120.0 . . ?
Cl13 C69 H69 1.4 . . ?
C69 C70 C65 121.1(6) . . ?
C69 C70 C58 125.7(6) . . ?
C65 C70 C58 113.2(5) . . ?
C72 C71 C76 119.5(6) . . ?
C72 C71 C57 126.0(6) . . ?
C76 C71 C57 114.4(5) . . ?
C71 C72 C73 120.1(6) . . ?
C71 C72 H72 119.9 . . ?
C73 C72 H72 119.9 . . ?
C74 C73 C72 119.9(6) . . ?
C74 C73 H73 120.0 . . ?
C72 C73 H73 120.0 . . ?
C73 C74 C75 119.2(6) . . ?
C73 C74 H74 120.4 . . ?
C75 C74 H74 120.4 . . ?
C76 C75 C74 120.1(6) . . ?
C76 C75 H75 119.9 . . ?
C74 C75 H75 119.9 . . ?
C75 C76 C71 121.1(6) . . ?
C75 C76 C58 126.1(6) . . ?
C71 C76 C58 112.9(5) . . ?
O3 C77 H77A 109.5 . . ?
O3 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
O3 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
O4 C78 H78A 109.5 . . ?
O4 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
O4 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
O4 C178 H17A 109.5 . . ?
O4 C178 H17B 109.5 . . ?
H17A C178 H17B 109.5 . . ?
O4 C178 H17C 109.5 . . ?
H17A C178 H17C 109.5 . . ?
H17B C178 H17C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -2.9(11) . . . . ?
C7 C1 C2 C3 -168.7(6) . . . . ?
C27 O1 C3 C4 4.1(11) . . . . ?
C27 O1 C3 C2 -178.6(7) . . . . ?
C1 C2 C3 C4 0.8(11) . . . . ?
C1 C2 C3 O1 -176.6(7) . . . . ?
O1 C3 C4 C5 178.7(7) . . . . ?
C2 C3 C4 C5 1.5(11) . . . . ?
C28 O2 C5 C6 172.5(7) . . . . ?
C28 O2 C5 C4 -7.8(10) . . . . ?
C3 C4 C5 O2 178.7(7) . . . . ?
C3 C4 C5 C6 -1.7(11) . . . . ?
C2 C1 C6 C5 2.7(10) . . . . ?
C7 C1 C6 C5 169.1(6) . . . . ?
O2 C5 C6 C1 179.3(6) . . . . ?
C4 C5 C6 C1 -0.4(11) . . . . ?
C2 C1 C7 C15 -31.2(9) . . . . ?
C6 C1 C7 C15 162.6(6) . . . . ?
C2 C1 C7 C21 89.5(8) . . . . ?
C6 C1 C7 C21 -76.8(7) . . . . ?
C2 C1 C7 C9 -150.4(7) . . . . ?
C6 C1 C7 C9 43.4(8) . . . . ?
C1 C7 C9 C14 -166.5(6) . . . . ?
C15 C7 C9 C14 64.1(6) . . . . ?
C21 C7 C9 C14 -46.7(7) . . . . ?
C1 C7 C9 C10 21.4(10) . . . . ?
C15 C7 C9 C10 -108.0(8) . . . . ?
C21 C7 C9 C10 141.2(7) . . . . ?
C14 C9 C10 C11 8.8(10) . . . . ?
C7 C9 C10 C11 -179.4(7) . . . . ?
C14 C9 C10 Cl1 -165.6(5) . . . . ?
C7 C9 C10 Cl1 6.2(11) . . . . ?
C9 C10 C11 C12 -3.0(12) . . . . ?
Cl1 C10 C11 C12 171.8(6) . . . . ?
C10 C11 C12 C13 -3.5(12) . . . . ?
C11 C12 C13 C14 4.0(11) . . . . ?
C11 C12 C13 Cl2 -175.8(6) . . . . ?
C12 C13 C14 C9 2.1(11) . . . . ?
Cl2 C13 C14 C9 -178.1(5) . . . . ?
C12 C13 C14 C8 -170.6(7) . . . . ?
Cl2 C13 C14 C8 9.3(9) . . . . ?
C10 C9 C14 C13 -8.3(9) . . . . ?
C7 C9 C14 C13 178.3(6) . . . . ?
C10 C9 C14 C8 165.2(6) . . . . ?
C7 C9 C14 C8 -8.1(8) . . . . ?
C20 C8 C14 C13 122.3(7) . . . . ?
C26 C8 C14 C13 -124.6(7) . . . . ?
C20 C8 C14 C9 -50.9(7) . . . . ?
C26 C8 C14 C9 62.2(7) . . . . ?
C1 C7 C15 C16 -17.0(9) . . . . ?
C21 C7 C15 C16 -137.6(7) . . . . ?
C9 C7 C15 C16 111.3(7) . . . . ?
C1 C7 C15 C20 168.5(5) . . . . ?
C21 C7 C15 C20 47.9(7) . . . . ?
C9 C7 C15 C20 -63.2(6) . . . . ?
C20 C15 C16 C17 -6.2(10) . . . . ?
C7 C15 C16 C17 179.7(6) . . . . ?
C15 C16 C17 C18 1.9(10) . . . . ?
C16 C17 C18 C19 1.9(10) . . . . ?
C17 C18 C19 C20 -1.5(10) . . . . ?
C17 C18 C19 Cl3 175.9(5) . . . . ?
C18 C19 C20 C15 -2.8(9) . . . . ?
Cl3 C19 C20 C15 179.8(5) . . . . ?
C18 C19 C20 C8 171.6(6) . . . . ?
Cl3 C19 C20 C8 -5.8(9) . . . . ?
C16 C15 C20 C19 6.7(9) . . . . ?
C7 C15 C20 C19 -178.3(5) . . . . ?
C16 C15 C20 C8 -168.3(6) . . . . ?
C7 C15 C20 C8 6.6(8) . . . . ?
C26 C8 C20 C19 124.1(7) . . . . ?
C14 C8 C20 C19 -122.4(7) . . . . ?
C26 C8 C20 C15 -61.2(7) . . . . ?
C14 C8 C20 C15 52.3(8) . . . . ?
C1 C7 C21 C26 179.5(6) . . . . ?
C15 C7 C21 C26 -52.4(8) . . . . ?
C9 C7 C21 C26 53.0(7) . . . . ?
C1 C7 C21 C22 -3.4(10) . . . . ?
C15 C7 C21 C22 124.8(8) . . . . ?
C9 C7 C21 C22 -129.8(8) . . . . ?
C26 C21 C22 C23 -1.8(12) . . . . ?
C7 C21 C22 C23 -178.8(8) . . . . ?
C21 C22 C23 C24 3.0(15) . . . . ?
C22 C23 C24 C25 -1.6(16) . . . . ?
C23 C24 C25 C26 -0.9(14) . . . . ?
C24 C25 C26 C21 2.1(13) . . . . ?
C24 C25 C26 C8 179.0(8) . . . . ?
C22 C21 C26 C25 -0.7(12) . . . . ?
C7 C21 C26 C25 176.7(7) . . . . ?
C22 C21 C26 C8 -178.0(7) . . . . ?
C7 C21 C26 C8 -0.6(9) . . . . ?
C20 C8 C26 C25 -120.7(9) . . . . ?
C14 C8 C26 C25 126.6(8) . . . . ?
C20 C8 C26 C21 56.5(7) . . . . ?
C14 C8 C26 C21 -56.2(8) . . . . ?
C56 C51 C52 C53 3.6(9) . . . . ?
C57 C51 C52 C53 171.7(5) . . . . ?
C77 O3 C53 C52 172.9(7) . . . . ?
C77 O3 C53 C54 -4.3(10) . . . . ?
C51 C52 C53 O3 -179.1(5) . . . . ?
C51 C52 C53 C54 -1.9(9) . . . . ?
