# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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_368a
_database_code_depnum_ccdc_archive 'CCDC 2233693'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2022-12-31 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_audit_creation_date             2019-05-21
_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            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H16 N8'
_chemical_formula_sum            'C20 H16 N8'
_chemical_formula_weight         368.41
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHN
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.3024(8)
_cell_length_b                   8.4285(10)
_cell_length_c                   9.2846(12)
_cell_angle_alpha                67.272(12)
_cell_angle_beta                 89.999(10)
_cell_angle_gamma                77.645(10)
_cell_volume                     442.49(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    999
_cell_measurement_temperature    172.97(10)
_cell_measurement_theta_max      74.4070
_cell_measurement_theta_min      5.1640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light red'
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.004
_exptl_crystal_size_min          0.004
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2679
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.836
_diffrn_reflns_theta_min         5.187
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -100.00  -8.00   1.00    4.05    --  -40.81 -77.00-150.00   92
  2  ω   -113.00 -25.00   1.00    4.05    --  -40.81 -38.00  90.00   88
  3  ω     60.00  94.00   1.00    4.05    --   40.81-125.00  60.00   34
  4  ω      4.00  41.00   1.00    4.05    --   40.81 -99.00 -30.00   37
  5  ω     76.00 102.00   1.00    4.05    --   40.81  38.00  60.00   26
  6  ω     20.00  70.00   1.00    4.05    --   40.81  38.00  60.00   50
  7  ω     79.00 167.00   1.00   16.22    --  107.77  30.00-180.00   88
  8  ω    106.00 178.00   1.00   16.22    --  107.77  30.00 -90.00   72
  9  ω    114.00 177.00   1.00   16.22    --  107.77  61.00-150.00   63
 10  ω     63.00 103.00   1.00   16.22    --  107.77 -95.00-120.00   40
 11  ω     29.00  55.00   1.00   16.22    --  107.77 -95.00 -30.00   26
 12  ω     63.00  97.00   1.00   16.22    --  107.77 -95.00 -30.00   34
 13  ω     45.00 125.00   1.00   16.22    --  107.77 -45.00 120.00   80
 14  ω     38.00 116.00   1.00   16.22    --  107.77-125.00  90.00   78
 15  ω     36.00 134.00   1.00   16.22    --  107.77 -45.00-120.00   98
 16  ω     36.00 117.00   1.00   16.22    --  107.77 -77.00  90.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1360052000
_diffrn_orient_matrix_UB_12      -0.1026697000
_diffrn_orient_matrix_UB_13      -0.0876884000
_diffrn_orient_matrix_UB_21      -0.1090561000
_diffrn_orient_matrix_UB_22      0.1453820000
_diffrn_orient_matrix_UB_23      -0.1578260000
_diffrn_orient_matrix_UB_31      0.1809960000
_diffrn_orient_matrix_UB_32      0.0991314000
_diffrn_orient_matrix_UB_33      -0.0061963000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1321
_reflns_number_total             1740
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.79
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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         0.255
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1740
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0558
_refine_ls_restrained_S_all      1.020
_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)+(0.0809P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1581
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_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
N001 N 0.2021(3) 0.8009(3) 0.1163(2) 0.0313(4) Uani 1 1 d . . . . .
N002 N 0.3690(3) 0.7108(3) 0.0701(2) 0.0311(4) Uani 1 1 d . . . . .
N003 N 0.4447(3) 0.9311(3) 0.2024(2) 0.0313(5) Uani 1 1 d . . . . .
N004 N 0.6119(3) 0.8402(3) 0.1573(2) 0.0307(4) Uani 1 1 d . . . . .
C005 C 0.5700(4) 0.7209(3) 0.1053(2) 0.0274(5) Uani 1 1 d . . . . .
C006 C 0.2485(4) 0.8955(3) 0.1941(2) 0.0280(5) Uani 1 1 d . . . . .
C007 C 0.8180(4) 0.4349(3) 0.2463(3) 0.0275(5) Uani 1 1 d . . . . .
C008 C 0.8952(4) 0.1701(3) 0.5500(3) 0.0271(5) Uani 1 1 d . . . . .
C009 C 0.7617(4) 0.5903(3) 0.0886(3) 0.0301(5) Uani 1 1 d . . . . .
C00A C 1.0037(4) 0.4085(3) 0.3413(3) 0.0308(5) Uani 1 1 d . . . . .
C00B C 0.7127(4) 0.1925(3) 0.4533(3) 0.0317(5) Uani 1 1 d . . . . .
C00C C 0.0736(4) 0.9639(3) 0.2791(3) 0.0308(5) Uani 1 1 d . . . . .
C00D C 1.0408(4) 0.2763(3) 0.4929(3) 0.0316(5) Uani 1 1 d . . . . .
C00E C 0.6747(4) 0.3237(3) 0.3029(3) 0.0322(5) Uani 1 1 d . . . . .
H00A H 0.886(4) 0.648(4) 0.052(3) 0.023(6) Uiso 1 1 d . . . . .
H00E H 0.095(5) 1.080(4) 0.272(4) 0.036(7) Uiso 1 1 d . . . . .
H00B H 0.722(5) 0.552(4) 0.007(4) 0.036(7) Uiso 1 1 d . . . . .
H00F H -0.076(5) 0.971(4) 0.236(3) 0.032(7) Uiso 1 1 d . . . . .
H00C H 1.106(5) 0.480(5) 0.304(4) 0.043(8) Uiso 1 1 d . . . . .
H00D H 0.608(5) 0.117(5) 0.494(4) 0.046(8) Uiso 1 1 d . . . . .
H00H H 0.545(5) 0.336(4) 0.235(4) 0.037(7) Uiso 1 1 d . . . . .
H00G H 1.174(6) 0.263(5) 0.552(4) 0.058(10) Uiso 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
N001 N002 1.333(3) . ?
N001 C006 1.337(3) . ?
N002 C005 1.337(3) . ?
N003 N004 1.332(3) . ?
N003 C006 1.343(3) . ?
N004 C005 1.343(3) . ?
C005 C009 1.503(3) . ?
C006 C00C 1.500(3) . ?
C007 C009 1.518(3) . ?
C007 C00A 1.391(3) . ?
C007 C00E 1.398(3) . ?
C008 C00B 1.393(3) . ?
C008 C00C 1.533(3) 2_666 ?
C008 C00D 1.382(3) . ?
C00A C00D 1.398(3) . ?
C00B C00E 1.387(3) . ?

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
N002 N001 C006 117.4(2) . . ?
N001 N002 C005 117.79(19) . . ?
N004 N003 C006 117.80(19) . . ?
N003 N004 C005 117.2(2) . . ?
N002 C005 N004 123.8(2) . . ?
N002 C005 C009 118.7(2) . . ?
N004 C005 C009 117.5(2) . . ?
N001 C006 N003 123.6(2) . . ?
N001 C006 C00C 118.6(2) . . ?
N003 C006 C00C 117.8(2) . . ?
C00A C007 C009 120.8(2) . . ?
C00A C007 C00E 119.0(2) . . ?
C00E C007 C009 120.1(2) . . ?
C00B C008 C00C 120.1(2) . 2_666 ?
C00D C008 C00B 119.3(2) . . ?
C00D C008 C00C 120.5(2) . 2_666 ?
C005 C009 C007 107.24(17) . . ?
C007 C00A C00D 120.1(2) . . ?
C00E C00B C008 120.2(2) . . ?
C006 C00C C008 107.32(18) . 2_666 ?
C008 C00D C00A 120.7(2) . . ?
C00B C00E C007 120.7(2) . . ?

_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 1.743
_oxdiff_exptl_absorpt_empirical_full_min 0.365
####################################################################### 
# 
# 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_tx1466c_tw
_database_code_depnum_ccdc_archive 'CCDC 2233698'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2022-12-31 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_audit_creation_date             2022-08-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H24 N12, 0.25(C H Cl3)'
_chemical_formula_sum            'C30.25 H24.25 Cl0.75 N12'
_chemical_formula_weight         582.45
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHN
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'
Cl Cl 0.3639 0.7018 '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'

