# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_TolHAT-1
_database_code_depnum_ccdc_archive 'CCDC 2081132'
loop_
_audit_author_name
_audit_author_address
'Ichiro Hisaki'
;Osaka University
Japan
;
_audit_update_record             
;
2021-04-30 deposited with the CCDC.	2021-06-21 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C102 H60 N6 O12'
_chemical_formula_moiety         'C102 H60 N6 O12'
_chemical_formula_weight         1561.56
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      trigonal
_space_group_name_H-M_alt        'R -3 c:H'
_space_group_name_Hall           '-R 3 2"c'
_space_group_IT_number           167
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'x, x-y, z+1/2'
'-x+y, y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, -z-1/2'
'-x, -x+y, -z-1/2'
'x-y, -y, -z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'y+2/3, x+1/3, -z-1/6'
'-x+2/3, -x+y+1/3, -z-1/6'
'x-y+2/3, -y+1/3, -z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'y+1/3, x+2/3, -z+1/6'
'-x+1/3, -x+y+2/3, -z+1/6'
'x-y+1/3, -y+2/3, -z+1/6'
#------------------------------------------------------------------------------
_cell_length_a                   59.5294(11)
_cell_length_b                   59.5294(11)
_cell_length_c                   6.96369(19)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_volume                     21371.4(8)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    5371
_cell_measurement_theta_min      1.56
_cell_measurement_theta_max      25.07
_cell_measurement_temperature    90
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            yellowishgreen
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    0.728
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4824.00
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.194
_exptl_absorpt_correction_T_max  1.000

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      90
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.81106
_diffrn_measurement_device_type  'SPring-8 BL40XU, Pilatus100K, DECTRIS'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            66289
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_av_R_equivalents  0.1398
_diffrn_reflns_theta_max         33.379
_diffrn_reflns_theta_min         1.561
_diffrn_reflns_theta_full        29.120
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -79
_diffrn_reflns_limit_h_max       80
_diffrn_reflns_limit_k_min       -76
_diffrn_reflns_limit_k_max       78
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             5840
_reflns_number_gt                2556
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1994
_refine_ls_R_factor_gt           0.1267
_refine_ls_wR_factor_ref         0.4200
_refine_ls_wR_factor_gt          0.3874
_refine_ls_number_restraints     31
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         5840
_refine_ls_number_parameters     181
_refine_ls_goodness_of_fit_ref   1.265
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.35665(8) 0.14646(12) 0.4823(8) 0.154(2) Uani 1 1 d D . . . .
H1O H 0.341664 0.141907 0.442245 0.185 Uiso 1 1 calc R U . . .
O2 O 0.35767(7) 0.18305(13) 0.4808(6) 0.149(2) Uani 1 1 d D . . . .
H3O H 0.342410 0.173609 0.441542 0.179 Uiso 1 1 calc R U . . .
N1 N 0.61328(4) 0.30656(4) 1.0438(4) 0.0240(6) Uani 1 1 d . . . . .
C1 C 0.63879(5) 0.31887(5) 1.0764(4) 0.0214(7) Uani 1 1 d . . . . .
C2 C 0.60077(6) 0.28061(6) 1.0480(5) 0.0293(7) Uani 1 1 d . . . . .
C3 C 0.57441(6) 0.26701(6) 0.9745(5) 0.0336(8) Uani 1 1 d D . . . .
C4 C 0.56391(6) 0.24280(6) 0.8835(5) 0.0383(9) Uani 1 1 d D . . . .
H4 H 0.574320 0.235075 0.862172 0.046 Uiso 1 1 calc R U . . .
C5 C 0.53771(6) 0.22999(7) 0.8239(6) 0.0487(10) Uani 1 1 d D . . . .
H5 H 0.530486 0.213431 0.764747 0.058 Uiso 1 1 calc R U . . .
C6 C 0.52256(7) 0.24106(7) 0.8500(5) 0.0484(10) Uani 1 1 d D . . . .
C7 C 0.53357(6) 0.26629(7) 0.9272(5) 0.0438(9) Uani 1 1 d D . . . .
H7 H 0.523561 0.274645 0.935726 0.053 Uiso 1 1 calc R U . . .
C8 C 0.55898(5) 0.27880(6) 0.9902(4) 0.0292(8) Uani 1 1 d D . . . .
H8 H 0.566185 0.295614 1.045044 0.035 Uiso 1 1 calc R U . . .
C9 C 0.49528(8) 0.22815(8) 0.7905(6) 0.0567(11) Uani 1 1 d . . . . .
C10 C 0.47381(9) 0.21871(9) 0.7400(6) 0.0687(14) Uani 1 1 d . . . . .
C11 C 0.44739(9) 0.20689(11) 0.6808(7) 0.0795(16) Uani 1 1 d D . . . .
C12 C 0.43309(9) 0.18062(13) 0.6512(10) 0.108(2) Uani 1 1 d D . . . .
H12 H 0.441300 0.170534 0.665613 0.130 Uiso 1 1 calc R U . . .
C13 C 0.40658(9) 0.16804(13) 0.6001(8) 0.098(2) Uani 1 1 d D . . . .
H13 H 0.396751 0.149731 0.585800 0.118 Uiso 1 1 calc R U . . .
C14 C 0.39557(10) 0.18320(15) 0.5720(8) 0.107(2) Uani 1 1 d D . . . .
C15 C 0.40915(10) 0.20913(13) 0.6014(8) 0.0912(18) Uani 1 1 d D . . . .
H15 H 0.401066 0.219300 0.585225 0.109 Uiso 1 1 calc R U . . .
C16 C 0.43523(9) 0.22080(12) 0.6558(7) 0.0780(16) Uani 1 1 d D . . . .
H16 H 0.444708 0.239023 0.675726 0.094 Uiso 1 1 calc R U . . .
C17 C 0.36814(12) 0.16920(15) 0.5091(10) 0.100(2) Uani 1 1 d D . . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/1 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 C17 1.187(7) . ?
O1 H1O 0.8400 . ?
O2 C17 1.273(7) . ?
O2 H3O 0.8400 . ?
N1 C1 1.335(3) . ?
N1 C2 1.339(4) . ?
C1 C1 1.388(5) 34_547 ?
C1 C1 1.494(5) 36_557 ?
C2 C2 1.445(6) 34_547 ?
C2 C3 1.452(4) . ?
C3 C4 1.403(4) . ?
C3 C8 1.412(4) . ?
C4 C5 1.413(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.369(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.410(5) . ?
C6 C9 1.467(5) . ?
C7 C8 1.381(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.164(6) . ?
C10 C11 1.425(6) . ?
C11 C16 1.356(7) . ?
C11 C12 1.372(7) . ?
C12 C13 1.413(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.368(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.353(8) . ?
C14 C17 1.481(8) . ?
C15 C16 1.399(6) . ?
C15 H15 0.9500 . ?
C16 H16 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
C17 O1 H1O 109.5 . . ?
C17 O2 H3O 109.5 . . ?
C1 N1 C2 117.0(2) . . ?
N1 C1 C1 121.34(15) . 34_547 ?
N1 C1 C1 119.07(15) . 36_557 ?
C1 C1 C1 119.54(6) 34_547 36_557 ?
N1 C2 C2 119.63(17) . 34_547 ?
N1 C2 C3 117.3(3) . . ?
C2 C2 C3 123.09(18) 34_547 . ?
C4 C3 C8 118.6(3) . . ?
C4 C3 C2 122.3(3) . . ?
C8 C3 C2 119.1(3) . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 121.1(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 119.7(3) . . ?
C5 C6 C9 122.2(3) . . ?
C7 C6 C9 118.0(4) . . ?
C8 C7 C6 119.7(3) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C7 C8 C3 121.1(3) . . ?
C7 C8 H8 119.4 . . ?
C3 C8 H8 119.4 . . ?
C10 C9 C6 177.6(5) . . ?
C9 C10 C11 179.1(6) . . ?
C16 C11 C12 117.4(5) . . ?
C16 C11 C10 122.0(5) . . ?
C12 C11 C10 120.6(5) . . ?
C11 C12 C13 122.3(6) . . ?
C11 C12 H12 118.9 . . ?
C13 C12 H12 118.9 . . ?
C14 C13 C12 117.6(6) . . ?
C14 C13 H13 121.2 . . ?
C12 C13 H13 121.2 . . ?
C15 C14 C13 121.4(5) . . ?
C15 C14 C17 123.3(7) . . ?
C13 C14 C17 115.4(6) . . ?
C14 C15 C16 119.3(6) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C11 C16 C15 122.0(5) . . ?
C11 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
O1 C17 O2 121.7(6) . . ?
O1 C17 C14 122.2(7) . . ?
O2 C17 C14 116.2(7) . . ?

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 N1 C1 C1 7.8(5) . . . 34_547 ?
C2 N1 C1 C1 -174.7(3) . . . 36_557 ?
C1 N1 C2 C2 10.6(5) . . . 34_547 ?
C1 N1 C2 C3 -167.6(3) . . . . ?
N1 C2 C3 C4 147.8(3) . . . . ?
C2 C2 C3 C4 -30.3(6) 34_547 . . . ?
N1 C2 C3 C8 -30.4(4) . . . . ?
C2 C2 C3 C8 151.4(4) 34_547 . . . ?
C8 C3 C4 C5 -4.9(5) . . . . ?