O3 C53 C54 C55 176.8(6) . . . . ?
C52 C53 C54 C55 -0.2(9) . . . . ?
C78 O4 C55 C56 -0.7(11) . . . . ?
C178 O4 C55 C56 -175.4(11) . . . . ?
C78 O4 C55 C54 179.7(8) . . . . ?
C178 O4 C55 C54 5.0(13) . . . . ?
C53 C54 C55 O4 -179.9(6) . . . . ?
C53 C54 C55 C56 0.5(9) . . . . ?
O4 C55 C56 C51 -178.3(5) . . . . ?
C54 C55 C56 C51 1.3(10) . . . . ?
C52 C51 C56 C55 -3.3(9) . . . . ?
C57 C51 C56 C55 -172.1(6) . . . . ?
C52 C51 C57 C59 150.6(5) . . . . ?
C56 C51 C57 C59 -41.2(7) . . . . ?
C52 C51 C57 C65 26.6(8) . . . . ?
C56 C51 C57 C65 -165.2(5) . . . . ?
C52 C51 C57 C71 -89.8(6) . . . . ?
C56 C51 C57 C71 78.5(6) . . . . ?
C51 C57 C59 C60 -22.9(9) . . . . ?
C65 C57 C59 C60 109.9(7) . . . . ?
C71 C57 C59 C60 -141.6(6) . . . . ?
C51 C57 C59 C64 165.3(5) . . . . ?
C65 C57 C59 C64 -61.8(6) . . . . ?
C71 C57 C59 C64 46.7(6) . . . . ?
C64 C59 C60 C61 -9.5(8) . . . . ?
C57 C59 C60 C61 179.1(6) . . . . ?
C64 C59 C60 Cl11 166.0(5) . . . . ?
C57 C59 C60 Cl11 -5.5(9) . . . . ?
C59 C60 C61 C62 3.7(10) . . . . ?
Cl11 C60 C61 C62 -172.2(6) . . . . ?
C60 C61 C62 C63 2.3(11) . . . . ?
C61 C62 C63 C64 -2.1(11) . . . . ?
C61 C62 C63 Cl12 176.5(6) . . . . ?
C62 C63 C64 C59 -4.1(10) . . . . ?
Cl12 C63 C64 C59 177.4(5) . . . . ?
C62 C63 C64 C58 170.8(6) . . . . ?
Cl12 C63 C64 C58 -7.7(9) . . . . ?
C60 C59 C64 C63 9.7(9) . . . . ?
C57 C59 C64 C63 -177.4(6) . . . . ?
C60 C59 C64 C58 -165.8(5) . . . . ?
C57 C59 C64 C58 7.1(7) . . . . ?
C76 C58 C64 C63 124.3(7) . . . . ?
C70 C58 C64 C63 -123.4(7) . . . . ?
C76 C58 C64 C59 -60.5(7) . . . . ?
C70 C58 C64 C59 51.8(7) . . . . ?
C51 C57 C65 C66 19.4(10) . . . . ?
C59 C57 C65 C66 -112.9(7) . . . . ?
C71 C57 C65 C66 136.3(7) . . . . ?
C51 C57 C65 C70 -168.4(5) . . . . ?
C59 C57 C65 C70 59.3(6) . . . . ?
C71 C57 C65 C70 -51.5(7) . . . . ?
C70 C65 C66 C67 6.2(10) . . . . ?
C57 C65 C66 C67 178.1(6) . . . . ?
C65 C66 C67 C68 -1.1(11) . . . . ?
C66 C67 C68 C69 -2.8(11) . . . . ?
C67 C68 C69 C70 1.4(10) . . . . ?
C67 C68 C69 Cl13 -177.2(5) . . . . ?
C68 C69 C70 C65 3.9(9) . . . . ?
Cl13 C69 C70 C65 -177.4(5) . . . . ?
C68 C69 C70 C58 -173.7(6) . . . . ?
Cl13 C69 C70 C58 4.9(9) . . . . ?
C66 C65 C70 C69 -7.7(9) . . . . ?
C57 C65 C70 C69 179.2(5) . . . . ?
C66 C65 C70 C58 170.2(6) . . . . ?
C57 C65 C70 C58 -2.9(7) . . . . ?
C76 C58 C70 C69 -122.5(6) . . . . ?
C64 C58 C70 C69 123.6(6) . . . . ?
C76 C58 C70 C65 59.8(6) . . . . ?
C64 C58 C70 C65 -54.2(7) . . . . ?
C51 C57 C71 C72 2.9(9) . . . . ?
C59 C57 C71 C72 130.0(7) . . . . ?
C65 C57 C71 C72 -123.8(7) . . . . ?
C51 C57 C71 C76 -179.6(5) . . . . ?
C59 C57 C71 C76 -52.4(7) . . . . ?
C65 C57 C71 C76 53.7(7) . . . . ?
C76 C71 C72 C73 0.2(10) . . . . ?
C57 C71 C72 C73 177.5(6) . . . . ?
C71 C72 C73 C74 1.5(11) . . . . ?
C72 C73 C74 C75 -0.7(11) . . . . ?
C73 C74 C75 C76 -1.9(11) . . . . ?
C74 C75 C76 C71 3.6(11) . . . . ?
C74 C75 C76 C58 -178.1(7) . . . . ?
C72 C71 C76 C75 -2.7(10) . . . . ?
C57 C71 C76 C75 179.6(7) . . . . ?
C72 C71 C76 C58 178.8(6) . . . . ?
C57 C71 C76 C58 1.1(8) . . . . ?
C64 C58 C76 C75 -123.5(7) . . . . ?
C70 C58 C76 C75 123.7(7) . . . . ?
C64 C58 C76 C71 54.9(7) . . . . ?
C70 C58 C76 C71 -57.9(7) . . . . ?

_refine_diff_density_max         0.766
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.075


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_chemical_compound_source        no
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TripPh(NH2)2
_database_code_depnum_ccdc_archive 'CCDC 2182984'
loop_
_audit_author_name
_audit_author_address
'Wataru Setaka'
;Tokyo Metropolitan University
Japan
;
_audit_update_record             
;
2022-06-30 deposited with the CCDC.	2022-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        (diaminophenyl)triptycene
_chemical_name_common            TripPh(NH2)2
_chemical_melting_point          '548 K (decomp.)'
_chemical_formula_moiety         'C26 H20 N2'
_chemical_formula_sum            'C26 H20 N2'
_chemical_formula_weight         360.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.58090(10)
_cell_length_b                   16.4594(3)
_cell_length_c                   20.4778(4)
_cell_angle_alpha                105.1070(10)
_cell_angle_beta                 97.6730(10)
_cell_angle_gamma                96.1400(10)
_cell_volume                     2736.72(8)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1846
_cell_measurement_theta_min      2.7528
_cell_measurement_theta_max      77.7531

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_F_000             1140
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.591
_shelx_estimated_absorpt_T_min   0.852
_shelx_estimated_absorpt_T_max   0.943
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_T_max  0.97


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed tube'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'

_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            23640
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.267
_diffrn_reflns_theta_max         72.424
_diffrn_reflns_theta_full        66.500
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 0.976
_reflns_number_total             10346
_reflns_number_gt                8987
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'Sir-2011 (IUCr, 2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2020)'
_computing_publication_material  'WinGX (Farrugia, 2020)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0524P)²+1.8253P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10346
_refine_ls_number_parameters     757
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1225
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.07097(19) 0.66883(10) 0.17019(7) 0.0293(3) Uani 1 1 d . . . . .
H1A H 0.003182 0.649034 0.131489 0.035 Uiso 1 1 calc R U . . .
H1B H 0.121004 0.721341 0.181711 0.035 Uiso 1 1 calc R U . . .