_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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   13.5363(2)
_cell_length_b                   10.3837(2)
_cell_length_c                   22.0547(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.2010(10)
_cell_angle_gamma                90
_cell_volume                     3081.80(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7856
_cell_measurement_temperature    169.98(11)
_cell_measurement_theta_max      73.2140
_cell_measurement_theta_min      2.0810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1210
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9424
_diffrn_reflns_point_group_measured_fraction_full 0.781
_diffrn_reflns_point_group_measured_fraction_max 0.738
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.566
_diffrn_reflns_theta_min         2.015
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.98(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -57.00  23.00   0.50    1.15    --  -47.45  47.00  27.00  160
  2  ω    -58.00  23.00   0.50    1.15    --  -47.45  38.00 120.00  162
  3  ω     45.00  78.00   0.50    1.15    --   47.45  47.00  27.00   66
  4  ω     92.00 169.00   0.50    4.62    --  103.25  47.00  27.00  154
  5  ω    123.00 155.00   0.50    4.62    --  103.25  45.00 -60.00   64
  6  ω     73.00 104.00   0.50    4.62    --  103.25 -94.00  30.00   62
  7  ω     39.00  68.00   0.50    4.62    --  103.25 -94.00  30.00   58
  8  ω     32.00  58.00   0.50    4.62    --  103.25 -94.00 -90.00   52
  9  ω     43.00 114.00   0.50    4.62    --  103.25 -47.00-121.00  142
 10  ω     39.00 105.00   0.50    4.62    --  103.25 -94.00-180.00  132
 11  ω    -21.00  39.00   0.50    1.15    --   47.45 -47.00-121.00  120
 12  ω   -101.00 -76.00   0.50    1.15    --  -47.45 -47.00-121.00   50
 13  ω    -62.00 -30.00   0.50    4.62    --  -99.00  45.00-150.00   64
 14  ω   -112.00 -25.00   0.50    4.62    --  -99.00  15.00-150.00  174
 15  ω   -112.00 -86.00   0.50    4.62    --  -99.00  47.00  27.00   52
 16  ω   -116.00 -87.00   0.50    4.62    --  -99.00 -47.00-121.00   58
 17  ω   -110.00 -80.00   0.50    4.62    --  -99.00  45.00-150.00   60
 18  ω   -168.00 -82.00   0.50    4.62    --  -99.00 -61.00-150.00  172
 19  ω   -118.00 -71.00   0.50    1.15    --  -47.45-125.00  30.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0545466000
_diffrn_orient_matrix_UB_12      0.0595403000
_diffrn_orient_matrix_UB_13      -0.0582755000
_diffrn_orient_matrix_UB_21      0.0754211000
_diffrn_orient_matrix_UB_22      -0.0633897000
_diffrn_orient_matrix_UB_23      -0.0382328000
_diffrn_orient_matrix_UB_31      -0.0666818000
_diffrn_orient_matrix_UB_32      -0.1202591000
_diffrn_orient_matrix_UB_33      -0.0086419000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.463
_reflns_Friedel_fraction_full    0.539
_reflns_Friedel_fraction_max     0.496
_reflns_number_gt                6832
_reflns_number_total             9424
_reflns_special_details          
;
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 
;
 Flack x determined using 1855 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.28(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         9424
_refine_ls_number_restraints     274
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.1239
_refine_ls_restrained_S_all      1.064
_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+1.7000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3253
_refine_ls_wR_factor_ref         0.3496
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.336(5)
 0.664(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 Cl3-C8 \\sim Cl7-C8 \\sim Cl4-C8
 with sigma of 0.02
 C3-Cl0A \\sim C3-Cl1 \\sim C3-Cl2
 with sigma of 0.02
 Cl7-Cl3 \\sim Cl4-Cl7 \\sim Cl3-Cl4
 with sigma of 0.02
4. Rigid bond restraints
 C01H, N01V, N02G, N01Y, N02H, C01M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C01Z, N01U, N01C, C01X, N02E, N02D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl3, C8, Cl7, Cl4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, C3, Cl0A, Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C01Z, C01X, N02E, N02D, N01U, N01C, C02A, C02B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C01H \\sim N01V \\sim N02G \\sim N01Y \\sim N02H \\sim C01M: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C01Z \\sim N01U \\sim N01C \\sim C01X \\sim N02E \\sim N02D: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C3 \\sim Cl2 \\sim Cl0A \\sim Cl1: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Cl3 \\sim C8 \\sim Cl7 \\sim Cl4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C01Z \\sim C01X \\sim N02E \\sim N02D \\sim N01U \\sim N01C \\sim C02A \\sim
C02B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
Uanis(C8) \\sim Ueq, Uanis(C017) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N02G) \\sim Ueq, Uanis(C01H) \\sim Ueq, Uanis(N01V) \\sim Ueq,
Uanis(N01Y) \\sim Ueq, Uanis(C01M) \\sim Ueq, Uanis(N02H) \\sim Ueq,
Uanis(N01C) \\sim Ueq, Uanis(C01S) \\sim Ueq, Uanis(N02H) \\sim Ueq,
Uanis(N02G) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01Z) \\sim Ueq, Uanis(C01X) \\sim Ueq, Uanis(N02E) \\sim Ueq,
Uanis(N02D) \\sim Ueq, Uanis(N01U) \\sim Ueq, Uanis(N01C) \\sim Ueq,
Uanis(C02A) \\sim Ueq, Uanis(C02B) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.014
6. Others
 Fixed Sof: Cl3(0.25) Cl4(0.25) Cl7(0.25) C8(0.25) H8(0.25) Cl1(0.25)
 Cl0A(0.25) Cl2(0.25) C3(0.25) H3(0.25)
7.a Ternary CH refined with riding coordinates:
 C8(H8), C3(H3)
7.b Secondary CH2 refined with riding coordinates:
 C00Z(H00A,H00B), C012(H01I,H01J), C017(H01A,H01B), C01A(H01K,H01L), C01D(H01C,
 H01D), C01E(H01E,H01F), C01I(H01S,H01T), C01S(H01G,H01H), C023(H02E,H02F),
 C02A(H02A,H02B), C02B(H02C,H02D), C02C(H02G,H02H)
7.c Aromatic/amide H refined with riding coordinates:
 C00X(H00X), C014(H014), C022(H022), C020(H020), C018(H018), C010(H010),
 C026(H026), C028(H028), C01F(H01M), C01K(H01N), C01B(H01P), C01L(H01R),
 C01Q(H01Q), C01O(H01O), C024(H024), C025(H025), C01W(H01W), C013(H013),
 C01R(H01U), C011(H011), C027(H027), C015(H015), C01J(H01V), C029(H029)
7.d Fitted hexagon refined as free rotating group:
 C00X(C014,C019,C022,C020,C00V), C00Y(C018,C010,C00M,C026,C028), C01F(C01K,
 C016,C01B,C01L,C00L), C01H(N01V,N01Y,C01M,N02H,N02G), C01Q(C01O,C00I,C024,C025,
 C00T), C01W(C013,C01N,C01R,C011,C00S), C027(C00O,C015,C01J,C00Q,C029)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
N001 N -0.0016(5) 1.1271(9) 0.3913(4) 0.0639(19) Uani 1 1 d . . . . .
N002 N 0.3750(7) 0.8033(12) 0.0594(5) 0.088(3) Uani 1 1 d . . . . .
N003 N 0.5261(6) 1.2218(11) 0.1882(4) 0.074(2) Uani 1 1 d . . . . .
N004 N 0.5868(6) 1.1227(9) 0.1941(3) 0.065(2) Uani 1 1 d . . . . .
N005 N 0.0217(6) 1.2159(10) 0.3528(4) 0.068(2) Uani 1 1 d . . . . .
N006 N 0.1189(7) 1.3208(12) 0.4314(6) 0.088(3) Uani 1 1 d . . . . .
N007 N 0.5023(6) 0.6205(11) 0.0955(5) 0.085(3) Uani 1 1 d . . . . .
N008 N 0.6014(9) 1.3009(12) 0.2839(5) 0.094(3) Uani 1 1 d . . . . .
N009 N 0.0974(6) 1.2333(15) 0.4691(5) 0.099(4) Uani 1 1 d . . . . .
N00A N -0.1031(8) 0.6288(11) 0.2996(4) 0.085(3) Uani 1 1 d . . . . .
N00B N 0.3896(8) 0.7162(13) 0.0206(5) 0.095(3) Uani 1 1 d . . . . .
N00C N 0.4846(7) 0.7098(13) 0.1365(5) 0.090(3) Uani 1 1 d . . . . .
N00D N -0.0833(10) 0.8199(12) 0.2216(6) 0.101(4) Uani 1 1 d . . . . .
N00E N -0.0311(9) 0.7097(12) 0.3112(5) 0.090(3) Uani 1 1 d . . . . .
N00F N 0.6623(6) 1.2024(13) 0.2864(4) 0.084(3) Uani 1 1 d . . . . .
N00G N -0.1591(7) 0.7388(13) 0.2095(5) 0.094(4) Uani 1 1 d . . . . .
C00H C 0.5369(8) 1.3097(12) 0.2323(6) 0.080(3) Uani 1 1 d . . . . .
C00J C 0.6552(6) 1.1193(11) 0.2424(4) 0.063(2) Uani 1 1 d . . . . .
C00K C 0.0357(6) 1.1440(13) 0.4475(5) 0.076(3) Uani 1 1 d . . . . .
C00N C -0.0255(11) 0.8039(14) 0.2736(6) 0.088(4) Uani 1 1 d . . . . .
C00P C -0.1689(7) 0.6441(12) 0.2509(5) 0.078(3) Uani 1 1 d . . . . .
C00R C 0.0778(6) 1.3142(12) 0.3728(6) 0.074(3) Uani 1 1 d . . . . .
C00U C 0.4219(8) 0.8016(15) 0.1161(7) 0.091(4) Uani 1 1 d . . . . .
C00W C 0.4560(8) 0.6313(15) 0.0387(7) 0.094(4) Uani 1 1 d . . . . .
C00X C 0.1359(5) 0.9331(7) 0.5656(3) 0.074(3) Uani 1 1 d G . . . .
H00X H 0.121070 0.991047 0.595506 0.089 Uiso 1 1 calc R U . . .
C014 C 0.2084(5) 0.8396(8) 0.5793(3) 0.076(3) Uani 1 1 d G . . . .
H014 H 0.242157 0.835105 0.618237 0.092 Uiso 1 1 calc R U . . .
C019 C 0.2306(6) 0.7530(7) 0.5346(4) 0.110(5) Uani 1 1 d G . . . .
C022 C 0.1801(8) 0.7598(9) 0.4764(4) 0.121(6) Uani 1 1 d G . . . .
H022 H 0.194954 0.701828 0.446496 0.145 Uiso 1 1 calc R U . . .
C020 C 0.1076(7) 0.8532(10) 0.4627(3) 0.117(5) Uani 1 1 d G . . . .
H020 H 0.073867 0.857769 0.423765 0.140 Uiso 1 1 calc R U . . .
C00V C 0.0855(5) 0.9399(8) 0.5074(3) 0.078(3) Uani 1 1 d G . . . .
C00Y C 0.6788(5) 0.7475(7) 0.3908(3) 0.085(4) Uani 1 1 d G . . . .
C018 C 0.7587(5) 0.8323(8) 0.3974(2) 0.074(3) Uani 1 1 d G . . . .
H018 H 0.801803 0.832316 0.433265 0.088 Uiso 1 1 calc R U . . .
C010 C 0.7742(4) 0.9169(7) 0.3506(3) 0.072(3) Uani 1 1 d G . . . .
H010 H 0.827694 0.973562 0.355022 0.086 Uiso 1 1 calc R U . . .
C00M C 0.7098(5) 0.9168(8) 0.2970(3) 0.074(3) Uani 1 1 d G . . . .
C026 C 0.6298(6) 0.8321(10) 0.2904(3) 0.136(7) Uani 1 1 d G . . . .
H026 H 0.586733 0.831997 0.254564 0.163 Uiso 1 1 calc R U . . .
C028 C 0.6143(5) 0.7474(9) 0.3373(4) 0.119(5) Uani 1 1 d G . . . .
H028 H 0.560841 0.690750 0.332807 0.142 Uiso 1 1 calc R U . . .
C00Z C -0.2498(9) 0.5523(15) 0.2369(7) 0.097(4) Uani 1 1 d . . . . .
H00A H -0.304253 0.595821 0.213062 0.117 Uiso 1 1 calc R U . . .
H00B H -0.273428 0.524901 0.274833 0.117 Uiso 1 1 calc R U . . .
C012 C 0.4780(10) 0.5252(17) -0.0087(7) 0.107(5) Uani 1 1 d . . . . .
H01I H 0.471961 0.562044 -0.049368 0.128 Uiso 1 1 calc R U . . .
H01J H 0.545475 0.493922 0.000605 0.128 Uiso 1 1 calc R U . . .
C017 C 0.0976(9) 1.4183(14) 0.3308(7) 0.101(4) Uani 1 1 d . U . . .
H01A H 0.093704 1.499819 0.351944 0.121 Uiso 1 1 calc R U . . .
H01B H 0.045796 1.417969 0.296859 0.121 Uiso 1 1 calc R U . . .
C01A C 0.4045(10) 0.9074(16) 0.1609(9) 0.122(6) Uani 1 1 d . . . . .
H01K H 0.459300 0.906734 0.193125 0.146 Uiso 1 1 calc R U . . .
H01L H 0.406244 0.989391 0.139990 0.146 Uiso 1 1 calc R U . . .
N01C N 0.4108(10) 0.5911(17) 0.4732(7) 0.138(4) Uani 1 1 d . U . . .
C01D C 0.0064(9) 1.044(2) 0.4946(7) 0.116(6) Uani 1 1 d . . . . .
H01C H -0.003380 1.087205 0.532394 0.140 Uiso 1 1 calc R U . . .
H01D H -0.056040 1.003466 0.479179 0.140 Uiso 1 1 calc R U . . .
C01E C 0.7255(9) 1.0112(17) 0.2470(6) 0.107(5) Uani 1 1 d . . . . .
H01E H 0.792514 1.045151 0.254109 0.129 Uiso 1 1 calc R U . . .
H01F H 0.719778 0.965708 0.208385 0.129 Uiso 1 1 calc R U . . .
C01F C -0.1489(4) 0.3520(7) 0.2296(2) 0.074(3) Uani 1 1 d G . . . .
H01M H -0.120197 0.368856 0.268997 0.089 Uiso 1 1 calc R U . . .
C01K C -0.1185(4) 0.2456(7) 0.1981(3) 0.075(3) Uani 1 1 d G . . . .
H01N H -0.069460 0.191295 0.216518 0.091 Uiso 1 1 calc R U . . .
C016 C -0.1614(6) 0.2204(8) 0.1392(3) 0.090(4) Uani 1 1 d G . . . .
C01B C -0.2347(6) 0.3015(10) 0.1117(2) 0.116(6) Uani 1 1 d G . . . .
H01P H -0.263377 0.284644 0.072267 0.139 Uiso 1 1 calc R U . . .
C01L C -0.2651(5) 0.4079(9) 0.1431(3) 0.110(6) Uani 1 1 d G . . . .
H01R H -0.314116 0.462206 0.124744 0.132 Uiso 1 1 calc R U . . .
C00L C -0.2222(4) 0.4331(6) 0.2021(3) 0.070(3) Uani 1 1 d G . . . .
C01H C -0.0403(6) 0.0986(11) 0.0828(5) 0.107(4) Uani 1 1 d G U . . .
N01V N 0.0326(6) 0.1917(9) 0.0964(3) 0.117(4) Uani 1 1 d G U . . .
N01Y N 0.1196(5) 0.1880(10) 0.0683(4) 0.117(4) Uani 1 1 d G U . . .
C01M C 0.1339(6) 0.0913(12) 0.0266(5) 0.118(4) Uani 1 1 d G U . . .
N02H N 0.0610(9) -0.0017(10) 0.0129(5) 0.179(6) Uani 1 1 d G U . . .
N02G N -0.0260(8) 0.0019(10) 0.0410(5) 0.181(6) Uani 1 1 d G U . . .
C01I C 0.0537(14) 0.9077(17) 0.2878(8) 0.130(6) Uani 1 1 d . . . . .
H01S H 0.023198 0.991363 0.279777 0.156 Uiso 1 1 calc R U . . .
H01T H 0.077054 0.903915 0.330893 0.156 Uiso 1 1 calc R U . . .
C01Q C 0.2911(7) 1.3739(8) 0.2205(2) 0.111(5) Uani 1 1 d G . . . .
H01Q H 0.293641 1.347383 0.180401 0.134 Uiso 1 1 calc R U . . .
C01O C 0.2015(5) 1.3710(8) 0.2459(4) 0.105(4) Uani 1 1 d G . . . .
H01O H 0.144099 1.342643 0.222781 0.126 Uiso 1 1 calc R U . . .
C00I C 0.1977(4) 1.4106(8) 0.3058(4) 0.074(3) Uani 1 1 d G . . . .
C024 C 0.2836(5) 1.4530(8) 0.3403(3) 0.085(3) Uani 1 1 d G . . . .
H024 H 0.281042 1.479445 0.380407 0.102 Uiso 1 1 calc R U . . .
C025 C 0.3732(4) 1.4558(8) 0.3149(3) 0.084(3) Uani 1 1 d G . . . .
H025 H 0.430584 1.484186 0.338028 0.100 Uiso 1 1 calc R U . . .
C00T C 0.3769(5) 1.4163(8) 0.2550(3) 0.080(3) Uani 1 1 d G . . . .
C01S C 0.4733(12) 1.4272(16) 0.2259(8) 0.119(5) Uani 1 1 d . U . . .
H01G H 0.457561 1.445947 0.182882 0.142 Uiso 1 1 calc R U . . .
H01H H 0.511060 1.499424 0.244218 0.142 Uiso 1 1 calc R U . . .
N01U N 0.4966(10) 0.5952(16) 0.4475(6) 0.129(4) Uani 1 1 d . U . . .
C01W C 0.4083(5) 0.3403(8) 0.0445(3) 0.093(4) Uani 1 1 d G . . . .
H01W H 0.451453 0.357964 0.079213 0.112 Uiso 1 1 calc R U . . .
C013 C 0.3441(6) 0.2358(8) 0.0437(3) 0.096(4) Uani 1 1 d G . . . .
H013 H 0.344182 0.183501 0.077973 0.115 Uiso 1 1 calc R U . . .
C01N C 0.2797(5) 0.2093(8) -0.0082(4) 0.090(4) Uani 1 1 d G . . . .
C01R C 0.2795(5) 0.2874(9) -0.0594(3) 0.110(6) Uani 1 1 d G . . . .
H01U H 0.236395 0.269757 -0.094163 0.132 Uiso 1 1 calc R U . . .
C011 C 0.3438(6) 0.3920(8) -0.0587(2) 0.090(4) Uani 1 1 d G . . . .
H011 H 0.343665 0.444219 -0.092925 0.108 Uiso 1 1 calc R U . . .
C00S C 0.4082(5) 0.4184(7) -0.0067(3) 0.077(3) Uani 1 1 d G . . . .
C01X C 0.4001(10) 0.6637(14) 0.5172(5) 0.089(3) Uani 1 1 d . U . . .
C01Z C 0.5677(9) 0.6691(14) 0.4681(6) 0.091(3) Uani 1 1 d . U . . .
C023 C -0.1320(10) 0.0993(16) 0.1076(6) 0.108(5) Uani 1 1 d . . . . .
H02E H -0.131223 0.029020 0.136648 0.130 Uiso 1 1 calc R U . . .
H02F H -0.183762 0.080402 0.074886 0.130 Uiso 1 1 calc R U . . .
C027 C 0.2904(6) 0.7936(7) 0.2247(4) 0.103(4) Uani 1 1 d G . . . .
H027 H 0.333450 0.723541 0.227293 0.124 Uiso 1 1 calc R U . . .
C00O C 0.3100(5) 0.8998(9) 0.1895(4) 0.084(3) Uani 1 1 d G . . . .
C015 C 0.2456(7) 1.0046(7) 0.1855(3) 0.090(3) Uani 1 1 d G . . . .
H015 H 0.258707 1.075633 0.162032 0.108 Uiso 1 1 calc R U . . .
C01J C 0.1617(6) 1.0031(7) 0.2168(4) 0.101(4) Uani 1 1 d G . . . .
H01V H 0.118688 1.073122 0.214107 0.121 Uiso 1 1 calc R U . . .
C00Q C 0.1422(6) 0.8968(9) 0.2519(4) 0.089(4) Uani 1 1 d G . . . .
C029 C 0.2065(7) 0.7921(7) 0.2559(4) 0.127(6) Uani 1 1 d G . . . .
H029 H 0.193428 0.721030 0.279369 0.152 Uiso 1 1 calc R U . . .
C02A C 0.3054(11) 0.6467(16) 0.5462(7) 0.115(4) Uani 1 1 d . U . . .
H02A H 0.274559 0.566593 0.531662 0.139 Uiso 1 1 calc R U . . .
H02B H 0.322140 0.638467 0.589962 0.139 Uiso 1 1 calc R U . . .
C02B C 0.6641(10) 0.6536(17) 0.4419(7) 0.117(4) Uani 1 1 d . U . . .
H02C H 0.667997 0.566470 0.426411 0.140 Uiso 1 1 calc R U . . .
H02D H 0.717913 0.664568 0.474219 0.140 Uiso 1 1 calc R U . . .
C02C C 0.2127(11) 0.0924(17) -0.0111(8) 0.128(6) Uani 1 1 d . . . . .
H02G H 0.183849 0.082021 -0.053052 0.154 Uiso 1 1 calc R U . . .
H02H H 0.253915 0.017439 -0.000877 0.154 Uiso 1 1 calc R U . . .
N02D N 0.5540(10) 0.7581(17) 0.5123(6) 0.136(4) Uani 1 1 d . U . . .
N02E N 0.4651(11) 0.7513(18) 0.5397(7) 0.140(4) Uani 1 1 d . U . . .
Cl3 Cl 0.2738(13) 1.0786(16) 0.3850(9) 0.144(6) Uani 0.25 1 d D U P . .
Cl4 Cl 0.4357(18) 1.0656(19) 0.3263(8) 0.169(8) Uani 0.25 1 d D U P . .
Cl7 Cl 0.3803(19) 0.865(3) 0.3867(16) 0.231(15) Uani 0.25 1 d D U P . .
C8 C 0.365(2) 1.005(2) 0.3671(15) 0.101(8) Uani 0.25 1 d D U P . .
H8 H 0.405223 1.035096 0.403785 0.121 Uiso 0.25 1 calc R U P . .
Cl1 Cl -0.0162(7) 0.0315(18) -0.1393(7) 0.115(5) Uani 0.25 1 d D U P . .
Cl0A Cl -0.0709(14) 0.2484(15) -0.0737(8) 0.136(5) Uani 0.25 1 d D U P . .
Cl2 Cl -0.1924(8) 0.0347(18) -0.0777(5) 0.111(5) Uani 0.25 1 d D U P . .
C3 C -0.1063(15) 0.116(2) -0.1112(11) 0.094(7) Uani 0.25 1 d D U P . .
H3 H -0.144421 0.149157 -0.148100 0.112 Uiso 0.25 1 calc R U 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
N001 N005 1.314(12) . ?
N001 C00K 1.299(14) . ?
N002 N00B 1.276(16) . ?
N002 C00U 1.339(18) . ?
N003 N004 1.315(13) . ?
N003 C00H 1.331(17) . ?
N004 C00J 1.334(12) . ?
N005 C00R 1.319(15) . ?
N006 N009 1.285(17) . ?
N006 C00R 1.353(16) . ?
N007 N00C 1.333(16) . ?
N007 C00W 1.344(17) . ?
N008 N00F 1.312(16) . ?
N008 C00H 1.360(18) . ?
N009 C00K 1.303(17) . ?
N00A N00E 1.290(15) . ?
N00A C00P 1.329(15) . ?
N00B C00W 1.292(17) . ?
N00C C00U 1.322(18) . ?
N00D N00G 1.332(17) . ?
N00D C00N 1.327(19) . ?
N00E C00N 1.290(18) . ?
N00F C00J 1.295(14) . ?
N00G C00P 1.358(13) . ?
C00H C01S 1.491(19) . ?
C00J C01E 1.467(16) . ?
C00K C01D 1.554(18) . ?
C00N C01I 1.53(2) . ?
C00P C00Z 1.460(19) . ?
C00R C017 1.466(17) . ?
C00U C01A 1.51(2) . ?
C00W C012 1.57(2) . ?
C00X H00X 0.9300 . ?
C00X C014 1.3900 . ?
C00X C00V 1.3900 . ?
C014 H014 0.9300 . ?
C014 C019 1.3900 . ?
C019 C022 1.3900 . ?
C019 C02A 1.501(15) . ?
C022 H022 0.9300 . ?
C022 C020 1.3900 . ?
C020 H020 0.9300 . ?
C020 C00V 1.3900 . ?
C00V C01D 1.523(15) . ?
C00Y C018 1.3900 . ?
C00Y C028 1.3900 . ?
C00Y C02B 1.520(14) . ?
C018 H018 0.9300 . ?
C018 C010 1.3900 . ?
C010 H010 0.9300 . ?
C010 C00M 1.3900 . ?
C00M C026 1.3900 . ?
C00M C01E 1.508(13) . ?
C026 H026 0.9300 . ?
C026 C028 1.3900 . ?
C028 H028 0.9300 . ?
C00Z H00A 0.9700 . ?
C00Z H00B 0.9700 . ?
C00Z C00L 1.524(17) . ?
C012 H01I 0.9700 . ?
C012 H01J 0.9700 . ?
C012 C00S 1.461(16) . ?
C017 H01A 0.9700 . ?
C017 H01B 0.9700 . ?
C017 C00I 1.520(11) . ?
C01A H01K 0.9700 . ?
C01A H01L 0.9700 . ?
C01A C00O 1.489(13) . ?
N01C N01U 1.346(15) . ?
N01C C01X 1.250(19) . ?
C01D H01C 0.9700 . ?
C01D H01D 0.9700 . ?
C01E H01E 0.9700 . ?
C01E H01F 0.9700 . ?
C01F H01M 0.9300 . ?
C01F C01K 1.3900 . ?
C01F C00L 1.3900 . ?
C01K H01N 0.9300 . ?
C01K C016 1.3900 . ?
C016 C01B 1.3900 . ?
C016 C023 1.512(17) . ?
C01B H01P 0.9300 . ?
C01B C01L 1.3900 . ?
C01L H01R 0.9300 . ?
C01L C00L 1.3900 . ?
C01H N01V 1.3900 . ?
C01H N02G 1.3900 . ?
C01H C023 1.410(13) . ?
N01V N01Y 1.3900 . ?
N01Y C01M 1.3900 . ?
C01M N02H 1.3900 . ?
C01M C02C 1.422(13) . ?
N02H N02G 1.3900 . ?
C01I H01S 0.9700 . ?
C01I H01T 0.9700 . ?
C01I C00Q 1.509(13) . ?
C01Q H01Q 0.9300 . ?
C01Q C01O 1.3900 . ?
C01Q C00T 1.3900 . ?
C01O H01O 0.9300 . ?
C01O C00I 1.3900 . ?
C00I C024 1.3900 . ?
C024 H024 0.9300 . ?
C024 C025 1.3900 . ?
C025 H025 0.9300 . ?
C025 C00T 1.3900 . ?
C00T C01S 1.519(12) . ?
C01S H01G 0.9700 . ?
C01S H01H 0.9700 . ?
N01U C01Z 1.275(19) . ?
C01W H01W 0.9300 . ?
C01W C013 1.3900 . ?
C01W C00S 1.3900 . ?
C013 H013 0.9300 . ?
C013 C01N 1.3900 . ?
C01N C01R 1.3900 . ?
C01N C02C 1.513(16) . ?
C01R H01U 0.9300 . ?
C01R C011 1.3900 . ?
C011 H011 0.9300 . ?
C011 C00S 1.3900 . ?
C01X C02A 1.504(16) . ?
C01X N02E 1.32(2) . ?
C01Z C02B 1.492(17) . ?
C01Z N02D 1.369(19) . ?
C023 H02E 0.9700 . ?
C023 H02F 0.9700 . ?
C027 H027 0.9300 . ?
C027 C00O 1.3900 . ?
C027 C029 1.3900 . ?
C00O C015 1.3900 . ?
C015 H015 0.9300 . ?
C015 C01J 1.3900 . ?
C01J H01V 0.9300 . ?
C01J C00Q 1.3900 . ?
C00Q C029 1.3900 . ?
C029 H029 0.9300 . ?
C02A H02A 0.9700 . ?
C02A H02B 0.9700 . ?
C02B H02C 0.9700 . ?
C02B H02D 0.9700 . ?
C02C H02G 0.9700 . ?
C02C H02H 0.9700 . ?
N02D N02E 1.405(17) . ?
Cl3 C8 1.536(19) . ?
Cl4 C8 1.523(19) . ?
Cl7 C8 1.529(19) . ?
C8 H8 0.9800 . ?
Cl1 C3 1.673(17) . ?
Cl0A C3 1.652(17) . ?
Cl2 C3 1.671(18) . ?
C3 H3 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
C00K N001 N005 115.2(10) . . ?
N00B N002 C00U 121.7(12) . . ?
N004 N003 C00H 116.6(9) . . ?
N003 N004 C00J 118.1(9) . . ?
N001 N005 C00R 119.8(9) . . ?
N009 N006 C00R 119.0(11) . . ?
N00C N007 C00W 118.3(11) . . ?
N00F N008 C00H 115.5(10) . . ?
N006 N009 C00K 116.6(10) . . ?
N00E N00A C00P 120.5(11) . . ?
N002 N00B C00W 115.4(12) . . ?
C00U N00C N007 115.2(11) . . ?
C00N N00D N00G 117.7(11) . . ?
C00N N00E N00A 117.5(12) . . ?
C00J N00F N008 119.6(10) . . ?
N00D N00G C00P 116.8(10) . . ?
N003 C00H N008 125.1(12) . . ?
N003 C00H C01S 118.4(13) . . ?
N008 C00H C01S 116.5(14) . . ?
N004 C00J C01E 117.7(11) . . ?
N00F C00J N004 124.7(10) . . ?
N00F C00J C01E 117.5(11) . . ?
N001 C00K N009 127.8(11) . . ?
N001 C00K C01D 116.5(13) . . ?
N009 C00K C01D 115.7(12) . . ?
N00D C00N C01I 115.1(15) . . ?
N00E C00N N00D 125.4(15) . . ?
N00E C00N C01I 119.5(15) . . ?
N00A C00P N00G 121.6(12) . . ?
N00A C00P C00Z 121.0(10) . . ?
N00G C00P C00Z 117.1(11) . . ?
N005 C00R N006 121.3(11) . . ?
N005 C00R C017 119.9(12) . . ?
N006 C00R C017 118.7(13) . . ?
N002 C00U C01A 120.5(15) . . ?
N00C C00U N002 123.3(15) . . ?
N00C C00U C01A 116.1(15) . . ?
N007 C00W C012 117.4(13) . . ?
N00B C00W N007 125.8(15) . . ?
N00B C00W C012 116.6(13) . . ?
C014 C00X H00X 120.0 . . ?
C014 C00X C00V 120.0 . . ?
C00V C00X H00X 120.0 . . ?
C00X C014 H014 120.0 . . ?
C019 C014 C00X 120.0 . . ?
C019 C014 H014 120.0 . . ?
C014 C019 C02A 123.2(9) . . ?
C022 C019 C014 120.0 . . ?
C022 C019 C02A 116.7(9) . . ?
C019 C022 H022 120.0 . . ?
C020 C022 C019 120.0 . . ?
C020 C022 H022 120.0 . . ?
C022 C020 H020 120.0 . . ?
C022 C020 C00V 120.0 . . ?
C00V C020 H020 120.0 . . ?
C00X C00V C01D 118.2(9) . . ?
C020 C00V C00X 120.0 . . ?
C020 C00V C01D 121.8(9) . . ?
C018 C00Y C028 120.0 . . ?
C018 C00Y C02B 119.4(8) . . ?
C028 C00Y C02B 120.6(8) . . ?
C00Y C018 H018 120.0 . . ?
C00Y C018 C010 120.0 . . ?
C010 C018 H018 120.0 . . ?
C018 C010 H010 120.0 . . ?
C00M C010 C018 120.0 . . ?
C00M C010 H010 120.0 . . ?
C010 C00M C026 120.0 . . ?
C010 C00M C01E 119.7(8) . . ?
C026 C00M C01E 120.3(8) . . ?
C00M C026 H026 120.0 . . ?
C028 C026 C00M 120.0 . . ?
C028 C026 H026 120.0 . . ?
C00Y C028 H028 120.0 . . ?
C026 C028 C00Y 120.0 . . ?
C026 C028 H028 120.0 . . ?
C00P C00Z H00A 108.6 . . ?
C00P C00Z H00B 108.6 . . ?
C00P C00Z C00L 114.7(8) . . ?
H00A C00Z H00B 107.6 . . ?
C00L C00Z H00A 108.6 . . ?
C00L C00Z H00B 108.6 . . ?
C00W C012 H01I 109.7 . . ?
C00W C012 H01J 109.7 . . ?
H01I C012 H01J 108.2 . . ?
C00S C012 C00W 110.0(8) . . ?
C00S C012 H01I 109.7 . . ?
C00S C012 H01J 109.7 . . ?
C00R C017 H01A 108.5 . . ?
C00R C017 H01B 108.5 . . ?
C00R C017 C00I 114.9(9) . . ?
H01A C017 H01B 107.5 . . ?
C00I C017 H01A 108.5 . . ?
C00I C017 H01B 108.5 . . ?
C00U C01A H01K 108.3 . . ?
C00U C01A H01L 108.3 . . ?
H01K C01A H01L 107.4 . . ?
C00O C01A C00U 116.1(10) . . ?
C00O C01A H01K 108.3 . . ?
C00O C01A H01L 108.3 . . ?
C01X N01C N01U 119.0(15) . . ?
C00K C01D H01C 109.2 . . ?
C00K C01D H01D 109.2 . . ?
C00V C01D C00K 111.9(8) . . ?
C00V C01D H01C 109.2 . . ?
C00V C01D H01D 109.2 . . ?
H01C C01D H01D 107.9 . . ?
C00J C01E C00M 114.0(8) . . ?
C00J C01E H01E 108.8 . . ?
C00J C01E H01F 108.8 . . ?
C00M C01E H01E 108.8 . . ?
C00M C01E H01F 108.8 . . ?
H01E C01E H01F 107.6 . . ?
C01K C01F H01M 120.0 . . ?
C01K C01F C00L 120.0 . . ?
C00L C01F H01M 120.0 . . ?
C01F C01K H01N 120.0 . . ?
C016 C01K C01F 120.0 . . ?
C016 C01K H01N 120.0 . . ?
C01K C016 C01B 120.0 . . ?
C01K C016 C023 118.9(8) . . ?
C01B C016 C023 121.0(8) . . ?
C016 C01B H01P 120.0 . . ?
C016 C01B C01L 120.0 . . ?
C01L C01B H01P 120.0 . . ?
C01B C01L H01R 120.0 . . ?
C00L C01L C01B 120.0 . . ?
C00L C01L H01R 120.0 . . ?
C01F C00L C00Z 118.3(7) . . ?
C01L C00L C00Z 121.6(7) . . ?
C01L C00L C01F 120.0 . . ?
N01V C01H N02G 120.0 . . ?
N01V C01H C023 123.1(9) . . ?
N02G C01H C023 116.8(9) . . ?
N01Y N01V C01H 120.0 . . ?
N01V N01Y C01M 120.0 . . ?
N01Y C01M C02C 123.2(9) . . ?
N02H C01M N01Y 120.0 . . ?
N02H C01M C02C 116.0(8) . . ?
C01M N02H N02G 120.0 . . ?
N02H N02G C01H 120.0 . . ?
C00N C01I H01S 108.6 . . ?
C00N C01I H01T 108.6 . . ?
H01S C01I H01T 107.6 . . ?
C00Q C01I C00N 114.7(10) . . ?
C00Q C01I H01S 108.6 . . ?
C00Q C01I H01T 108.6 . . ?
C01O C01Q H01Q 120.0 . . ?
C01O C01Q C00T 120.0 . . ?
C00T C01Q H01Q 120.0 . . ?
C01Q C01O H01O 120.0 . . ?
C01Q C01O C00I 120.0 . . ?
C00I C01O H01O 120.0 . . ?
C01O C00I C017 119.1(9) . . ?
C01O C00I C024 120.0 . . ?
C024 C00I C017 120.6(9) . . ?
C00I C024 H024 120.0 . . ?
C025 C024 C00I 120.0 . . ?
C025 C024 H024 120.0 . . ?
C024 C025 H025 120.0 . . ?
C024 C025 C00T 120.0 . . ?
C00T C025 H025 120.0 . . ?
C01Q C00T C01S 119.8(9) . . ?
C025 C00T C01Q 120.0 . . ?
C025 C00T C01S 120.0(10) . . ?
C00H C01S C00T 114.3(10) . . ?
C00H C01S H01G 108.7 . . ?
C00H C01S H01H 108.7 . . ?
C00T C01S H01G 108.7 . . ?
C00T C01S H01H 108.7 . . ?
H01G C01S H01H 107.6 . . ?
C01Z N01U N01C 121.4(14) . . ?
C013 C01W H01W 120.0 . . ?
C013 C01W C00S 120.0 . . ?
C00S C01W H01W 120.0 . . ?
C01W C013 H013 120.0 . . ?
C01W C013 C01N 120.0 . . ?
C01N C013 H013 120.0 . . ?
C013 C01N C02C 120.9(10) . . ?
C01R C01N C013 120.0 . . ?
C01R C01N C02C 119.1(10) . . ?
C01N C01R H01U 120.0 . . ?
C011 C01R C01N 120.0 . . ?
C011 C01R H01U 120.0 . . ?
C01R C011 H011 120.0 . . ?
C01R C011 C00S 120.0 . . ?
C00S C011 H011 120.0 . . ?
C01W C00S C012 121.5(9) . . ?
C011 C00S C012 118.4(9) . . ?
C011 C00S C01W 120.0 . . ?
N01C C01X C02A 115.8(15) . . ?
N01C C01X N02E 125.2(12) . . ?
N02E C01X C02A 118.9(14) . . ?
N01U C01Z C02B 117.0(14) . . ?
N01U C01Z N02D 120.3(12) . . ?
N02D C01Z C02B 122.7(14) . . ?
C016 C023 H02E 107.8 . . ?
C016 C023 H02F 107.8 . . ?
C01H C023 C016 118.0(10) . . ?
C01H C023 H02E 107.8 . . ?
C01H C023 H02F 107.8 . . ?
H02E C023 H02F 107.1 . . ?
C00O C027 H027 120.0 . . ?
C00O C027 C029 120.0 . . ?
C029 C027 H027 120.0 . . ?
C027 C00O C01A 120.1(10) . . ?
C027 C00O C015 120.0 . . ?
C015 C00O C01A 119.6(10) . . ?
C00O C015 H015 120.0 . . ?
C00O C015 C01J 120.0 . . ?
C01J C015 H015 120.0 . . ?
C015 C01J H01V 120.0 . . ?
C00Q C01J C015 120.0 . . ?
C00Q C01J H01V 120.0 . . ?
C01J C00Q C01I 116.3(9) . . ?
C01J C00Q C029 120.0 . . ?
C029 C00Q C01I 123.6(10) . . ?
C027 C029 H029 120.0 . . ?
C00Q C029 C027 120.0 . . ?
C00Q C029 H029 120.0 . . ?
C019 C02A C01X 115.5(11) . . ?
C019 C02A H02A 108.4 . . ?
C019 C02A H02B 108.4 . . ?
C01X C02A H02A 108.4 . . ?
C01X C02A H02B 108.4 . . ?
H02A C02A H02B 107.5 . . ?
C00Y C02B H02C 108.7 . . ?
C00Y C02B H02D 108.7 . . ?
C01Z C02B C00Y 114.1(10) . . ?
C01Z C02B H02C 108.7 . . ?
C01Z C02B H02D 108.7 . . ?
H02C C02B H02D 107.6 . . ?
C01M C02C C01N 117.8(10) . . ?
C01M C02C H02G 107.9 . . ?
C01M C02C H02H 107.9 . . ?
C01N C02C H02G 107.9 . . ?
C01N C02C H02H 107.9 . . ?
H02G C02C H02H 107.2 . . ?
C01Z N02D N02E 117.4(14) . . ?
C01X N02E N02D 116.0(14) . . ?
Cl3 C8 H8 91.2 . . ?
Cl4 C8 Cl3 121.4(14) . . ?
Cl4 C8 Cl7 119.0(13) . . ?
Cl4 C8 H8 91.2 . . ?
Cl7 C8 Cl3 119.5(13) . . ?
Cl7 C8 H8 91.2 . . ?
Cl1 C3 H3 102.5 . . ?
Cl0A C3 Cl1 115.9(14) . . ?
Cl0A C3 Cl2 112.1(14) . . ?
Cl0A C3 H3 102.5 . . ?
Cl2 C3 Cl1 118.2(15) . . ?
Cl2 C3 H3 102.5 . . ?

