# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_ydkr
_database_code_depnum_ccdc_archive 'CCDC 1871606'
_audit_update_record             
;
2018-10-05 deposited with the CCDC.
2018-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C22 H18 N2 O3'
_chemical_formula_sum            'C22 H18 N2 O3'
_chemical_formula_weight         358.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-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                   21.323(2)
_cell_length_b                   4.9429(7)
_cell_length_c                   15.810(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.652(8)
_cell_angle_gamma                90
_cell_volume                     1658.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    4139
_cell_measurement_theta_min      3.377
_cell_measurement_theta_max      27.965

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_F_000             752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.097
_shelx_estimated_absorpt_T_min   0.996
_shelx_estimated_absorpt_T_max   0.999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.78228
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'

_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_detector_area_resol_mean 29
_diffrn_reflns_number            4139
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.377
_diffrn_reflns_theta_max         27.965
_diffrn_reflns_theta_full        27.965
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             1467
_reflns_number_gt                1232
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0676P)²+0.4601P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1467
_refine_ls_number_parameters     126
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1122
_refine_ls_wR_factor_gt          0.1030
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.61857(6) 0.1351(3) 0.30142(9) 0.0170(4) Uani 1 1 d . . . . .
H1 H 0.583650 0.242123 0.279627 0.020 Uiso 1 1 calc R U . . .
C2 C 0.64293(6) -0.0587(3) 0.25011(9) 0.0182(4) Uani 1 1 d . . . . .
H2 H 0.624433 -0.082895 0.193460 0.022 Uiso 1 1 calc R U . . .
C3 C 0.69383(6) -0.2173(3) 0.28042(9) 0.0189(4) Uani 1 1 d . . . . .
H3 H 0.710105 -0.350134 0.245057 0.023 Uiso 1 1 calc R U . . .
C4 C 0.72066(6) -0.1795(3) 0.36289(9) 0.0193(4) Uani 1 1 d . . . . .
H4 H 0.755759 -0.286196 0.384236 0.023 Uiso 1 1 calc R U . . .
C5 C 0.69664(6) 0.0126(3) 0.41430(9) 0.0180(4) Uani 1 1 d . . . . .
H5 H 0.715460 0.036175 0.470816 0.022 Uiso 1 1 calc R U . . .
C6 C 0.64502(6) 0.1733(3) 0.38460(9) 0.0159(3) Uani 1 1 d . . . . .
C7 C 0.61933(6) 0.3712(3) 0.44090(9) 0.0157(4) Uani 1 1 d . . . . .
C8 C 0.63240(6) 0.4098(3) 0.52788(9) 0.0178(4) Uani 1 1 d . . . . .
H6 H 0.662194 0.310878 0.564330 0.021 Uiso 1 1 calc R U . . .
C9 C 0.59420(6) 0.6187(3) 0.55239(9) 0.0175(4) Uani 1 1 d . . . . .
H7 H 0.593190 0.686958 0.608412 0.021 Uiso 1 1 calc R U . . .
C10 C 0.55765(6) 0.7098(3) 0.47975(9) 0.0157(3) Uani 1 1 d . . . . .
C11 C 0.50991(6) 0.9147(3) 0.46299(9) 0.0155(4) Uani 1 1 d . . . . .
N1 N 0.57442(5) 0.5534(2) 0.41362(7) 0.0152(3) Uani 1 1 d . . . . .
H8 H 0.558096 0.569580 0.360539 0.018 Uiso 1 1 calc R U . . .
O1 O 0.48471(4) 0.9576(2) 0.39070(6) 0.0198(3) Uani 1 1 d . . . . .
O2 O 0.500000 0.6381(3) 0.250000 0.0187(4) Uani 1 2 d DS T P . .
H9 H 0.4861(8) 0.764(3) 0.2913(9) 0.028 Uiso 1 1 d 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
C1 C2 1.389(2) . ?
C1 C6 1.392(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.385(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.400(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.4644(19) . ?
C7 N1 1.3537(18) . ?
C7 C8 1.389(2) . ?
C8 C9 1.394(2) . ?
C8 H6 0.9500 . ?
C9 C10 1.397(2) . ?
C9 H7 0.9500 . ?
C10 N1 1.3759(18) . ?
C10 C11 1.442(2) . ?
C11 O1 1.2324(17) . ?
C11 C11 1.535(3) 5_676 ?
N1 H8 0.8800 . ?
O2 H9 0.970(13) . ?

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
C2 C1 C6 120.37(13) . . ?
C2 C1 H1 119.8 . . ?
C6 C1 H1 119.8 . . ?
C3 C2 C1 120.90(14) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C4 C3 C2 119.11(13) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C5 C4 C3 120.30(13) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.18(13) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 118.14(13) . . ?
C1 C6 C7 121.60(12) . . ?
C5 C6 C7 120.25(13) . . ?
N1 C7 C8 106.90(12) . . ?
N1 C7 C6 123.07(12) . . ?
C8 C7 C6 130.00(13) . . ?
C7 C8 C9 108.13(13) . . ?
C7 C8 H6 125.9 . . ?
C9 C8 H6 125.9 . . ?
C8 C9 C10 107.72(12) . . ?
C8 C9 H7 126.1 . . ?