N2 N -0.02329(19) 0.39838(10) 0.22121(8) 0.0300(3) Uani 1 1 d . . . . .
H2A H -0.088527 0.377307 0.181900 0.036 Uiso 1 1 calc R U . . .
H2B H -0.004674 0.366260 0.248819 0.036 Uiso 1 1 calc R U . . .
C1 C 0.22763(17) 0.60049(10) 0.32169(8) 0.0157(3) Uani 1 1 d . . . . .
C2 C 0.20112(19) 0.65026(10) 0.27663(8) 0.0180(3) Uani 1 1 d . . . . .
H2 H 0.252722 0.707429 0.288949 0.022 Uiso 1 1 calc R U . . .
C3 C 0.0992(2) 0.61678(11) 0.21344(8) 0.0210(3) Uani 1 1 d . . . . .
C4 C 0.02126(19) 0.53361(11) 0.19613(8) 0.0220(3) Uani 1 1 d . . . . .
H4 H -0.052101 0.511527 0.154457 0.026 Uiso 1 1 calc R U . . .
C5 C 0.05050(19) 0.48257(11) 0.23974(8) 0.0208(3) Uani 1 1 d . . . . .
C6 C 0.15815(18) 0.51542(10) 0.30134(8) 0.0177(3) Uani 1 1 d . . . . .
H6 H 0.183944 0.479423 0.329421 0.021 Uiso 1 1 calc R U . . .
C7 C 0.34747(17) 0.63755(9) 0.38782(8) 0.0142(3) Uani 1 1 d . . . . .
C8 C 0.58010(18) 0.70149(10) 0.49304(8) 0.0156(3) Uani 1 1 d . . . . .
H8 H 0.667952 0.725737 0.533081 0.019 Uiso 1 1 calc R U . . .
C9 C 0.34837(18) 0.73296(9) 0.42470(8) 0.0147(3) Uani 1 1 d . . . . .
C10 C 0.22927(19) 0.78163(10) 0.41527(8) 0.0177(3) Uani 1 1 d . . . . .
H10 H 0.139894 0.758853 0.379874 0.021 Uiso 1 1 calc R U . . .
C11 C 0.2413(2) 0.86402(11) 0.45791(8) 0.0218(3) Uani 1 1 d . . . . .
H11 H 0.159413 0.897079 0.451381 0.026 Uiso 1 1 calc R U . . .
C12 C 0.3709(2) 0.89846(10) 0.50967(8) 0.0219(3) Uani 1 1 d . . . . .
H12 H 0.380125 0.955631 0.536977 0.026 Uiso 1 1 calc R U . . .
C13 C 0.48788(19) 0.84878(10) 0.52152(8) 0.0183(3) Uani 1 1 d . . . . .
H13 H 0.575114 0.871166 0.558010 0.022 Uiso 1 1 calc R U . . .
C14 C 0.47563(18) 0.76667(10) 0.47967(8) 0.0152(3) Uani 1 1 d . . . . .
C15 C 0.33419(18) 0.59895(9) 0.44903(8) 0.0149(3) Uani 1 1 d . . . . .
C16 C 0.20733(18) 0.54564(10) 0.45817(8) 0.0163(3) Uani 1 1 d . . . . .
H16 H 0.115483 0.526623 0.423624 0.020 Uiso 1 1 calc R U . . .
C17 C 0.21492(19) 0.51996(10) 0.51829(8) 0.0186(3) Uani 1 1 d . . . . .
H17 H 0.128928 0.482230 0.523723 0.022 Uiso 1 1 calc R U . . .
C18 C 0.34591(19) 0.54871(10) 0.57003(8) 0.0193(3) Uani 1 1 d . . . . .
H18 H 0.351525 0.529290 0.609969 0.023 Uiso 1 1 calc R U . . .
C19 C 0.46909(19) 0.60622(10) 0.56304(8) 0.0179(3) Uani 1 1 d . . . . .
H19 H 0.557586 0.628078 0.599005 0.021 Uiso 1 1 calc R U . . .
C20 C 0.46237(18) 0.63154(9) 0.50352(8) 0.0157(3) Uani 1 1 d . . . . .
C21 C 0.51621(18) 0.62810(9) 0.37150(8) 0.0151(3) Uani 1 1 d . . . . .
C22 C 0.55100(19) 0.58611(10) 0.30827(8) 0.0175(3) Uani 1 1 d . . . . .
H22 H 0.467942 0.562182 0.270194 0.021 Uiso 1 1 calc R U . . .
C23 C 0.7086(2) 0.57926(10) 0.30099(9) 0.0204(3) Uani 1 1 d . . . . .
H23 H 0.732743 0.549428 0.258043 0.024 Uiso 1 1 calc R U . . .
C24 C 0.83085(19) 0.61583(10) 0.35619(9) 0.0210(3) Uani 1 1 d . . . . .
H24 H 0.938161 0.612054 0.350492 0.025 Uiso 1 1 calc R U . . .
C25 C 0.79646(19) 0.65804(10) 0.41988(8) 0.0185(3) Uani 1 1 d . . . . .
H25 H 0.879667 0.683068 0.457706 0.022 Uiso 1 1 calc R U . . .
C26 C 0.63928(18) 0.66296(9) 0.42723(8) 0.0159(3) Uani 1 1 d . . . . .
N3 N -0.2437(2) -0.25623(9) 0.22941(8) 0.0309(4) Uani 1 1 d . . . . .
H3A H -0.291985 -0.299403 0.240502 0.037 Uiso 1 1 calc R U . . .
H3B H -0.226711 -0.262259 0.187080 0.037 Uiso 1 1 calc R U . . .
N4 N -0.17510(18) -0.08410(10) 0.46438(8) 0.0265(3) Uani 1 1 d . . . . .
H4A H -0.215034 -0.128648 0.476192 0.032 Uiso 1 1 calc R U . . .
H4B H -0.140888 -0.035397 0.495875 0.032 Uiso 1 1 calc R U . . .
C31 C -0.07505(18) -0.02936(10) 0.30923(8) 0.0186(3) Uani 1 1 d . . . . .
C32 C -0.1209(2) -0.10869(10) 0.26103(8) 0.0208(3) Uani 1 1 d . . . . .
H32 H -0.102372 -0.115792 0.215310 0.025 Uiso 1 1 calc R U . . .
C33 C -0.1939(2) -0.17786(10) 0.27916(9) 0.0228(3) Uani 1 1 d . . . . .
C34 C -0.2202(2) -0.16773(11) 0.34609(9) 0.0228(3) Uani 1 1 d . . . . .
H34 H -0.275324 -0.213555 0.358002 0.027 Uiso 1 1 calc R U . . .
C35 C -0.16603(19) -0.09070(11) 0.39567(9) 0.0207(3) Uani 1 1 d . . . . .
C36 C -0.09341(18) -0.02157(10) 0.37733(8) 0.0187(3) Uani 1 1 d . . . . .
H36 H -0.056339 0.030983 0.411348 0.022 Uiso 1 1 calc R U . . .
C37 C 0.01892(18) 0.04224(10) 0.28970(8) 0.0178(3) Uani 1 1 d . . . . .
C38 C 0.21148(19) 0.15481(10) 0.25618(9) 0.0216(3) Uani 1 1 d . . . . .
H38 H 0.284085 0.197808 0.243543 0.026 Uiso 1 1 calc R U . . .
C39 C -0.02520(19) 0.04631(10) 0.21463(8) 0.0187(3) Uani 1 1 d . . . . .
C40 C -0.1637(2) 0.00754(10) 0.16879(9) 0.0227(3) Uani 1 1 d . . . . .
H40 H -0.241885 -0.028140 0.181383 0.027 Uiso 1 1 calc R U . . .
C41 C -0.1869(2) 0.02145(11) 0.10413(9) 0.0276(4) Uani 1 1 d . . . . .