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
N001 N005 C00R N006 5.3(14) . . . . ?
N001 N005 C00R C017 -175.3(9) . . . . ?
N001 C00K C01D C00V 97.5(14) . . . . ?
N002 N00B C00W N007 6.8(19) . . . . ?
N002 N00B C00W C012 -178.2(10) . . . . ?
N002 C00U C01A C00O 77.2(19) . . . . ?
N003 N004 C00J N00F 4.9(14) . . . . ?
N003 N004 C00J C01E -177.3(9) . . . . ?
N003 C00H C01S C00T 92.2(15) . . . . ?
N004 N003 C00H N008 -3.8(14) . . . . ?
N004 N003 C00H C01S 176.8(8) . . . . ?
N004 C00J C01E C00M -109.6(13) . . . . ?
N005 N001 C00K N009 -4.4(15) . . . . ?
N005 N001 C00K C01D 177.7(9) . . . . ?
N005 C00R C017 C00I -99.7(13) . . . . ?
N006 N009 C00K N001 5.3(17) . . . . ?
N006 N009 C00K C01D -176.8(10) . . . . ?
N006 C00R C017 C00I 79.7(15) . . . . ?
N007 N00C C00U N002 3.2(15) . . . . ?
N007 N00C C00U C01A -177.2(9) . . . . ?
N007 C00W C012 C00S 89.3(14) . . . . ?
N008 N00F C00J N004 -2.5(16) . . . . ?
N008 N00F C00J C01E 179.6(10) . . . . ?
N008 C00H C01S C00T -87.3(16) . . . . ?
N009 N006 C00R N005 -4.4(16) . . . . ?
N009 N006 C00R C017 176.3(10) . . . . ?
N009 C00K C01D C00V -80.7(17) . . . . ?
N00A N00E C00N N00D -5.0(17) . . . . ?
N00A N00E C00N C01I 175.5(10) . . . . ?
N00A C00P C00Z C00L -83.8(13) . . . . ?
N00B N002 C00U N00C -1.5(18) . . . . ?
N00B N002 C00U C01A 178.9(10) . . . . ?
N00B C00W C012 C00S -86.1(15) . . . . ?
N00C N007 C00W N00B -5.1(18) . . . . ?
N00C N007 C00W C012 179.9(9) . . . . ?
N00C C00U C01A C00O -102.4(15) . . . . ?
N00D N00G C00P N00A -3.5(16) . . . . ?
N00D N00G C00P C00Z -178.0(11) . . . . ?
N00D C00N C01I C00Q -76.4(18) . . . . ?
N00E N00A C00P N00G 4.8(16) . . . . ?
N00E N00A C00P C00Z 179.2(10) . . . . ?
N00E C00N C01I C00Q 103.2(15) . . . . ?
N00F N008 C00H N003 6.1(16) . . . . ?
N00F N008 C00H C01S -174.5(9) . . . . ?
N00F C00J C01E C00M 68.4(16) . . . . ?
N00G N00D C00N N00E 6.2(18) . . . . ?
N00G N00D C00N C01I -174.3(10) . . . . ?
N00G C00P C00Z C00L 90.8(12) . . . . ?
C00H N003 N004 C00J -1.6(12) . . . . ?
C00H N008 N00F C00J -2.8(15) . . . . ?
C00K N001 N005 C00R -1.2(12) . . . . ?
C00N N00D N00G C00P -1.7(16) . . . . ?
C00N C01I C00Q C01J 122.0(13) . . . . ?
C00N C01I C00Q C029 -62.5(18) . . . . ?
C00P N00A N00E C00N -0.7(15) . . . . ?
C00P C00Z C00L C01F 61.8(11) . . . . ?
C00P C00Z C00L C01L -115.2(9) . . . . ?
C00R N006 N009 C00K -0.7(16) . . . . ?
C00R C017 C00I C01O 104.9(13) . . . . ?
C00R C017 C00I C024 -80.6(14) . . . . ?
C00U N002 N00B C00W -3.4(17) . . . . ?
C00U C01A C00O C027 60.7(18) . . . . ?
C00U C01A C00O C015 -125.2(13) . . . . ?
C00W N007 N00C C00U -0.1(15) . . . . ?
C00W C012 C00S C01W -65.9(13) . . . . ?
C00W C012 C00S C011 117.2(11) . . . . ?
C00X C014 C019 C022 0.0 . . . . ?
C00X C014 C019 C02A -177.9(9) . . . . ?
C00X C00V C01D C00K 114.6(12) . . . . ?
C014 C00X C00V C020 0.0 . . . . ?
C014 C00X C00V C01D 179.8(9) . . . . ?
C014 C019 C022 C020 0.0 . . . . ?
C014 C019 C02A C01X -109.2(12) . . . . ?
C019 C022 C020 C00V 0.0 . . . . ?
C022 C019 C02A C01X 72.8(15) . . . . ?
C022 C020 C00V C00X 0.0 . . . . ?
C022 C020 C00V C01D -179.8(10) . . . . ?
C020 C00V C01D C00K -65.6(17) . . . . ?
C00V C00X C014 C019 0.0 . . . . ?
C00Y C018 C010 C00M 0.0 . . . . ?
C018 C00Y C028 C026 0.0 . . . . ?
C018 C00Y C02B C01Z 119.6(12) . . . . ?
C018 C010 C00M C026 0.0 . . . . ?
C018 C010 C00M C01E 178.4(8) . . . . ?
C010 C00M C026 C028 0.0 . . . . ?
C010 C00M C01E C00J -104.6(12) . . . . ?
C00M C026 C028 C00Y 0.0 . . . . ?
C026 C00M C01E C00J 73.8(15) . . . . ?
C028 C00Y C018 C010 0.0 . . . . ?
C028 C00Y C02B C01Z -61.7(16) . . . . ?
C017 C00I C024 C025 -174.4(9) . . . . ?
C01A C00O C015 C01J -174.1(10) . . . . ?
N01C N01U C01Z C02B 172.0(16) . . . . ?
N01C N01U C01Z N02D -8(3) . . . . ?
N01C C01X C02A C019 -108.3(18) . . . . ?
N01C C01X N02E N02D -2(3) . . . . ?
C01E C00M C026 C028 -178.4(9) . . . . ?
C01F C01K C016 C01B 0.0 . . . . ?
C01F C01K C016 C023 -175.9(7) . . . . ?
C01K C01F C00L C00Z -177.1(7) . . . . ?
C01K C01F C00L C01L 0.0 . . . . ?
C01K C016 C01B C01L 0.0 . . . . ?
C01K C016 C023 C01H -78.1(13) . . . . ?
C016 C01B C01L C00L 0.0 . . . . ?
C01B C016 C023 C01H 106.0(12) . . . . ?
C01B C01L C00L C00Z 177.0(7) . . . . ?
C01B C01L C00L C01F 0.0 . . . . ?
C00L C01F C01K C016 0.0 . . . . ?
C01H N01V N01Y C01M 0.0 . . . . ?
N01V C01H N02G N02H 0.0 . . . . ?
N01V C01H C023 C016 13.6(18) . . . . ?
N01V N01Y C01M N02H 0.0 . . . . ?
N01V N01Y C01M C02C 169.6(15) . . . . ?
N01Y C01M N02H N02G 0.0 . . . . ?
N01Y C01M C02C C01N -4(2) . . . . ?
C01M N02H N02G C01H 0.0 . . . . ?
N02H C01M C02C C01N 165.7(11) . . . . ?
N02G C01H N01V N01Y 0.0 . . . . ?
N02G C01H C023 C016 -163.8(9) . . . . ?
C01I C00Q C029 C027 -175.3(11) . . . . ?
C01Q C01O C00I C017 174.5(9) . . . . ?
C01Q C01O C00I C024 0.0 . . . . ?
C01Q C00T C01S C00H -92.0(15) . . . . ?
C01O C01Q C00T C025 0.0 . . . . ?
C01O C01Q C00T C01S -176.1(9) . . . . ?
C01O C00I C024 C025 0.0 . . . . ?
C00I C024 C025 C00T 0.0 . . . . ?
C024 C025 C00T C01Q 0.0 . . . . ?
C024 C025 C00T C01S 176.1(9) . . . . ?
C025 C00T C01S C00H 91.9(15) . . . . ?
C00T C01Q C01O C00I 0.0 . . . . ?
N01U N01C C01X C02A -175.7(16) . . . . ?
N01U N01C C01X N02E 4(3) . . . . ?
N01U C01Z C02B C00Y 96.4(18) . . . . ?
N01U C01Z N02D N02E 9(2) . . . . ?
C01W C013 C01N C01R 0.0 . . . . ?
C01W C013 C01N C02C 177.0(8) . . . . ?
C013 C01W C00S C012 -176.9(8) . . . . ?
C013 C01W C00S C011 0.0 . . . . ?
C013 C01N C01R C011 0.0 . . . . ?
C013 C01N C02C C01M 68.7(17) . . . . ?
C01N C01R C011 C00S 0.0 . . . . ?
C01R C01N C02C C01M -114.3(14) . . . . ?
C01R C011 C00S C012 177.0(8) . . . . ?
C01R C011 C00S C01W 0.0 . . . . ?
C00S C01W C013 C01N 0.0 . . . . ?
C01X N01C N01U C01Z 2(3) . . . . ?
C01Z N02D N02E C01X -4(2) . . . . ?
C023 C016 C01B C01L 175.8(7) . . . . ?
C023 C01H N01V N01Y -177.4(14) . . . . ?
C023 C01H N02G N02H 177.5(13) . . . . ?
C027 C00O C015 C01J 0.0 . . . . ?
C00O C027 C029 C00Q 0.0 . . . . ?
C00O C015 C01J C00Q 0.0 . . . . ?
C015 C01J C00Q C01I 175.7(11) . . . . ?
C015 C01J C00Q C029 0.0 . . . . ?
C01J C00Q C029 C027 0.0 . . . . ?
C029 C027 C00O C01A 174.1(10) . . . . ?
C029 C027 C00O C015 0.0 . . . . ?
C02A C019 C022 C020 178.0(9) . . . . ?
C02A C01X N02E N02D 177.1(14) . . . . ?
C02B C00Y C018 C010 178.7(9) . . . . ?
C02B C00Y C028 C026 -178.7(9) . . . . ?
C02B C01Z N02D N02E -171.0(14) . . . . ?
C02C C01M N02H N02G -170.3(14) . . . . ?
C02C C01N C01R C011 -177.0(8) . . . . ?
N02D C01Z C02B C00Y -83.5(18) . . . . ?
N02E C01X C02A C019 72.3(18) . . . . ?

_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 3.036
_oxdiff_exptl_absorpt_empirical_full_min 0.668
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.336(5)
2 0.664(5)

####################################################################### 
# 
# 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_tx715
_database_code_depnum_ccdc_archive 'CCDC 2233700'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2022-12-31 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_audit_creation_date             2022-08-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H24 N12, C10 H8 N2'
_chemical_formula_sum            'C40 H32 N14'
_chemical_formula_weight         708.79
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHN
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'

_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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   10.96920(10)
_cell_length_b                   22.0100(2)
_cell_length_c                   14.5393(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3510.25(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8415
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      74.5440
_cell_measurement_theta_min      3.0340
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'translucent light red'
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.135
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13311
_diffrn_reflns_point_group_measured_fraction_full 0.830
_diffrn_reflns_point_group_measured_fraction_max 0.781
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.272
_diffrn_reflns_theta_min         3.643
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     43.00 120.00   0.50    0.05    --   47.20  80.00 -33.00  154
  2  ω    -79.00 -26.00   0.50    0.15    --  -99.00  80.00 -33.00  106
  3  ω     95.00 169.00   0.50    0.15    --  103.25  46.00 129.00  148
  4  ω     31.00 110.00   0.50    0.15    --  103.25-107.00 116.00  158
  5  ω     41.00  94.00   0.50    0.05    --   47.20-125.00-180.00  106
  6  ω     35.00  97.00   0.50    0.05    --   47.20  38.00  90.00  124
  7  ω   -163.00-123.00   0.50    0.15    --  -99.00 -45.00-120.00   80
  8  ω     51.00  88.00   0.50    0.15    --  103.25 -94.00-150.00   74
  9  ω     31.00 106.00   0.50    0.15    --  103.25 -94.00-180.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1321335000
_diffrn_orient_matrix_UB_12      -0.0084882000
_diffrn_orient_matrix_UB_13      -0.0229460000
_diffrn_orient_matrix_UB_21      0.0330666000
_diffrn_orient_matrix_UB_22      -0.0904122000
_diffrn_orient_matrix_UB_23      -0.0326587000
_diffrn_orient_matrix_UB_31      -0.0340230000
_diffrn_orient_matrix_UB_32      -0.0546660000
_diffrn_orient_matrix_UB_33      0.0575004000
_diffrn_oxdiff_ac3_digest_frames 
;
015c160d27648b9729b7239f5604a6e3bc01100acf9
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.549
_reflns_Friedel_fraction_full    0.646
_reflns_Friedel_fraction_max     0.577
_reflns_number_gt                5330
_reflns_number_total             5654
_reflns_odcompleteness_completeness 99.94
_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.
 