C10 C9 H7 126.1 . . ?
N1 C10 C9 106.12(12) . . ?
N1 C10 C11 119.14(12) . . ?
C9 C10 C11 134.74(13) . . ?
O1 C11 C10 121.77(12) . . ?
O1 C11 C11 119.02(15) . 5_676 ?
C10 C11 C11 119.21(15) . 5_676 ?
C7 N1 C10 111.13(12) . . ?
C7 N1 H8 124.4 . . ?
C10 N1 H8 124.4 . . ?

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
C6 C1 C2 C3 0.0(2) . . . . ?
C1 C2 C3 C4 -0.3(2) . . . . ?
C2 C3 C4 C5 0.4(2) . . . . ?
C3 C4 C5 C6 -0.1(2) . . . . ?
C2 C1 C6 C5 0.3(2) . . . . ?
C2 C1 C6 C7 -178.39(12) . . . . ?
C4 C5 C6 C1 -0.25(19) . . . . ?
C4 C5 C6 C7 178.47(12) . . . . ?
C1 C6 C7 N1 -9.1(2) . . . . ?
C5 C6 C7 N1 172.22(12) . . . . ?
C1 C6 C7 C8 168.93(13) . . . . ?
C5 C6 C7 C8 -9.8(2) . . . . ?
N1 C7 C8 C9 0.18(15) . . . . ?
C6 C7 C8 C9 -178.10(13) . . . . ?
C7 C8 C9 C10 -0.29(15) . . . . ?
C8 C9 C10 N1 0.29(15) . . . . ?
C8 C9 C10 C11 179.53(14) . . . . ?
N1 C10 C11 O1 -1.64(19) . . . . ?
C9 C10 C11 O1 179.20(14) . . . . ?
N1 C10 C11 C11 178.66(13) . . . 5_676 ?
C9 C10 C11 C11 -0.5(3) . . . 5_676 ?
C8 C7 N1 C10 0.00(15) . . . . ?
C6 C7 N1 C10 178.42(11) . . . . ?
C9 C10 N1 C7 -0.18(15) . . . . ?
C11 C10 N1 C7 -179.56(11) . . . . ?

_refine_diff_density_max         0.225
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_40719m3
_database_code_depnum_ccdc_archive 'CCDC 1871607'
_audit_update_record             
;
2018-10-05 deposited with the CCDC.
2018-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H20 N4'
_chemical_formula_sum            'C28 H20 N4'
_chemical_formula_weight         412.48

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_Int_Tables_number      33

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

_cell_length_a                   14.990(6)
_cell_length_b                   24.357(9)
_cell_length_c                   5.395(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1969.8(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    2247
_cell_measurement_theta_min      26.0
_cell_measurement_theta_max      68.2

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6573
_exptl_absorpt_correction_T_max  0.9375
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.8140
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7193
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         6.94
_diffrn_reflns_theta_max         66.00
_reflns_number_total             3094
_reflns_number_gt                3023
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.1260P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.4(4)
_refine_ls_number_reflns         3094
_refine_ls_number_parameters     289
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0843
_refine_ls_wR_factor_gt          0.0833
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.18802(8) 0.65396(5) 0.0852(2) 0.0163(3) Uani 1 1 d . . .
H1 H 0.2131 0.6699 0.2138 0.020 Uiso 1 1 calc R . .
N2 N 0.16832(8) 0.41388(5) 0.1059(3) 0.0169(3) Uani 1 1 d . . .
H2 H 0.2142 0.3978 0.1772 0.020 Uiso 1 1 calc R . .
N3 N 0.28100(8) 0.58908(5) 0.3829(3) 0.0174(3) Uani 1 1 d . . .
N4 N 0.25619(8) 0.47605(5) 0.4371(3) 0.0187(3) Uani 1 1 d . . .
C1 C 0.09961(10) 0.76546(6) -0.3269(3) 0.0188(3) Uani 1 1 d . . .
H3 H 0.0732 0.7428 -0.4500 0.023 Uiso 1 1 calc R . .
C2 C 0.09324(10) 0.82214(6) -0.3466(3) 0.0207(3) Uani 1 1 d . . .
H4 H 0.0620 0.8379 -0.4822 0.025 Uiso 1 1 calc R . .
C3 C 0.13200(10) 0.85584(6) -0.1704(3) 0.0207(3) Uani 1 1 d . . .
H5 H 0.1274 0.8946 -0.1844 0.025 Uiso 1 1 calc R . .
C4 C 0.17777(10) 0.83243(6) 0.0275(3) 0.0210(4) Uani 1 1 d . . .
H6 H 0.2050 0.8554 0.1480 0.025 Uiso 1 1 calc R . .
C5 C 0.18393(10) 0.77559(6) 0.0503(3) 0.0185(3) Uani 1 1 d . . .
H7 H 0.2149 0.7601 0.1869 0.022 Uiso 1 1 calc R . .
C6 C 0.14474(10) 0.74121(6) -0.1269(3) 0.0168(3) Uani 1 1 d . . .
C7 C 0.14988(9) 0.68118(6) -0.1102(3) 0.0165(3) Uani 1 1 d . . .