H41 H -0.280965 -0.005720 0.072548 0.033 Uiso 1 1 calc R U . . .
C42 C -0.0757(2) 0.07400(12) 0.08507(9) 0.0285(4) Uani 1 1 d . . . . .
H42 H -0.090748 0.080345 0.039953 0.034 Uiso 1 1 calc R U . . .
C43 C 0.0587(2) 0.11766(11) 0.13227(9) 0.0247(4) Uani 1 1 d . . . . .
H43 H 0.133237 0.156152 0.120494 0.030 Uiso 1 1 calc R U . . .
C44 C 0.08192(19) 0.10405(10) 0.19666(9) 0.0209(3) Uani 1 1 d . . . . .
C45 C 0.01316(19) 0.13612(10) 0.33003(8) 0.0187(3) Uani 1 1 d . . . . .
C46 C -0.0916(2) 0.16652(10) 0.37348(8) 0.0208(3) Uani 1 1 d . . . . .
H46 H -0.165772 0.127692 0.385064 0.025 Uiso 1 1 calc R U . . .
C47 C -0.0881(2) 0.25433(11) 0.40031(9) 0.0247(4) Uani 1 1 d . . . . .
H47 H -0.158770 0.274829 0.430666 0.030 Uiso 1 1 calc R U . . .
C48 C 0.0175(2) 0.31115(11) 0.38276(9) 0.0259(4) Uani 1 1 d . . . . .
H48 H 0.019752 0.370619 0.401183 0.031 Uiso 1 1 calc R U . . .
C49 C 0.1207(2) 0.28140(11) 0.33816(9) 0.0242(4) Uani 1 1 d . . . . .
H49 H 0.192547 0.320566 0.325758 0.029 Uiso 1 1 calc R U . . .
C50 C 0.11878(19) 0.19472(10) 0.31180(8) 0.0203(3) Uani 1 1 d . . . . .
C51 C 0.19640(19) 0.03090(10) 0.29969(8) 0.0187(3) Uani 1 1 d . . . . .
C52 C 0.2582(2) -0.03193(10) 0.32492(8) 0.0205(3) Uani 1 1 d . . . . .
H52 H 0.190167 -0.072009 0.338158 0.025 Uiso 1 1 calc R U . . .
C53 C 0.4207(2) -0.03540(11) 0.33055(8) 0.0234(4) Uani 1 1 d . . . . .
H53 H 0.463863 -0.077345 0.348632 0.028 Uiso 1 1 calc R U . . .
C54 C 0.5200(2) 0.02188(12) 0.30997(9) 0.0259(4) Uani 1 1 d . . . . .
H54 H 0.630128 0.017673 0.312552 0.031 Uiso 1 1 calc R U . . .
C55 C 0.4592(2) 0.08557(11) 0.28553(9) 0.0243(4) Uani 1 1 d . . . . .
H55 H 0.527290 0.125255 0.271932 0.029 Uiso 1 1 calc R U . . .
C56 C 0.2978(2) 0.09023(10) 0.28133(8) 0.0205(3) Uani 1 1 d . . . . .
N5 N 0.6371(2) -0.00296(10) -0.07229(8) 0.0339(4) Uani 1 1 d . . . . .
H5A H 0.649940 -0.040728 -0.109710 0.041 Uiso 1 1 calc R U . . .
H5B H 0.631824 -0.017927 -0.034316 0.041 Uiso 1 1 calc R U . . .
N6 N 0.6054(2) 0.20785(10) -0.19750(8) 0.0325(4) Uani 1 1 d . . . . .
H6A H 0.625749 0.171705 -0.234245 0.039 Uiso 1 1 calc R U . . .
H6B H 0.586229 0.258851 -0.198995 0.039 Uiso 1 1 calc R U . . .
C61 C 0.57381(19) 0.22211(11) -0.01659(9) 0.0213(3) Uani 1 1 d . . . . .
C62 C 0.5936(2) 0.13954(11) -0.01500(9) 0.0233(4) Uani 1 1 d . . . . .
H62 H 0.585575 0.123019 0.025695 0.028 Uiso 1 1 calc R U . . .
C63 C 0.6252(2) 0.08075(11) -0.07318(9) 0.0253(4) Uani 1 1 d . . . . .
C64 C 0.6337(2) 0.10388(11) -0.13332(9) 0.0272(4) Uani 1 1 d . . . . .
H64 H 0.659906 0.065001 -0.172031 0.033 Uiso 1 1 calc R U . . .
C65 C 0.6036(2) 0.18419(11) -0.13662(9) 0.0244(4) Uani 1 1 d . . . . .
C66 C 0.5758(2) 0.24302(11) -0.07834(9) 0.0227(3) Uani 1 1 d . . . . .
H66 H 0.557904 0.298247 -0.080672 0.027 Uiso 1 1 calc R U . . .
C67 C 0.5191(2) 0.28513(11) 0.04156(8) 0.0219(3) Uani 1 1 d . . . . .
C68 C 0.3849(2) 0.38937(12) 0.13039(9) 0.0285(4) Uani 1 1 d . . . . .
H68 H 0.334225 0.429009 0.164237 0.034 Uiso 1 1 calc R U . . .
C69 C 0.5606(2) 0.27945(11) 0.11623(8) 0.0222(3) Uani 1 1 d . . . . .
C70 C 0.6712(2) 0.23490(11) 0.14186(9) 0.0230(3) Uani 1 1 d . . . . .
H70 H 0.728074 0.200203 0.111695 0.028 Uiso 1 1 calc R U . . .
C71 C 0.6989(2) 0.24101(11) 0.21190(9) 0.0257(4) Uani 1 1 d . . . . .
H71 H 0.772194 0.209017 0.228903 0.031 Uiso 1 1 calc R U . . .
C72 C 0.6201(2) 0.29339(11) 0.25673(9) 0.0273(4) Uani 1 1 d . . . . .
H72 H 0.639348 0.296993 0.304245 0.033 Uiso 1 1 calc R U . . .
C73 C 0.5132(2) 0.34061(11) 0.23235(9) 0.0272(4) Uani 1 1 d . . . . .
H73 H 0.460412 0.377201 0.263139 0.033 Uiso 1 1 calc R U . . .
C74 C 0.4841(2) 0.33404(11) 0.16288(9) 0.0253(4) Uani 1 1 d . . . . .
C75 C 0.5771(2) 0.38133(11) 0.05124(8) 0.0235(4) Uani 1 1 d . . . . .
C76 C 0.6974(2) 0.41623(11) 0.02354(9) 0.0255(4) Uani 1 1 d . . . . .
H76 H 0.755686 0.380142 -0.004871 0.031 Uiso 1 1 calc R U . . .
C77 C 0.7333(2) 0.50489(12) 0.03739(10) 0.0306(4) Uani 1 1 d . . . . .
H77 H 0.813135 0.528571 0.016897 0.037 Uiso 1 1 calc R U . . .
C78 C 0.6532(2) 0.55779(12) 0.08057(10) 0.0331(4) Uani 1 1 d . . . . .
H78 H 0.676723 0.617728 0.089158 0.040 Uiso 1 1 calc R U . . .
C79 C 0.5380(2) 0.52337(12) 0.11159(9) 0.0315(4) Uani 1 1 d . . . . .
H79 H 0.484957 0.559760 0.142404 0.038 Uiso 1 1 calc R U . . .
C80 C 0.5010(2) 0.43571(11) 0.09734(9) 0.0268(4) Uani 1 1 d . . . . .
C81 C 0.3350(2) 0.27345(11) 0.02519(9) 0.0238(4) Uani 1 1 d . . . . .
C82 C 0.2402(2) 0.21306(12) -0.03047(9) 0.0275(4) Uani 1 1 d . . . . .
H82 H 0.287441 0.174932 -0.062650 0.033 Uiso 1 1 calc R U . . .