C2 C3 C4 C5 176.8(3) . . . . ?
C3 C4 C5 C6 1.3(5) . . . . ?
C4 C5 C6 C7 3.8(6) . . . . ?
C4 C5 C6 C9 -179.7(3) . . . . ?
C5 C6 C7 C8 -5.2(6) . . . . ?
C9 C6 C7 C8 178.1(3) . . . . ?
C6 C7 C8 C3 1.6(5) . . . . ?
C4 C3 C8 C7 3.5(5) . . . . ?
C2 C3 C8 C7 -178.2(3) . . . . ?
C16 C11 C12 C13 -1.2(9) . . . . ?
C10 C11 C12 C13 177.4(5) . . . . ?
C11 C12 C13 C14 2.9(9) . . . . ?
C12 C13 C14 C15 -3.3(9) . . . . ?
C12 C13 C14 C17 177.0(5) . . . . ?
C13 C14 C15 C16 2.0(9) . . . . ?
C17 C14 C15 C16 -178.3(5) . . . . ?
C12 C11 C16 C15 -0.2(8) . . . . ?
C10 C11 C16 C15 -178.7(5) . . . . ?
C14 C15 C16 C11 -0.2(8) . . . . ?
C15 C14 C17 O1 179.2(7) . . . . ?
C13 C14 C17 O1 -1.1(10) . . . . ?
C15 C14 C17 O2 0.8(9) . . . . ?
C13 C14 C17 O2 -179.5(6) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.





#==============================================================================

# start Validation Reply Form
_vrf_PLAT312_TolHAT-1            
;
PROBLEM: Strange C-O-H Geometry (C-O < 1.25 Ang) ..... O1 Check 
RESPONSE: Due to disorder of the hydrogen atom of the carboxy group
;
_vrf_PLAT417_TolHAT-1            
;
PROBLEM: Short Inter D-H..H-D H1O ..H1O . 0.93 Ang. 
RESPONSE: Due to disorder of the hydrogen atom of the carboxy group
;
# end Validation Reply Form
#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        
"4,4',4'',4''',4'''',4'''''-((dipyrazino[2,3-f:2',3'-h]quinoxaline-2,3,6,7,10,11-hexaylhexakis(benzene-4,1-diyl))hexakis(ethyne-2,1-diyl))hexabenzoic acid"
_chemical_name_common            TolHAT
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: N,N-dimethylacetamide, 1,2,4-trichlorobenzene'
####################################################################### 
# 
# 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_BPTp-1-TCB
_database_code_depnum_ccdc_archive 'CCDC 2081133'
loop_
_audit_author_name
_audit_author_address
'Ichiro Hisaki'
;Osaka University
Japan
;
_audit_update_record             
;
2021-04-30 deposited with the CCDC.	2021-06-21 downloaded from the CCDC.
;
_audit_creation_date             2019-09-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            BPTp
_chemical_name_systematic        
"4',4''',4''''',4''''''',4'''''''''-(11-(4'-methyl-[1,1'-biphenyl]-4-yl)triphenylene-2,3,6,7,10-pentayl)pentakis(([1,1'-biphenyl]-4-carboxylic acid))"
_chemical_formula_moiety         'C96 H66 O12, 2(C6 H3 Cl3)'
_chemical_formula_sum            'C108 H72 Cl6 O12'
_chemical_formula_weight         1774.35
_chemical_melting_point          ?
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   9.3082(3)
_cell_length_b                   53.6910(12)
_cell_length_c                   30.7096(6)
_cell_angle_alpha                90
_cell_angle_beta                 97.504(2)
_cell_angle_gamma                90
_cell_volume                     15216.2(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8497
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      74.0530
_cell_measurement_theta_min      4.8260
_shelx_estimated_absorpt_T_max   0.935
_shelx_estimated_absorpt_T_min   0.935
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    ?
_exptl_crystal_density_diffrn    0.775
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6023
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       65
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            37007
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.469
_diffrn_reflns_theta_min         3.337
_diffrn_ambient_temperature      93(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -17.00  89.00   0.50    2.00    --    0.00  37.00   0.00  212
  2  ω     -8.00  21.00   0.50    2.00    --    0.00  57.00-120.00   58
  3  ω     37.00  62.00   0.50    2.00    --    0.00  57.00-120.00   50
  4  ω      5.00 108.00   0.50   18.00    --   94.90 -61.00  90.00  206
  5  ω     90.00 180.00   0.50   18.00    --   94.90  82.00 120.00  180
  6  ω      6.00 113.00   0.50   18.00    --   94.90 -82.00  90.00  214
  7  ω    151.00 184.00   0.50   18.00    --   94.90  30.00 -30.00   66
  8  ω     71.00 125.00   0.50   18.00    --   94.90 -82.00 -90.00  108
  9  ω     75.00 153.00   0.50   18.00    --   94.90  77.00  30.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0092102000
_diffrn_orient_matrix_UB_12      -0.0022466000
_diffrn_orient_matrix_UB_13      -0.0503249000
_diffrn_orient_matrix_UB_21      -0.0037957000
_diffrn_orient_matrix_UB_22      0.0286064000
_diffrn_orient_matrix_UB_23      -0.0040381000
_diffrn_orient_matrix_UB_31      0.1665330000
_diffrn_orient_matrix_UB_32      0.0005271000
_diffrn_orient_matrix_UB_33      0.0037350000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7913
_reflns_number_total             14857
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.377
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         14857
_refine_ls_number_restraints     826
_refine_ls_R_factor_all          0.1786
_refine_ls_R_factor_gt           0.1349
_refine_ls_restrained_S_all      1.351
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3858
_refine_ls_wR_factor_ref         0.4215
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C44B-C47B
 1.488 with sigma of 0.02
 O6B-C47B
 1.253 with sigma of 0.02
 O5B-C47B
 1.253 with sigma of 0.02
 O5B-O6B
 2.221 with sigma of 0.04
 C44B-O5B
 2.35 with sigma of 0.08
 O6B-C44B
 2.35 with sigma of 0.08
 O1A-C23A \\sim O1B-C23B
 with sigma of 0.02
 C16-C17A \\sim C16-C17B
 with sigma of 0.02
 C17A-C18A \\sim C17B-C18B
 with sigma of 0.02
 C17A-C22A \\sim C17B-C22B
 with sigma of 0.02
 C18A-C19A \\sim C18B-C19B
 with sigma of 0.02
 C19A-C20A \\sim C19B-C20B
 with sigma of 0.02
 C20A-C21A \\sim C20B-C21B
 with sigma of 0.02
 C20A-C23A \\sim C20B-C23B
 with sigma of 0.02
 C21A-C22A \\sim C21B-C22B
 with sigma of 0.02
 O2A-C23A \\sim O2B-C23B
 with sigma of 0.02
 O1A-C20A \\sim O1B-C20B
 with sigma of 0.04
 O1A-O2A \\sim O1B-O2B
 with sigma of 0.04
 C16-C18A \\sim C16-C18B
 with sigma of 0.04
 C16-C22A \\sim C16-C22B
 with sigma of 0.04
 C17A-C19A \\sim C17B-C19B
 with sigma of 0.04
 C17A-C21A \\sim C17B-C21B
 with sigma of 0.04
 C18A-C20A \\sim C18B-C20B
 with sigma of 0.04
 C18A-C22A \\sim C18B-C22B
 with sigma of 0.04
 C19A-C21A \\sim C19B-C21B
 with sigma of 0.04
 C19A-C23A \\sim C19B-C23B
 with sigma of 0.04
 C20A-C22A \\sim C20B-C22B
 with sigma of 0.04
 C20A-O2A \\sim C20B-O2B
 with sigma of 0.04
 C21A-C23A \\sim C21B-C23B
 with sigma of 0.04
 O5B-C47B \\sim O6A-C47A
 with sigma of 0.02
 C40-C41B \\sim C40-C41A
 with sigma of 0.02
 C41B-C46B \\sim C41A-C42A
 with sigma of 0.02
 C41B-C42B \\sim C41A-C46A
 with sigma of 0.02
 C46B-C45B \\sim C42A-C43A
 with sigma of 0.02
 C45B-C44B \\sim C43A-C44A
 with sigma of 0.02
 C44B-C43B \\sim C44A-C45A
 with sigma of 0.02
 C44B-C47B \\sim C44A-C47A
 with sigma of 0.02
 C43B-C42B \\sim C45A-C46A
 with sigma of 0.02
 O6B-C47B \\sim O5A-C47A
 with sigma of 0.02
 O5B-C44B \\sim O6A-C44A
 with sigma of 0.04
 O5B-O6B \\sim O6A-O5A
 with sigma of 0.04
 C40-C46B \\sim C40-C42A
 with sigma of 0.04
 C40-C42B \\sim C40-C46A
 with sigma of 0.04
 C41B-C45B \\sim C41A-C43A
 with sigma of 0.04
 C41B-C43B \\sim C41A-C45A
 with sigma of 0.04
 C46B-C44B \\sim C42A-C44A
 with sigma of 0.04
 C46B-C42B \\sim C42A-C46A
 with sigma of 0.04
 C45B-C43B \\sim C43A-C45A
 with sigma of 0.04
 C45B-C47B \\sim C43A-C47A
 with sigma of 0.04
 C44B-C42B \\sim C44A-C46A
 with sigma of 0.04
 C44B-O6B \\sim C44A-O5A
 with sigma of 0.04
 C43B-C47B \\sim C45A-C47A
 with sigma of 0.04
3. Restrained planarity
 C41B, C42B, C43B, C44B, C45B, C46B, C47B, O5B, O6B
 with sigma of 0.1
4. Rigid bond restraints
 C41B, C46B, C45B, C44B, C43B, C42B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C41A, C46A, C42A, C43A, C45A, C44A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C37, C38, C39, C40, C41, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17A, C22A, C21A, C20A, C19A, C18A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
6. Others
 Sof(C17B)=Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(C21B)=
 Sof(H21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(O1B)=Sof(H1B)=Sof(O2B)=Sof(H2B)=1-
 FVAR(1)
 Sof(O1A)=Sof(H1A)=Sof(C17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=
 Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(O2A)=Sof(H2A)=Sof(C23A)=FVAR(1)
 Sof(C41A)=Sof(C46A)=Sof(H46A)=Sof(C45A)=Sof(H45A)=Sof(C44A)=Sof(C43A)=
 Sof(H43A)=Sof(C42A)=Sof(H42A)=Sof(C47A)=Sof(O6A)=Sof(H6A)=Sof(O5A)=Sof(H5A)=1-
 FVAR(2)
 Sof(O5B)=Sof(H5B)=Sof(C41B)=Sof(C46B)=Sof(H46B)=Sof(C45B)=Sof(H45B)=Sof(C44B)=
 Sof(C43B)=Sof(H43B)=Sof(C42B)=Sof(H42B)=Sof(O6B)=Sof(H6B)=Sof(C47B)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C38(H38), C39(H39), C2(H2), C42(H42), C25(H25), C28(H28),
 C41(H41), C26(H26), C15(H15), C29(H29), C46B(H46B), C45B(H45B), C43B(H43B),
 C42B(H42B), C14(H14), C31(H31), C35(H35), C11(H11), C50(H50), C53(H53),
 C52(H52), C18A(H18A), C19A(H19A), C21A(H21A), C22A(H22A), C12(H12), C34(H34),
 C32(H32), C18B(H18B), C19B(H19B), C21B(H21B), C22B(H22B), C46A(H46A),
 C45A(H45A), C43A(H43A), C42A(H42A)
7.b Fitted hexagon refined as free rotating group:
 C41B(C46B,C45B,C44B,C43B,C42B), C51(C50,C49,C48,C53,C52), C17A(C18A,C19A,C20A,
 C21A,C22A)
7.c Tetrahedral OH refined with riding coordinates:
 O5B(H5B), O1A(H1A), O3(H3), O4(H4), O6B(H6B), O2A(H2A), O1B(H1B), O2B(H2B),
 O6A(H6A), O5A(H5A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Cl3 Cl 0.2084(3) 0.49490(5) 0.65369(7) 0.1444(9) Uani 1 1 d . U . . .