 _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 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 
;
 Flack x determined using 1800 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.31(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         5654
_refine_ls_number_restraints     99
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0431
_refine_ls_restrained_S_all      1.202
_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)+(0.0659P)²+1.3128P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1259
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C50, N54, C53, C52, C46, H52a, H52b, C47, C45, C48, H47, C44, H45, C43, H48,
 H44, C49, H49a, H49b, N51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C46) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C49) \\sim Ueq,
Uanis(C50) \\sim Ueq, Uanis(N51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(N54) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C28(H28a,H28b), C35(H35a,H35b), C12(H12a,H12b), C21(H21a,H21b), C42(H42a,
 H42b), C7(H7a,H7b), C49(H49a,H49b), C52(H52a,H52b)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C33(H33), C2(H2), C31(H31), C16(H16), C6(H6), C34(H34), C17(H17),
 C30(H30), C5(H5), C19(H19), C20(H20), C48(H48), C44(H44), C47(H47), C45(H45)
;
_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
N10 N 0.8344(2) 0.69166(11) 0.7628(2) 0.0385(6) Uani 1 1 d . . . . .
N41 N 0.7824(2) 0.30155(11) 0.7588(2) 0.0389(6) Uani 1 1 d . . . . .
N40 N 0.7360(2) 0.33253(11) 0.8280(2) 0.0379(6) Uani 1 1 d . . . . .
N9 N 0.7873(2) 0.66183(11) 0.83284(19) 0.0355(6) Uani 1 1 d . . . . .
N38 N 0.5368(2) 0.31438(12) 0.7721(2) 0.0396(6) Uani 1 1 d . . . . .
N37 N 0.5840(2) 0.28175(12) 0.7034(2) 0.0408(6) Uani 1 1 d . . . . .
N14 N 0.6369(2) 0.72265(12) 0.71773(19) 0.0380(6) Uani 1 1 d . . . . .
N13 N 0.5890(2) 0.69129(12) 0.78722(19) 0.0376(6) Uani 1 1 d . . . . .
C36 C 0.7046(3) 0.27482(12) 0.7006(2) 0.0319(6) Uani 1 1 d . . . . .
N26 N 0.8036(3) 0.53805(12) 0.3175(3) 0.0619(10) Uani 1 1 d . . . . .
C11 C 0.7580(3) 0.72414(12) 0.7100(2) 0.0323(6) Uani 1 1 d . . . . .
C15 C 0.8430(3) 0.72611(12) 0.5508(2) 0.0321(6) Uani 1 1 d . . . . .
C22 C 0.8910(3) 0.44423(14) 0.3109(2) 0.0360(7) Uani 1 1 d . . . . .
C29 C 0.7868(3) 0.27466(12) 0.5405(2) 0.0325(6) Uani 1 1 d . . . . .
N24 N 1.0144(3) 0.52641(15) 0.3217(3) 0.0639(10) Uani 1 1 d . . . . .
C32 C 0.8434(3) 0.34243(12) 0.3827(2) 0.0327(6) Uani 1 1 d . . . . .
C39 C 0.6144(3) 0.33665(12) 0.8344(2) 0.0327(6) Uani 1 1 d . . . . .
C28 C 0.8757(3) 0.37727(14) 0.2956(2) 0.0398(7) Uani 1 1 d . . . . .
H28A H 0.950898 0.360981 0.270563 0.048 Uiso 1 1 calc R U . . .
H28B H 0.812030 0.370883 0.250297 0.048 Uiso 1 1 calc R U . . .
N23 N 1.0011(3) 0.46636(14) 0.3197(3) 0.0640(10) Uani 1 1 d . . . . .
C4 C 0.5755(3) 0.43858(13) 0.9084(2) 0.0332(6) Uani 1 1 d . . . . .
N27 N 0.7903(3) 0.47859(14) 0.3165(3) 0.0629(11) Uani 1 1 d . . . . .
C8 C 0.6666(3) 0.66485(12) 0.8454(2) 0.0313(6) Uani 1 1 d . . . . .
C3 C 0.4750(3) 0.47571(14) 0.9201(2) 0.0353(6) Uani 1 1 d . . . . .
H3 H 0.398106 0.458345 0.925947 0.042 Uiso 1 1 calc R U . . .
C35 C 0.7580(3) 0.23689(13) 0.6254(2) 0.0384(7) Uani 1 1 d . . . . .
H35A H 0.700849 0.205026 0.609050 0.046 Uiso 1 1 calc R U . . .
H35B H 0.832089 0.217751 0.647389 0.046 Uiso 1 1 calc R U . . .
C33 C 0.7273(3) 0.31867(13) 0.3955(2) 0.0364(7) Uani 1 1 d . . . . .
H33 H 0.667141 0.325828 0.351776 0.044 Uiso 1 1 calc R U . . .
C18 C 0.9003(3) 0.66164(13) 0.3903(2) 0.0339(6) Uani 1 1 d . . . . .
C2 C 0.4869(3) 0.53824(13) 0.9232(2) 0.0369(7) Uani 1 1 d . . . . .
H2 H 0.417975 0.562367 0.930560 0.044 Uiso 1 1 calc R U . . .
C25 C 0.9172(3) 0.55999(14) 0.3136(2) 0.0377(7) Uani 1 1 d . . . . .
C31 C 0.9305(3) 0.33254(15) 0.4505(2) 0.0395(7) Uani 1 1 d . . . . .
H31 H 1.008578 0.348346 0.443317 0.047 Uiso 1 1 calc R U . . .
C1 C 0.6003(3) 0.56520(13) 0.9156(2) 0.0322(6) Uani 1 1 d . . . . .
C16 C 0.9593(3) 0.70392(15) 0.5361(2) 0.0405(7) Uani 1 1 d . . . . .
H16 H 1.019111 0.710419 0.580333 0.049 Uiso 1 1 calc R U . . .
C6 C 0.7008(3) 0.52832(14) 0.8996(3) 0.0421(8) Uani 1 1 d . . . . .
H6 H 0.777144 0.545835 0.891136 0.051 Uiso 1 1 calc R U . . .
C12 C 0.8125(3) 0.76250(13) 0.6363(2) 0.0390(7) Uani 1 1 d . . . . .
H12A H 0.886247 0.781386 0.659554 0.047 Uiso 1 1 calc R U . . .
H12B H 0.755755 0.794583 0.620283 0.047 Uiso 1 1 calc R U . . .
C34 C 0.7005(3) 0.28455(13) 0.4724(2) 0.0370(7) Uani 1 1 d . . . . .
H34 H 0.623126 0.267846 0.478791 0.044 Uiso 1 1 calc R U . . .
C21 C 0.9310(3) 0.62751(14) 0.3024(2) 0.0434(8) Uani 1 1 d . . . . .
H21A H 0.877701 0.641320 0.253449 0.052 Uiso 1 1 calc R U . . .
H21B H 1.014238 0.636676 0.284711 0.052 Uiso 1 1 calc R U . . .
C42 C 0.5631(3) 0.37002(13) 0.9150(2) 0.0391(7) Uani 1 1 d . . . . .
H42A H 0.604182 0.356232 0.970272 0.047 Uiso 1 1 calc R U . . .
H42B H 0.477445 0.359840 0.920982 0.047 Uiso 1 1 calc R U . . .
C17 C 0.9883(3) 0.67218(15) 0.4567(2) 0.0413(7) Uani 1 1 d . . . . .
H17 H 1.067262 0.657889 0.448050 0.050 Uiso 1 1 calc R U . . .
C30 C 0.9025(3) 0.29958(14) 0.5282(2) 0.0391(7) Uani 1 1 d . . . . .
H30 H 0.961696 0.293854 0.573119 0.047 Uiso 1 1 calc R U . . .
C7 C 0.6158(3) 0.63338(13) 0.9283(2) 0.0382(7) Uani 1 1 d . . . . .
H7A H 0.537161 0.651053 0.943097 0.046 Uiso 1 1 calc R U . . .
H7B H 0.669603 0.640555 0.980150 0.046 Uiso 1 1 calc R U . . .
C5 C 0.6887(3) 0.46633(13) 0.8962(3) 0.0415(8) Uani 1 1 d . . . . .
H5 H 0.757127 0.442391 0.885626 0.050 Uiso 1 1 calc R U . . .
C19 C 0.7835(3) 0.68300(14) 0.4051(2) 0.0399(7) Uani 1 1 d . . . . .
H19 H 0.723295 0.675632 0.361413 0.048 Uiso 1 1 calc R U . . .
C20 C 0.7550(3) 0.71500(14) 0.4833(2) 0.0393(7) Uani 1 1 d . . . . .
H20 H 0.676124 0.729464 0.491532 0.047 Uiso 1 1 calc R U . . .
N54 N -0.1271(6) 0.5799(2) 0.0915(4) 0.1084(17) Uani 1 1 d . U . . .
C49 C 0.5223(8) 0.5074(2) 0.1685(5) 0.111(2) Uani 1 1 d . U . . .
H49A H 0.553676 0.542757 0.136523 0.133 Uiso 1 1 calc R U . . .
H49B H 0.528371 0.515378 0.233949 0.133 Uiso 1 1 calc R U . . .
C43 C 0.3901(8) 0.50009(19) 0.1443(4) 0.0962(18) Uani 1 1 d . U . . .
C48 C 0.3337(8) 0.4429(2) 0.1347(4) 0.106(2) Uani 1 1 d . U . . .
H48 H 0.378263 0.407472 0.144128 0.128 Uiso 1 1 calc R U . . .
C46 C 0.1404(8) 0.4902(2) 0.0985(4) 0.0976(17) Uani 1 1 d . U . . .
C44 C 0.3178(8) 0.5513(2) 0.1316(4) 0.0947(18) Uani 1 1 d . U . . .
H44 H 0.352315 0.589552 0.138757 0.114 Uiso 1 1 calc R U . . .
C47 C 0.2117(9) 0.4398(2) 0.1112(4) 0.110(2) Uani 1 1 d . U . . .
H47 H 0.176386 0.401742 0.103662 0.132 Uiso 1 1 calc R U . . .
C53 C -0.0686(7) 0.5373(3) 0.0833(4) 0.0936(18) Uani 1 1 d . U . . .
C45 C 0.1962(8) 0.5468(2) 0.1087(4) 0.0995(19) Uani 1 1 d . U . . .
H45 H 0.150726 0.581926 0.099927 0.119 Uiso 1 1 calc R U . . .
C50 C 0.6002(9) 0.4554(3) 0.1466(4) 0.127(3) Uani 1 1 d . U . . .
C52 C 0.0065(9) 0.4836(3) 0.0740(4) 0.110(2) Uani 1 1 d . U . . .
H52A H 0.001083 0.469687 0.010844 0.132 Uiso 1 1 calc R U . . .
H52B H -0.028028 0.451958 0.112558 0.132 Uiso 1 1 calc R U . . .
N51 N 0.6668(9) 0.4160(3) 0.1273(4) 0.181(4) Uani 1 1 d . U . . .


_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
N10 N9 1.318(4) . ?
N10 C11 1.343(4) . ?
N41 N40 1.317(4) . ?
N41 C36 1.339(4) . ?
N40 C39 1.341(4) . ?
N9 C8 1.338(4) . ?
N38 N37 1.335(4) . ?
N38 C39 1.336(4) . ?
N37 C36 1.332(4) . ?
N14 N13 1.331(4) . ?
N14 C11 1.334(4) . ?
N13 C8 1.334(4) . ?
C36 C35 1.495(4) . ?
N26 N27 1.317(4) . ?
N26 C25 1.338(4) . ?
C11 C12 1.489(4) . ?
C15 C16 1.383(4) . ?
C15 C12 1.517(4) . ?
C15 C20 1.397(4) . ?
C22 C28 1.500(4) . ?
C22 N23 1.308(4) . ?
C22 N27 1.341(4) . ?
C29 C35 1.522(4) . ?
C29 C34 1.386(4) . ?
C29 C30 1.394(4) . ?
N24 N23 1.330(4) . ?
N24 C25 1.302(5) . ?
C32 C28 1.522(5) . ?
C32 C33 1.389(4) . ?
C32 C31 1.391(5) . ?
C39 C42 1.493(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C4 C3 1.382(4) . ?
C4 C42 1.518(4) . ?
C4 C5 1.395(4) . ?
C8 C7 1.498(5) . ?
C3 H3 0.9300 . ?
C3 C2 1.383(4) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C33 H33 0.9300 . ?
C33 C34 1.379(5) . ?
C18 C21 1.520(4) . ?
C18 C17 1.385(5) . ?
C18 C19 1.382(4) . ?
C2 H2 0.9300 . ?
C2 C1 1.383(4) . ?
C25 C21 1.503(4) . ?
C31 H31 0.9300 . ?
C31 C30 1.377(5) . ?
C1 C6 1.389(4) . ?
C1 C7 1.522(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.386(5) . ?
C6 H6 0.9300 . ?
C6 C5 1.372(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C34 H34 0.9300 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C17 H17 0.9300 . ?
C30 H30 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C5 H5 0.9300 . ?
C19 H19 0.9300 . ?
C19 C20 1.374(5) . ?
C20 H20 0.9300 . ?
N54 C53 1.143(8) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C49 C43 1.501(11) . ?
C49 C50 1.462(9) . ?
C43 C48 1.409(9) . ?
C43 C44 1.390(8) . ?
C48 H48 0.9300 . ?
C48 C47 1.384(10) . ?
C46 C47 1.368(9) . ?
C46 C45 1.396(8) . ?
C46 C52 1.518(11) . ?
C44 H44 0.9300 . ?
C44 C45 1.378(10) . ?
C47 H47 0.9300 . ?
C53 C52 1.447(10) . ?
C45 H45 0.9300 . ?
C50 N51 1.169(8) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?

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
N9 N10 C11 117.5(3) . . ?
N40 N41 C36 117.6(3) . . ?
N41 N40 C39 118.2(3) . . ?
N10 N9 C8 118.0(3) . . ?
N37 N38 C39 117.2(3) . . ?
C36 N37 N38 118.0(3) . . ?
N13 N14 C11 118.0(3) . . ?
N14 N13 C8 117.2(3) . . ?
N41 C36 C35 117.3(3) . . ?
N37 C36 N41 124.3(3) . . ?
N37 C36 C35 118.4(3) . . ?
N27 N26 C25 117.5(3) . . ?
N10 C11 C12 117.5(3) . . ?
N14 C11 N10 124.1(3) . . ?
N14 C11 C12 118.4(3) . . ?
C16 C15 C12 121.1(3) . . ?
C16 C15 C20 117.9(3) . . ?
C20 C15 C12 121.1(3) . . ?
N23 C22 C28 118.9(3) . . ?
N23 C22 N27 123.0(3) . . ?
N27 C22 C28 118.1(3) . . ?
C34 C29 C35 121.5(3) . . ?
C34 C29 C30 117.9(3) . . ?
C30 C29 C35 120.6(3) . . ?
C25 N24 N23 118.2(3) . . ?
C33 C32 C28 121.0(3) . . ?
C33 C32 C31 118.4(3) . . ?
C31 C32 C28 120.6(3) . . ?
N40 C39 C42 117.5(3) . . ?
N38 C39 N40 124.2(3) . . ?
N38 C39 C42 118.2(3) . . ?
C22 C28 C32 113.4(3) . . ?
C22 C28 H28A 108.9 . . ?
C22 C28 H28B 108.9 . . ?
C32 C28 H28A 108.9 . . ?
C32 C28 H28B 108.9 . . ?
H28A C28 H28B 107.7 . . ?
C22 N23 N24 118.2(3) . . ?
C3 C4 C42 120.6(3) . . ?
C3 C4 C5 117.8(3) . . ?
C5 C4 C42 121.5(3) . . ?
N26 N27 C22 118.0(3) . . ?
N9 C8 C7 117.1(3) . . ?
N13 C8 N9 124.5(3) . . ?
N13 C8 C7 118.4(3) . . ?
C4 C3 H3 119.4 . . ?
C4 C3 C2 121.1(3) . . ?
C2 C3 H3 119.4 . . ?
C36 C35 C29 111.7(2) . . ?
C36 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C29 C35 H35A 109.3 . . ?
C29 C35 H35B 109.3 . . ?
H35A C35 H35B 107.9 . . ?
C32 C33 H33 119.7 . . ?
C34 C33 C32 120.6(3) . . ?
C34 C33 H33 119.7 . . ?
C17 C18 C21 121.0(3) . . ?
C19 C18 C21 120.3(3) . . ?
C19 C18 C17 118.8(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 C3 120.6(3) . . ?
C1 C2 H2 119.7 . . ?
N26 C25 C21 117.1(3) . . ?
N24 C25 N26 123.6(3) . . ?
N24 C25 C21 119.3(3) . . ?
C32 C31 H31 119.6 . . ?
C30 C31 C32 120.7(3) . . ?
C30 C31 H31 119.6 . . ?
C2 C1 C6 118.5(3) . . ?
C2 C1 C7 120.9(3) . . ?
C6 C1 C7 120.5(3) . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121.2(3) . . ?
C17 C16 H16 119.4 . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.7(3) . . ?
C5 C6 H6 119.7 . . ?
C11 C12 C15 112.3(2) . . ?
C11 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
C15 C12 H12A 109.1 . . ?
C15 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
C29 C34 H34 119.4 . . ?
C33 C34 C29 121.3(3) . . ?
C33 C34 H34 119.4 . . ?
C18 C21 H21A 109.2 . . ?
C18 C21 H21B 109.2 . . ?
C25 C21 C18 112.1(3) . . ?
C25 C21 H21A 109.2 . . ?
C25 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C39 C42 C4 113.9(3) . . ?
C39 C42 H42A 108.8 . . ?
C39 C42 H42B 108.8 . . ?
C4 C42 H42A 108.8 . . ?
C4 C42 H42B 108.8 . . ?
H42A C42 H42B 107.7 . . ?
C18 C17 C16 120.3(3) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C29 C30 H30 119.5 . . ?
C31 C30 C29 121.1(3) . . ?
C31 C30 H30 119.5 . . ?
C8 C7 C1 113.5(3) . . ?
C8 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
C1 C7 H7A 108.9 . . ?
C1 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C4 C5 H5 119.4 . . ?
C6 C5 C4 121.1(3) . . ?
C6 C5 H5 119.4 . . ?
C18 C19 H19 119.5 . . ?
C20 C19 C18 120.9(3) . . ?
C20 C19 H19 119.6 . . ?
C15 C20 H20 119.5 . . ?
C19 C20 C15 120.9(3) . . ?
C19 C20 H20 119.5 . . ?
H49A C49 H49B 107.5 . . ?
C43 C49 H49A 108.4 . . ?
C43 C49 H49B 108.4 . . ?
C50 C49 H49A 108.4 . . ?
C50 C49 H49B 108.4 . . ?
C50 C49 C43 115.4(6) . . ?
C48 C43 C49 122.9(6) . . ?
C44 C43 C49 119.7(6) . . ?
C44 C43 C48 117.4(8) . . ?
C43 C48 H48 120.3 . . ?
C47 C48 C43 119.5(6) . . ?
C47 C48 H48 120.3 . . ?
C47 C46 C45 117.2(8) . . ?
C47 C46 C52 120.5(6) . . ?
C45 C46 C52 122.3(6) . . ?
C43 C44 H44 119.1 . . ?
C45 C44 C43 121.7(6) . . ?
C45 C44 H44 119.1 . . ?
C48 C47 H47 118.4 . . ?
C46 C47 C48 123.2(6) . . ?
C46 C47 H47 118.4 . . ?
N54 C53 C52 179.2(7) . . ?
C46 C45 H45 119.5 . . ?
C44 C45 C46 121.0(6) . . ?
C44 C45 H45 119.5 . . ?
N51 C50 C49 176.5(10) . . ?
C46 C52 H52A 108.1 . . ?
C46 C52 H52B 108.1 . . ?
C53 C52 C46 116.8(5) . . ?
C53 C52 H52A 108.1 . . ?
C53 C52 H52B 108.1 . . ?
H52A C52 H52B 107.3 . . ?

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
N10 N9 C8 N13 6.5(4) . . . . ?
N10 N9 C8 C7 -176.8(2) . . . . ?
N10 C11 C12 C15 81.3(4) . . . . ?
N41 N40 C39 N38 -4.2(4) . . . . ?
N41 N40 C39 C42 177.8(3) . . . . ?
N41 C36 C35 C29 -88.0(3) . . . . ?
N40 N41 C36 N37 6.0(5) . . . . ?
N40 N41 C36 C35 -176.7(3) . . . . ?
N40 C39 C42 C4 74.7(4) . . . . ?
N9 N10 C11 N14 -7.8(5) . . . . ?
N9 N10 C11 C12 174.3(3) . . . . ?
N9 C8 C7 C1 -80.3(4) . . . . ?
N38 N37 C36 N41 -4.3(5) . . . . ?
N38 N37 C36 C35 178.3(3) . . . . ?
N38 C39 C42 C4 -103.4(3) . . . . ?
N37 N38 C39 N40 5.7(4) . . . . ?
N37 N38 C39 C42 -176.3(3) . . . . ?
N37 C36 C35 C29 89.5(3) . . . . ?
N14 N13 C8 N9 -8.1(4) . . . . ?
N14 N13 C8 C7 175.3(3) . . . . ?
N14 C11 C12 C15 -96.7(3) . . . . ?
N13 N14 C11 N10 6.2(5) . . . . ?
N13 N14 C11 C12 -175.9(3) . . . . ?
N13 C8 C7 C1 96.5(3) . . . . ?
C36 N41 N40 C39 -1.6(4) . . . . ?
N26 C25 C21 C18 73.5(4) . . . . ?
C11 N10 N9 C8 1.4(4) . . . . ?
C11 N14 N13 C8 1.6(4) . . . . ?
C15 C16 C17 C18 -0.5(5) . . . . ?
N24 C25 C21 C18 -104.5(4) . . . . ?
C32 C33 C34 C29 2.2(4) . . . . ?
C32 C31 C30 C29 0.8(5) . . . . ?
C39 N38 N37 C36 -1.5(4) . . . . ?
C28 C22 N23 N24 171.7(3) . . . . ?
C28 C22 N27 N26 -171.0(4) . . . . ?
C28 C32 C33 C34 176.7(3) . . . . ?
C28 C32 C31 C30 -178.2(3) . . . . ?
N23 C22 C28 C32 99.2(4) . . . . ?
N23 C22 N27 N26 10.3(6) . . . . ?
N23 N24 C25 N26 10.6(6) . . . . ?
N23 N24 C25 C21 -171.6(4) . . . . ?
C4 C3 C2 C1 -0.6(5) . . . . ?
N27 N26 C25 N24 -9.8(6) . . . . ?
N27 N26 C25 C21 172.3(4) . . . . ?
N27 C22 C28 C32 -79.6(4) . . . . ?
N27 C22 N23 N24 -9.5(6) . . . . ?
C3 C4 C42 C39 127.7(3) . . . . ?
C3 C4 C5 C6 2.7(5) . . . . ?
C3 C2 C1 C6 3.5(5) . . . . ?
C3 C2 C1 C7 -173.9(3) . . . . ?
C35 C29 C34 C33 -179.8(3) . . . . ?
C35 C29 C30 C31 178.3(3) . . . . ?
C33 C32 C28 C22 108.4(3) . . . . ?
C33 C32 C31 C30 0.4(4) . . . . ?
C18 C19 C20 C15 -0.9(5) . . . . ?
C2 C1 C6 C5 -3.3(5) . . . . ?
C2 C1 C7 C8 -120.0(3) . . . . ?
C25 N26 N27 C22 -0.7(6) . . . . ?
C25 N24 N23 C22 -0.8(6) . . . . ?
C31 C32 C28 C22 -73.0(4) . . . . ?
C31 C32 C33 C34 -1.9(4) . . . . ?
C1 C6 C5 C4 0.2(6) . . . . ?
C16 C15 C12 C11 -96.2(3) . . . . ?
C16 C15 C20 C19 0.0(5) . . . . ?
C6 C1 C7 C8 62.7(4) . . . . ?
C12 C15 C16 C17 -178.1(3) . . . . ?
C12 C15 C20 C19 178.8(3) . . . . ?
C34 C29 C35 C36 -88.1(3) . . . . ?
C34 C29 C30 C31 -0.5(4) . . . . ?
C21 C18 C17 C16 179.3(3) . . . . ?
C21 C18 C19 C20 -178.7(3) . . . . ?
C42 C4 C3 C2 173.6(3) . . . . ?
C42 C4 C5 C6 -173.4(3) . . . . ?
C17 C18 C21 C25 87.6(4) . . . . ?
C17 C18 C19 C20 1.0(4) . . . . ?
C30 C29 C35 C36 93.1(3) . . . . ?
C30 C29 C34 C33 -0.9(4) . . . . ?
C7 C1 C6 C5 174.1(3) . . . . ?
C5 C4 C3 C2 -2.5(5) . . . . ?
C5 C4 C42 C39 -56.4(4) . . . . ?
C19 C18 C21 C25 -92.7(4) . . . . ?
C19 C18 C17 C16 -0.4(5) . . . . ?
C20 C15 C16 C17 0.6(5) . . . . ?
C20 C15 C12 C11 85.1(4) . . . . ?
C49 C43 C48 C47 -179.3(6) . . . . ?
C49 C43 C44 C45 179.6(6) . . . . ?
C43 C48 C47 C46 -1.6(9) . . . . ?
C43 C44 C45 C46 0.9(9) . . . . ?
C48 C43 C44 C45 -1.3(8) . . . . ?
C44 C43 C48 C47 1.6(8) . . . . ?
C47 C46 C45 C44 -0.7(8) . . . . ?
C47 C46 C52 C53 165.7(5) . . . . ?
C45 C46 C47 C48 1.1(9) . . . . ?
C45 C46 C52 C53 -14.5(8) . . . . ?
C50 C49 C43 C48 23.3(9) . . . . ?
C50 C49 C43 C44 -157.6(6) . . . . ?
C52 C46 C47 C48 -179.1(6) . . . . ?
C52 C46 C45 C44 179.5(6) . . . . ?