C83 C 0.0754(2) 0.20900(13) -0.03858(11) 0.0338(4) Uani 1 1 d . . . . .
H83 H 0.010140 0.167657 -0.076306 0.041 Uiso 1 1 calc R U . . .
C84 C 0.0064(2) 0.26474(14) 0.00789(12) 0.0382(5) Uani 1 1 d . . . . .
H84 H -0.105985 0.261742 0.001844 0.046 Uiso 1 1 calc R U . . .
C85 C 0.1013(2) 0.32545(13) 0.06371(11) 0.0352(4) Uani 1 1 d . . . . .
H85 H 0.053930 0.364025 0.095505 0.042 Uiso 1 1 calc R U . . .
C86 C 0.2646(2) 0.32895(12) 0.07231(9) 0.0278(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C3 1.400(2) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
N2 C5 1.392(2) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
C1 C6 1.393(2) . ?
C1 C2 1.397(2) . ?
C1 C7 1.525(2) . ?
C2 C3 1.402(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(2) . ?
C4 C5 1.394(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.401(2) . ?
C6 H6 0.9500 . ?
C7 C21 1.544(2) . ?
C7 C9 1.554(2) . ?
C7 C15 1.557(2) . ?
C8 C26 1.511(2) . ?
C8 C14 1.524(2) . ?
C8 C20 1.527(2) . ?
C8 H8 1.0000 . ?
C9 C10 1.388(2) . ?
C9 C14 1.409(2) . ?
C10 C11 1.393(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.396(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(2) . ?
C13 H13 0.9500 . ?
C15 C16 1.388(2) . ?
C15 C20 1.406(2) . ?
C16 C17 1.398(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(2) . ?
C19 H19 0.9500 . ?
C21 C22 1.387(2) . ?
C21 C26 1.398(2) . ?
C22 C23 1.394(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.391(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.395(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(2) . ?
C25 H25 0.9500 . ?
N3 C33 1.402(2) . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
N4 C35 1.396(2) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
C31 C32 1.396(2) . ?
C31 C36 1.399(2) . ?
C31 C37 1.526(2) . ?
C32 C33 1.398(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.389(2) . ?
C34 C35 1.390(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.399(2) . ?
C36 H36 0.9500 . ?
C37 C51 1.547(2) . ?
C37 C39 1.554(2) . ?
C37 C45 1.560(2) . ?
C38 C56 1.515(2) . ?
C38 C50 1.525(2) . ?
C38 C44 1.526(2) . ?
C38 H38 1.0000 . ?
C39 C40 1.389(2) . ?
C39 C44 1.403(2) . ?
C40 C41 1.394(2) . ?
C40 H40 0.9500 . ?
C41 C42 1.382(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.394(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.386(2) . ?
C43 H43 0.9500 . ?
C45 C46 1.388(2) . ?
C45 C50 1.408(2) . ?
C46 C47 1.401(2) . ?
C46 H46 0.9500 . ?
C47 C48 1.381(3) . ?
C47 H47 0.9500 . ?
C48 C49 1.390(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.385(2) . ?
C49 H49 0.9500 . ?
C51 C52 1.393(2) . ?
C51 C56 1.396(2) . ?
C52 C53 1.392(2) . ?
C52 H52 0.9500 . ?
C53 C54 1.387(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.394(3) . ?
C54 H54 0.9500 . ?
C55 C56 1.387(2) . ?
C55 H55 0.9500 . ?
N5 C63 1.397(2) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N6 C65 1.401(2) . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8800 . ?
C61 C62 1.396(2) . ?
C61 C66 1.396(2) . ?
C61 C67 1.524(2) . ?
C62 C63 1.404(2) . ?
C62 H62 0.9500 . ?
C63 C64 1.389(3) . ?
C64 C65 1.390(3) . ?
C64 H64 0.9500 . ?
C65 C66 1.394(2) . ?
C66 H66 0.9500 . ?
C67 C81 1.551(2) . ?
C67 C69 1.552(2) . ?
C67 C75 1.561(2) . ?
C68 C86 1.518(3) . ?
C68 C80 1.523(3) . ?
C68 C74 1.526(2) . ?
C68 H68 1.0000 . ?
C69 C70 1.389(2) . ?
C69 C74 1.413(2) . ?
C70 C71 1.397(2) . ?
C70 H70 0.9500 . ?
C71 C72 1.386(3) . ?
C71 H71 0.9500 . ?
C72 C73 1.388(3) . ?
C72 H72 0.9500 . ?
C73 C74 1.385(2) . ?
C73 H73 0.9500 . ?
C75 C76 1.384(3) . ?
C75 C80 1.403(2) . ?
C76 C77 1.403(3) . ?
C76 H76 0.9500 . ?
C77 C78 1.379(3) . ?
C77 H77 0.9500 . ?
C78 C79 1.392(3) . ?
C78 H78 0.9500 . ?
C79 C80 1.388(3) . ?
C79 H79 0.9500 . ?
C81 C82 1.392(3) . ?
C81 C86 1.395(2) . ?
C82 C83 1.394(3) . ?
C82 H82 0.9500 . ?
C83 C84 1.382(3) . ?
C83 H83 0.9500 . ?
C84 C85 1.396(3) . ?
C84 H84 0.9500 . ?
C85 C86 1.382(3) . ?
C85 H85 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 N1 H1A 120.0 . . ?
C3 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C5 N2 H2A 120.0 . . ?
C5 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C6 C1 C2 118.96(14) . . ?
C6 C1 C7 121.60(13) . . ?
C2 C1 C7 119.01(14) . . ?
C1 C2 C3 120.74(15) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C4 C3 N1 120.85(15) . . ?
C4 C3 C2 119.52(15) . . ?
N1 C3 C2 119.55(15) . . ?
C3 C4 C5 120.19(15) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N2 C5 C4 120.13(15) . . ?
N2 C5 C6 120.04(15) . . ?
C4 C5 C6 119.80(15) . . ?
C1 C6 C5 120.48(15) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C1 C7 C21 108.72(12) . . ?
C1 C7 C9 115.92(12) . . ?
C21 C7 C9 107.14(12) . . ?
C1 C7 C15 118.77(13) . . ?
C21 C7 C15 105.45(11) . . ?
C9 C7 C15 99.76(11) . . ?
C26 C8 C14 107.62(12) . . ?
C26 C8 C20 106.20(12) . . ?
C14 C8 C20 103.33(12) . . ?
C26 C8 H8 113.0 . . ?
C14 C8 H8 113.0 . . ?
C20 C8 H8 113.0 . . ?
C10 C9 C14 118.98(14) . . ?
C10 C9 C7 127.06(14) . . ?
C14 C9 C7 113.28(13) . . ?
C9 C10 C11 119.74(15) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 121.00(15) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 119.71(15) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 119.41(15) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C9 121.02(14) . . ?
C13 C14 C8 124.75(14) . . ?
C9 C14 C8 113.74(13) . . ?
C16 C15 C20 118.46(14) . . ?
C16 C15 C7 128.12(13) . . ?
C20 C15 C7 113.02(13) . . ?
C15 C16 C17 119.89(14) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C18 C17 C16 120.97(15) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C17 C18 C19 119.43(14) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C20 C19 C18 119.75(14) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C15 121.25(14) . . ?
C19 C20 C8 124.53(14) . . ?
C15 C20 C8 113.96(13) . . ?
C22 C21 C26 119.78(14) . . ?
C22 C21 C7 125.24(14) . . ?
C26 C21 C7 114.93(13) . . ?
C21 C22 C23 119.54(15) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 120.41(15) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 120.24(15) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C26 C25 C24 119.09(15) . . ?
C26 C25 H25 120.5 . . ?
C24 C25 H25 120.5 . . ?
C25 C26 C21 120.90(14) . . ?