C7 C 0.2804(4) 0.46558(5) 0.52211(8) 0.0290(7) Uani 1 1 d . U . . .
C9 C 0.2840(4) 0.51112(5) 0.52209(9) 0.0301(7) Uani 1 1 d . U . . .
C37 C 0.3149(4) 0.53447(5) 0.54790(10) 0.0322(7) Uani 1 1 d . U . . .
C8 C 0.3169(4) 0.48849(5) 0.54258(9) 0.0309(7) Uani 1 1 d . U . . .
H8 H 0.365248 0.488476 0.571066 0.037 Uiso 1 1 calc R . . . .
Cl1 Cl 0.5926(4) 0.52707(9) 0.82526(11) 0.2117(17) Uani 1 1 d . U . . .
C4 C 0.3790(4) 0.41936(6) 0.61450(9) 0.0412(9) Uani 1 1 d . U . . .
C5 C 0.3606(4) 0.44100(5) 0.59071(9) 0.0343(8) Uani 1 1 d . U . . .
H5 H 0.382832 0.455936 0.605383 0.041 Uiso 1 1 calc R . . . .
C6 C 0.3102(4) 0.44204(5) 0.54559(9) 0.0358(8) Uani 1 1 d . U . . .
C38 C 0.4497(4) 0.53888(6) 0.57136(11) 0.0413(9) Uani 1 1 d . U . . .
H38 H 0.524416 0.527540 0.569930 0.050 Uiso 1 1 calc R . . . .
C1 C 0.2786(5) 0.41920(5) 0.52332(9) 0.0430(10) Uani 1 1 d . U . . .
C3 C 0.3483(5) 0.39644(6) 0.59209(10) 0.0525(12) Uani 1 1 d . U . . .
C39 C 0.4742(4) 0.56018(6) 0.59708(13) 0.0457(9) Uani 1 1 d . U . . .
H39 H 0.565317 0.562742 0.612856 0.055 Uiso 1 1 calc R . . . .
O5B O 0.5609(17) 0.6688(3) 0.7289(5) 0.094(5) Uani 0.594(5) 1 d D U P A 2
H5B H 0.569686 0.682752 0.739673 0.142 Uiso 0.594(5) 1 calc R . P A 2
C24 C 0.4280(5) 0.42188(7) 0.66276(10) 0.0476(10) Uani 1 1 d . U . . .
O1A O 0.3931(16) 0.2120(3) 0.7283(5) 0.065(4) Uani 0.481(6) 1 d D U P B 1
H1A H 0.415222 0.198967 0.741423 0.098 Uiso 0.481(6) 1 calc R . P B 1
C2 C 0.2985(5) 0.39708(6) 0.54758(10) 0.0578(13) Uani 1 1 d . U . . .
H2 H 0.277211 0.382060 0.533059 0.069 Uiso 1 1 calc R . . . .
C42 C 0.2046(4) 0.55170(6) 0.55166(15) 0.0508(10) Uani 1 1 d . U . . .
H42 H 0.111726 0.548727 0.537437 0.061 Uiso 1 1 calc R . . . .
C40 C 0.3678(4) 0.57738(7) 0.59971(15) 0.0546(11) Uani 1 1 d D U . . .
C25 C 0.3606(5) 0.40842(7) 0.69368(11) 0.0527(10) Uani 1 1 d . U . . .
H25 H 0.287351 0.397156 0.684067 0.063 Uiso 1 1 calc R . . . .
C10 C 0.3691(6) 0.37159(6) 0.61368(11) 0.0658(14) Uani 1 1 d . U . . .
C28 C 0.5734(6) 0.44198(9) 0.72303(12) 0.0731(15) Uani 1 1 d . U . . .
H28 H 0.643925 0.453769 0.732383 0.088 Uiso 1 1 calc R . . . .
Cl2 Cl 0.5630(6) 0.56036(9) 0.7437(2) 0.309(4) Uani 1 1 d . U . . .
C41 C 0.2317(5) 0.57273(8) 0.57586(19) 0.0710(15) Uani 1 1 d . U . . .
H41 H 0.157996 0.584348 0.576632 0.085 Uiso 1 1 calc R . . . .
C27 C 0.5115(6) 0.42853(9) 0.75337(11) 0.0614(12) Uani 1 1 d . U . . .
C26 C 0.4019(5) 0.41175(9) 0.73848(11) 0.0590(12) Uani 1 1 d . U . . .
H26 H 0.356192 0.402724 0.758578 0.071 Uiso 1 1 calc R . . . .
C15 C 0.4907(6) 0.36508(7) 0.64059(14) 0.0682(14) Uani 1 1 d . U . . .
H15 H 0.564607 0.376733 0.646512 0.082 Uiso 1 1 calc R . . . .
C29 C 0.5321(6) 0.43829(8) 0.67813(11) 0.0686(15) Uani 1 1 d . U . . .
H29 H 0.577894 0.447423 0.658196 0.082 Uiso 1 1 calc R . . . .
C41B C 0.3909(7) 0.60241(7) 0.62027(17) 0.051(3) Uani 0.594(5) 1 d D U P A 2
C46B C 0.3364(7) 0.62485(8) 0.60259(15) 0.065(2) Uani 0.594(5) 1 d DG U P A 2
H46B H 0.282044 0.625171 0.574944 0.078 Uiso 0.594(5) 1 calc R . P A 2
C45B C 0.3631(7) 0.64681(7) 0.62623(18) 0.073(3) Uani 0.594(5) 1 d DG U P A 2
H45B H 0.326663 0.661824 0.614405 0.088 Uiso 0.594(5) 1 calc R . P A 2
C44B C 0.4444(7) 0.64633(8) 0.66755(17) 0.072(3) Uani 0.594(5) 1 d DG U P A 2
C43B C 0.4989(7) 0.62388(9) 0.68523(15) 0.069(2) Uani 0.594(5) 1 d DG U P A 2
H43B H 0.553217 0.623562 0.712881 0.082 Uiso 0.594(5) 1 calc R . P A 2
C42B C 0.4721(7) 0.60192(7) 0.66159(18) 0.071(3) Uani 0.594(5) 1 d DG U P A 2
H42B H 0.508599 0.586909 0.673420 0.086 Uiso 0.594(5) 1 calc R . P A 2
C30 C 0.5573(7) 0.43252(10) 0.80162(13) 0.0809(17) Uani 1 1 d . U . . .
C14 C 0.5087(7) 0.34167(8) 0.65955(16) 0.0771(16) Uani 1 1 d . U . . .
H14 H 0.594115 0.338029 0.677703 0.093 Uiso 1 1 calc R . . . .