C8 C 0.11922(9) 0.64185(6) -0.2728(3) 0.0185(3) Uani 1 1 d . . .
H8 H 0.0897 0.6487 -0.4255 0.022 Uiso 1 1 calc R . .
C9 C 0.13911(10) 0.59005(6) -0.1741(3) 0.0188(3) Uani 1 1 d . . .
H9 H 0.1258 0.5557 -0.2490 0.023 Uiso 1 1 calc R . .
C10 C 0.18149(10) 0.59759(6) 0.0516(3) 0.0165(3) Uani 1 1 d . . .
C11 C 0.22429(9) 0.56250(6) 0.2369(3) 0.0164(3) Uani 1 1 d . . .
C12 C 0.21002(9) 0.50365(6) 0.2692(3) 0.0165(3) Uani 1 1 d . . .
C13 C 0.14922(10) 0.46942(6) 0.1217(3) 0.0171(3) Uani 1 1 d . . .
C14 C 0.07033(10) 0.47726(6) -0.0071(3) 0.0195(3) Uani 1 1 d . . .
H10 H 0.0394 0.5111 -0.0248 0.023 Uiso 1 1 calc R . .
C15 C 0.04414(10) 0.42663(6) -0.1070(3) 0.0192(3) Uani 1 1 d . . .
H11 H -0.0072 0.4203 -0.2062 0.023 Uiso 1 1 calc R . .
C16 C 0.10606(9) 0.38749(6) -0.0361(3) 0.0174(3) Uani 1 1 d . . .
C17 C 0.10889(9) 0.32843(6) -0.0883(3) 0.0164(3) Uani 1 1 d . . .
C18 C 0.06527(9) 0.30740(6) -0.2973(3) 0.0190(3) Uani 1 1 d . . .
H12 H 0.0348 0.3316 -0.4065 0.023 Uiso 1 1 calc R . .
C19 C 0.06624(10) 0.25134(6) -0.3459(3) 0.0204(3) Uani 1 1 d . . .
H13 H 0.0364 0.2376 -0.4883 0.024 Uiso 1 1 calc R . .
C20 C 0.11026(9) 0.21535(6) -0.1889(3) 0.0190(3) Uani 1 1 d . . .
H14 H 0.1106 0.1771 -0.2228 0.023 Uiso 1 1 calc R . .
C21 C 0.15381(10) 0.23590(6) 0.0185(3) 0.0200(3) Uani 1 1 d . . .
H15 H 0.1843 0.2116 0.1269 0.024 Uiso 1 1 calc R . .
C22 C 0.15299(9) 0.29179(6) 0.0683(3) 0.0177(3) Uani 1 1 d . . .
H16 H 0.1829 0.3053 0.2111 0.021 Uiso 1 1 calc R . .
C23 C 0.32567(10) 0.56101(6) 0.5633(3) 0.0170(3) Uani 1 1 d . . .
C24 C 0.38383(10) 0.58894(6) 0.7261(3) 0.0200(3) Uani 1 1 d . . .
H17 H 0.3928 0.6274 0.7085 0.024 Uiso 1 1 calc R . .
C25 C 0.42739(10) 0.56072(6) 0.9092(3) 0.0207(3) Uani 1 1 d . . .
H18 H 0.4655 0.5798 1.0203 0.025 Uiso 1 1 calc R . .
C26 C 0.41605(10) 0.50326(6) 0.9344(3) 0.0210(4) Uani 1 1 d . . .
H19 H 0.4470 0.4840 1.0612 0.025 Uiso 1 1 calc R . .
C27 C 0.36081(10) 0.47535(6) 0.7770(3) 0.0201(3) Uani 1 1 d . . .
H20 H 0.3538 0.4368 0.7945 0.024 Uiso 1 1 calc R . .
C28 C 0.31399(10) 0.50355(6) 0.5882(3) 0.0169(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C7 1.370(2) . ?
N1 C10 1.3882(18) . ?
N1 H1 0.8800 . ?
N2 C16 1.368(2) . ?
N2 C13 1.3853(18) . ?
N2 H2 0.8800 . ?
N3 C11 1.328(2) . ?
N3 C23 1.365(2) . ?
N4 C12 1.323(2) . ?
N4 C28 1.365(2) . ?
C1 C2 1.388(2) . ?
C1 C6 1.404(2) . ?
C1 H3 0.9500 . ?
C2 C3 1.384(2) . ?
C2 H4 0.9500 . ?
C3 C4 1.391(2) . ?
C3 H5 0.9500 . ?
C4 C5 1.393(2) . ?
C4 H6 0.9500 . ?
C5 C6 1.400(2) . ?
C5 H7 0.9500 . ?
C6 C7 1.467(2) . ?
C7 C8 1.378(2) . ?
C8 C9 1.402(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.386(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.463(2) . ?
C11 C12 1.460(2) . ?
C12 C13 1.469(2) . ?
C13 C14 1.385(2) . ?
C14 C15 1.402(2) . ?
C14 H10 0.9500 . ?
C15 C16 1.384(2) . ?
C15 H11 0.9500 . ?
C16 C17 1.467(2) . ?
C17 C22 1.395(2) . ?
C17 C18 1.400(2) . ?
C18 C19 1.390(2) . ?
C18 H12 0.9500 . ?