C25 C26 C8 126.15(14) . . ?
C21 C26 C8 112.92(13) . . ?
C33 N3 H3A 120.0 . . ?
C33 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C35 N4 H4A 120.0 . . ?
C35 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C32 C31 C36 118.73(15) . . ?
C32 C31 C37 119.46(14) . . ?
C36 C31 C37 120.98(14) . . ?
C31 C32 C33 120.88(15) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C34 C33 C32 119.64(15) . . ?
C34 C33 N3 120.42(15) . . ?
C32 C33 N3 119.93(16) . . ?
C33 C34 C35 120.13(15) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C34 C35 N4 119.82(15) . . ?
C34 C35 C36 119.98(15) . . ?
N4 C35 C36 120.07(15) . . ?
C31 C36 C35 120.41(15) . . ?
C31 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C31 C37 C51 107.95(12) . . ?
C31 C37 C39 116.42(13) . . ?
C51 C37 C39 106.37(12) . . ?
C31 C37 C45 118.61(13) . . ?
C51 C37 C45 105.78(12) . . ?
C39 C37 C45 100.65(12) . . ?
C56 C38 C50 106.95(13) . . ?
C56 C38 C44 106.37(13) . . ?
C50 C38 C44 103.66(13) . . ?
C56 C38 H38 113.0 . . ?
C50 C38 H38 113.0 . . ?
C44 C38 H38 113.0 . . ?
C40 C39 C44 118.90(15) . . ?
C40 C39 C37 127.12(15) . . ?
C44 C39 C37 113.52(14) . . ?
C39 C40 C41 119.39(16) . . ?
C39 C40 H40 120.3 . . ?
C41 C40 H40 120.3 . . ?
C42 C41 C40 121.27(16) . . ?
C42 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C41 C42 C43 119.78(16) . . ?
C41 C42 H42 120.1 . . ?
C43 C42 H42 120.1 . . ?
C44 C43 C42 118.97(16) . . ?
C44 C43 H43 120.5 . . ?
C42 C43 H43 120.5 . . ?
C43 C44 C39 121.39(15) . . ?
C43 C44 C38 124.75(15) . . ?
C39 C44 C38 113.56(14) . . ?
C46 C45 C50 118.99(15) . . ?
C46 C45 C37 128.30(15) . . ?
C50 C45 C37 112.29(14) . . ?
C45 C46 C47 120.20(16) . . ?
C45 C46 H46 119.9 . . ?
C47 C46 H46 119.9 . . ?
C48 C47 C46 120.22(16) . . ?
C48 C47 H47 119.9 . . ?
C46 C47 H47 119.9 . . ?
C47 C48 C49 120.07(16) . . ?
C47 C48 H48 120.0 . . ?
C49 C48 H48 120.0 . . ?
C50 C49 C48 120.06(16) . . ?
C50 C49 H49 120.0 . . ?
C48 C49 H49 120.0 . . ?
C49 C50 C45 120.44(16) . . ?
C49 C50 C38 124.56(15) . . ?
C45 C50 C38 114.61(14) . . ?
C52 C51 C56 119.85(15) . . ?
C52 C51 C37 125.33(15) . . ?
C56 C51 C37 114.82(14) . . ?
C53 C52 C51 119.33(16) . . ?
C53 C52 H52 120.3 . . ?
C51 C52 H52 120.3 . . ?
C54 C53 C52 120.56(15) . . ?
C54 C53 H53 119.7 . . ?
C52 C53 H53 119.7 . . ?
C53 C54 C55 120.33(16) . . ?
C53 C54 H54 119.8 . . ?
C55 C54 H54 119.8 . . ?
C56 C55 C54 119.12(16) . . ?
C56 C55 H55 120.4 . . ?
C54 C55 H55 120.4 . . ?
C55 C56 C51 120.74(15) . . ?
C55 C56 C38 126.33(15) . . ?
C51 C56 C38 112.91(14) . . ?
C63 N5 H5A 120.0 . . ?
C63 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C65 N6 H6A 120.0 . . ?
C65 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C62 C61 C66 118.58(16) . . ?
C62 C61 C67 122.70(15) . . ?
C66 C61 C67 117.67(15) . . ?
C61 C62 C63 120.39(16) . . ?
C61 C62 H62 119.8 . . ?
C63 C62 H62 119.8 . . ?
C64 C63 N5 119.66(16) . . ?
C64 C63 C62 120.14(16) . . ?
N5 C63 C62 120.05(17) . . ?
C63 C64 C65 119.71(16) . . ?
C63 C64 H64 120.1 . . ?
C65 C64 H64 120.1 . . ?
C64 C65 C66 119.92(16) . . ?
C64 C65 N6 120.78(16) . . ?
C66 C65 N6 119.27(16) . . ?
C65 C66 C61 121.06(16) . . ?
C65 C66 H66 119.5 . . ?
C61 C66 H66 119.5 . . ?
C61 C67 C81 106.94(13) . . ?
C61 C67 C69 119.57(14) . . ?
C81 C67 C69 105.85(13) . . ?
C61 C67 C75 116.40(14) . . ?
C81 C67 C75 105.99(13) . . ?
C69 C67 C75 100.95(13) . . ?
C86 C68 C80 106.74(14) . . ?
C86 C68 C74 106.49(14) . . ?
C80 C68 C74 104.26(15) . . ?
C86 C68 H68 112.9 . . ?
C80 C68 H68 112.9 . . ?
C74 C68 H68 112.9 . . ?
C70 C69 C74 118.55(15) . . ?
C70 C69 C67 128.15(15) . . ?
C74 C69 C67 112.99(14) . . ?
C69 C70 C71 120.14(16) . . ?
C69 C70 H70 119.9 . . ?
C71 C70 H70 119.9 . . ?
C72 C71 C70 120.48(16) . . ?
C72 C71 H71 119.8 . . ?
C70 C71 H71 119.8 . . ?
C71 C72 C73 120.14(16) . . ?
C71 C72 H72 119.9 . . ?
C73 C72 H72 119.9 . . ?
C74 C73 C72 119.57(17) . . ?
C74 C73 H73 120.2 . . ?
C72 C73 H73 120.2 . . ?
C73 C74 C69 121.03(16) . . ?
C73 C74 C68 124.95(16) . . ?
C69 C74 C68 113.71(15) . . ?
C76 C75 C80 119.04(16) . . ?
C76 C75 C67 127.66(16) . . ?
C80 C75 C67 113.16(16) . . ?
C75 C76 C77 120.04(17) . . ?
C75 C76 H76 120.0 . . ?
C77 C76 H76 120.0 . . ?
C78 C77 C76 120.35(19) . . ?
C78 C77 H77 119.8 . . ?
C76 C77 H77 119.8 . . ?
C77 C78 C79 120.00(17) . . ?
C77 C78 H78 120.0 . . ?
C79 C78 H78 120.0 . . ?
C80 C79 C78 119.76(18) . . ?
C80 C79 H79 120.1 . . ?
C78 C79 H79 120.1 . . ?
C79 C80 C75 120.64(18) . . ?
C79 C80 C68 125.47(17) . . ?
C75 C80 C68 113.84(16) . . ?
C82 C81 C86 119.87(16) . . ?
C82 C81 C67 125.47(15) . . ?
C86 C81 C67 114.65(15) . . ?
C81 C82 C83 119.45(17) . . ?
C81 C82 H82 120.3 . . ?
C83 C82 H82 120.3 . . ?
C84 C83 C82 120.42(18) . . ?
C84 C83 H83 119.8 . . ?
C82 C83 H83 119.8 . . ?
C83 C84 C85 120.23(18) . . ?
C83 C84 H84 119.9 . . ?
C85 C84 H84 119.9 . . ?
C86 C85 C84 119.46(18) . . ?
C86 C85 H85 120.3 . . ?
C84 C85 H85 120.3 . . ?