_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 2.350
_oxdiff_exptl_absorpt_empirical_full_min 0.750
####################################################################### 
# 
# 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_tx1465
_database_code_depnum_ccdc_archive 'CCDC 2233697'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2022-12-31 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_audit_creation_date             2022-08-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.667(C H2 Cl2), 0.667(C30 H24 N12), C10.333 H8.667 Cl0.667 N4'
_chemical_formula_sum            'C31 H26 Cl2 N12'
_chemical_formula_weight         637.54
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHN
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'
Cl Cl 0.3639 0.7018 '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'

_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      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   24.4461(4)
_cell_length_b                   37.2074(6)
_cell_length_c                   10.1093(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9195.2(3)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    10383
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      74.8240
_cell_measurement_theta_min      3.6140
_shelx_estimated_absorpt_T_max   0.805
_shelx_estimated_absorpt_T_min   0.660
_exptl_absorpt_coefficient_mu    2.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3960
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            35548
_diffrn_reflns_point_group_measured_fraction_full 0.889
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.658
_diffrn_reflns_theta_min         2.162
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     48.00  77.00   0.50    1.50    --   47.20  53.00  13.00   58
  2  ω    110.00 137.00   0.50    5.00    --  103.25  53.00  13.00   54
  3  ω     92.00 168.00   0.50    5.00    --  103.25  45.00   0.00  152
  4  ω    140.00 166.00   0.50    5.00    --  103.25  45.00-120.00   52
  5  ω     92.00 123.00   0.50    5.00    --  103.25  45.00-120.00   62
  6  ω     31.00 117.00   0.50    5.00    --  103.25 -53.00-130.00  172
  7  ω     92.00 169.00   0.50    5.00    --  103.25  45.00  90.00  154
  8  ω    -24.00  50.00   0.50    1.50    --   47.20 -53.00-130.00  148
  9  ω    -61.00  23.00   0.50    1.50    --  -47.20  53.00  13.00  168
 10  ω    -70.00 -41.00   0.50    5.00    --  -99.00  53.00  13.00   58
 11  ω    -54.00 -29.00   0.50    5.00    --  -99.00  61.00  90.00   50
 12  ω    -61.00  22.00   0.50    1.50    --  -47.20  57.00  90.00  166
 13  ω    -62.00 -36.00   0.50    1.50    --  -47.20 -53.00-130.00   52
 14  ω   -104.00 -79.00   0.50    1.50    --  -47.20 -53.00-130.00   50
 15  ω   -127.00-102.00   0.50    5.00    --  -99.00 -53.00-130.00   50
 16  ω   -134.00-109.00   0.50    5.00    --  -99.00 -30.00 -60.00   50
 17  ω   -112.00 -27.00   0.50    5.00    --  -99.00  45.00-120.00  170
 18  ω   -111.00 -25.00   0.50    5.00    --  -99.00  30.00-150.00  172
 19  ω   -117.00 -76.00   0.50    1.50    --  -47.20-125.00   0.00   82
 20  ω   -147.00 -93.00   0.50    5.00    --  -99.00 -15.00  90.00  108
 21  ω   -115.00 -72.00   0.50    5.00    --  -99.00  61.00  90.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0589472000
_diffrn_orient_matrix_UB_12      0.0046250000
_diffrn_orient_matrix_UB_13      -0.0513986000
_diffrn_orient_matrix_UB_21      0.0061618000
_diffrn_orient_matrix_UB_22      0.0343902000
_diffrn_orient_matrix_UB_23      0.0835290000
_diffrn_orient_matrix_UB_31      0.0215003000
_diffrn_orient_matrix_UB_32      -0.0225595000
_diffrn_orient_matrix_UB_33      0.1166223000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.657
_reflns_Friedel_fraction_full    0.768
_reflns_Friedel_fraction_max     0.715
_reflns_number_gt                6422
_reflns_number_total             8295
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 
;
 Flack x determined using 2032 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         8295
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0997
_refine_ls_restrained_S_all      1.087
_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+8.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2787
_refine_ls_wR_factor_ref         0.3014
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C016-C01V \\sim C016-C01W
 with sigma of 0.02
 C01V-C3 \\sim C01W-C3
 with sigma of 0.02
 C01V-C3A \\sim C01W-C3A
 with sigma of 0.02
3. Rigid bond restraints
 C01V, C01W, C016, C3A, C3, N4, N4A, N1, N1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C00H, C01M, C01N, C014
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C01U) \\sim Ueq, Uanis(C01D) \\sim Ueq, Uanis(C011) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C01V) \\sim Ueq, Uanis(C01W) \\sim Ueq, Uanis(C016) \\sim Ueq, Uanis(C3A)
\\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C00H) \\sim Ueq, Uanis(C01M) \\sim Ueq, Uanis(C01N) \\sim Ueq,
Uanis(C014) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=0.5*(1-FVAR(2))
 Sof(C1)=Sof(H1A)=Sof(H1B)=0.5*FVAR(2)
 Sof(N1A)=Sof(C3A)=Sof(N4A)=1-FVAR(2)
 Sof(N1)=Sof(C3)=Sof(N4)=FVAR(2)
 Sof(C01W)=Sof(H01F)=Sof(H01G)=1-FVAR(3)
 Sof(C01V)=Sof(H01D)=Sof(H01E)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C00W(H00A,H00B), C010(H01H,H01I), C014(H01A,H01B), C015(H01J,H01K), C01A(H01T,
 H01U), C01C(H01V,H01W), C01H(H3,H), C01K(H2,HA), C01R(H01R,H01S), C01U(H1,HB),
 C01V(H01D,H01E), C1(H1A,H1B), C1A(H1AA,H1AB), C01W(H01F,H01G)
6.b Aromatic/amide H refined with riding coordinates:
 C00Q(H00Q), C00R(H00R), C00Z(H00Z), C013(H013), C017(H017), C018(H018),
 C019(H019), C01B(H01C), C01E(H01O), C01F(H01X), C01G(H01P), C01I(H01Y),
 C01J(H01Q), C01L(H01L), C01M(H01M), C01N(H01N), C01P(H01Z), C01T(H01)
;
_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
Cl01 Cl 0.44037(7) 0.41701(5) 1.2012(3) 0.0823(7) Uani 1 1 d . . . . .
Cl02 Cl 0.44024(8) 0.75214(6) 0.1886(3) 0.0883(8) Uani 1 1 d . . . . .
N004 N 0.3115(2) 0.58484(12) 0.8972(6) 0.0511(13) Uani 1 1 d . . . . .
N005 N 0.34198(19) 0.56987(13) 0.9902(5) 0.0492(12) Uani 1 1 d . . . . .
N006 N 0.1869(2) 0.75360(13) 0.8891(7) 0.0537(14) Uani 1 1 d . . . . .
N007 N 0.33044(18) 0.51366(11) 0.8869(6) 0.0467(11) Uani 1 1 d . . . . .
N008 N 0.19733(19) 0.69592(12) 0.8006(6) 0.0470(11) Uani 1 1 d . . . . .
N009 N 0.15458(19) 0.40376(13) 1.9968(6) 0.0503(12) Uani 1 1 d . . . . .
N00A N 0.16685(19) 0.68257(12) 0.8979(6) 0.0516(13) Uani 1 1 d . . . . .
N00B N 0.1838(2) 0.42027(13) 1.9074(6) 0.0520(13) Uani 1 1 d . . . . .
N00C N 0.29955(19) 0.52871(11) 0.7936(5) 0.0463(11) Uani 1 1 d . . . . .
N00D N 0.1571(2) 0.74094(14) 0.9875(6) 0.0529(13) Uani 1 1 d . . . . .
N00E N 0.1689(2) 0.34843(12) 1.8875(6) 0.0517(12) Uani 1 1 d . . . . .
N00F N 0.1993(2) 0.36534(13) 1.7962(6) 0.0515(12) Uani 1 1 d . . . . .
C00G C 0.29015(18) 0.56360(13) 0.8051(6) 0.0414(12) Uani 1 1 d . . . . .
C00H C 0.0575(2) 0.35129(15) 2.0830(6) 0.0450(12) Uani 1 1 d . U . . .
C00I C 0.20650(19) 0.40032(14) 1.8109(7) 0.0452(13) Uani 1 1 d . . . . .
C00J C 0.20761(18) 0.73082(14) 0.8027(7) 0.0426(12) Uani 1 1 d . . . . .
C00K C 0.28862(18) 0.60108(12) 0.6011(6) 0.0415(12) Uani 1 1 d . . . . .
C00L C 0.4428(2) 0.51916(15) 1.0749(6) 0.0448(13) Uani 1 1 d . . . . .
C00M C 0.34980(19) 0.53425(14) 0.9818(6) 0.0435(13) Uani 1 1 d . . . . .
C00N C 0.14911(19) 0.36819(15) 1.9856(6) 0.0456(13) Uani 1 1 d . . . . .
C00O C 0.1492(2) 0.70540(18) 0.9886(6) 0.0502(14) Uani 1 1 d . . . . .
C00P C 0.0572(2) 0.69133(18) 1.0910(7) 0.0585(18) Uani 1 1 d . . . . .
C00Q C 0.2898(2) 0.63845(13) 0.5991(8) 0.0516(15) Uani 1 1 d . . . . .
H00Q H 0.269449 0.651539 0.660053 0.062 Uiso 1 1 calc R U . . .
C00R C 0.2130(2) 0.80500(14) 0.5990(8) 0.0551(16) Uani 1 1 d . . . . .
H00R H 0.235505 0.816743 0.659252 0.066 Uiso 1 1 calc R U . . .
C00S C 0.2108(2) 0.76773(13) 0.5975(7) 0.0461(14) Uani 1 1 d . . . . .
C00T C 0.2073(2) 0.43506(13) 1.5995(6) 0.0429(12) Uani 1 1 d . . . . .
N00U N 0.4721(2) 0.62727(18) 0.3090(8) 0.0747(18) Uani 1 1 d . . . . .
N00V N 0.0266(3) 0.84810(18) 0.4473(10) 0.091(2) Uani 1 1 d . . . . .
C00W C 0.2413(2) 0.4197(2) 1.7107(9) 0.0650(19) Uani 1 1 d . . . . .
H00A H 0.267992 0.403135 1.674471 0.078 Uiso 1 1 calc R U . . .
H00B H 0.260947 0.439014 1.754175 0.078 Uiso 1 1 calc R U . . .
C00X C 0.3529(2) 0.63827(19) 0.4173(8) 0.065(2) Uani 1 1 d . . . . .
C00Y C 0.4487(3) 0.65705(19) 0.3467(9) 0.065(2) Uani 1 1 d . . . . .
C00Z C 0.4716(2) 0.54599(17) 1.1378(7) 0.0562(15) Uani 1 1 d . . . . .
H00Z H 0.452739 0.564311 1.180751 0.067 Uiso 1 1 calc R U . . .
C010 C 0.3815(2) 0.5167(2) 1.0919(8) 0.0634(18) Uani 1 1 d . . . . .
H01H H 0.371113 0.491584 1.097013 0.076 Uiso 1 1 calc R U . . .
H01I H 0.371444 0.527965 1.175001 0.076 Uiso 1 1 calc R U . . .
C011 C 0.1475(3) 0.8089(2) 0.4238(9) 0.071(2) Uani 1 1 d . U . . .
N012 N 0.4730(3) 0.68309(17) 0.4106(10) 0.090(2) Uani 1 1 d . . . . .
C013 C 0.3513(3) 0.6008(2) 0.4183(8) 0.0662(18) Uani 1 1 d . . . . .
H013 H 0.372203 0.588054 0.357514 0.079 Uiso 1 1 calc R U . . .
C014 C 0.1187(2) 0.34918(18) 2.0954(8) 0.0597(16) Uani 1 1 d . U . . .
H01A H 0.129557 0.324098 2.096182 0.072 Uiso 1 1 calc R U . . .
H01B H 0.129509 0.359609 2.179378 0.072 Uiso 1 1 calc R U . . .
C015 C 0.2550(2) 0.5817(2) 0.7025(9) 0.0627(18) Uani 1 1 d . . . . .
H01J H 0.232584 0.563742 0.658728 0.075 Uiso 1 1 calc R U . . .
H01K H 0.230737 0.598644 0.745655 0.075 Uiso 1 1 calc R U . . .
C016 C 0.1446(2) 0.4634(2) 1.3907(9) 0.0668(18) Uani 1 1 d D U . . .
C017 C 0.1458(3) 0.4270(2) 1.4177(8) 0.0654(18) Uani 1 1 d . . . . .
H017 H 0.124549 0.411494 1.366933 0.079 Uiso 1 1 calc R U . . .
C018 C 0.1769(3) 0.41331(14) 1.5153(7) 0.0502(15) Uani 1 1 d . . . . .
H018 H 0.178046 0.388528 1.526900 0.060 Uiso 1 1 calc R U . . .
C019 C 0.1454(3) 0.7721(2) 0.4201(9) 0.073(2) Uani 1 1 d . . . . .
H019 H 0.122186 0.760897 0.360097 0.088 Uiso 1 1 calc R U . . .
C01A C 0.2433(3) 0.7467(2) 0.6978(9) 0.074(2) Uani 1 1 d . . . . .
H01T H 0.262959 0.727563 0.653163 0.088 Uiso 1 1 calc R U . . .
H01U H 0.270061 0.762419 0.738742 0.088 Uiso 1 1 calc R U . . .
C01B C 0.2063(3) 0.47196(15) 1.5782(8) 0.061(2) Uani 1 1 d . . . . .
H01C H 0.225864 0.487401 1.633057 0.073 Uiso 1 1 calc R U . . .
C01C C 0.1188(3) 0.6893(2) 1.1044(9) 0.083(3) Uani 1 1 d . . . . .
H01V H 0.129682 0.701715 1.184493 0.099 Uiso 1 1 calc R U . . .
H01W H 0.129429 0.664290 1.113517 0.099 Uiso 1 1 calc R U . . .
C01D C 0.0509(3) 0.8291(2) 0.3582(9) 0.0645(18) Uani 1 1 d . U . . .
C01E C 0.3198(2) 0.58269(14) 0.5067(7) 0.0515(15) Uani 1 1 d . . . . .
H01O H 0.318920 0.557705 0.504336 0.062 Uiso 1 1 calc R U . . .
C01F C 0.1820(3) 0.82452(17) 0.5117(10) 0.072(2) Uani 1 1 d . . . . .
H01X H 0.184723 0.849447 0.512833 0.086 Uiso 1 1 calc R U . . .
C01G C 0.3212(2) 0.65588(15) 0.5068(9) 0.064(2) Uani 1 1 d . . . . .
H01P H 0.320779 0.680873 0.505291 0.077 Uiso 1 1 calc R U . . .
C01H C 0.500000 0.7645(2) 0.2706(12) 0.061(2) Uani 1 2 d S T P . .
H3 H 0.500000 0.753565 0.357672 0.074 Uiso 1 2 calc R U P . .
H H 0.499999 0.790363 0.282503 0.074 Uiso 1 2 calc R U P . .
C01I C 0.1769(3) 0.75152(16) 0.5032(8) 0.0565(17) Uani 1 1 d . . . . .
H01Y H 0.175715 0.726595 0.496656 0.068 Uiso 1 1 calc R U . . .
C01J C 0.4712(3) 0.49400(16) 1.0045(8) 0.0605(16) Uani 1 1 d . . . . .
H01Q H 0.452373 0.476727 0.956070 0.073 Uiso 1 1 calc R U . . .
C01K C 0.500000 0.4322(2) 1.2767(11) 0.060(2) Uani 1 2 d S T P . .
H2 H 0.499999 0.458272 1.276149 0.072 Uiso 1 2 calc R U P . .
HA H 0.500001 0.424442 1.368339 0.072 Uiso 1 2 calc R U P . .
C01L C 0.1752(3) 0.48558(17) 1.4720(10) 0.079(3) Uani 1 1 d . . . . .
H01L H 0.175301 0.510198 1.456117 0.095 Uiso 1 1 calc R U . . .
C01M C 0.0287(3) 0.3685(3) 2.1739(11) 0.098(3) Uani 1 1 d . U . . .
H01M H 0.047148 0.381084 2.239805 0.117 Uiso 1 1 calc R U . . .
C01N C 0.0287(3) 0.3339(2) 1.9886(9) 0.075(2) Uani 1 1 d . U . . .
H01N H 0.047261 0.321710 1.922197 0.090 Uiso 1 1 calc R U . . .
N01O N 0.0285(3) 0.8047(3) 0.2872(10) 0.113(3) Uani 1 1 d . . . . .
C01P C 0.0284(2) 0.7214(2) 1.1273(9) 0.081(3) Uani 1 1 d . . . . .
H01Z H 0.047146 0.742078 1.152143 0.097 Uiso 1 1 calc R U . . .
C01R C 0.3878(3) 0.6588(3) 0.3207(11) 0.098(4) Uani 1 1 d . . . . .
H01R H 0.376577 0.683769 0.321905 0.118 Uiso 1 1 calc R U . . .
H01S H 0.380874 0.649549 0.232555 0.118 Uiso 1 1 calc R U . . .
C01T C 0.0284(3) 0.6628(2) 1.0517(15) 0.122(5) Uani 1 1 d . . . . .
H01 H 0.046852 0.642369 1.023468 0.147 Uiso 1 1 calc R U . . .
C01U C 0.1120(4) 0.8308(3) 0.3325(12) 0.104(3) Uani 1 1 d . U . . .
H1 H 0.118733 0.822901 0.242525 0.125 Uiso 1 1 calc R U . . .
HB H 0.123509 0.855727 0.338369 0.125 Uiso 1 1 calc R U . . .
C01V C 0.1134(4) 0.4727(3) 1.2599(12) 0.040(3) Uani 0.47(2) 1 d D U P A 1
H01D H 0.122460 0.497090 1.234559 0.048 Uiso 0.47(2) 1 calc R U P A 1
H01E H 0.126501 0.456875 1.190462 0.048 Uiso 0.47(2) 1 calc R U P A 1
Cl1 Cl 0.05942(9) 0.42244(10) -0.2812(5) 0.1396(18) Uani 1 1 d . . . . .
C1 C 0.000000 0.4043(7) -0.222(3) 0.089(8) Uani 0.57(3) 2 d S T P B 1
H1A H 0.000000 0.406536 -0.126849 0.106 Uiso 0.57(3) 2 calc R U P B 1
H1B H 0.000002 0.378802 -0.242959 0.106 Uiso 0.57(3) 2 calc R U P B 1
C1A C 0.000000 0.4282(6) -0.158(2) 0.053(7) Uani 0.43(3) 2 d S T P B 2
H1AA H -0.000001 0.451821 -0.116637 0.064 Uiso 0.43(3) 2 calc R U P B 2
H1AB H 0.000002 0.409781 -0.089869 0.064 Uiso 0.43(3) 2 calc R U P B 2
N1 N 0.0271(4) 0.4565(3) 1.1594(12) 0.048(3) Uani 0.444(12) 1 d . U P A 1
C3 C 0.0530(4) 0.4695(3) 1.2672(14) 0.031(2) Uani 0.444(12) 1 d . U P A 1
N4 N 0.0270(4) 0.4803(5) 1.3763(16) 0.066(4) Uani 0.444(12) 1 d . U P A 1
N1A N 0.0298(7) 0.4604(6) 1.305(3) 0.139(9) Uani 0.556(12) 1 d . U P A 2
C3A C 0.0493(8) 0.4917(6) 1.348(2) 0.093(5) Uani 0.556(12) 1 d . U P A 2
N4A N 0.0263(7) 0.5150(4) 1.423(2) 0.112(6) Uani 0.556(12) 1 d . U P A 2
C01W C 0.1115(7) 0.4924(5) 1.323(2) 0.090(5) Uani 0.53(2) 1 d D U P A 2
H01F H 0.117676 0.490540 1.228253 0.107 Uiso 0.53(2) 1 calc R U P A 2
H01G H 0.125381 0.515583 1.351002 0.107 Uiso 0.53(2) 1 calc R U P A 2


_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
Cl01 C01K 1.740(6) . ?
Cl02 C01H 1.741(7) . ?
N004 N005 1.323(8) . ?
N004 C00G 1.328(8) . ?
N005 C00M 1.342(7) . ?
N006 N00D 1.320(8) . ?
N006 C00J 1.318(8) . ?
N007 N00C 1.331(7) . ?
N007 C00M 1.317(8) . ?
N008 N00A 1.330(8) . ?
N008 C00J 1.323(7) . ?
N009 N00B 1.306(8) . ?
N009 C00N 1.335(8) . ?
N00A C00O 1.323(9) . ?
N00B C00I 1.345(8) . ?
N00C C00G 1.323(7) . ?
N00D C00O 1.337(8) . ?
N00E N00F 1.341(8) . ?
N00E C00N 1.326(8) . ?
N00F C00I 1.322(7) . ?
C00G C015 1.506(9) . ?
C00H C014 1.505(8) . ?
C00H C01M 1.323(10) . ?
C00H C01N 1.350(10) . ?
C00I C00W 1.507(9) . ?
C00J C01A 1.495(9) . ?
C00K C00Q 1.391(7) . ?
C00K C015 1.499(9) . ?
C00K C01E 1.400(9) . ?
C00L C00Z 1.376(8) . ?
C00L C010 1.512(8) . ?
C00L C01J 1.366(9) . ?
C00M C010 1.505(8) . ?
C00N C014 1.511(9) . ?
C00O C01C 1.510(9) . ?
C00P C01C 1.515(8) . ?
C00P C01P 1.372(10) . ?
C00P C01T 1.334(11) . ?
C00Q H00Q 0.9300 . ?
C00Q C01G 1.371(10) . ?
C00R H00R 0.9300 . ?
C00R C00S 1.388(7) . ?
C00R C01F 1.372(10) . ?
C00S C01A 1.508(9) . ?
C00S C01I 1.400(9) . ?
C00T C00W 1.509(10) . ?
C00T C018 1.390(8) . ?
C00T C01B 1.390(7) . ?
N00U N00U 1.362(11) 4_655 ?
N00U C00Y 1.305(10) . ?
N00V N00V 1.300(15) 4 ?
N00V C01D 1.289(12) . ?
C00W H00A 0.9700 . ?
C00W H00B 0.9700 . ?
C00X C013 1.393(10) . ?
C00X C01G 1.360(11) . ?
C00X C01R 1.504(10) . ?
C00Y N012 1.307(12) . ?
C00Y C01R 1.512(10) . ?
C00Z C00Z 1.391(12) 4_655 ?
C00Z H00Z 0.9300 . ?
C010 H01H 0.9700 . ?
C010 H01I 0.9700 . ?
C011 C019 1.370(11) . ?
C011 C01F 1.355(12) . ?
C011 C01U 1.506(11) . ?
N012 N012 1.322(15) 4_655 ?
C013 H013 0.9300 . ?
C013 C01E 1.359(10) . ?
C014 H01A 0.9700 . ?
C014 H01B 0.9700 . ?
C015 H01J 0.9700 . ?
C015 H01K 0.9700 . ?
C016 C017 1.384(10) . ?
C016 C01L 1.384(12) . ?
C016 C01V 1.565(13) . ?
C016 C01W 1.513(16) . ?
C017 H017 0.9300 . ?
C017 C018 1.345(10) . ?
C018 H018 0.9300 . ?
C019 H019 0.9300 . ?
C019 C01I 1.373(10) . ?
C01A H01T 0.9700 . ?
C01A H01U 0.9700 . ?
C01B H01C 0.9300 . ?
C01B C01L 1.410(12) . ?
C01C H01V 0.9700 . ?
C01C H01W 0.9700 . ?
C01D N01O 1.280(11) . ?
C01D C01U 1.519(11) . ?
C01E H01O 0.9300 . ?
C01F H01X 0.9300 . ?
C01G H01P 0.9300 . ?
C01H H3 0.9700 . ?
C01H H 0.9700 . ?
C01I H01Y 0.9300 . ?
C01J C01J 1.407(13) 4_655 ?
C01J H01Q 0.9300 . ?
C01K H2 0.9700 . ?
C01K HA 0.9700 . ?
C01L H01L 0.9300 . ?
C01M C01M 1.404(15) 4 ?
C01M H01M 0.9300 . ?
C01N C01N 1.401(14) 4 ?
C01N H01N 0.9300 . ?
N01O N01O 1.394(14) 4 ?
C01P C01P 1.387(12) 4 ?
C01P H01Z 0.9300 . ?
C01R H01R 0.9700 . ?
C01R H01S 0.9700 . ?
C01T C01T 1.387(17) 4 ?
C01T H01 0.9300 . ?
C01U H1 0.9700 . ?
C01U HB 0.9700 . ?
C01V H01D 0.9700 . ?
C01V H01E 0.9700 . ?
C01V C3 1.483(14) . ?
Cl1 C1 1.709(13) . ?
Cl1 C1A 1.928(16) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
N1 N1 1.327(18) 4 ?
N1 C3 1.349(18) . ?
C3 N4 1.33(2) . ?
N4 N4 1.32(2) 4 ?
N1A N1A 1.46(3) 4 ?
N1A C3A 1.33(3) . ?
C3A N4A 1.29(3) . ?
C3A C01W 1.54(3) . ?
N4A N4A 1.29(3) 4 ?
C01W H01F 0.9700 . ?
C01W H01G 0.9700 . ?