C16 C 0.4041(7) 0.32390(8) 0.65219(16) 0.090(2) Uani 1 1 d D U . . .
O3 O 0.8191(7) 0.44520(14) 0.95219(12) 0.167(3) Uani 1 1 d . U . . .
H3 H 0.829487 0.446479 0.979020 0.251 Uiso 1 1 calc R . . . .
C31 C 0.6992(8) 0.43714(14) 0.81688(15) 0.105(2) Uani 1 1 d . U . . .
H31 H 0.767865 0.437905 0.797468 0.126 Uiso 1 1 calc R . . . .
C35 C 0.4543(7) 0.43186(11) 0.83055(12) 0.0849(17) Uani 1 1 d . U . . .
H35 H 0.357292 0.429057 0.820128 0.102 Uiso 1 1 calc R . . . .
C11 C 0.2589(8) 0.35340(8) 0.60562(17) 0.109(3) Uani 1 1 d . U . . .
H11 H 0.174103 0.357120 0.587252 0.131 Uiso 1 1 calc R . . . .
O4 O 0.5905(8) 0.44359(13) 0.96337(13) 0.155(3) Uani 1 1 d . U . . .
H4 H 0.627000 0.444816 0.989074 0.233 Uiso 1 1 calc R . . . .
C51 C 0.3164(6) 0.50344(12) 0.70043(18) 0.108(2) Uani 1 1 d . U . . .
C50 C 0.3906(7) 0.52596(11) 0.70204(19) 0.129(3) Uani 1 1 d G U . . .
H50 H 0.383341 0.536153 0.677364 0.155 Uiso 1 1 calc R . . . .
C49 C 0.4757(6) 0.53323(11) 0.7405(2) 0.150(4) Uani 1 1 d G U . . .
C48 C 0.4866(7) 0.51799(15) 0.77739(18) 0.126(3) Uani 1 1 d G U . . .
C53 C 0.4124(8) 0.49548(14) 0.77579(19) 0.149(4) Uani 1 1 d G U . . .
H53 H 0.419633 0.485285 0.800458 0.179 Uiso 1 1 calc R . . . .
C52 C 0.3273(7) 0.48820(9) 0.7373(3) 0.141(3) Uani 1 1 d G U . . .
H52 H 0.277604 0.473140 0.736229 0.169 Uiso 1 1 calc R . . . .
C17A C 0.4476(9) 0.29724(11) 0.6682(3) 0.062(3) Uani 0.481(6) 1 d D U P B 1
C18A C 0.3284(8) 0.28462(17) 0.6801(4) 0.081(5) Uani 0.481(6) 1 d DG U P B 1
H18A H 0.236956 0.291881 0.675375 0.097 Uiso 0.481(6) 1 calc R . P B 1
C19A C 0.3457(8) 0.26115(17) 0.6992(4) 0.076(5) Uani 0.481(6) 1 d DG U P B 1
H19A H 0.265934 0.252707 0.707193 0.092 Uiso 0.481(6) 1 calc R . P B 1
C20A C 0.4824(9) 0.25030(11) 0.7063(3) 0.071(3) Uani 0.481(6) 1 d DG U P B 1
C21A C 0.6016(7) 0.26292(12) 0.6944(3) 0.077(3) Uani 0.481(6) 1 d DG U P B 1
H21A H 0.693043 0.255655 0.699170 0.093 Uiso 0.481(6) 1 calc R . P B 1
C22A C 0.5843(8) 0.28639(11) 0.6753(3) 0.072(3) Uani 0.481(6) 1 d DG U P B 1
H22A H 0.664068 0.294829 0.667352 0.086 Uiso 0.481(6) 1 calc R . P B 1
C33 C 0.6433(9) 0.43987(13) 0.89063(16) 0.102(2) Uani 1 1 d . U . . .
C12 C 0.2764(9) 0.33014(9) 0.6249(2) 0.127(3) Uani 1 1 d . U . . .
H12 H 0.202488 0.318447 0.619639 0.152 Uiso 1 1 calc R . . . .
C34 C 0.4980(9) 0.43546(14) 0.87581(15) 0.104(2) Uani 1 1 d . U . . .
H34 H 0.430318 0.434890 0.895545 0.125 Uiso 1 1 calc R . . . .
C36 C 0.6907(11) 0.44273(16) 0.93861(18) 0.119(3) Uani 1 1 d . U . . .
C32 C 0.7408(9) 0.44072(16) 0.86201(16) 0.116(3) Uani 1 1 d . U . . .
H32 H 0.837679 0.443742 0.872319 0.139 Uiso 1 1 calc R . . . .
O6B O 0.4246(9) 0.68923(11) 0.6747(3) 0.131(4) Uani 0.594(5) 1 d D U P A 2
H6B H 0.446518 0.701101 0.691039 0.197 Uiso 0.594(5) 1 calc R . P A 2
C47B C 0.4762(13) 0.66972(15) 0.6926(4) 0.087(4) Uani 0.594(5) 1 d D U P A 2
O2A O 0.6205(9) 0.21455(15) 0.7270(4) 0.111(4) Uani 0.481(6) 1 d D U P B 1
H2A H 0.619693 0.200717 0.738244 0.166 Uiso 0.481(6) 1 calc R . P B 1
C23A C 0.5008(12) 0.2249(2) 0.7283(6) 0.083(4) Uani 0.481(6) 1 d D U P B 1
C17B C 0.3947(14) 0.30127(17) 0.6799(4) 0.070(4) Uani 0.519(6) 1 d D U P B 2
C18B C 0.3125(14) 0.28043(19) 0.6655(4) 0.062(3) Uani 0.519(6) 1 d D U P B 2
H18B H 0.242091 0.282015 0.641282 0.074 Uiso 0.519(6) 1 calc R . P B 2
C19B C 0.3319(16) 0.2573(2) 0.6861(4) 0.070(3) Uani 0.519(6) 1 d D U P B 2
H19B H 0.282416 0.243360 0.674113 0.084 Uiso 0.519(6) 1 calc R . P B 2
C20B C 0.4246(13) 0.25555(17) 0.7242(3) 0.071(3) Uani 0.519(6) 1 d D U P B 2
C21B C 0.5087(15) 0.27564(17) 0.7383(4) 0.110(5) Uani 0.519(6) 1 d D U P B 2
H21B H 0.577665 0.273831 0.762858 0.131 Uiso 0.519(6) 1 calc R . P B 2
C22B C 0.4954(13) 0.29818(17) 0.7177(4) 0.097(4) Uani 0.519(6) 1 d D U P B 2
H22B H 0.553023 0.311489 0.728734 0.116 Uiso 0.519(6) 1 calc R . P B 2
C23B C 0.4408(15) 0.2314(2) 0.7508(4) 0.076(3) Uani 0.519(6) 1 d D U P B 2
O1B O 0.366(2) 0.2137(3) 0.7398(6) 0.104(7) Uani 0.519(6) 1 d D U P B 2
H1B H 0.386811 0.202226 0.756994 0.156 Uiso 0.519(6) 1 calc R . P B 2
O2B O 0.5325(9) 0.23092(13) 0.7829(3) 0.115(4) Uani 0.519(6) 1 d D U P B 2
H2B H 0.545556 0.216500 0.791332 0.173 Uiso 0.519(6) 1 calc R . P B 2
C41A C 0.4009(12) 0.59748(15) 0.6354(3) 0.034(2) Uani 0.406(5) 1 d D U P A 1
C46A C 0.5167(10) 0.61304(16) 0.6343(3) 0.048(2) Uani 0.406(5) 1 d D U P A 1
H46A H 0.582517 0.609776 0.614681 0.057 Uiso 0.406(5) 1 calc R . P A 1
C45A C 0.5382(11) 0.63363(18) 0.6618(4) 0.053(3) Uani 0.406(5) 1 d D U P A 1
H45A H 0.618546 0.643764 0.660556 0.063 Uiso 0.406(5) 1 calc R . P A 1
C44A C 0.4422(11) 0.63929(18) 0.6911(4) 0.052(3) Uani 0.406(5) 1 d D U P A 1
C43A C 0.3253(10) 0.62317(14) 0.6940(3) 0.044(2) Uani 0.406(5) 1 d D U P A 1
H43A H 0.260850 0.626449 0.714041 0.053 Uiso 0.406(5) 1 calc R . P A 1
C42A C 0.3056(10) 0.60248(14) 0.6674(3) 0.046(2) Uani 0.406(5) 1 d D U P A 1
H42A H 0.229426 0.591632 0.670145 0.055 Uiso 0.406(5) 1 calc R . P A 1
C47A C 0.4605(16) 0.6617(2) 0.7196(6) 0.068(4) Uani 0.406(5) 1 d D U P A 1
O6A O 0.582(2) 0.6737(4) 0.7203(9) 0.094(8) Uani 0.406(5) 1 d D U P A 1
H6A H 0.586076 0.684762 0.738779 0.141 Uiso 0.406(5) 1 calc R . P A 1
O5A O 0.3604(9) 0.66920(14) 0.7385(3) 0.079(3) Uani 0.406(5) 1 d D U P A 1
H5A H 0.385357 0.681929 0.752210 0.119 Uiso 0.406(5) 1 calc R . P A 1


_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
Cl3 C51 1.704(5) . ?
C7 C7 1.401(5) 2_556 ?
C7 C8 1.403(4) . ?