C85 C86 C81 120.56(18) . . ?
C85 C86 C68 126.47(17) . . ?
C81 C86 C68 112.96(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 3.5(2) . . . . ?
C7 C1 C2 C3 176.13(14) . . . . ?
C1 C2 C3 C4 1.3(2) . . . . ?
C1 C2 C3 N1 178.06(15) . . . . ?
N1 C3 C4 C5 -179.94(15) . . . . ?
C2 C3 C4 C5 -3.2(2) . . . . ?
C3 C4 C5 N2 -177.71(15) . . . . ?
C3 C4 C5 C6 0.3(2) . . . . ?
C2 C1 C6 C5 -6.5(2) . . . . ?
C7 C1 C6 C5 -178.88(14) . . . . ?
N2 C5 C6 C1 -177.36(15) . . . . ?
C4 C5 C6 C1 4.6(2) . . . . ?
C6 C1 C7 C21 90.74(16) . . . . ?
C2 C1 C7 C21 -81.67(16) . . . . ?
C6 C1 C7 C9 -148.54(14) . . . . ?
C2 C1 C7 C9 39.05(19) . . . . ?
C6 C1 C7 C15 -29.7(2) . . . . ?
C2 C1 C7 C15 157.86(13) . . . . ?
C1 C7 C9 C10 18.2(2) . . . . ?
C21 C7 C9 C10 139.73(15) . . . . ?
C15 C7 C9 C10 -110.64(16) . . . . ?
C1 C7 C9 C14 -171.47(13) . . . . ?
C21 C7 C9 C14 -49.91(16) . . . . ?
C15 C7 C9 C14 59.72(15) . . . . ?
C14 C9 C10 C11 3.1(2) . . . . ?
C7 C9 C10 C11 173.00(15) . . . . ?
C9 C10 C11 C12 0.2(2) . . . . ?
C10 C11 C12 C13 -3.0(3) . . . . ?
C11 C12 C13 C14 2.4(2) . . . . ?
C12 C13 C14 C9 1.0(2) . . . . ?
C12 C13 C14 C8 -170.48(15) . . . . ?
C10 C9 C14 C13 -3.7(2) . . . . ?
C7 C9 C14 C13 -174.95(13) . . . . ?
C10 C9 C14 C8 168.61(13) . . . . ?
C7 C9 C14 C8 -2.61(18) . . . . ?
C26 C8 C14 C13 -131.63(15) . . . . ?
C20 C8 C14 C13 116.28(16) . . . . ?
C26 C8 C14 C9 56.36(16) . . . . ?
C20 C8 C14 C9 -55.74(16) . . . . ?
C1 C7 C15 C16 -14.8(2) . . . . ?
C21 C7 C15 C16 -136.88(15) . . . . ?
C9 C7 C15 C16 112.15(16) . . . . ?
C1 C7 C15 C20 172.69(13) . . . . ?
C21 C7 C15 C20 50.57(16) . . . . ?
C9 C7 C15 C20 -60.40(15) . . . . ?
C20 C15 C16 C17 -5.3(2) . . . . ?
C7 C15 C16 C17 -177.45(14) . . . . ?
C15 C16 C17 C18 1.7(2) . . . . ?
C16 C17 C18 C19 2.2(2) . . . . ?
C17 C18 C19 C20 -2.5(2) . . . . ?
C18 C19 C20 C15 -1.2(2) . . . . ?
C18 C19 C20 C8 172.71(14) . . . . ?
C16 C15 C20 C19 5.1(2) . . . . ?
C7 C15 C20 C19 178.40(13) . . . . ?
C16 C15 C20 C8 -169.45(13) . . . . ?
C7 C15 C20 C8 3.89(18) . . . . ?
C26 C8 C20 C19 127.62(15) . . . . ?
C14 C8 C20 C19 -119.25(15) . . . . ?
C26 C8 C20 C15 -58.08(16) . . . . ?
C14 C8 C20 C15 55.05(16) . . . . ?
C1 C7 C21 C22 -5.2(2) . . . . ?
C9 C7 C21 C22 -131.14(15) . . . . ?
C15 C7 C21 C22 123.23(15) . . . . ?
C1 C7 C21 C26 177.34(13) . . . . ?
C9 C7 C21 C26 51.35(16) . . . . ?
C15 C7 C21 C26 -54.27(16) . . . . ?
C26 C21 C22 C23 -0.1(2) . . . . ?
C7 C21 C22 C23 -177.50(14) . . . . ?
C21 C22 C23 C24 -1.4(2) . . . . ?
C22 C23 C24 C25 1.5(2) . . . . ?
C23 C24 C25 C26 0.0(2) . . . . ?
C24 C25 C26 C21 -1.5(2) . . . . ?
C24 C25 C26 C8 176.22(14) . . . . ?
C22 C21 C26 C25 1.6(2) . . . . ?
C7 C21 C26 C25 179.25(13) . . . . ?
C22 C21 C26 C8 -176.42(13) . . . . ?
C7 C21 C26 C8 1.24(18) . . . . ?
C14 C8 C26 C25 126.76(16) . . . . ?
C20 C8 C26 C25 -123.10(16) . . . . ?
C14 C8 C26 C21 -55.34(16) . . . . ?
C20 C8 C26 C21 54.79(16) . . . . ?
C36 C31 C32 C33 4.3(2) . . . . ?
C37 C31 C32 C33 173.93(14) . . . . ?
C31 C32 C33 C34 -0.4(2) . . . . ?
C31 C32 C33 N3 177.92(15) . . . . ?
C32 C33 C34 C35 -3.7(2) . . . . ?
N3 C33 C34 C35 177.95(15) . . . . ?
C33 C34 C35 N4 -172.05(15) . . . . ?
C33 C34 C35 C36 3.9(2) . . . . ?
C32 C31 C36 C35 -4.1(2) . . . . ?
C37 C31 C36 C35 -173.60(14) . . . . ?
C34 C35 C36 C31 0.1(2) . . . . ?
N4 C35 C36 C31 176.02(14) . . . . ?
C32 C31 C37 C51 -83.35(17) . . . . ?
C36 C31 C37 C51 86.02(17) . . . . ?
C32 C31 C37 C39 36.1(2) . . . . ?
C36 C31 C37 C39 -154.52(14) . . . . ?
C32 C31 C37 C45 156.50(14) . . . . ?
C36 C31 C37 C45 -34.1(2) . . . . ?
C31 C37 C39 C40 17.9(2) . . . . ?
C51 C37 C39 C40 138.20(16) . . . . ?
C45 C37 C39 C40 -111.70(17) . . . . ?
C31 C37 C39 C44 -169.96(13) . . . . ?
C51 C37 C39 C44 -49.66(17) . . . . ?
C45 C37 C39 C44 60.43(16) . . . . ?
C44 C39 C40 C41 5.1(2) . . . . ?
C37 C39 C40 C41 176.90(15) . . . . ?
C39 C40 C41 C42 -0.9(3) . . . . ?
C40 C41 C42 C43 -3.4(3) . . . . ?
C41 C42 C43 C44 3.2(3) . . . . ?
C42 C43 C44 C39 1.2(2) . . . . ?
C42 C43 C44 C38 -172.18(16) . . . . ?
C40 C39 C44 C43 -5.4(2) . . . . ?
C37 C39 C44 C43 -178.21(14) . . . . ?
C40 C39 C44 C38 168.68(14) . . . . ?
C37 C39 C44 C38 -4.16(19) . . . . ?
C56 C38 C44 C43 -127.98(17) . . . . ?
C50 C38 C44 C43 119.43(17) . . . . ?
C56 C38 C44 C39 58.20(18) . . . . ?
C50 C38 C44 C39 -54.39(17) . . . . ?
C31 C37 C45 C46 -14.3(2) . . . . ?