C19 C20 1.386(2) . ?
C19 H13 0.9500 . ?
C20 C21 1.389(2) . ?
C20 H14 0.9500 . ?
C21 C22 1.388(2) . ?
C21 H15 0.9500 . ?
C22 H16 0.9500 . ?
C23 C24 1.412(2) . ?
C23 C28 1.417(2) . ?
C24 C25 1.369(2) . ?
C24 H17 0.9500 . ?
C25 C26 1.416(2) . ?
C25 H18 0.9500 . ?
C26 C27 1.367(2) . ?
C26 H19 0.9500 . ?
C27 C28 1.415(2) . ?
C27 H20 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 N1 C10 110.40(12) . . ?
C7 N1 H1 124.8 . . ?
C10 N1 H1 124.8 . . ?
C16 N2 C13 110.64(12) . . ?
C16 N2 H2 124.7 . . ?
C13 N2 H2 124.7 . . ?
C11 N3 C23 119.55(13) . . ?
C12 N4 C28 119.42(13) . . ?
C2 C1 C6 120.70(14) . . ?
C2 C1 H3 119.7 . . ?
C6 C1 H3 119.7 . . ?
C3 C2 C1 120.56(15) . . ?
C3 C2 H4 119.7 . . ?
C1 C2 H4 119.7 . . ?
C2 C3 C4 119.41(14) . . ?
C2 C3 H5 120.3 . . ?
C4 C3 H5 120.3 . . ?
C3 C4 C5 120.52(15) . . ?
C3 C4 H6 119.7 . . ?
C5 C4 H6 119.7 . . ?
C4 C5 C6 120.41(15) . . ?
C4 C5 H7 119.8 . . ?
C6 C5 H7 119.8 . . ?
C5 C6 C1 118.39(13) . . ?
C5 C6 C7 122.14(14) . . ?
C1 C6 C7 119.47(13) . . ?
N1 C7 C8 107.01(13) . . ?
N1 C7 C6 123.48(13) . . ?
C8 C7 C6 129.51(15) . . ?
C7 C8 C9 108.25(15) . . ?
C7 C8 H8 125.9 . . ?
C9 C8 H8 125.9 . . ?
C10 C9 C8 108.16(14) . . ?
C10 C9 H9 125.9 . . ?
C8 C9 H9 125.9 . . ?
C9 C10 N1 106.17(13) . . ?
C9 C10 C11 136.36(14) . . ?
N1 C10 C11 117.22(13) . . ?
N3 C11 C12 120.11(13) . . ?
N3 C11 C10 113.66(13) . . ?
C12 C11 C10 126.24(13) . . ?
N4 C12 C11 120.28(13) . . ?
N4 C12 C13 113.99(13) . . ?
C11 C12 C13 125.68(13) . . ?
C14 C13 N2 106.27(13) . . ?
C14 C13 C12 136.32(13) . . ?
N2 C13 C12 117.35(13) . . ?
C13 C14 C15 108.11(13) . . ?
C13 C14 H10 125.9 . . ?
C15 C14 H10 125.9 . . ?
C16 C15 C14 108.16(14) . . ?
C16 C15 H11 125.9 . . ?
C14 C15 H11 125.9 . . ?
N2 C16 C15 106.78(13) . . ?
N2 C16 C17 123.29(12) . . ?
C15 C16 C17 129.92(14) . . ?
C22 C17 C18 118.34(14) . . ?
C22 C17 C16 121.64(14) . . ?
C18 C17 C16 120.00(13) . . ?
C19 C18 C17 120.42(14) . . ?
C19 C18 H12 119.8 . . ?
C17 C18 H12 119.8 . . ?
C20 C19 C18 120.70(15) . . ?
C20 C19 H13 119.6 . . ?
C18 C19 H13 119.6 . . ?
C19 C20 C21 119.22(14) . . ?
C19 C20 H14 120.4 . . ?
C21 C20 H14 120.4 . . ?
C22 C21 C20 120.35(15) . . ?
C22 C21 H15 119.8 . . ?
C20 C21 H15 119.8 . . ?
C21 C22 C17 120.96(15) . . ?
C21 C22 H16 119.5 . . ?
C17 C22 H16 119.5 . . ?
N3 C23 C24 120.34(13) . . ?
N3 C23 C28 120.10(13) . . ?
C24 C23 C28 119.56(14) . . ?
C25 C24 C23 120.09(14) . . ?
C25 C24 H17 120.0 . . ?
C23 C24 H17 120.0 . . ?
C24 C25 C26 120.52(14) . . ?
C24 C25 H18 119.7 . . ?
C26 C25 H18 119.7 . . ?
C27 C26 C25 120.30(14) . . ?
C27 C26 H19 119.8 . . ?
C25 C26 H19 119.8 . . ?
C26 C27 C28 120.41(14) . . ?
C26 C27 H20 119.8 . . ?
C28 C27 H20 119.8 . . ?
N4 C28 C27 120.42(13) . . ?
N4 C28 C23 120.45(14) . . ?
C27 C28 C23 119.10(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.6(2) . . . . ?
C1 C2 C3 C4 0.1(2) . . . . ?
C2 C3 C4 C5 -0.7(2) . . . . ?