C7 C6 1.464(4) . ?
C9 C9 1.420(6) 2_556 ?
C9 C37 1.491(4) . ?
C9 C8 1.384(4) . ?
C37 C38 1.383(5) . ?
C37 C42 1.398(5) . ?
Cl1 C48 1.730(6) . ?
C4 C5 1.371(4) . ?
C4 C3 1.420(4) . ?
C4 C24 1.499(4) . ?
C5 C6 1.405(4) . ?
C6 C1 1.416(4) . ?
C38 C39 1.391(4) . ?
C1 C1 1.461(5) 2_556 ?
C1 C2 1.401(4) . ?
C3 C2 1.385(4) . ?
C3 C10 1.492(4) . ?
C39 C40 1.365(5) . ?
O5B C47B 1.280(12) . ?
C24 C25 1.405(5) . ?
C24 C29 1.348(6) . ?
O1A C23A 1.220(12) . ?
C42 C41 1.357(5) . ?
C40 C41 1.400(6) . ?
C40 C41B 1.488(4) . ?
C40 C41A 1.540(9) . ?
C25 C26 1.391(5) . ?
C10 C15 1.357(6) . ?
C10 C11 1.414(7) . ?
C28 C27 1.364(7) . ?
C28 C29 1.397(5) . ?
Cl2 C49 1.664(6) . ?
C27 C26 1.393(6) . ?
C27 C30 1.503(5) . ?
C15 C14 1.386(5) . ?
C41B C46B 1.3900 . ?
C41B C42B 1.3900 . ?
C46B C45B 1.3900 . ?
C45B C44B 1.3900 . ?
C44B C43B 1.3900 . ?
C44B C47B 1.482(7) . ?
C43B C42B 1.3900 . ?
C30 C31 1.366(9) . ?
C30 C35 1.390(9) . ?
C14 C16 1.361(7) . ?
C16 C17A 1.550(6) . ?
C16 C12 1.402(8) . ?
C16 C17B 1.494(9) . ?
O3 C36 1.221(10) . ?
C31 C32 1.403(6) . ?
C35 C34 1.410(6) . ?
C11 C12 1.383(5) . ?
O4 C36 1.278(10) . ?
C51 C50 1.3900 . ?
C51 C52 1.3900 . ?
C50 C49 1.3900 . ?
C49 C48 1.3900 . ?
C48 C53 1.3900 . ?
C53 C52 1.3900 . ?
C17A C18A 1.3900 . ?
C17A C22A 1.3900 . ?
C18A C19A 1.3900 . ?
C19A C20A 1.3900 . ?
C20A C21A 1.3900 . ?
C20A C23A 1.518(8) . ?
C21A C22A 1.3900 . ?
C33 C34 1.390(10) . ?
C33 C36 1.490(7) . ?
C33 C32 1.344(11) . ?
O6B C47B 1.248(9) . ?
O2A C23A 1.252(13) . ?
C17B C18B 1.394(11) . ?
C17B C22B 1.403(11) . ?
C18B C19B 1.394(10) . ?
C19B C20B 1.362(12) . ?
C20B C21B 1.369(12) . ?
C20B C23B 1.531(11) . ?
C21B C22B 1.363(9) . ?
C23B O1B 1.199(14) . ?
C23B O2B 1.217(11) . ?
C41A C46A 1.368(12) . ?
C41A C42A 1.432(12) . ?
C46A C45A 1.391(10) . ?
C45A C44A 1.381(12) . ?
C44A C43A 1.402(12) . ?
C44A C47A 1.484(12) . ?
C43A C42A 1.378(9) . ?
C47A O6A 1.298(19) . ?
C47A O5A 1.230(12) . ?

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
C7 C7 C8 118.55(16) 2_556 . ?
C7 C7 C6 120.25(15) 2_556 . ?
C8 C7 C6 121.1(2) . . ?
C9 C9 C37 122.60(16) 2_556 . ?
C8 C9 C9 118.62(16) . 2_556 ?
C8 C9 C37 118.7(3) . . ?
C38 C37 C9 121.3(3) . . ?
C38 C37 C42 118.0(3) . . ?
C42 C37 C9 120.5(3) . . ?
C9 C8 C7 122.7(3) . . ?
C5 C4 C3 118.2(2) . . ?
C5 C4 C24 116.8(3) . . ?
C3 C4 C24 125.0(3) . . ?
C4 C5 C6 124.2(3) . . ?
C5 C6 C7 122.5(2) . . ?
C5 C6 C1 117.6(2) . . ?
C1 C6 C7 119.7(2) . . ?
C37 C38 C39 120.5(3) . . ?
C6 C1 C1 119.96(15) . 2_556 ?
C2 C1 C6 118.2(2) . . ?
C2 C1 C1 121.80(17) . 2_556 ?
C4 C3 C10 123.6(3) . . ?
C2 C3 C4 118.5(3) . . ?
C2 C3 C10 117.9(3) . . ?
C40 C39 C38 121.5(3) . . ?
C25 C24 C4 121.1(3) . . ?
C29 C24 C4 121.1(3) . . ?
C29 C24 C25 117.6(3) . . ?
C3 C2 C1 123.3(3) . . ?
C41 C42 C37 120.6(4) . . ?
C39 C40 C41 117.5(3) . . ?
C39 C40 C41B 124.8(4) . . ?
C39 C40 C41A 115.9(5) . . ?
C41 C40 C41B 117.0(4) . . ?
C41 C40 C41A 125.5(5) . . ?
C26 C25 C24 120.8(4) . . ?
C15 C10 C3 123.4(4) . . ?
C15 C10 C11 117.2(3) . . ?
C11 C10 C3 119.4(4) . . ?
C27 C28 C29 120.9(4) . . ?
C42 C41 C40 121.7(4) . . ?
C28 C27 C26 118.4(3) . . ?
C28 C27 C30 120.5(4) . . ?
C26 C27 C30 121.1(4) . . ?
C25 C26 C27 120.2(4) . . ?
C10 C15 C14 122.3(4) . . ?
C24 C29 C28 122.1(4) . . ?
C46B C41B C40 126.3(3) . . ?
C46B C41B C42B 120.0 . . ?
C42B C41B C40 113.7(3) . . ?
C41B C46B C45B 120.0 . . ?
C46B C45B C44B 120.0 . . ?
C45B C44B C47B 120.4(5) . . ?
C43B C44B C45B 120.0 . . ?
C43B C44B C47B 119.6(5) . . ?
C44B C43B C42B 120.0 . . ?
C43B C42B C41B 120.0 . . ?
C31 C30 C27 120.1(5) . . ?
C31 C30 C35 120.2(4) . . ?
C35 C30 C27 119.7(5) . . ?
C16 C14 C15 121.4(4) . . ?
C14 C16 C17A 116.3(5) . . ?
C14 C16 C12 117.6(4) . . ?
C14 C16 C17B 124.7(5) . . ?
C12 C16 C17A 125.2(5) . . ?
C12 C16 C17B 115.3(6) . . ?
C30 C31 C32 119.6(6) . . ?
C30 C35 C34 119.5(6) . . ?
C12 C11 C10 120.4(5) . . ?
C50 C51 Cl3 120.0(5) . . ?
C50 C51 C52 120.0 . . ?
C52 C51 Cl3 120.0(5) . . ?
C49 C50 C51 120.0 . . ?
C50 C49 Cl2 121.1(5) . . ?
C50 C49 C48 120.0 . . ?
C48 C49 Cl2 118.9(5) . . ?
C49 C48 Cl1 119.9(5) . . ?
C53 C48 Cl1 120.1(5) . . ?
C53 C48 C49 120.0 . . ?
C52 C53 C48 120.0 . . ?
C53 C52 C51 120.0 . . ?
C18A C17A C16 110.4(6) . . ?
C18A C17A C22A 120.0 . . ?
C22A C17A C16 129.3(6) . . ?
C17A C18A C19A 120.0 . . ?
C20A C19A C18A 120.0 . . ?
C19A C20A C23A 119.6(6) . . ?
C21A C20A C19A 120.0 . . ?
C21A C20A C23A 120.4(6) . . ?
C22A C21A C20A 120.0 . . ?
C21A C22A C17A 120.0 . . ?
C34 C33 C36 119.4(7) . . ?
C32 C33 C34 120.2(5) . . ?
C32 C33 C36 120.4(7) . . ?
C11 C12 C16 121.0(5) . . ?
C33 C34 C35 119.3(6) . . ?
O3 C36 O4 123.4(6) . . ?
O3 C36 C33 119.9(8) . . ?
O4 C36 C33 116.6(8) . . ?
C33 C32 C31 121.2(7) . . ?
O5B C47B C44B 118.5(9) . . ?
O6B C47B O5B 125.0(9) . . ?
O6B C47B C44B 116.4(7) . . ?
O1A C23A C20A 117.8(11) . . ?
O1A C23A O2A 118.8(13) . . ?
O2A C23A C20A 115.8(9) . . ?
C18B C17B C16 122.9(8) . . ?
C18B C17B C22B 116.6(7) . . ?
C22B C17B C16 119.0(8) . . ?
C19B C18B C17B 122.5(9) . . ?
C20B C19B C18B 118.7(10) . . ?
C19B C20B C21B 119.2(8) . . ?
C19B C20B C23B 121.6(9) . . ?
C21B C20B C23B 119.1(8) . . ?