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
N005 N004 C00G 118.0(4) . . ?
N004 N005 C00M 116.8(5) . . ?
C00J N006 N00D 118.8(5) . . ?
C00M N007 N00C 118.4(4) . . ?
C00J N008 N00A 117.5(5) . . ?
N00B N009 C00N 117.5(5) . . ?
C00O N00A N008 117.1(5) . . ?
N009 N00B C00I 117.9(5) . . ?
C00G N00C N007 116.7(5) . . ?
N006 N00D C00O 116.1(5) . . ?
C00N N00E N00F 117.2(5) . . ?
C00I N00F N00E 117.3(5) . . ?
N004 C00G C015 116.2(5) . . ?
N00C C00G N004 125.2(5) . . ?
N00C C00G C015 118.5(6) . . ?
C01M C00H C014 119.7(7) . . ?
C01M C00H C01N 116.5(6) . . ?
C01N C00H C014 123.6(6) . . ?
N00B C00I C00W 117.1(5) . . ?
N00F C00I N00B 124.8(5) . . ?
N00F C00I C00W 118.1(6) . . ?
N006 C00J N008 124.7(6) . . ?
N006 C00J C01A 116.1(6) . . ?
N008 C00J C01A 119.2(6) . . ?
C00Q C00K C015 120.2(6) . . ?
C00Q C00K C01E 117.9(5) . . ?
C01E C00K C015 121.9(5) . . ?
C00Z C00L C010 119.8(6) . . ?
C01J C00L C00Z 118.5(5) . . ?
C01J C00L C010 121.5(6) . . ?
N005 C00M C010 117.1(6) . . ?
N007 C00M N005 124.7(5) . . ?
N007 C00M C010 118.2(5) . . ?
N009 C00N C014 116.8(6) . . ?
N00E C00N N009 125.2(6) . . ?
N00E C00N C014 118.0(5) . . ?
N00A C00O N00D 125.6(6) . . ?
N00A C00O C01C 116.3(6) . . ?
N00D C00O C01C 118.1(7) . . ?
C01P C00P C01C 121.8(7) . . ?
C01T C00P C01C 120.8(7) . . ?
C01T C00P C01P 117.2(6) . . ?
C00K C00Q H00Q 120.2 . . ?
C01G C00Q C00K 119.6(6) . . ?
C01G C00Q H00Q 120.2 . . ?
C00S C00R H00R 120.0 . . ?
C01F C00R H00R 120.0 . . ?
C01F C00R C00S 120.1(7) . . ?
C00R C00S C01A 119.4(7) . . ?
C00R C00S C01I 117.4(6) . . ?
C01I C00S C01A 123.1(6) . . ?
C018 C00T C00W 122.0(5) . . ?
C01B C00T C00W 119.9(6) . . ?
C01B C00T C018 118.1(6) . . ?
C00Y N00U N00U 116.1(4) . 4_655 ?
C01D N00V N00V 117.4(5) . 4 ?
C00I C00W C00T 111.8(5) . . ?
C00I C00W H00A 109.2 . . ?
C00I C00W H00B 109.2 . . ?
C00T C00W H00A 109.2 . . ?
C00T C00W H00B 109.2 . . ?
H00A C00W H00B 107.9 . . ?
C013 C00X C01R 121.9(8) . . ?
C01G C00X C013 117.4(6) . . ?
C01G C00X C01R 120.7(7) . . ?
N00U C00Y C01R 114.7(8) . . ?
N012 C00Y N00U 125.0(7) . . ?
N012 C00Y C01R 120.1(8) . . ?
C00L C00Z C00Z 120.7(3) . 4_655 ?
C00L C00Z H00Z 119.6 . . ?
C00Z C00Z H00Z 119.6 4_655 . ?
C00L C010 H01H 108.8 . . ?
C00L C010 H01I 108.8 . . ?
C00M C010 C00L 113.6(5) . . ?
C00M C010 H01H 108.8 . . ?
C00M C010 H01I 108.8 . . ?
H01H C010 H01I 107.7 . . ?
C019 C011 C01U 120.2(9) . . ?
C01F C011 C019 118.0(7) . . ?
C01F C011 C01U 121.9(8) . . ?
C00Y N012 N012 117.0(4) . 4_655 ?
C00X C013 H013 119.4 . . ?
C01E C013 C00X 121.2(7) . . ?
C01E C013 H013 119.4 . . ?
C00H C014 C00N 113.8(5) . . ?
C00H C014 H01A 108.8 . . ?
C00H C014 H01B 108.8 . . ?
C00N C014 H01A 108.8 . . ?
C00N C014 H01B 108.8 . . ?
H01A C014 H01B 107.7 . . ?
C00G C015 H01J 109.2 . . ?
C00G C015 H01K 109.2 . . ?
C00K C015 C00G 111.9(4) . . ?
C00K C015 H01J 109.2 . . ?
C00K C015 H01K 109.2 . . ?
H01J C015 H01K 107.9 . . ?
C017 C016 C01L 117.1(7) . . ?
C017 C016 C01V 113.1(8) . . ?
C017 C016 C01W 143.0(10) . . ?
C01L C016 C01V 129.5(7) . . ?
C01L C016 C01W 97.8(11) . . ?
C016 C017 H017 119.1 . . ?
C018 C017 C016 121.8(7) . . ?
C018 C017 H017 119.1 . . ?
C00T C018 H018 118.9 . . ?
C017 C018 C00T 122.1(6) . . ?
C017 C018 H018 118.9 . . ?
C011 C019 H019 119.3 . . ?
C011 C019 C01I 121.3(7) . . ?
C01I C019 H019 119.3 . . ?
C00J C01A C00S 112.0(5) . . ?
C00J C01A H01T 109.2 . . ?
C00J C01A H01U 109.2 . . ?
C00S C01A H01T 109.2 . . ?
C00S C01A H01U 109.2 . . ?
H01T C01A H01U 107.9 . . ?
C00T C01B H01C 120.6 . . ?
C00T C01B C01L 118.8(6) . . ?
C01L C01B H01C 120.6 . . ?
C00O C01C C00P 113.6(5) . . ?
C00O C01C H01V 108.8 . . ?
C00O C01C H01W 108.8 . . ?
C00P C01C H01V 108.8 . . ?
C00P C01C H01W 108.8 . . ?
H01V C01C H01W 107.7 . . ?
N00V C01D C01U 123.4(9) . . ?
N01O C01D N00V 125.7(7) . . ?
N01O C01D C01U 110.7(9) . . ?
C00K C01E H01O 119.6 . . ?
C013 C01E C00K 120.9(5) . . ?
C013 C01E H01O 119.6 . . ?
C00R C01F H01X 118.7 . . ?
C011 C01F C00R 122.6(6) . . ?
C011 C01F H01X 118.7 . . ?
C00Q C01G H01P 118.5 . . ?
C00X C01G C00Q 122.9(5) . . ?
C00X C01G H01P 118.5 . . ?
Cl02 C01H Cl02 114.1(7) . 4_655 ?
Cl02 C01H H3 108.7 . . ?
Cl02 C01H H3 108.7 4_655 . ?
Cl02 C01H H 108.7 . . ?
Cl02 C01H H 108.7 4_655 . ?
H3 C01H H 107.6 . . ?
C00S C01I H01Y 119.7 . . ?
C019 C01I C00S 120.5(6) . . ?
C019 C01I H01Y 119.7 . . ?
C00L C01J C01J 120.6(4) . 4_655 ?
C00L C01J H01Q 119.7 . . ?
C01J C01J H01Q 119.7 4_655 . ?
Cl01 C01K Cl01 113.8(6) 4_655 . ?
Cl01 C01K H2 108.8 4_655 . ?
Cl01 C01K H2 108.8 . . ?
Cl01 C01K HA 108.8 . . ?
Cl01 C01K HA 108.8 4_655 . ?
H2 C01K HA 107.7 . . ?
C016 C01L C01B 122.0(6) . . ?
C016 C01L H01L 119.0 . . ?
C01B C01L H01L 119.0 . . ?
C00H C01M C01M 122.1(4) . 4 ?
C00H C01M H01M 119.0 . . ?
C01M C01M H01M 119.0 4 . ?
C00H C01N C01N 121.4(4) . 4 ?
C00H C01N H01N 119.3 . . ?
C01N C01N H01N 119.3 4 . ?
C01D N01O N01O 115.3(5) . 4 ?
C00P C01P C01P 120.9(4) . 4 ?
C00P C01P H01Z 119.6 . . ?
C01P C01P H01Z 119.6 4 . ?
C00X C01R C00Y 115.1(6) . . ?
C00X C01R H01R 108.5 . . ?
C00X C01R H01S 108.5 . . ?
C00Y C01R H01R 108.5 . . ?
C00Y C01R H01S 108.5 . . ?
H01R C01R H01S 107.5 . . ?
C00P C01T C01T 121.9(5) . 4 ?
C00P C01T H01 119.1 . . ?
C01T C01T H01 119.1 4 . ?
C011 C01U C01D 116.1(7) . . ?
C011 C01U H1 108.3 . . ?
C011 C01U HB 108.3 . . ?
C01D C01U H1 108.3 . . ?
C01D C01U HB 108.3 . . ?
H1 C01U HB 107.4 . . ?
C016 C01V H01D 108.5 . . ?
C016 C01V H01E 108.5 . . ?
H01D C01V H01E 107.5 . . ?
C3 C01V C016 115.2(9) . . ?
C3 C01V H01D 108.5 . . ?
C3 C01V H01E 108.5 . . ?
Cl1 C1 Cl1 116.4(14) . 4 ?
Cl1 C1 H1A 108.2 . . ?
Cl1 C1 H1A 108.2 4 . ?
Cl1 C1 H1B 108.2 . . ?
Cl1 C1 H1B 108.2 4 . ?
H1A C1 H1B 107.3 . . ?
Cl1 C1A Cl1 97.8(11) . 4 ?
Cl1 C1A H1AA 112.2 4 . ?
Cl1 C1A H1AA 112.2 . . ?
Cl1 C1A H1AB 112.2 . . ?
Cl1 C1A H1AB 112.2 4 . ?
H1AA C1A H1AB 109.8 . . ?
N1 N1 C3 117.9(6) 4 . ?
N1 C3 C01V 117.0(11) . . ?
N1 C3 N4 123.7(11) . . ?
N4 C3 C01V 119.3(12) . . ?
N4 N4 C3 118.3(8) 4 . ?
N1A C3A C01W 108(2) . . ?
N4A C3A N1A 129(2) . . ?
N4A C3A C01W 121(2) . . ?
C3A N4A N4A 115.9(13) . 4 ?
C016 C01W C3A 116.2(13) . . ?
C016 C01W H01F 108.2 . . ?
C016 C01W H01G 108.2 . . ?
C3A C01W H01F 108.2 . . ?
C3A C01W H01G 108.2 . . ?
H01F C01W H01G 107.4 . . ?

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
N004 N005 C00M N007 1.6(8) . . . . ?
N004 N005 C00M C010 -176.3(5) . . . . ?
N004 C00G C015 C00K 76.9(8) . . . . ?
N005 N004 C00G N00C -4.5(8) . . . . ?
N005 N004 C00G C015 179.0(5) . . . . ?
N005 C00M C010 C00L -83.4(8) . . . . ?
N006 N00D C00O N00A -2.5(8) . . . . ?
N006 N00D C00O C01C 175.8(5) . . . . ?
N006 C00J C01A C00S -72.1(9) . . . . ?
N007 N00C C00G N004 4.1(8) . . . . ?
N007 N00C C00G C015 -179.5(5) . . . . ?
N007 C00M C010 C00L 98.5(6) . . . . ?
N008 N00A C00O N00D 3.4(8) . . . . ?
N008 N00A C00O C01C -174.9(5) . . . . ?
N008 C00J C01A C00S 105.5(7) . . . . ?
N009 N00B C00I N00F 3.4(9) . . . . ?
N009 N00B C00I C00W -178.5(5) . . . . ?
N009 C00N C014 C00H 81.1(7) . . . . ?
N00A N008 C00J N006 -4.7(8) . . . . ?
N00A N008 C00J C01A 177.9(5) . . . . ?
N00A C00O C01C C00P -98.2(8) . . . . ?
N00B N009 C00N N00E -3.3(8) . . . . ?
N00B N009 C00N C014 175.5(5) . . . . ?
N00B C00I C00W C00T -85.5(8) . . . . ?
N00C N007 C00M N005 -1.9(8) . . . . ?
N00C N007 C00M C010 175.9(5) . . . . ?
N00C C00G C015 C00K -99.8(7) . . . . ?
N00D N006 C00J N008 5.7(9) . . . . ?
N00D N006 C00J C01A -176.9(5) . . . . ?
N00D C00O C01C C00P 83.3(9) . . . . ?
N00E N00F C00I N00B -2.9(8) . . . . ?
N00E N00F C00I C00W 179.0(5) . . . . ?
N00E C00N C014 C00H -100.0(6) . . . . ?
N00F N00E C00N N009 3.7(8) . . . . ?
N00F N00E C00N C014 -175.1(5) . . . . ?
N00F C00I C00W C00T 92.8(7) . . . . ?
C00G N004 N005 C00M 1.5(8) . . . . ?
C00J N006 N00D C00O -1.9(8) . . . . ?
C00J N008 N00A C00O 0.2(7) . . . . ?
C00K C00Q C01G C00X -1.7(10) . . . . ?
C00M N007 N00C C00G -0.8(7) . . . . ?
C00N N009 N00B C00I -0.3(8) . . . . ?
C00N N00E N00F C00I -0.6(7) . . . . ?
C00Q C00K C015 C00G -108.7(7) . . . . ?
C00Q C00K C01E C013 1.7(9) . . . . ?
C00R C00S C01A C00J 106.2(7) . . . . ?
C00R C00S C01I C019 -2.9(10) . . . . ?
C00S C00R C01F C011 1.6(11) . . . . ?
C00T C01B C01L C016 1.7(10) . . . . ?
N00U N00U C00Y N012 -16.1(10) 4_655 . . . ?
N00U N00U C00Y C01R 168.7(5) 4_655 . . . ?
N00U C00Y N012 N012 16.2(10) . . . 4_655 ?
N00U C00Y C01R C00X 78.2(12) . . . . ?
N00V N00V C01D N01O -15.2(11) 4 . . . ?
N00V N00V C01D C01U 170.5(6) 4 . . . ?
N00V C01D N01O N01O 14.9(11) . . . 4 ?
N00V C01D C01U C011 81.7(12) . . . . ?
C00W C00T C018 C017 178.8(6) . . . . ?
C00W C00T C01B C01L 178.7(6) . . . . ?
C00X C013 C01E C00K -1.1(11) . . . . ?
C00Z C00L C010 C00M 96.5(8) . . . . ?
C00Z C00L C01J C01J 4.7(7) . . . 4_655 ?
C010 C00L C00Z C00Z 171.5(4) . . . 4_655 ?
C010 C00L C01J C01J -171.4(4) . . . 4_655 ?
C011 C019 C01I C00S 2.2(11) . . . . ?
N012 C00Y C01R C00X -97.3(10) . . . . ?
C013 C00X C01G C00Q 2.3(11) . . . . ?
C013 C00X C01R C00Y -71.9(13) . . . . ?
C014 C00H C01M C01M -174.0(4) . . . 4 ?
C014 C00H C01N C01N 173.8(4) . . . 4 ?
C015 C00K C00Q C01G 179.3(6) . . . . ?
C015 C00K C01E C013 -177.9(6) . . . . ?
C016 C017 C018 C00T 3.6(11) . . . . ?
C016 C01V C3 N1 -142.6(10) . . . . ?
C016 C01V C3 N4 39.6(16) . . . . ?
C017 C016 C01L C01B -0.1(11) . . . . ?
C017 C016 C01V C3 73.6(12) . . . . ?
C017 C016 C01W C3A 45(3) . . . . ?
C018 C00T C00W C00I -62.3(9) . . . . ?
C018 C00T C01B C01L -0.7(9) . . . . ?
C019 C011 C01F C00R -2.3(12) . . . . ?
C019 C011 C01U C01D 67.7(13) . . . . ?
C01A C00S C01I C019 175.6(7) . . . . ?
C01B C00T C00W C00I 118.3(6) . . . . ?
C01B C00T C018 C017 -1.9(9) . . . . ?
C01C C00P C01P C01P -173.2(5) . . . 4 ?
C01C C00P C01T C01T 173.3(5) . . . 4 ?
C01E C00K C00Q C01G -0.4(9) . . . . ?
C01E C00K C015 C00G 71.0(9) . . . . ?
C01F C00R C00S C01A -177.5(6) . . . . ?
C01F C00R C00S C01I 1.1(9) . . . . ?
C01F C011 C019 C01I 0.4(12) . . . . ?
C01F C011 C01U C01D -112.0(10) . . . . ?
C01G C00X C013 C01E -0.9(11) . . . . ?
C01G C00X C01R C00Y 108.7(9) . . . . ?
C01I C00S C01A C00J -72.3(10) . . . . ?
C01J C00L C00Z C00Z -4.7(7) . . . 4_655 ?
C01J C00L C010 C00M -87.4(8) . . . . ?
C01L C016 C017 C018 -2.5(11) . . . . ?
C01L C016 C01V C3 -114.1(10) . . . . ?
C01L C016 C01W C3A -115.8(19) . . . . ?
C01M C00H C014 C00N -115.6(8) . . . . ?
C01M C00H C01N C01N -0.8(9) . . . 4 ?
C01N C00H C014 C00N 69.9(9) . . . . ?
C01N C00H C01M C01M 0.8(9) . . . 4 ?
N01O C01D C01U C011 -93.4(12) . . . . ?
C01P C00P C01C C00O -84.4(11) . . . . ?
C01P C00P C01T C01T -2.4(11) . . . 4 ?
C01R C00X C013 C01E 179.7(7) . . . . ?
C01R C00X C01G C00Q -178.2(7) . . . . ?
C01R C00Y N012 N012 -168.8(5) . . . 4_655 ?
C01T C00P C01C C00O 100.2(11) . . . . ?
C01T C00P C01P C01P 2.3(11) . . . 4 ?
C01U C011 C019 C01I -179.4(8) . . . . ?
C01U C011 C01F C00R 177.4(8) . . . . ?
C01U C01D N01O N01O -170.2(5) . . . 4 ?
C01V C016 C017 C018 170.8(7) . . . . ?
C01V C016 C01L C01B -172.1(8) . . . . ?
C01V C3 N4 N4 173.9(6) . . . 4 ?
N1 N1 C3 C01V -173.9(6) 4 . . . ?
N1 N1 C3 N4 3.8(15) 4 . . . ?
N1 C3 N4 N4 -3.8(15) . . . 4 ?
N1A N1A C3A N4A 24(3) 4 . . . ?
N1A N1A C3A C01W -170.4(11) 4 . . . ?
N1A C3A N4A N4A -25(3) . . . 4 ?
N1A C3A C01W C016 -60(3) . . . . ?
N4A C3A C01W C016 106(2) . . . . ?
C01W C016 C017 C018 -161.0(17) . . . . ?
C01W C016 C01L C01B 167.0(10) . . . . ?
C01W C3A N4A N4A 171.0(13) . . . 4 ?