C3 C4 C5 C6 0.5(2) . . . . ?
C4 C5 C6 C1 0.1(2) . . . . ?
C4 C5 C6 C7 179.83(13) . . . . ?
C2 C1 C6 C5 -0.7(2) . . . . ?
C2 C1 C6 C7 179.60(14) . . . . ?
C10 N1 C7 C8 -0.59(16) . . . . ?
C10 N1 C7 C6 178.87(13) . . . . ?
C5 C6 C7 N1 4.2(2) . . . . ?
C1 C6 C7 N1 -176.14(13) . . . . ?
C5 C6 C7 C8 -176.49(15) . . . . ?
C1 C6 C7 C8 3.2(2) . . . . ?
N1 C7 C8 C9 0.01(16) . . . . ?
C6 C7 C8 C9 -179.40(14) . . . . ?
C7 C8 C9 C10 0.56(17) . . . . ?
C8 C9 C10 N1 -0.90(16) . . . . ?
C8 C9 C10 C11 -174.74(16) . . . . ?
C7 N1 C10 C9 0.93(16) . . . . ?
C7 N1 C10 C11 176.15(13) . . . . ?
C23 N3 C11 C12 -0.1(2) . . . . ?
C23 N3 C11 C10 -179.78(12) . . . . ?
C9 C10 C11 N3 158.82(17) . . . . ?
N1 C10 C11 N3 -14.52(19) . . . . ?
C9 C10 C11 C12 -20.9(3) . . . . ?
N1 C10 C11 C12 165.80(14) . . . . ?
C28 N4 C12 C11 3.3(2) . . . . ?
C28 N4 C12 C13 -179.03(13) . . . . ?
N3 C11 C12 N4 -2.8(2) . . . . ?
C10 C11 C12 N4 176.82(14) . . . . ?
N3 C11 C12 C13 179.75(14) . . . . ?
C10 C11 C12 C13 -0.6(2) . . . . ?
C16 N2 C13 C14 2.36(18) . . . . ?
C16 N2 C13 C12 179.81(14) . . . . ?
N4 C12 C13 C14 153.78(18) . . . . ?
C11 C12 C13 C14 -28.7(3) . . . . ?
N4 C12 C13 N2 -22.7(2) . . . . ?
C11 C12 C13 N2 154.87(14) . . . . ?
N2 C13 C14 C15 -2.02(18) . . . . ?
C12 C13 C14 C15 -178.75(18) . . . . ?
C13 C14 C15 C16 1.01(19) . . . . ?
C13 N2 C16 C15 -1.75(17) . . . . ?
C13 N2 C16 C17 179.51(13) . . . . ?
C14 C15 C16 N2 0.43(18) . . . . ?
C14 C15 C16 C17 179.07(15) . . . . ?
N2 C16 C17 C22 24.1(2) . . . . ?
C15 C16 C17 C22 -154.36(16) . . . . ?
N2 C16 C17 C18 -157.11(15) . . . . ?
C15 C16 C17 C18 24.5(2) . . . . ?
C22 C17 C18 C19 0.0(2) . . . . ?
C16 C17 C18 C19 -178.86(13) . . . . ?
C17 C18 C19 C20 0.0(2) . . . . ?
C18 C19 C20 C21 -0.1(2) . . . . ?
C19 C20 C21 C22 0.2(2) . . . . ?
C20 C21 C22 C17 -0.2(2) . . . . ?
C18 C17 C22 C21 0.1(2) . . . . ?
C16 C17 C22 C21 178.92(13) . . . . ?
C11 N3 C23 C24 -177.74(14) . . . . ?
C11 N3 C23 C28 2.3(2) . . . . ?
N3 C23 C24 C25 178.96(13) . . . . ?
C28 C23 C24 C25 -1.1(2) . . . . ?
C23 C24 C25 C26 1.3(2) . . . . ?
C24 C25 C26 C27 -0.5(2) . . . . ?
C25 C26 C27 C28 -0.3(2) . . . . ?
C12 N4 C28 C27 176.90(14) . . . . ?
C12 N4 C28 C23 -1.0(2) . . . . ?
C26 C27 C28 N4 -177.45(14) . . . . ?
C26 C27 C28 C23 0.5(2) . . . . ?
N3 C23 C28 N4 -1.9(2) . . . . ?
C24 C23 C28 N4 178.18(14) . . . . ?
N3 C23 C28 C27 -179.83(14) . . . . ?
C24 C23 C28 C27 0.3(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        66.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.072
####################################################################### 
# 
# 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_41105m3
_database_code_depnum_ccdc_archive 'CCDC 1871610'
_audit_update_record             
;
2018-10-05 deposited with the CCDC.
2018-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(C28 H20 N4), 2(C7 H8) '
_chemical_formula_sum            'C98 H76 Cl0 N12'
_chemical_formula_weight         1421.71

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.7878(12)
_cell_length_b                   16.2197(8)
_cell_length_c                   19.920(2)
_cell_angle_alpha                72.109(15)
_cell_angle_beta                 85.164(15)
_cell_angle_gamma                66.730(15)
_cell_volume                     3890.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9056
_exptl_absorpt_correction_T_max  0.9888
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.8140
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            51030
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         6.53
_diffrn_reflns_theta_max         68.37
_reflns_number_total             13851
_reflns_number_gt                10434
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0577P)²+1.4258P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13851
_refine_ls_number_parameters     1031
_refine_ls_number_restraints     169
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1125
_refine_ls_wR_factor_gt          0.1015
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N9 N 0.94425(10) 0.26616(10) 0.32072(7) 0.0192(3) Uani 1 1 d . . .