C22B C21B C20B 122.7(9) . . ?
C21B C22B C17B 119.9(9) . . ?
O1B C23B C20B 120.3(12) . . ?
O1B C23B O2B 122.2(12) . . ?
O2B C23B C20B 117.4(10) . . ?
C46A C41A C40 119.7(8) . . ?
C46A C41A C42A 117.6(7) . . ?
C42A C41A C40 122.3(7) . . ?
C41A C46A C45A 121.4(9) . . ?
C44A C45A C46A 121.1(9) . . ?
C45A C44A C43A 118.6(8) . . ?
C45A C44A C47A 121.8(9) . . ?
C43A C44A C47A 119.6(9) . . ?
C42A C43A C44A 120.2(8) . . ?
C43A C42A C41A 120.8(8) . . ?
O6A C47A C44A 116.4(13) . . ?
O5A C47A C44A 120.5(11) . . ?
O5A C47A O6A 122.8(13) . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.284 0.500 0.000 3628 1118 ' '
2 0.187 0.000 0.500 3628 1118 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.507
_oxdiff_exptl_absorpt_empirical_full_min 0.640

#==============================================================================
# start Validation Reply Form
_vrf_PLAT213_BPTp-1-TCB          
;
PROBLEM: Atom O6B has ADP max/min Ratio ..... 5.1 prolat
RESPONSE: Due to severe disorder of the carboxy group. 
;
_vrf_PLAT417_BPTp-1-TCB          
;
PROBLEM: Short Inter D-H..H-D H3 ..H4 . 1.01 Ang. 
RESPONSE: Due to disorder of the H atom in the carboxy gruop.
;
# end Validation Reply Form
#==============================================================================
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: N,N-dimethylformamide, 1,2,4-trichlorobenzene'
####################################################################### 
# 
# 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_ThiaHAT-1
_database_code_depnum_ccdc_archive 'CCDC 2081131'
loop_
_audit_author_name
_audit_author_address
'Ichiro Hisaki'
;Osaka University
Japan
;
_audit_update_record             
;
2021-05-07 deposited with the CCDC.	2021-06-21 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C126 H66 N18 O12 S6'
_chemical_formula_moiety         'C126 H66 N18 O12 S6'
_chemical_formula_weight         2216.33
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      trigonal
_space_group_name_H-M_alt        'R -3 c:H'
_space_group_name_Hall           '-R 3 2"c'
_space_group_IT_number           167
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'x, x-y, z+1/2'
'-x+y, y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, -z-1/2'
'-x, -x+y, -z-1/2'
'x-y, -y, -z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'y+2/3, x+1/3, -z-1/6'
'-x+2/3, -x+y+1/3, -z-1/6'
'x-y+2/3, -y+1/3, -z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'y+1/3, x+2/3, -z+1/6'
'-x+1/3, -x+y+2/3, -z+1/6'
'x-y+1/3, -y+2/3, -z+1/6'
#------------------------------------------------------------------------------
_cell_length_a                   65.827(5)
_cell_length_b                   65.827(5)
_cell_length_c                   6.9879(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     26223(4)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    1350
_cell_measurement_theta_min      1.88
_cell_measurement_theta_max      23.88
_cell_measurement_temperature    95
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            yeloow
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.008
_exptl_crystal_density_diffrn    0.842
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6840.00
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_T_max  1.000

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      95
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.81128
_diffrn_measurement_device_type  'SPring-8 BL40XU, Pilatus100K, DECTRIS'
_diffrn_reflns_number            79883
_diffrn_reflns_av_unetI/netI     0.1226
_diffrn_reflns_av_R_equivalents  0.3517
_diffrn_reflns_theta_max         28.247
_diffrn_reflns_theta_min         1.869
_diffrn_reflns_theta_full        28.247
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -76
_diffrn_reflns_limit_h_max       76
_diffrn_reflns_limit_k_min       -76
_diffrn_reflns_limit_k_max       76
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             4863
_reflns_number_gt                2899
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.2018
_refine_ls_R_factor_gt           0.1673
_refine_ls_wR_factor_ref         0.4353
_refine_ls_wR_factor_gt          0.4068
_refine_ls_number_restraints     741
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4863
_refine_ls_number_parameters     394
_refine_ls_goodness_of_fit_ref   1.363
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.64280(4) 0.35749(4) 0.1275(4) 0.0420(9) Uani 1 1 d . . . . .
C1 C 0.65438(5) 0.34618(5) 0.0883(6) 0.0416(10) Uani 1 1 d . . . . .
C2 C 0.65504(5) 0.38096(5) 0.1197(6) 0.0453(10) Uani 1 1 d . . . . .
C3 C 0.64402(6) 0.39392(6) 0.1933(6) 0.0483(11) Uani 1 1 d . . . . .
C4 C 0.62027(6) 0.38583(7) 0.1667(6) 0.0564(12) Uani 1 1 d . . . . .
H4 H 0.610840 0.371399 0.108289 0.068 Uiso 1 1 calc R U . . .
C5 C 0.61065(8) 0.39915(9) 0.2265(8) 0.0834(16) Uani 1 1 d . . . . .
H5 H 0.594808 0.393708 0.205216 0.100 Uiso 1 1 calc R U . . .
C6 C 0.62431(10) 0.42079(9) 0.3191(9) 0.0881(17) Uani 1 1 d D . . . .
C7 C 0.64759(8) 0.42827(7) 0.3495(7) 0.0747(15) Uani 1 1 d . . . . .
H7 H 0.656900 0.442487 0.411338 0.090 Uiso 1 1 calc R U . . .
C8 C 0.65738(7) 0.41530(6) 0.2911(7) 0.0658(14) Uani 1 1 d . . . . .
H8 H 0.673136 0.420669 0.316307 0.079 Uiso 1 1 calc R U . . .
S1A S 0.63739(9) 0.46583(10) 0.8682(10) 0.166(2) Uani 0.662 1 d D U P A 1
O1A O 0.5276(5) 0.5110(4) 0.593(4) 0.425(11) Uani 0.662 1 d D U P A 1
O2A O 0.5399(4) 0.5127(4) 0.883(4) 0.449(12) Uani 0.662 1 d D U P A 1
H2OA H 0.531694 0.518586 0.900771 0.539 Uiso 0.662 1 calc DR U P A 1
N2A N 0.6372(2) 0.4494(2) 0.691(2) 0.134(4) Uani 0.662 1 d D U P A 1
N3A N 0.6167(2) 0.4709(3) 0.793(3) 0.194(6) Uani 0.662 1 d D U P A 1
C9A C 0.6141(3) 0.43482(19) 0.391(3) 0.122(5) Uani 0.662 1 d D U P A 1
C10A C 0.5976(3) 0.4370(3) 0.303(3) 0.155(6) Uani 0.662 1 d D U P A 1
H10A H 0.592138 0.428779 0.188135 0.187 Uiso 0.662 1 calc R U P A 1
C11A C 0.5874(4) 0.4499(4) 0.359(3) 0.171(6) Uani 0.662 1 d D U P A 1
H11A H 0.575889 0.449868 0.282097 0.205 Uiso 0.662 1 calc R U P A 1
C12A C 0.5935(4) 0.4623(3) 0.519(3) 0.202(6) Uani 0.662 1 d D U P A 1
C13A C 0.6101(3) 0.4603(3) 0.627(3) 0.173(6) Uani 0.662 1 d D U P A 1
C14A C 0.6210(3) 0.4478(3) 0.567(3) 0.132(5) Uani 0.662 1 d D U P A 1
C15A C 0.5802(3) 0.4752(3) 0.554(4) 0.261(7) Uani 0.662 1 d D U P A 1
C16A C 0.5681(4) 0.4798(4) 0.413(4) 0.340(9) Uani 0.662 1 d D U P A 1
H16A H 0.568897 0.475927 0.286418 0.408 Uiso 0.662 1 calc R U P A 1
C17A C 0.5549(4) 0.4902(4) 0.463(4) 0.360(9) Uani 0.662 1 d D U P A 1
H17A H 0.547206 0.493849 0.368661 0.433 Uiso 0.662 1 calc R U P A 1
C18A C 0.5533(5) 0.4950(5) 0.652(4) 0.368(9) Uani 0.662 1 d D U P A 1
C19A C 0.5669(4) 0.4932(4) 0.790(4) 0.370(12) Uani 0.662 1 d D U P A 1
H19A H 0.568608 0.499599 0.911558 0.444 Uiso 0.662 1 calc R U P A 1
C20A C 0.5783(4) 0.4807(4) 0.735(4) 0.307(9) Uani 0.662 1 d D U P A 1
H20A H 0.584940 0.476072 0.830203 0.369 Uiso 0.662 1 calc R U P A 1
C21A C 0.5391(4) 0.5074(5) 0.715(4) 0.395(10) Uani 0.662 1 d D U P A 1
S1B S 0.6277(3) 0.4684(2) 0.842(3) 0.235(6) Uani 0.338 1 d D U P A 2
O1B O 0.5388(6) 0.5221(6) 0.451(7) 0.396(9) Uani 0.338 1 d D U P A 2
H1OB H 0.531284 0.528658 0.473006 0.476 Uiso 0.169 1 calc DR U P A 2
O2B O 0.5153(6) 0.4928(6) 0.675(7) 0.396(9) Uani 0.338 1 d D U P A 2
H2OB H 0.508021 0.499714 0.693982 0.476 Uiso 0.169 1 calc DR U P A 2
N2B N 0.6321(6) 0.4534(6) 0.662(4) 0.163(8) Uani 0.338 1 d D U P A 2
N3B N 0.6097(5) 0.4721(5) 0.694(4) 0.209(9) Uani 0.338 1 d D U P A 2
C9B C 0.6143(5) 0.4360(4) 0.357(5) 0.121(7) Uani 0.338 1 d D U P A 2
C10B C 0.5982(6) 0.4358(6) 0.243(5) 0.146(7) Uani 0.338 1 d D U P A 2
H10B H 0.595092 0.427212 0.130890 0.175 Uiso 0.338 1 calc R U P A 2
C11B C 0.5857(6) 0.4468(7) 0.272(5) 0.177(7) Uani 0.338 1 d D U P A 2
H11B H 0.574996 0.445158 0.178018 0.212 Uiso 0.338 1 calc R U P A 2
C12B C 0.5878(5) 0.4599(5) 0.428(4) 0.199(8) Uani 0.338 1 d D U P A 2
C13B C 0.6065(5) 0.4626(5) 0.532(4) 0.179(7) Uani 0.338 1 d D U P A 2
C14B C 0.6186(6) 0.4507(6) 0.514(5) 0.148(6) Uani 0.338 1 d D U P A 2
C15B C 0.5713(5) 0.4693(5) 0.469(5) 0.286(8) Uani 0.338 1 d D U P A 2
C16B C 0.5772(6) 0.4895(6) 0.364(6) 0.312(9) Uani 0.338 1 d D U P A 2
H16B H 0.589754 0.495391 0.279275 0.374 Uiso 0.338 1 calc R U P A 2
C17B C 0.5645(6) 0.5010(6) 0.387(6) 0.349(9) Uani 0.338 1 d D U P A 2
H17B H 0.568257 0.514401 0.316929 0.419 Uiso 0.338 1 calc R U P A 2
C18B C 0.5461(4) 0.4919(5) 0.517(4) 0.372(9) Uani 0.338 1 d D U P A 2
C19B C 0.5390(6) 0.4710(6) 0.614(6) 0.348(10) Uani 0.338 1 d D U P A 2
H19B H 0.526021 0.464725 0.693953 0.417 Uiso 0.338 1 calc R U P A 2
C20B C 0.5519(6) 0.4599(6) 0.588(6) 0.309(9) Uani 0.338 1 d D U P A 2
H20B H 0.547403 0.445854 0.652172 0.371 Uiso 0.338 1 calc R U P A 2
C21B C 0.5312(5) 0.5040(5) 0.552(5) 0.396(9) Uani 0.338 1 d D U P A 2


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT Version 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/1 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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 C1 1.333(4) . ?