_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 2.343
_oxdiff_exptl_absorpt_empirical_full_min 0.635
####################################################################### 
# 
# 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_ch2_8_400004
_database_code_depnum_ccdc_archive 'CCDC 2233701'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2022-12-31 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_audit_creation_date             2019-06-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C20 H16 N8)'
_chemical_formula_sum            'C40 H32 N16'
_chemical_formula_weight         736.81
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N'
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'

_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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.1552(3)
_cell_length_b                   33.0314(8)
_cell_length_c                   11.9403(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.094(2)
_cell_angle_gamma                90
_cell_volume                     3605.59(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3802
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.8960
_cell_measurement_theta_min      4.5520
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light purple'
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14596
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.136
_diffrn_reflns_theta_min         3.942
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -104.00 -71.00   1.00   12.81    --  -40.81 -38.00 -60.00   33
  2  ω    -44.00 -19.00   1.00   12.81    --  -40.81 -38.00 -60.00   25
  3  ω    -65.00  32.00   1.00   12.81    --  -40.81  38.00 120.00   97
  4  ω     25.00  97.00   1.00   12.81    --   40.81-125.00   0.00   72
  5  ω     49.00  75.00   1.00   12.81    --   40.81-125.00-180.00   26
  6  ω     35.00 132.00   1.00   55.24    --  107.77 -45.00 120.00   97
  7  ω     32.00 107.00   1.00   55.24    --  107.77 -95.00 150.00   75
  8  ω    140.00 178.00   1.00   55.24    --  107.77 125.00   0.00   38
  9  ω     99.00 124.00   1.00   55.24    --  107.77 125.00   0.00   25
 10  ω     85.00 177.00   1.00   55.24    --  107.77  61.00 -90.00   92
 11  ω     68.00 165.00   1.00   55.24    --  107.77   0.00  30.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0360320000
_diffrn_orient_matrix_UB_12      -0.0448322000
_diffrn_orient_matrix_UB_13      0.0237377000
_diffrn_orient_matrix_UB_21      -0.1592961000
_diffrn_orient_matrix_UB_22      -0.0073329000
_diffrn_orient_matrix_UB_23      0.0303183000
_diffrn_orient_matrix_UB_31      -0.0418428000
_diffrn_orient_matrix_UB_32      -0.0104905000
_diffrn_orient_matrix_UB_33      -0.1233263000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5019
_reflns_number_total             7203
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.79
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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         0.254
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7203
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0499
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0402P)²+0.8181P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1243
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C013(H01A,H01B), C018(H01K,H01L), C01A(H01C,H01D), C01F(H01N,H01O), C01G(H01P,
 H01Q), C01I(H01F,H01G), C01J(H01I,H01J), C01K(H01R,H01S)
2.b Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00O(H00O), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W),
 C00Y(H00Y), C012(H012), C014(H014), C015(H015), C016(H016), C017(H017),
 C019(H019), C01B(H01M), C01E(H01E), C01H(H01H)
;
_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
N001 N 0.1388(2) 0.29854(5) 0.51380(14) 0.0329(4) Uani 1 1 d . . . . .
N002 N 0.2237(2) 0.32912(5) 0.54982(14) 0.0333(4) Uani 1 1 d . . . . .
N003 N 0.3138(2) 0.81372(6) 0.87866(14) 0.0332(4) Uani 1 1 d . . . . .
N004 N 0.4088(2) 0.78994(6) 0.82972(14) 0.0340(4) Uani 1 1 d . . . . .
N005 N 0.2793(2) 0.80021(6) 0.65509(15) 0.0373(4) Uani 1 1 d . . . . .
N006 N 0.2293(2) 0.30611(6) 0.33291(15) 0.0374(4) Uani 1 1 d . . . . .
N007 N 0.1835(2) 0.82327(6) 0.70385(15) 0.0367(4) Uani 1 1 d . . . . .
N008 N 0.3137(2) 0.33644(6) 0.36939(15) 0.0378(4) Uani 1 1 d . . . . .
N009 N 0.2843(2) 0.54674(6) 0.75461(16) 0.0389(5) Uani 1 1 d . . . . .
N00A N 0.3465(2) 0.58296(6) 0.76256(16) 0.0412(5) Uani 1 1 d . . . . .
N00B N 0.3370(3) 1.05254(6) 0.64695(17) 0.0459(5) Uani 1 1 d . . . . .
N00C N 0.2196(3) 0.55142(6) 0.94277(17) 0.0480(5) Uani 1 1 d . . . . .
C00D C 0.3068(2) 0.34730(6) 0.47656(17) 0.0282(4) Uani 1 1 d . . . . .
N00E N 0.2820(3) 0.58779(6) 0.95109(17) 0.0476(5) Uani 1 1 d . . . . .
N00F N 0.2668(3) 1.07815(7) 0.57663(17) 0.0497(6) Uani 1 1 d . . . . .
C00G C 0.2475(2) 0.95860(6) 0.74391(17) 0.0306(4) Uani 1 1 d . . . . .
H00G H 0.2572 0.9700 0.6735 0.037 Uiso 1 1 calc R . . . .
C00H C 0.0875(2) 0.72187(6) 0.70188(17) 0.0286(4) Uani 1 1 d . . . . .
C00I C 0.6127(2) 0.79038(6) 0.60847(17) 0.0299(4) Uani 1 1 d . . . . .
C00J C 0.2059(2) 0.83046(6) 0.81348(18) 0.0304(4) Uani 1 1 d . . . . .
N00K N 0.0985(3) 1.09279(7) 0.71264(18) 0.0532(6) Uani 1 1 d . . . . .
C00L C 0.1433(2) 0.28838(6) 0.40507(17) 0.0296(4) Uani 1 1 d . . . . .
N00M N 0.1679(3) 1.06708(8) 0.78276(18) 0.0562(6) Uani 1 1 d . . . . .
C00N C 0.3910(3) 0.78485(6) 0.71909(17) 0.0309(4) Uani 1 1 d . . . . .
C00O C 0.1878(2) 0.92033(7) 0.75249(17) 0.0320(5) Uani 1 1 d . . . . .
H00O H 0.1577 0.9062 0.6879 0.038 Uiso 1 1 calc R . . . .
C00P C 0.3365(2) 0.40954(6) 0.60067(17) 0.0316(5) Uani 1 1 d . . . . .
C00Q C 0.1724(2) 0.90276(6) 0.85726(17) 0.0299(4) Uani 1 1 d . . . . .
C00R C 0.2933(2) 0.98017(6) 0.83966(17) 0.0305(4) Uani 1 1 d . . . . .
C00S C 0.3034(2) 0.67371(6) 0.81033(18) 0.0318(5) Uani 1 1 d . . . . .
C00T C 0.2179(2) 0.92419(6) 0.95249(17) 0.0322(5) Uani 1 1 d . . . . .
H00T H 0.2091 0.9126 1.0228 0.039 Uiso 1 1 calc R . . . .
C00U C 0.1861(3) 0.70035(6) 0.64096(17) 0.0329(5) Uani 1 1 d . . . . .
H00U H 0.1807 0.7021 0.5631 0.040 Uiso 1 1 calc R . . . .
C00V C 0.1020(2) 0.72081(6) 0.81744(17) 0.0311(4) Uani 1 1 d . . . . .
H00V H 0.0393 0.7360 0.8596 0.037 Uiso 1 1 calc R . . . .
C00W C 0.6482(2) 0.78580(7) 0.49786(17) 0.0323(5) Uani 1 1 d . . . . .
H00W H 0.6045 0.7654 0.4540 0.039 Uiso 1 1 calc R . . . .
C00X C 0.2872(3) 1.04880(6) 0.74930(18) 0.0340(5) Uani 1 1 d . . . . .
C00Y C 0.2766(2) 0.96277(7) 0.94403(17) 0.0333(5) Uani 1 1 d . . . . .
H00Y H 0.3050 0.9771 1.0087 0.040 Uiso 1 1 calc R . . . .
C00Z C 0.2230(3) 0.53216(7) 0.84522(18) 0.0335(5) Uani 1 1 d . . . . .
C010 C 0.8137(3) 0.84246(7) 0.51515(19) 0.0360(5) Uani 1 1 d . . . . .
C011 C 0.3434(2) 0.60231(6) 0.86068(19) 0.0342(5) Uani 1 1 d . . . . .
C012 C 0.2105(3) 0.69707(6) 0.87134(17) 0.0332(5) Uani 1 1 d . . . . .
H012 H 0.2206 0.6969 0.9493 0.040 Uiso 1 1 calc R . . . .
C013 C 0.0393(3) 0.25669(6) 0.35903(18) 0.0358(5) Uani 1 1 d . . . . .
H01A H 0.0044 0.2403 0.4195 0.043 Uiso 1 1 calc R . . . .
H01B H 0.0880 0.2391 0.3078 0.043 Uiso 1 1 calc R . . . .
C014 C 0.2048(3) 0.42914(7) 0.57465(18) 0.0345(5) Uani 1 1 d . . . . .
H014 H 0.1557 0.4245 0.5056 0.041 Uiso 1 1 calc R . . . .
C015 C 0.2921(3) 0.67643(6) 0.69401(19) 0.0351(5) Uani 1 1 d . . . . .
H015 H 0.3566 0.6620 0.6516 0.042 Uiso 1 1 calc R . . . .
C016 C 0.6790(3) 0.82110(7) 0.67184(17) 0.0347(5) Uani 1 1 d . . . . .
H016 H 0.6569 0.8243 0.7464 0.042 Uiso 1 1 calc R . . . .
C017 C 0.7489(3) 0.81158(7) 0.45257(17) 0.0362(5) Uani 1 1 d . . . . .
H017 H 0.7732 0.8080 0.3786 0.043 Uiso 1 1 calc R . . . .
C018 C 0.1088(3) 0.86040(7) 0.86646(19) 0.0351(5) Uani 1 1 d . . . . .
H01K H 0.0999 0.8535 0.9448 0.042 Uiso 1 1 calc R . . . .
H01L H 0.0120 0.8596 0.8293 0.042 Uiso 1 1 calc R . . . .
C019 C 0.4073(3) 0.41712(7) 0.70452(19) 0.0375(5) Uani 1 1 d . . . . .
H019 H 0.4959 0.4044 0.7235 0.045 Uiso 1 1 calc R . . . .
C01A C 0.4040(2) 0.38153(7) 0.51794(19) 0.0348(5) Uani 1 1 d . . . . .
H01C H 0.4314 0.3973 0.4539 0.042 Uiso 1 1 calc R . . . .
H01D H 0.4929 0.3702 0.5530 0.042 Uiso 1 1 calc R . . . .
C01B C 0.7778(3) 0.84705(7) 0.62544(19) 0.0365(5) Uani 1 1 d . . . . .
H01M H 0.8203 0.8677 0.6687 0.044 Uiso 1 1 calc R . . . .
C01C C 0.1535(3) 1.09847(7) 0.61312(19) 0.0362(5) Uani 1 1 d . . . . .
C01D C 0.2161(3) 0.46302(7) 0.75388(19) 0.0366(5) Uani 1 1 d . . . . .
C01E C 0.1453(3) 0.45553(7) 0.65001(19) 0.0369(5) Uani 1 1 d . . . . .
H01E H 0.0571 0.4684 0.6309 0.044 Uiso 1 1 calc R . . . .
C01F C 0.3671(3) 1.02110(7) 0.83024(19) 0.0374(5) Uani 1 1 d . . . . .
H01N H 0.3740 1.0338 0.9036 0.045 Uiso 1 1 calc R . . . .
H01O H 0.4657 1.0171 0.8066 0.045 Uiso 1 1 calc R . . . .
C01G C 0.5047(3) 0.76199(7) 0.66013(19) 0.0383(5) Uani 1 1 d . . . . .
H01P H 0.4576 0.7454 0.6017 0.046 Uiso 1 1 calc R . . . .
H01Q H 0.5568 0.7442 0.7130 0.046 Uiso 1 1 calc R . . . .
C01H C 0.3472(3) 0.44338(7) 0.7801(2) 0.0420(6) Uani 1 1 d . . . . .
H01H H 0.3956 0.4479 0.8494 0.050 Uiso 1 1 calc R . . . .
C01I C 0.4091(3) 0.64390(7) 0.8673(2) 0.0422(6) Uani 1 1 d . . . . .
H01F H 0.5010 0.6442 0.8305 0.051 Uiso 1 1 calc R . . . .
H01G H 0.4284 0.6515 0.9451 0.051 Uiso 1 1 calc R . . . .
C01J C 0.1502(3) 0.49142(7) 0.8365(2) 0.0472(6) Uani 1 1 d . . . . .
H01I H 0.0476 0.4953 0.8145 0.057 Uiso 1 1 calc R . . . .
H01J H 0.1556 0.4788 0.9099 0.057 Uiso 1 1 calc R . . . .
C01K C 0.9208(3) 0.87146(9) 0.4647(2) 0.0494(7) Uani 1 1 d . . . . .
H01R H 0.9743 0.8859 0.5247 0.059 Uiso 1 1 calc R . . . .
H01S H 0.9909 0.8561 0.4240 0.059 Uiso 1 1 calc R . . . .


_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
N001 N002 1.331(3) . ?
N001 C00L 1.344(3) . ?
N002 C00D 1.333(3) . ?
N003 N004 1.330(3) . ?
N003 C00J 1.344(3) . ?
N004 C00N 1.333(3) . ?
N005 N007 1.321(3) . ?
N005 C00N 1.342(3) . ?
N006 N008 1.324(3) . ?
N006 C00L 1.334(3) . ?
N007 C00J 1.335(3) . ?
N008 C00D 1.334(3) . ?
N009 N00A 1.327(3) . ?
N009 C00Z 1.335(3) . ?
N00A C011 1.336(3) . ?
N00B N00F 1.332(3) . ?
N00B C00X 1.333(3) . ?
N00C N00E 1.332(3) . ?
N00C C00Z 1.329(3) . ?
C00D C01A 1.505(3) . ?
N00E C011 1.333(3) . ?
N00F C01C 1.329(3) . ?
C00G H00G 0.9300 . ?
C00G C00O 1.383(3) . ?
C00G C00R 1.392(3) . ?
C00H C00U 1.386(3) . ?
C00H C00V 1.380(3) . ?
C00H C013 1.512(3) 3_566 ?
C00I C00W 1.385(3) . ?
C00I C016 1.386(3) . ?
C00I C01G 1.518(3) . ?
C00J C018 1.493(3) . ?
N00K N00M 1.330(3) . ?
N00K C01C 1.329(3) . ?
C00L C013 1.500(3) . ?
N00M C00X 1.328(3) . ?
C00N C01G 1.493(3) . ?
C00O H00O 0.9300 . ?
C00O C00Q 1.393(3) . ?
C00P C014 1.389(3) . ?
C00P C019 1.390(3) . ?
C00P C01A 1.510(3) . ?
C00Q C00T 1.384(3) . ?
C00Q C018 1.522(3) . ?
C00R C00Y 1.388(3) . ?
C00R C01F 1.518(3) . ?
C00S C012 1.384(3) . ?
C00S C015 1.390(3) . ?
C00S C01I 1.516(3) . ?
C00T H00T 0.9300 . ?
C00T C00Y 1.389(3) . ?
C00U H00U 0.9300 . ?
C00U C015 1.379(3) . ?
C00V H00V 0.9300 . ?
C00V C012 1.395(3) . ?
C00W H00W 0.9300 . ?
C00W C017 1.386(3) . ?
C00X C01F 1.493(3) . ?
C00Y H00Y 0.9300 . ?
C00Z C01J 1.503(3) . ?
C010 C017 1.379(3) . ?
C010 C01B 1.383(3) . ?
C010 C01K 1.519(3) . ?
C011 C01I 1.500(3) . ?
C012 H012 0.9300 . ?
C013 C00H 1.512(3) 3_566 ?
C013 H01A 0.9700 . ?
C013 H01B 0.9700 . ?
C014 H014 0.9300 . ?
C014 C01E 1.385(3) . ?
C015 H015 0.9300 . ?
C016 H016 0.9300 . ?
C016 C01B 1.383(3) . ?
C017 H017 0.9300 . ?
C018 H01K 0.9700 . ?
C018 H01L 0.9700 . ?
C019 H019 0.9300 . ?
C019 C01H 1.386(3) . ?
C01A H01C 0.9700 . ?
C01A H01D 0.9700 . ?
C01B H01M 0.9300 . ?
C01C C01K 1.498(3) 3_676 ?
C01D C01E 1.390(3) . ?
C01D C01H 1.385(4) . ?
C01D C01J 1.510(3) . ?
C01E H01E 0.9300 . ?
C01F H01N 0.9700 . ?
C01F H01O 0.9700 . ?
C01G H01P 0.9700 . ?
C01G H01Q 0.9700 . ?
C01H H01H 0.9300 . ?
C01I H01F 0.9700 . ?
C01I H01G 0.9700 . ?
C01J H01I 0.9700 . ?
C01J H01J 0.9700 . ?
C01K C01C 1.498(3) 3_676 ?
C01K H01R 0.9700 . ?
C01K H01S 0.9700 . ?

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
N002 N001 C00L 116.99(18) . . ?
N001 N002 C00D 118.27(18) . . ?
N004 N003 C00J 117.81(18) . . ?
N003 N004 C00N 117.50(19) . . ?
N007 N005 C00N 118.07(18) . . ?
N008 N006 C00L 118.29(18) . . ?
N005 N007 C00J 117.68(19) . . ?
N006 N008 C00D 117.52(19) . . ?
N00A N009 C00Z 117.71(19) . . ?
N009 N00A C011 117.7(2) . . ?
N00F N00B C00X 117.4(2) . . ?
C00Z N00C N00E 117.8(2) . . ?
N002 C00D N008 124.5(2) . . ?
N002 C00D C01A 118.12(18) . . ?
N008 C00D C01A 117.33(19) . . ?
N00C N00E C011 117.5(2) . . ?
C01C N00F N00B 118.2(2) . . ?
C00O C00G H00G 119.7 . . ?
C00O C00G C00R 120.63(19) . . ?
C00R C00G H00G 119.7 . . ?
C00U C00H C013 119.51(19) . 3_566 ?
C00V C00H C00U 118.8(2) . . ?
C00V C00H C013 121.5(2) . 3_566 ?
C00W C00I C016 118.8(2) . . ?
C00W C00I C01G 120.8(2) . . ?
C016 C00I C01G 120.41(19) . . ?
N003 C00J C018 117.60(19) . . ?
N007 C00J N003 124.3(2) . . ?
N007 C00J C018 118.0(2) . . ?
C01C N00K N00M 117.5(2) . . ?
N001 C00L C013 118.5(2) . . ?
N006 C00L N001 124.4(2) . . ?
N006 C00L C013 117.08(19) . . ?
C00X N00M N00K 118.3(2) . . ?
N004 C00N N005 124.4(2) . . ?
N004 C00N C01G 118.7(2) . . ?
N005 C00N C01G 116.85(19) . . ?
C00G C00O H00O 119.8 . . ?
C00G C00O C00Q 120.4(2) . . ?
C00Q C00O H00O 119.8 . . ?
C014 C00P C019 118.2(2) . . ?
C014 C00P C01A 121.4(2) . . ?
C019 C00P C01A 120.4(2) . . ?
C00O C00Q C018 120.4(2) . . ?
C00T C00Q C00O 118.9(2) . . ?
C00T C00Q C018 120.67(19) . . ?
C00G C00R C01F 120.68(19) . . ?
C00Y C00R C00G 118.8(2) . . ?
C00Y C00R C01F 120.4(2) . . ?
C012 C00S C015 118.4(2) . . ?
C012 C00S C01I 121.4(2) . . ?
C015 C00S C01I 120.1(2) . . ?
C00Q C00T H00T 119.7 . . ?
C00Q C00T C00Y 120.66(19) . . ?
C00Y C00T H00T 119.7 . . ?
C00H C00U H00U 119.5 . . ?
C015 C00U C00H 121.0(2) . . ?
C015 C00U H00U 119.5 . . ?
C00H C00V H00V 119.9 . . ?
C00H C00V C012 120.2(2) . . ?
C012 C00V H00V 119.9 . . ?
C00I C00W H00W 120.0 . . ?
C00I C00W C017 120.0(2) . . ?
C017 C00W H00W 120.0 . . ?
N00B C00X C01F 118.1(2) . . ?
N00M C00X N00B 124.1(2) . . ?
N00M C00X C01F 117.8(2) . . ?
C00R C00Y C00T 120.5(2) . . ?
C00R C00Y H00Y 119.8 . . ?
C00T C00Y H00Y 119.8 . . ?
N009 C00Z C01J 118.08(19) . . ?
N00C C00Z N009 124.6(2) . . ?
N00C C00Z C01J 117.3(2) . . ?
C017 C010 C01B 118.7(2) . . ?
C017 C010 C01K 121.3(2) . . ?
C01B C010 C01K 120.0(2) . . ?
N00A C011 C01I 117.2(2) . . ?
N00E C011 N00A 124.6(2) . . ?
N00E C011 C01I 118.2(2) . . ?
C00S C012 C00V 120.84(19) . . ?
C00S C012 H012 119.6 . . ?
C00V C012 H012 119.6 . . ?
C00H C013 H01A 110.2 3_566 . ?
C00H C013 H01B 110.2 3_566 . ?
C00L C013 C00H 107.78(17) . 3_566 ?
C00L C013 H01A 110.2 . . ?
C00L C013 H01B 110.2 . . ?
H01A C013 H01B 108.5 . . ?
C00P C014 H014 119.5 . . ?
C01E C014 C00P 121.0(2) . . ?
C01E C014 H014 119.5 . . ?
C00S C015 H015 119.7 . . ?
C00U C015 C00S 120.6(2) . . ?
C00U C015 H015 119.7 . . ?
C00I C016 H016 119.6 . . ?
C01B C016 C00I 120.8(2) . . ?
C01B C016 H016 119.6 . . ?
C00W C017 H017 119.4 . . ?
C010 C017 C00W 121.2(2) . . ?
C010 C017 H017 119.4 . . ?
C00J C018 C00Q 109.86(18) . . ?
C00J C018 H01K 109.7 . . ?
C00J C018 H01L 109.7 . . ?
C00Q C018 H01K 109.7 . . ?
C00Q C018 H01L 109.7 . . ?
H01K C018 H01L 108.2 . . ?
C00P C019 H019 119.6 . . ?
C01H C019 C00P 120.7(2) . . ?
C01H C019 H019 119.6 . . ?
C00D C01A C00P 114.80(19) . . ?
C00D C01A H01C 108.6 . . ?
C00D C01A H01D 108.6 . . ?
C00P C01A H01C 108.6 . . ?
C00P C01A H01D 108.6 . . ?
H01C C01A H01D 107.5 . . ?
C010 C01B C016 120.5(2) . . ?
C010 C01B H01M 119.7 . . ?
C016 C01B H01M 119.7 . . ?
N00F C01C C01K 117.9(2) . 3_676 ?
N00K C01C N00F 124.2(2) . . ?
N00K C01C C01K 117.8(2) . 3_676 ?
C01E C01D C01J 120.6(2) . . ?
C01H C01D C01E 118.3(2) . . ?
C01H C01D C01J 121.0(2) . . ?
C014 C01E C01D 120.7(2) . . ?
C014 C01E H01E 119.6 . . ?
C01D C01E H01E 119.6 . . ?
C00R C01F H01N 109.0 . . ?
C00R C01F H01O 109.0 . . ?
C00X C01F C00R 112.93(19) . . ?
C00X C01F H01N 109.0 . . ?
C00X C01F H01O 109.0 . . ?
H01N C01F H01O 107.8 . . ?
C00I C01G H01P 109.3 . . ?
C00I C01G H01Q 109.3 . . ?
C00N C01G C00I 111.43(18) . . ?
C00N C01G H01P 109.3 . . ?
C00N C01G H01Q 109.3 . . ?
H01P C01G H01Q 108.0 . . ?
C019 C01H H01H 119.5 . . ?
C01D C01H C019 121.0(2) . . ?
C01D C01H H01H 119.5 . . ?
C00S C01I H01F 109.9 . . ?
C00S C01I H01G 109.9 . . ?
C011 C01I C00S 109.09(18) . . ?
C011 C01I H01F 109.9 . . ?
C011 C01I H01G 109.9 . . ?
H01F C01I H01G 108.3 . . ?
C00Z C01J C01D 114.2(2) . . ?
C00Z C01J H01I 108.7 . . ?
C00Z C01J H01J 108.7 . . ?
C01D C01J H01I 108.7 . . ?
C01D C01J H01J 108.7 . . ?
H01I C01J H01J 107.6 . . ?
C010 C01K H01R 109.1 . . ?
C010 C01K H01S 109.1 . . ?
C01C C01K C010 112.5(2) 3_676 . ?
C01C C01K H01R 109.1 3_676 . ?
C01C C01K H01S 109.1 3_676 . ?
H01R C01K H01S 107.8 . . ?