N1 N 1.50517(10) -0.15317(10) 0.28227(7) 0.0206(3) Uani 1 1 d . . .
N5 N 1.76455(10) -0.66710(10) 0.41651(7) 0.0188(3) Uani 1 1 d . . .
H1 H 1.8132 -0.6899 0.3881 0.023 Uiso 1 1 calc R . .
N6 N 1.62400(10) -0.29714(10) 0.41774(7) 0.0193(3) Uani 1 1 d . . .
H2 H 1.5895 -0.2530 0.3796 0.023 Uiso 1 1 calc R . .
N7 N 1.73057(11) -0.34736(10) 0.29746(7) 0.0225(3) Uani 1 1 d . . .
N3 N 1.32836(10) 0.18360(10) 0.17078(7) 0.0184(3) Uani 1 1 d . . .
H3 H 1.2679 0.1865 0.1903 0.022 Uiso 1 1 calc R . .
N8 N 1.75682(11) -0.52595(10) 0.29218(7) 0.0214(3) Uani 1 1 d . . .
N11 N 1.12878(10) 0.14396(10) 0.13155(7) 0.0180(3) Uani 1 1 d . . .
H4 H 1.1900 0.1137 0.1553 0.022 Uiso 1 1 calc R . .
N2 N 1.32578(10) 0.00527(10) 0.21849(7) 0.0192(3) Uani 1 1 d . . .
N12 N 0.74807(10) 0.30745(10) 0.26268(7) 0.0197(3) Uani 1 1 d . . .
H5 H 0.7456 0.3523 0.2796 0.024 Uiso 1 1 calc R . .
N10 N 1.12878(10) 0.19311(10) 0.25108(7) 0.0190(3) Uani 1 1 d . . .
N4 N 1.69474(10) -0.14253(10) 0.30221(7) 0.0181(3) Uani 1 1 d . . .
H6 H 1.7038 -0.1993 0.3022 0.022 Uiso 1 1 calc R . .
C13 C 1.03939(13) 0.25819(12) 0.34358(8) 0.0195(4) Uani 1 1 d . . .
C14 C 1.41765(12) 0.01230(12) 0.22158(8) 0.0173(3) Uani 1 1 d . . .
C15 C 1.42029(12) 0.10386(12) 0.18344(8) 0.0184(3) Uani 1 1 d . . .
C16 C 0.83912(13) 0.24102(12) 0.24789(8) 0.0192(4) Uani 1 1 d . . .
C17 C 1.30100(13) 0.11134(12) 0.03172(9) 0.0225(4) Uani 1 1 d . . .
H7 H 1.3140 0.1248 0.0724 0.027 Uiso 1 1 calc R . .
C18 C 1.13296(13) 0.21625(12) 0.31085(8) 0.0195(4) Uani 1 1 d . . .
C19 C 1.62255(13) 0.01134(12) 0.28651(9) 0.0212(4) Uani 1 1 d . . .
H8 H 1.5745 0.0753 0.2740 0.025 Uiso 1 1 calc R . .
C20 C 0.94135(13) 0.23788(12) 0.26572(8) 0.0185(3) Uani 1 1 d . . .
C21 C 1.50894(12) -0.06898(12) 0.25848(8) 0.0179(3) Uani 1 1 d . . .
C22 C 1.41234(13) -0.16177(12) 0.27425(9) 0.0214(4) Uani 1 1 d . . .
C23 C 1.03488(12) 0.19111(12) 0.15832(8) 0.0182(3) Uani 1 1 d . . .
C24 C 1.03559(12) 0.20547(11) 0.22695(8) 0.0176(3) Uani 1 1 d . . .
C26 C 1.20123(13) 0.11496(12) 0.01906(8) 0.0192(4) Uani 1 1 d . . .
C27 C 1.60496(12) -0.06241(12) 0.27684(8) 0.0180(3) Uani 1 1 d . . .
C28 C 1.32047(13) -0.08129(12) 0.24597(8) 0.0197(4) Uani 1 1 d . . .
C29 C 1.71419(13) -0.57345(12) 0.41135(9) 0.0200(4) Uani 1 1 d . . .
C30 C 1.73253(12) -0.50311(12) 0.35144(8) 0.0187(3) Uani 1 1 d . . .
C32 C 1.72084(12) -0.41172(12) 0.35433(9) 0.0193(4) Uani 1 1 d . . .
C34 C 1.72831(13) -0.72004(12) 0.47210(8) 0.0204(4) Uani 1 1 d . . .
C35 C 1.49635(13) 0.12883(12) 0.14252(8) 0.0209(4) Uani 1 1 d . . .
H9 H 1.5678 0.0883 0.1403 0.025 Uiso 1 1 calc R . .
C36 C 1.69616(13) -0.38512(12) 0.41924(9) 0.0206(4) Uani 1 1 d . . .