C51 C37 C45 C46 -135.52(16) . . . . ?
C39 C37 C45 C46 113.93(17) . . . . ?
C31 C37 C45 C50 173.37(13) . . . . ?
C51 C37 C45 C50 52.12(16) . . . . ?
C39 C37 C45 C50 -58.44(16) . . . . ?
C50 C45 C46 C47 -2.0(2) . . . . ?
C37 C45 C46 C47 -173.89(15) . . . . ?
C45 C46 C47 C48 1.1(2) . . . . ?
C46 C47 C48 C49 0.2(2) . . . . ?
C47 C48 C49 C50 -0.7(2) . . . . ?
C48 C49 C50 C45 -0.2(2) . . . . ?
C48 C49 C50 C38 172.26(15) . . . . ?
C46 C45 C50 C49 1.5(2) . . . . ?
C37 C45 C50 C49 174.69(14) . . . . ?
C46 C45 C50 C38 -171.66(14) . . . . ?
C37 C45 C50 C38 1.49(19) . . . . ?
C56 C38 C50 C49 131.11(16) . . . . ?
C44 C38 C50 C49 -116.72(17) . . . . ?
C56 C38 C50 C45 -56.02(17) . . . . ?
C44 C38 C50 C45 56.15(17) . . . . ?
C31 C37 C51 C52 -2.5(2) . . . . ?
C39 C37 C51 C52 -128.11(16) . . . . ?
C45 C37 C51 C52 125.45(16) . . . . ?
C31 C37 C51 C56 177.70(13) . . . . ?
C39 C37 C51 C56 52.07(17) . . . . ?
C45 C37 C51 C56 -54.38(17) . . . . ?
C56 C51 C52 C53 -0.9(2) . . . . ?
C37 C51 C52 C53 179.26(15) . . . . ?
C51 C52 C53 C54 -1.3(2) . . . . ?
C52 C53 C54 C55 2.2(3) . . . . ?
C53 C54 C55 C56 -0.7(3) . . . . ?
C54 C55 C56 C51 -1.5(2) . . . . ?
C54 C55 C56 C38 179.99(16) . . . . ?
C52 C51 C56 C55 2.4(2) . . . . ?
C37 C51 C56 C55 -177.79(15) . . . . ?
C52 C51 C56 C38 -178.96(14) . . . . ?
C37 C51 C56 C38 0.9(2) . . . . ?
C50 C38 C56 C55 -127.19(17) . . . . ?
C44 C38 C56 C55 122.51(18) . . . . ?
C50 C38 C56 C51 54.23(18) . . . . ?
C44 C38 C56 C51 -56.07(18) . . . . ?
C66 C61 C62 C63 4.1(2) . . . . ?
C67 C61 C62 C63 172.18(15) . . . . ?
C61 C62 C63 C64 -1.4(3) . . . . ?
C61 C62 C63 N5 -176.87(16) . . . . ?
N5 C63 C64 C65 172.61(17) . . . . ?
C62 C63 C64 C65 -2.9(3) . . . . ?
C63 C64 C65 C66 4.3(3) . . . . ?
C63 C64 C65 N6 -177.53(16) . . . . ?
C64 C65 C66 C61 -1.5(3) . . . . ?
N6 C65 C66 C61 -179.69(16) . . . . ?
C62 C61 C66 C65 -2.7(2) . . . . ?
C67 C61 C66 C65 -171.35(15) . . . . ?
C62 C61 C67 C81 -90.18(18) . . . . ?
C66 C61 C67 C81 77.95(18) . . . . ?
C62 C61 C67 C69 29.9(2) . . . . ?
C66 C61 C67 C69 -161.97(15) . . . . ?
C62 C61 C67 C75 151.61(15) . . . . ?
C66 C61 C67 C75 -40.3(2) . . . . ?
C61 C67 C69 C70 14.7(3) . . . . ?
C81 C67 C69 C70 135.34(18) . . . . ?
C75 C67 C69 C70 -114.37(19) . . . . ?
C61 C67 C69 C74 -171.90(15) . . . . ?
C81 C67 C69 C74 -51.27(18) . . . . ?
C75 C67 C69 C74 59.01(18) . . . . ?
C74 C69 C70 C71 3.4(3) . . . . ?
C67 C69 C70 C71 176.42(16) . . . . ?
C69 C70 C71 C72 -2.0(3) . . . . ?
C70 C71 C72 C73 -0.3(3) . . . . ?
C71 C72 C73 C74 1.0(3) . . . . ?
C72 C73 C74 C69 0.5(3) . . . . ?
C72 C73 C74 C68 -172.67(17) . . . . ?
C70 C69 C74 C73 -2.7(3) . . . . ?
C67 C69 C74 C73 -176.75(16) . . . . ?
C70 C69 C74 C68 171.24(16) . . . . ?
C67 C69 C74 C68 -2.8(2) . . . . ?
C86 C68 C74 C73 -128.98(19) . . . . ?
C80 C68 C74 C73 118.37(19) . . . . ?
C86 C68 C74 C69 57.4(2) . . . . ?
C80 C68 C74 C69 -55.26(19) . . . . ?
C61 C67 C75 C76 -14.7(2) . . . . ?
C81 C67 C75 C76 -133.41(17) . . . . ?
C69 C67 C75 C76 116.41(18) . . . . ?
C61 C67 C75 C80 169.64(14) . . . . ?
C81 C67 C75 C80 50.92(18) . . . . ?
C69 C67 C75 C80 -59.26(17) . . . . ?
C80 C75 C76 C77 -5.0(2) . . . . ?
C67 C75 C76 C77 179.57(15) . . . . ?
C75 C76 C77 C78 2.4(2) . . . . ?
C76 C77 C78 C79 1.1(3) . . . . ?
C77 C78 C79 C80 -1.8(3) . . . . ?
C78 C79 C80 C75 -0.8(3) . . . . ?
C78 C79 C80 C68 176.37(16) . . . . ?
C76 C75 C80 C79 4.2(2) . . . . ?
C67 C75 C80 C79 -179.68(15) . . . . ?
C76 C75 C80 C68 -173.27(15) . . . . ?
C67 C75 C80 C68 2.8(2) . . . . ?
C86 C68 C80 C79 125.38(18) . . . . ?
C74 C68 C80 C79 -122.15(18) . . . . ?
C86 C68 C80 C75 -57.25(18) . . . . ?
C74 C68 C80 C75 55.22(18) . . . . ?
C61 C67 C81 C82 3.2(2) . . . . ?
C69 C67 C81 C82 -125.30(18) . . . . ?
C75 C67 C81 C82 128.02(18) . . . . ?
C61 C67 C81 C86 -177.69(15) . . . . ?
C69 C67 C81 C86 53.79(19) . . . . ?
C75 C67 C81 C86 -52.88(19) . . . . ?
C86 C81 C82 C83 0.2(3) . . . . ?
C67 C81 C82 C83 179.28(17) . . . . ?
C81 C82 C83 C84 0.4(3) . . . . ?
C82 C83 C84 C85 -0.3(3) . . . . ?
C83 C84 C85 C86 -0.4(3) . . . . ?
C84 C85 C86 C81 1.1(3) . . . . ?
C84 C85 C86 C68 -178.80(19) . . . . ?
C82 C81 C86 C85 -1.0(3) . . . . ?
C67 C81 C86 C85 179.86(17) . . . . ?
C82 C81 C86 C68 178.90(16) . . . . ?
C67 C81 C86 C68 -0.3(2) . . . . ?
C80 C68 C86 C85 -124.5(2) . . . . ?
C74 C68 C86 C85 124.5(2) . . . . ?
C80 C68 C86 C81 55.57(19) . . . . ?
C74 C68 C86 C81 -55.4(2) . . . . ?

_refine_diff_density_max         0.439
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.046


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_chemical_compound_source        no