N1 C2 1.340(4) . ?
C1 C1 1.402(6) 35_655 ?
C1 C1 1.467(6) 36 ?
C2 C2 1.420(6) 35_655 ?
C2 C3 1.462(5) . ?
C3 C4 1.389(5) . ?
C3 C8 1.409(5) . ?
C4 C5 1.378(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.405(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.372(7) . ?
C6 C9B 1.474(14) . ?
C6 C9A 1.478(10) . ?
C7 C8 1.364(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
S1A N2A 1.638(11) . ?
S1A N3A 1.642(11) . ?
O1A C21A 1.243(17) . ?
O2A C21A 1.223(16) . ?
O2A H2OA 0.8200 . ?
N2A C14A 1.340(14) . ?
N3A C13A 1.305(15) . ?
C9A C10A 1.317(13) . ?
C9A C14A 1.438(15) . ?
C10A C11A 1.375(13) . ?
C10A H10A 0.9300 . ?
C11A C12A 1.324(15) . ?
C11A H11A 0.9300 . ?
C12A C13A 1.390(15) . ?
C12A C15A 1.511(14) . ?
C13A C14A 1.396(13) . ?
C15A C20A 1.337(17) . ?
C15A C16A 1.389(18) . ?
C16A C17A 1.397(16) . ?
C16A H16A 0.9300 . ?
C17A C18A 1.379(17) . ?
C17A H17A 0.9300 . ?
C18A C19A 1.364(17) . ?
C18A C21A 1.573(14) . ?
C19A C20A 1.413(14) . ?
C19A H19A 0.9300 . ?
C20A H20A 0.9300 . ?
S1B N3B 1.686(18) . ?
S1B N2B 1.713(18) . ?
O1B C21B 1.253(17) . ?
O1B H1OB 0.8200 . ?
O2B C21B 1.264(17) . ?
O2B H2OB 0.8200 . ?
N2B C14B 1.313(19) . ?
N3B C13B 1.261(18) . ?
C9B C10B 1.321(18) . ?
C9B C14B 1.393(17) . ?
C10B C11B 1.348(18) . ?
C10B H10B 0.9300 . ?
C11B C12B 1.356(18) . ?
C11B H11B 0.9300 . ?
C12B C13B 1.366(18) . ?
C12B C15B 1.517(18) . ?
C13B C14B 1.373(17) . ?
C15B C20B 1.389(18) . ?
C15B C16B 1.393(19) . ?
C16B C17B 1.387(17) . ?
C16B H16B 0.9300 . ?
C17B C18B 1.391(18) . ?
C17B H17B 0.9300 . ?
C18B C19B 1.386(18) . ?
C18B C21B 1.559(17) . ?
C19B C20B 1.380(17) . ?
C19B H19B 0.9300 . ?
C20B H20B 0.9300 . ?

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
C1 N1 C2 117.0(3) . . ?
N1 C1 C1 120.31(18) . 35_655 ?
N1 C1 C1 119.52(18) . 36 ?
C1 C1 C1 119.76(6) 35_655 36 ?
N1 C2 C2 120.06(19) . 35_655 ?
N1 C2 C3 118.1(3) . . ?
C2 C2 C3 121.81(19) 35_655 . ?
C4 C3 C8 117.9(3) . . ?
C4 C3 C2 121.4(3) . . ?
C8 C3 C2 120.7(3) . . ?
C5 C4 C3 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C7 C6 C5 117.9(4) . . ?
C7 C6 C9B 121.8(14) . . ?
C5 C6 C9B 119.7(14) . . ?
C7 C6 C9A 120.0(9) . . ?
C5 C6 C9A 122.0(8) . . ?
C8 C7 C6 121.5(4) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C7 C8 C3 121.1(4) . . ?
C7 C8 H8 119.5 . . ?
C3 C8 H8 119.5 . . ?
N2A S1A N3A 99.1(8) . . ?
C21A O2A H2OA 109.5 . . ?
C14A N2A S1A 106.3(10) . . ?
C13A N3A S1A 105.4(10) . . ?
C10A C9A C14A 111.7(11) . . ?
C10A C9A C6 124.4(16) . . ?
C14A C9A C6 123.9(15) . . ?
C9A C10A C11A 127.8(14) . . ?
C9A C10A H10A 116.1 . . ?
C11A C10A H10A 116.1 . . ?
C12A C11A C10A 122.3(14) . . ?
C12A C11A H11A 118.8 . . ?
C10A C11A H11A 118.8 . . ?
C11A C12A C13A 114.2(12) . . ?
C11A C12A C15A 113.8(17) . . ?
C13A C12A C15A 132.0(17) . . ?
N3A C13A C12A 120.0(14) . . ?
N3A C13A C14A 116.6(14) . . ?
C12A C13A C14A 123.4(13) . . ?
N2A C14A C13A 112.6(13) . . ?
N2A C14A C9A 127.0(14) . . ?
C13A C14A C9A 120.4(11) . . ?
C20A C15A C16A 117.9(12) . . ?
C20A C15A C12A 117.7(17) . . ?
C16A C15A C12A 124.2(18) . . ?
C15A C16A C17A 119.9(18) . . ?
C15A C16A H16A 120.1 . . ?
C17A C16A H16A 120.1 . . ?
C18A C17A C16A 119.3(17) . . ?
C18A C17A H17A 120.4 . . ?
C16A C17A H17A 120.4 . . ?
C19A C18A C17A 121.9(13) . . ?
C19A C18A C21A 116.0(17) . . ?
C17A C18A C21A 121.2(17) . . ?
C18A C19A C20A 115.0(16) . . ?
C18A C19A H19A 122.5 . . ?
C20A C19A H19A 122.5 . . ?
C15A C20A C19A 124.5(17) . . ?
C15A C20A H20A 117.7 . . ?
C19A C20A H20A 117.7 . . ?
O2A C21A O1A 123.2(14) . . ?
O2A C21A C18A 117.4(17) . . ?
O1A C21A C18A 119.3(18) . . ?
N3B S1B N2B 88.0(13) . . ?
C21B O1B H1OB 109.5 . . ?
C21B O2B H2OB 109.5 . . ?
C14B N2B S1B 111.0(17) . . ?
C13B N3B S1B 115.6(17) . . ?
C10B C9B C14B 111.6(16) . . ?
C10B C9B C6 121(2) . . ?
C14B C9B C6 127(2) . . ?
C9B C10B C11B 127(2) . . ?
C9B C10B H10B 116.4 . . ?
C11B C10B H10B 116.4 . . ?
C10B C11B C12B 125(2) . . ?
C10B C11B H11B 117.7 . . ?
C12B C11B H11B 117.7 . . ?