_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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.865
####################################################################### 
# 
# 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_tx1388
_database_code_depnum_ccdc_archive 'CCDC 2233699'
loop_
_audit_author_name
_audit_author_address
'Mei-Xiang Wang'
;Tsinghua University
China
;
_audit_update_record             
;
2022-12-31 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_audit_creation_date             2019-12-05
_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            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H24 N12, C2 H3 N'
_chemical_formula_sum            'C32 H27 N13'
_chemical_formula_weight         593.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNK
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8117(2)
_cell_length_b                   13.6872(4)
_cell_length_c                   13.7913(5)
_cell_angle_alpha                118.189(3)
_cell_angle_beta                 95.231(2)
_cell_angle_gamma                93.932(2)
_cell_volume                     1448.09(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13835
_cell_measurement_temperature    169.99(12)
_cell_measurement_theta_max      74.9300
_cell_measurement_theta_min      3.6600
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light red'
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27345
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.589
_diffrn_reflns_theta_min         3.673
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -81.00  25.00   0.50    0.30    --  -47.20 100.00 -71.00  212
  2  ω    -18.00  81.00   0.50    0.30    --   47.20-100.00-176.00  198
  3  ω   -168.00 -83.00   0.50    0.90    --  -99.00-100.00-176.00  170
  4  ω   -110.00 -26.00   0.50    0.90    --  -99.00 100.00 -71.00  168
  5  ω     89.00 169.00   0.50    0.90    --  103.25 100.00 -71.00  160
  6  ω     31.00 109.00   0.50    0.90    --  103.25-100.00-176.00  156
  7  ω    -60.00  26.00   0.50    0.30    --  -47.20  38.00 -30.00  172
  8  ω   -120.00 -71.00   0.50    0.30    --  -47.20-125.00 -30.00   98
  9  ω    -60.00  28.00   0.50    0.30    --  -47.20  19.00-120.00  176
 10  ω    -26.00  60.00   0.50    0.30    --   47.20 -38.00 -30.00  172
 11  ω   -122.00 -26.00   0.50    0.90    --  -99.00  77.00 -60.00  192
 12  ω   -117.00 -26.00   0.50    0.90    --  -99.00 125.00  90.00  182
 13  ω   -115.00 -26.00   0.50    0.90    --  -99.00  61.00 -60.00  178
 14  ω   -168.00 -86.00   0.50    0.90    --  -99.00 -45.00-180.00  164
 15  ω   -112.00 -24.00   0.50    0.90    --  -99.00  30.00 150.00  176
 16  ω     31.00 126.00   0.50    0.90    --  103.25 -77.00  30.00  190
 17  ω     77.00 169.00   0.50    0.90    --  103.25 125.00 120.00  184
 18  ω     90.00 169.00   0.50    0.90    --  103.25  15.00-120.00  158
 19  ω     31.00 117.00   0.50    0.90    --  103.25-125.00   0.00  172
 20  ω     91.00 169.00   0.50    0.90    --  103.25  45.00  60.00  156
 21  ω     90.00 169.00   0.50    0.90    --  103.25  15.00 -90.00  158
 22  ω     31.00 109.00   0.50    0.90    --  103.25 -94.00  30.00  156
 23  ω   -120.00 -24.00   0.50    0.30    --  -47.20 -77.00 -30.00  192
 24  ω     32.00 120.00   0.50    0.30    --   47.20  57.00-150.00  176
 25  ω     32.00 120.00   0.50    0.30    --   47.20  57.00  30.00  176
 26  ω     25.00 120.00   0.50    0.30    --   47.20  77.00-120.00  190
 27  ω     25.00 120.00   0.50    0.30    --   47.20  77.00  90.00  190
 28  ω   -168.00 -76.00   0.50    0.90    --  -99.00 -77.00 120.00  184
 29  ω     91.00 169.00   0.50    0.90    --  103.25  30.00  30.00  156
 30  ω     87.00 129.00   0.50    0.90    --  103.25  61.00 -90.00   84
 31  ω     91.00 169.00   0.50    0.90    --  103.25  30.00 -30.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0293252000
_diffrn_orient_matrix_UB_12      0.0600574000
_diffrn_orient_matrix_UB_13      -0.0682145000
_diffrn_orient_matrix_UB_21      0.0185644000
_diffrn_orient_matrix_UB_22      -0.1123572000
_diffrn_orient_matrix_UB_23      -0.1004168000
_diffrn_orient_matrix_UB_31      -0.1735644000
_diffrn_orient_matrix_UB_32      -0.0185696000
_diffrn_orient_matrix_UB_33      -0.0406089000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5203
_reflns_number_total             5806
_reflns_odcompleteness_completeness 99.98
_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.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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         0.397
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5806
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0912
_refine_ls_restrained_S_all      1.108
_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)+(0.0951P)²+4.9834P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2763
_refine_ls_wR_factor_ref         0.2800
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9904(7)
 0.0096(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
3. Others
 Fixed Sof: H1AA(0.5) H1AB(0.5) H1AC(0.5) H1BD(0.5) H1BE(0.5) H1BF(0.5)
 C2(0.5) N1(0.5) N2(0.5) C3(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C00R(H00A,H00B), C00T(H00C,H00D), C00V(H00E,H00F), C00Z(H00I,H00J), C013(H01A,
 H01B), C015(H01C,H01D)
4.b Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00H(H00H), C00K(H00K), C00O(H00O), C00S(H00S), C00U(H00U),
 C00X(H00X), C010(H010), C011(H011), C012(H012), C014(H014), C016(H016)
4.c Idealised Me refined as rotating group:
 C1(H1AA,H1AB,H1AC), C1(H1BD,H1BE,H1BF)
;
_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
N001 N 0.3930(4) 0.1874(3) 0.7318(3) 0.0365(8) Uani 1 1 d . . . . .
N002 N 0.3904(4) 0.1349(3) 0.6229(3) 0.0363(8) Uani 1 1 d . . . . .
N003 N 0.1031(4) 0.8119(3) 1.0163(3) 0.0394(8) Uani 1 1 d . . . . .
N004 N 0.3829(4) 0.4746(3) 0.3165(3) 0.0415(9) Uani 1 1 d . . . . .
N005 N 0.1051(5) 0.8665(3) 0.9581(3) 0.0416(9) Uani 1 1 d . . . . .
N006 N 0.1182(4) 0.1150(3) 0.5982(3) 0.0401(9) Uani 1 1 d . . . . .
N007 N 0.1204(4) 0.1651(3) 0.7075(3) 0.0400(8) Uani 1 1 d . . . . .
N008 N 0.1230(4) 0.4226(3) 0.2386(3) 0.0438(9) Uani 1 1 d . . . . .
N009 N 0.3615(5) 0.5818(3) 0.3660(4) 0.0459(9) Uani 1 1 d . . . . .
N00A N 0.3683(5) 0.7996(4) 1.0095(4) 0.0502(10) Uani 1 1 d . . . . .
N00B N 0.1016(5) 0.5306(4) 0.2861(4) 0.0482(10) Uani 1 1 d . . . . .
N00C N 0.3704(5) 0.8546(4) 0.9525(4) 0.0522(11) Uani 1 1 d . . . . .
C00D C 0.2527(5) 0.0963(3) 0.5593(3) 0.0330(9) Uani 1 1 d . . . . .
C00E C 0.2567(5) 0.1001(3) 0.3774(3) 0.0336(9) Uani 1 1 d . . . . .
C00F C 0.2627(5) 0.3991(4) 0.2505(3) 0.0332(9) Uani 1 1 d . . . . .
C00G C 0.1938(5) 0.0514(3) 0.2656(3) 0.0379(10) Uani 1 1 d . . . . .
H00G H 0.142689 -0.020982 0.230310 0.045 Uiso 1 1 calc R . . . .
C00H C 0.3506(5) 0.5625(4) 1.1017(3) 0.0338(9) Uani 1 1 d . . . . .
H00H H 0.416116 0.608019 1.167467 0.041 Uiso 1 1 calc R . . . .
C00I C 0.2582(5) 0.1981(3) 0.7705(3) 0.0334(9) Uani 1 1 d . . . . .
C00J C 0.2364(5) 0.7856(3) 1.0446(3) 0.0367(9) Uani 1 1 d . . . . .
C00K C 0.3313(5) 0.2090(4) 0.4278(4) 0.0389(10) Uani 1 1 d . . . . .
H00K H 0.374443 0.243272 0.502087 0.047 Uiso 1 1 calc R . . . .
C00L C 0.2804(5) 0.2184(4) 0.2576(4) 0.0354(9) Uani 1 1 d . . . . .
C00M C 0.2230(5) 0.6059(4) 0.3456(4) 0.0384(10) Uani 1 1 d . . . . .
C00N C 0.2386(5) 0.8970(4) 0.7522(4) 0.0388(10) Uani 1 1 d . . . . .
C00O C 0.3417(5) 0.2667(4) 0.3684(4) 0.0387(10) Uani 1 1 d . . . . .
H00O H 0.390986 0.339668 0.403915 0.046 Uiso 1 1 calc R . . . .
C00P C 0.2593(5) 0.3773(4) 0.9489(3) 0.0348(9) Uani 1 1 d . . . . .
C00Q C 0.2492(5) 0.6092(4) 1.0585(3) 0.0356(9) Uani 1 1 d . . . . .
C00R C 0.2502(5) 0.0310(3) 0.4363(4) 0.0372(9) Uani 1 1 d . . . . .
H00A H 0.157263 -0.021916 0.404781 0.045 Uiso 1 1 calc R . . . .
H00B H 0.336790 -0.011613 0.421559 0.045 Uiso 1 1 calc R . . . .
C00S C 0.3556(5) 0.4472(4) 1.0473(3) 0.0352(9) Uani 1 1 d . . . . .
H00S H 0.424343 0.416793 1.077462 0.042 Uiso 1 1 calc R . . . .
C00T C 0.2387(5) 0.7340(4) 1.1196(4) 0.0387(10) Uani 1 1 d . . . . .
H00C H 0.146089 0.746488 1.154562 0.046 Uiso 1 1 calc R . . . .
H00D H 0.325837 0.770841 1.177872 0.046 Uiso 1 1 calc R . . . .
C00U C 0.2065(6) 0.1092(4) 0.2069(4) 0.0397(10) Uani 1 1 d . . . . .
H00U H 0.165052 0.074729 0.132196 0.048 Uiso 1 1 calc R . . . .
C00V C 0.2616(6) 0.2518(4) 0.8939(4) 0.0386(10) Uani 1 1 d . . . . .
H00E H 0.353499 0.236432 0.925970 0.046 Uiso 1 1 calc R . . . .
H00F H 0.173583 0.218221 0.910078 0.046 Uiso 1 1 calc R . . . .
C00W C 0.2394(6) 0.8908(4) 0.9332(4) 0.0407(10) Uani 1 1 d . . . . .
C00X C 0.3310(6) 0.8731(4) 0.5847(4) 0.0440(11) Uani 1 1 d . . . . .
H00X H 0.401958 0.895083 0.550528 0.053 Uiso 1 1 calc R . . . .
C00Y C 0.2155(6) 0.7869(4) 0.5201(4) 0.0409(10) Uani 1 1 d . . . . .
C00Z C 0.2911(6) 0.2790(4) 0.1897(4) 0.0404(10) Uani 1 1 d . . . . .
H00I H 0.392581 0.276111 0.167259 0.048 Uiso 1 1 calc R . . . .
H00J H 0.216908 0.239837 0.122833 0.048 Uiso 1 1 calc R . . . .
C010 C 0.1605(6) 0.4250(4) 0.9049(4) 0.0431(11) Uani 1 1 d . . . . .
H010 H 0.096979 0.379683 0.838159 0.052 Uiso 1 1 calc R . . . .
C011 C 0.3436(5) 0.9279(4) 0.6999(4) 0.0423(10) Uani 1 1 d . . . . .
H011 H 0.422879 0.985547 0.741892 0.051 Uiso 1 1 calc R . . . .
C012 C 0.1545(6) 0.5391(4) 0.9586(4) 0.0460(11) Uani 1 1 d . . . . .
H012 H 0.086516 0.569344 0.927792 0.055 Uiso 1 1 calc R . . . .
C013 C 0.2031(7) 0.7282(4) 0.3944(4) 0.0523(13) Uani 1 1 d . . . . .
H01A H 0.103323 0.734971 0.363675 0.063 Uiso 1 1 calc R . . . .
H01B H 0.280827 0.765035 0.372949 0.063 Uiso 1 1 calc R . . . .
C014 C 0.1114(6) 0.7546(4) 0.5731(4) 0.0497(12) Uani 1 1 d . . . . .
H014 H 0.033580 0.695752 0.531202 0.060 Uiso 1 1 calc R . . . .
C015 C 0.2466(7) 0.9627(4) 0.8782(4) 0.0481(12) Uani 1 1 d . . . . .
H01C H 0.341594 1.013595 0.908788 0.058 Uiso 1 1 calc R . . . .
H01D H 0.162236 1.007412 0.895996 0.058 Uiso 1 1 calc R . . . .
C016 C 0.1234(6) 0.8096(4) 0.6877(4) 0.0492(12) Uani 1 1 d . . . . .
H016 H 0.052853 0.787516 0.722028 0.059 Uiso 1 1 calc R . . . .
C1 C 0.7542(9) 0.4303(9) 0.3064(11) 0.113(4) Uani 1 1 d . . . . .
H1AA H 0.800899 0.387966 0.241194 0.169 Uiso 0.5 1 calc GR . P A -1
H1AB H 0.654331 0.392713 0.298978 0.169 Uiso 0.5 1 calc GR . P A -1
H1AC H 0.817189 0.437408 0.370476 0.169 Uiso 0.5 1 calc GR . P A -1
H1BD H 0.836506 0.430662 0.265438 0.169 Uiso 0.5 1 calc GR . P B 1
H1BE H 0.678926 0.474209 0.297788 0.169 Uiso 0.5 1 calc GR . P B 1
H1BF H 0.707305 0.354951 0.278649 0.169 Uiso 0.5 1 calc GR . P B 1
C2 C 0.7390(12) 0.5424(11) 0.3194(11) 0.056(3) Uani 0.5 1 d . . P C -1
N1 N 0.8601(18) 0.5093(10) 0.4990(12) 0.089(4) Uani 0.5 1 d . . P C 1
N2 N 0.7194(15) 0.6242(9) 0.3175(10) 0.076(3) Uani 0.5 1 d . . P C -1
C3 C 0.8079(17) 0.4725(11) 0.4107(13) 0.069(3) Uani 0.5 1 d . . P C 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
N001 N002 1.322(5) . ?
N001 C00I 1.335(6) . ?
N002 C00D 1.342(5) . ?
N003 N005 1.331(6) . ?
N003 C00J 1.331(6) . ?
N004 N009 1.331(5) . ?
N004 C00F 1.342(6) . ?
N005 C00W 1.326(6) . ?
N006 N007 1.326(5) . ?
N006 C00D 1.337(6) . ?
N007 C00I 1.339(6) . ?
N008 N00B 1.340(6) . ?
N008 C00F 1.309(6) . ?
N009 C00M 1.325(6) . ?
N00A N00C 1.322(6) . ?
N00A C00J 1.335(6) . ?
N00B C00M 1.330(6) . ?
N00C C00W 1.340(6) . ?
C00D C00R 1.495(6) . ?
C00E C00G 1.396(6) . ?
C00E C00K 1.393(6) . ?
C00E C00R 1.511(6) . ?
C00F C00Z 1.504(6) . ?
C00G C00U 1.380(6) . ?
C00H C00Q 1.380(6) . ?
C00H C00S 1.397(6) . ?
C00I C00V 1.499(6) . ?
C00J C00T 1.502(6) . ?
C00K C00O 1.385(6) . ?
C00L C00O 1.382(6) . ?
C00L C00U 1.394(6) . ?
C00L C00Z 1.521(6) . ?
C00M C013 1.512(6) . ?
C00N C011 1.383(7) . ?
C00N C015 1.525(6) . ?
C00N C016 1.385(7) . ?
C00P C00S 1.389(6) . ?
C00P C00V 1.518(6) . ?
C00P C010 1.381(6) . ?
C00Q C00T 1.521(6) . ?
C00Q C012 1.395(6) . ?
C00W C015 1.501(7) . ?
C00X C00Y 1.378(7) . ?
C00X C011 1.388(7) . ?
C00Y C013 1.516(7) . ?
C00Y C014 1.395(7) . ?
C010 C012 1.384(6) . ?
C014 C016 1.382(7) . ?
C1 C2 1.475(15) . ?
C1 C3 1.297(18) . ?
C2 N2 1.156(15) . ?
C2 C3 1.99(2) . ?
N1 C3 1.111(19) . ?

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
N002 N001 C00I 117.4(4) . . ?
N001 N002 C00D 117.7(4) . . ?
N005 N003 C00J 117.3(4) . . ?
N009 N004 C00F 117.7(4) . . ?
C00W N005 N003 117.6(4) . . ?
N007 N006 C00D 117.7(4) . . ?
N006 N007 C00I 117.2(4) . . ?
C00F N008 N00B 117.7(4) . . ?
C00M N009 N004 117.3(4) . . ?
N00C N00A C00J 117.5(4) . . ?
C00M N00B N008 117.4(4) . . ?
N00A N00C C00W 117.5(4) . . ?
N002 C00D C00R 117.5(4) . . ?
N006 C00D N002 124.5(4) . . ?
N006 C00D C00R 118.0(4) . . ?
C00G C00E C00R 119.2(4) . . ?
C00K C00E C00G 117.9(4) . . ?
C00K C00E C00R 122.8(4) . . ?
N004 C00F C00Z 117.0(4) . . ?
N008 C00F N004 124.6(4) . . ?
N008 C00F C00Z 118.3(4) . . ?
C00U C00G C00E 121.0(4) . . ?
C00Q C00H C00S 120.4(4) . . ?
N001 C00I N007 125.1(4) . . ?
N001 C00I C00V 117.3(4) . . ?
N007 C00I C00V 117.6(4) . . ?
N003 C00J N00A 124.7(4) . . ?
N003 C00J C00T 117.9(4) . . ?
N00A C00J C00T 117.3(4) . . ?
C00O C00K C00E 120.7(4) . . ?
C00O C00L C00U 118.0(4) . . ?
C00O C00L C00Z 122.8(4) . . ?
C00U C00L C00Z 119.2(4) . . ?
N009 C00M N00B 124.9(4) . . ?
N009 C00M C013 117.0(4) . . ?
N00B C00M C013 118.2(4) . . ?
C011 C00N C015 119.9(4) . . ?
C011 C00N C016 118.7(4) . . ?
C016 C00N C015 121.4(4) . . ?
C00L C00O C00K 121.4(4) . . ?
C00S C00P C00V 120.1(4) . . ?
C010 C00P C00S 118.2(4) . . ?
C010 C00P C00V 121.7(4) . . ?
C00H C00Q C00T 120.7(4) . . ?
C00H C00Q C012 118.6(4) . . ?
C012 C00Q C00T 120.8(4) . . ?
C00D C00R C00E 115.1(3) . . ?
C00P C00S C00H 121.0(4) . . ?
C00J C00T C00Q 112.9(3) . . ?
C00G C00U C00L 121.0(4) . . ?
C00I C00V C00P 113.5(3) . . ?
N005 C00W N00C 124.6(5) . . ?
N005 C00W C015 118.3(4) . . ?
N00C C00W C015 117.0(4) . . ?
C00Y C00X C011 121.3(4) . . ?
C00X C00Y C013 120.6(5) . . ?
C00X C00Y C014 118.4(4) . . ?
C014 C00Y C013 121.0(5) . . ?
C00F C00Z C00L 114.0(4) . . ?
C00P C010 C012 121.1(4) . . ?
C00N C011 C00X 120.2(4) . . ?
C010 C012 C00Q 120.7(4) . . ?
C00M C013 C00Y 112.7(4) . . ?
C016 C014 C00Y 120.3(5) . . ?
C00W C015 C00N 113.9(4) . . ?
C014 C016 C00N 121.1(5) . . ?
C3 C1 C2 91.4(11) . . ?
C1 C2 C3 40.7(7) . . ?
N2 C2 C1 172.4(14) . . ?
N2 C2 C3 146.8(13) . . ?
C1 C3 C2 47.9(8) . . ?
N1 C3 C1 177.0(16) . . ?
N1 C3 C2 131.8(13) . . ?

_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 1.948
_oxdiff_exptl_absorpt_empirical_full_min 0.351
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9904(7)
2 0.0096(7)