C37 C 1.34515(13) 0.25779(12) 0.12319(8) 0.0195(4) Uani 1 1 d . . .
C39 C 1.76010(14) -0.87381(13) 0.56149(9) 0.0259(4) Uani 1 1 d . . .
H10 H 1.7198 -0.8414 0.5934 0.031 Uiso 1 1 calc R . .
C40 C 1.87118(13) -0.18870(12) 0.35965(8) 0.0202(4) Uani 1 1 d . . .
C41 C 0.69912(14) 0.21541(13) 0.22372(9) 0.0260(4) Uani 1 1 d . . .
H11 H 0.6571 0.1886 0.2098 0.031 Uiso 1 1 calc R . .
C42 C 1.14092(14) 0.27194(13) 0.42869(9) 0.0281(4) Uani 1 1 d . . .
H12 H 1.1445 0.2912 0.4685 0.034 Uiso 1 1 calc R . .
C44 C 1.50495(14) -0.11627(13) 0.45009(9) 0.0248(4) Uani 1 1 d . . .
H13 H 1.5352 -0.1093 0.4051 0.030 Uiso 1 1 calc R . .
C45 C 1.76772(12) -0.12019(12) 0.32742(8) 0.0189(4) Uani 1 1 d . . .
C46 C 1.18462(13) 0.09295(12) -0.04038(9) 0.0228(4) Uani 1 1 d . . .
H14 H 1.1175 0.0944 -0.0498 0.027 Uiso 1 1 calc R . .
C47 C 1.23087(13) 0.20149(13) 0.33912(9) 0.0244(4) Uani 1 1 d . . .
H15 H 1.2945 0.1729 0.3178 0.029 Uiso 1 1 calc R . .
C48 C 1.89850(14) -0.28501(13) 0.38016(10) 0.0273(4) Uani 1 1 d . . .
H16 H 1.8488 -0.3093 0.3736 0.033 Uiso 1 1 calc R . .
C49 C 1.75495(13) -0.37072(12) 0.23603(9) 0.0229(4) Uani 1 1 d . . .
C50 C 1.65077(14) -0.65789(13) 0.50162(9) 0.0246(4) Uani 1 1 d . . .
H17 H 1.6103 -0.6743 0.5406 0.030 Uiso 1 1 calc R . .
C51 C 1.04500(14) 0.28688(13) 0.40263(9) 0.0246(4) Uani 1 1 d . . .
H18 H 0.9822 0.3166 0.4242 0.030 Uiso 1 1 calc R . .
C52 C 1.53655(13) -0.20483(12) 0.50000(9) 0.0215(4) Uani 1 1 d . . .
C53 C 1.94591(13) -0.15554(13) 0.37086(9) 0.0248(4) Uani 1 1 d . . .
H19 H 1.9286 -0.0897 0.3571 0.030 Uiso 1 1 calc R . .
C55 C 1.23425(14) 0.22829(14) 0.39711(9) 0.0284(4) Uani 1 1 d . . .
H20 H 1.3005 0.2173 0.4164 0.034 Uiso 1 1 calc R . .
C56 C 1.26154(13) 0.35160(12) 0.09838(9) 0.0223(4) Uani 1 1 d . . .
C57 C 1.41796(14) -0.13448(14) 0.58144(10) 0.0289(4) Uani 1 1 d . . .
H21 H 1.3886 -0.1408 0.6267 0.035 Uiso 1 1 calc R . .
C58 C 1.26595(14) 0.06900(13) -0.08556(9) 0.0266(4) Uani 1 1 d . . .
H22 H 1.2543 0.0536 -0.1257 0.032 Uiso 1 1 calc R . .
C59 C 0.66203(13) 0.29382(13) 0.24736(9) 0.0222(4) Uani 1 1 d . . .
C60 C 1.64203(13) -0.56666(13) 0.46429(9) 0.0238(4) Uani 1 1 d . . .
H23 H 1.5952 -0.5103 0.4735 0.029 Uiso 1 1 calc R . .
C61 C 1.38125(14) 0.08839(13) -0.01407(9) 0.0253(4) Uani 1 1 d . . .
H24 H 1.4485 0.0871 -0.0050 0.030 Uiso 1 1 calc R . .
C62 C 1.68393(15) -0.37143(13) 0.52839(9) 0.0278(4) Uani 1 1 d . . .
H25 H 1.6954 -0.3852 0.5777 0.033 Uiso 1 1 calc R . .
C63 C 1.72361(13) -0.02467(12) 0.31786(9) 0.0215(4) Uani 1 1 d . . .
H26 H 1.7563 0.0106 0.3304 0.026 Uiso 1 1 calc R . .
C64 C 1.76938(13) -0.46069(12) 0.23331(9) 0.0224(4) Uani 1 1 d . . .
C65 C 1.77327(13) -0.82256(12) 0.49320(9) 0.0214(4) Uani 1 1 d . . .
C67 C 1.61380(13) -0.28841(12) 0.48438(9) 0.0216(4) Uani 1 1 d . . .
C68 C 1.36403(14) 0.06725(13) -0.07298(9) 0.0265(4) Uani 1 1 d . . .
H27 H 1.4191 0.0516 -0.1046 0.032 Uiso 1 1 calc R . .