C11B C12B C13B 107.6(17) . . ?
C11B C12B C15B 123(2) . . ?
C13B C12B C15B 129(2) . . ?
N3B C13B C12B 117(2) . . ?
N3B C13B C14B 111.6(19) . . ?
C12B C13B C14B 128.7(19) . . ?
N2B C14B C13B 113.4(19) . . ?
N2B C14B C9B 127(2) . . ?
C13B C14B C9B 119.2(18) . . ?
C20B C15B C16B 119.7(19) . . ?
C20B C15B C12B 128(2) . . ?
C16B C15B C12B 112(2) . . ?
C17B C16B C15B 120(2) . . ?
C17B C16B H16B 119.9 . . ?
C15B C16B H16B 119.9 . . ?
C16B C17B C18B 118(2) . . ?
C16B C17B H17B 120.8 . . ?
C18B C17B H17B 120.8 . . ?
C19B C18B C17B 122.1(18) . . ?
C19B C18B C21B 117(2) . . ?
C17B C18B C21B 121(2) . . ?
C20B C19B C18B 118(2) . . ?
C20B C19B H19B 120.8 . . ?
C18B C19B H19B 120.8 . . ?
C19B C20B C15B 121(2) . . ?
C19B C20B H20B 119.6 . . ?
C15B C20B H20B 119.6 . . ?
O1B C21B O2B 139(2) . . ?
O1B C21B C18B 110(2) . . ?
O2B C21B C18B 111(2) . . ?

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 N1 C1 C1 12.5(7) . . . 35_655 ?
C2 N1 C1 C1 -174.8(4) . . . 36 ?
C1 N1 C2 C2 8.4(6) . . . 35_655 ?
C1 N1 C2 C3 -169.6(3) . . . . ?
N1 C2 C3 C4 -37.9(6) . . . . ?
C2 C2 C3 C4 144.1(5) 35_655 . . . ?
N1 C2 C3 C8 143.2(4) . . . . ?
C2 C2 C3 C8 -34.8(7) 35_655 . . . ?
C8 C3 C4 C5 3.2(6) . . . . ?
C2 C3 C4 C5 -175.7(4) . . . . ?
C3 C4 C5 C6 -1.5(7) . . . . ?
C4 C5 C6 C7 -0.4(8) . . . . ?
C4 C5 C6 C9B 171.6(16) . . . . ?
C4 C5 C6 C9A -177.5(8) . . . . ?
C5 C6 C7 C8 0.4(8) . . . . ?
C9B C6 C7 C8 -171.4(17) . . . . ?
C9A C6 C7 C8 177.6(8) . . . . ?
C6 C7 C8 C3 1.4(7) . . . . ?
C4 C3 C8 C7 -3.2(6) . . . . ?
C2 C3 C8 C7 175.7(4) . . . . ?
N3A S1A N2A C14A 0.8(13) . . . . ?
N2A S1A N3A C13A -1.8(15) . . . . ?
C7 C6 C9A C10A 144.9(9) . . . . ?
C5 C6 C9A C10A -38.1(9) . . . . ?
C7 C6 C9A C14A -35.1(12) . . . . ?
C5 C6 C9A C14A 141.9(12) . . . . ?
C14A C9A C10A C11A 0.9(17) . . . . ?
C6 C9A C10A C11A -179.1(14) . . . . ?
C9A C10A C11A C12A 0(3) . . . . ?
C10A C11A C12A C13A -3(3) . . . . ?
C10A C11A C12A C15A 179.9(17) . . . . ?
S1A N3A C13A C12A -176.4(16) . . . . ?
S1A N3A C13A C14A 2(2) . . . . ?
C11A C12A C13A N3A -176.7(18) . . . . ?
C15A C12A C13A N3A 0(3) . . . . ?
C11A C12A C13A C14A 5(3) . . . . ?
C15A C12A C13A C14A -178.4(19) . . . . ?
S1A N2A C14A C13A 0.4(17) . . . . ?
S1A N2A C14A C9A -178.5(15) . . . . ?
N3A C13A C14A N2A -2(2) . . . . ?
C12A C13A C14A N2A 176.7(18) . . . . ?
N3A C13A C14A C9A 177.1(16) . . . . ?
C12A C13A C14A C9A -4(3) . . . . ?
C10A C9A C14A N2A -179.9(16) . . . . ?
C6 C9A C14A N2A 0(2) . . . . ?
C10A C9A C14A C13A 1.2(19) . . . . ?
C6 C9A C14A C13A -178.8(13) . . . . ?
C11A C12A C15A C20A 156(2) . . . . ?
C13A C12A C15A C20A -21(3) . . . . ?
C11A C12A C15A C16A -18(3) . . . . ?
C13A C12A C15A C16A 165(2) . . . . ?
C20A C15A C16A C17A 1.0(17) . . . . ?
C12A C15A C16A C17A 175.0(15) . . . . ?
C15A C16A C17A C18A -2.4(16) . . . . ?
C16A C17A C18A C19A 10(4) . . . . ?
C16A C17A C18A C21A 178.2(18) . . . . ?
C17A C18A C19A C20A -15(4) . . . . ?
C21A C18A C19A C20A 176(2) . . . . ?
C16A C15A C20A C19A -7(3) . . . . ?
C12A C15A C20A C19A 179(2) . . . . ?
C18A C19A C20A C15A 14(4) . . . . ?
C19A C18A C21A O2A -6(4) . . . . ?
C17A C18A C21A O2A -175(3) . . . . ?
C19A C18A C21A O1A 175(3) . . . . ?
C17A C18A C21A O1A 6(4) . . . . ?
N3B S1B N2B C14B -5(3) . . . . ?
N2B S1B N3B C13B 2.3(14) . . . . ?
C7 C6 C9B C10B 141.8(14) . . . . ?
C5 C6 C9B C10B -30(2) . . . . ?
C7 C6 C9B C14B -43(3) . . . . ?
C5 C6 C9B C14B 146(3) . . . . ?
C14B C9B C10B C11B -4.1(18) . . . . ?
C6 C9B C10B C11B 172(2) . . . . ?
C9B C10B C11B C12B -0.5(19) . . . . ?
C10B C11B C12B C13B 8(3) . . . . ?
C10B C11B C12B C15B -171(2) . . . . ?
S1B N3B C13B C12B 164(2) . . . . ?
S1B N3B C13B C14B 0.9(19) . . . . ?
C11B C12B C13B N3B -172(2) . . . . ?
C15B C12B C13B N3B 7(3) . . . . ?
C11B C12B C13B C14B -13(3) . . . . ?
C15B C12B C13B C14B 167(3) . . . . ?
S1B N2B C14B C13B 7(4) . . . . ?
S1B N2B C14B C9B -168(3) . . . . ?
N3B C13B C14B N2B -5(3) . . . . ?
C12B C13B C14B N2B -165(3) . . . . ?
N3B C13B C14B C9B 170(3) . . . . ?
C12B C13B C14B C9B 10(4) . . . . ?
C10B C9B C14B N2B 174(3) . . . . ?
C6 C9B C14B N2B -2(5) . . . . ?
C10B C9B C14B C13B 0(3) . . . . ?
C6 C9B C14B C13B -176(3) . . . . ?
C11B C12B C15B C20B 97(3) . . . . ?
C13B C12B C15B C20B -82(3) . . . . ?
C11B C12B C15B C16B -81(3) . . . . ?
C13B C12B C15B C16B 99(3) . . . . ?
C20B C15B C16B C17B 3(4) . . . . ?
C12B C15B C16B C17B -178(3) . . . . ?
C15B C16B C17B C18B 1(5) . . . . ?
C16B C17B C18B C19B -5(4) . . . . ?
C16B C17B C18B C21B 179(2) . . . . ?
C17B C18B C19B C20B 4(3) . . . . ?
C21B C18B C19B C20B -179(2) . . . . ?
C18B C19B C20B C15B 0(4) . . . . ?
C16B C15B C20B C19B -4(3) . . . . ?
C12B C15B C20B C19B 178(3) . . . . ?
C19B C18B C21B O1B -177(2) . . . . ?
C17B C18B C21B O1B -1(2) . . . . ?
C19B C18B C21B O2B 3(2) . . . . ?
C17B C18B C21B O2B 180(2) . . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.







#==============================================================================
# start Validation Reply Form
_vrf_RINTA01_ThiaHAT-1           
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: Due to weak diffraction because of small crystal size
;
_vrf_PLAT020_ThiaHAT-1           
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.352 Report
RESPONSE: Due to weak diffraction because of small crystal size
;
_vrf_PLAT213_ThiaHAT-1           
;
PROBLEM: Atom O1A             has ADP max/min Ratio .....        6.1 oblate
RESPONSE: Due to severe disorder of the peripheral group
;
_vrf_PLAT250_ThiaHAT-1           
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....       15.3 Note  
RESPONSE: Due to severe disorder of the peripheral group
;
# end Validation Reply Form
#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        
"4,4',4'',4''',4'''',4'''''-((dipyrazino[2,3-f:2',3'-h]quinoxaline-2,3,6,7,10,11-hexaylhexakis(benzene-4,1-diyl))hexakis(benzo[c][1,2,5]thiadiazole-7,4-diyl))hexabenzoic acid"
_chemical_name_common            ThiaHAT
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: N,N-dimethylacetamide, 1,2,4-trichlorobenzene'