C70 C 1.44919(13) 0.22455(12) 0.10500(9) 0.0219(4) Uani 1 1 d . . .
H28 H 1.4830 0.2603 0.0727 0.026 Uiso 1 1 calc R . .
C71 C 1.83236(14) -0.87206(13) 0.44747(10) 0.0257(4) Uani 1 1 d . . .
H29 H 1.8416 -0.8387 0.4007 0.031 Uiso 1 1 calc R . .
C72 C 1.73513(15) -0.43168(13) 0.48774(9) 0.0269(4) Uani 1 1 d . . .
H30 H 1.7874 -0.4936 0.5044 0.032 Uiso 1 1 calc R . .
C73 C 1.80510(15) -0.97105(14) 0.58312(10) 0.0313(4) Uani 1 1 d . . .
H31 H 1.7955 -1.0050 0.6296 0.038 Uiso 1 1 calc R . .
C74 C 1.87768(14) -0.96929(13) 0.46967(10) 0.0302(4) Uani 1 1 d . . .
H32 H 1.9185 -1.0022 0.4382 0.036 Uiso 1 1 calc R . .
C75 C 0.80979(14) 0.18245(13) 0.22400(9) 0.0234(4) Uani 1 1 d . . .
H33 H 0.8561 0.1295 0.2103 0.028 Uiso 1 1 calc R . .
C76 C 1.49248(14) -0.21280(14) 0.56610(9) 0.0267(4) Uani 1 1 d . . .
H34 H 1.5138 -0.2725 0.6009 0.032 Uiso 1 1 calc R . .
C78 C 1.79347(15) -0.48186(14) 0.16888(9) 0.0292(4) Uani 1 1 d . . .
H35 H 1.8030 -0.5422 0.1665 0.035 Uiso 1 1 calc R . .
C79 C 1.80309(15) -0.41557(14) 0.10965(10) 0.0339(5) Uani 1 1 d . . .
H36 H 1.8181 -0.4297 0.0661 0.041 Uiso 1 1 calc R . .
C80 C 1.38613(14) -0.04720(14) 0.53129(10) 0.0288(4) Uani 1 1 d . . .
H37 H 1.3347 0.0064 0.5418 0.035 Uiso 1 1 calc R . .
C81 C 1.86390(15) -1.01882(14) 0.53738(11) 0.0328(4) Uani 1 1 d . . .
H38 H 1.8949 -1.0856 0.5523 0.039 Uiso 1 1 calc R . .
C82 C 2.07089(15) -0.31211(15) 0.42107(11) 0.0357(5) Uani 1 1 d . . .
H39 H 2.1388 -0.3543 0.4418 0.043 Uiso 1 1 calc R . .
C83 C 1.42977(14) -0.03852(14) 0.46563(10) 0.0285(4) Uani 1 1 d . . .
H40 H 1.4079 0.0213 0.4309 0.034 Uiso 1 1 calc R . .
C85 C 0.55395(14) 0.35497(14) 0.25764(9) 0.0266(4) Uani 1 1 d . . .
C86 C 1.28527(16) 0.42970(14) 0.06569(11) 0.0357(5) Uani 1 1 d . . .
H41 H 1.3570 0.4223 0.0599 0.043 Uiso 1 1 calc R . .
C87 C 1.76731(16) -0.30460(14) 0.17463(10) 0.0355(5) Uani 1 1 d . . .
H42 H 1.7592 -0.2443 0.1762 0.043 Uiso 1 1 calc R . .
C88 C 1.99798(15) -0.34624(15) 0.41027(11) 0.0365(5) Uani 1 1 d . . .
H43 H 2.0162 -0.4122 0.4236 0.044 Uiso 1 1 calc R . .
C89 C 1.15549(16) 0.36531(15) 0.10423(12) 0.0410(5) Uani 1 1 d . . .
H44 H 1.1367 0.3129 0.1252 0.049 Uiso 1 1 calc R . .
C90 C 1.79088(17) -0.32684(15) 0.11289(10) 0.0391(5) Uani 1 1 d . . .
H45 H 1.7991 -0.2818 0.0717 0.047 Uiso 1 1 calc R . .
C91 C 1.20616(18) 0.51816(15) 0.04140(12) 0.0413(5) Uani 1 1 d . . .
H46 H 1.2243 0.5706 0.0191 0.050 Uiso 1 1 calc R . .
C92 C 1.10273(17) 0.53122(15) 0.04894(11) 0.0408(5) Uani 1 1 d . . .
H47 H 1.0488 0.5925 0.0331 0.049 Uiso 1 1 calc R . .
C96 C 0.34804(16) 0.46936(18) 0.27921(12) 0.0487(6) Uani 1 1 d . . .
H48 H 0.2780 0.5098 0.2848 0.058 Uiso 1 1 calc R . .
C97 C 0.53490(15) 0.41502(15) 0.29929(12) 0.0397(5) Uani 1 1 d . . .
H49 H 0.5929 0.4168 0.3205 0.048 Uiso 1 1 calc R . .
C98 C 2.04432(14) -0.21670(14) 0.40152(10) 0.0305(4) Uani 1 1 d . . .
H50 H 2.0938 -0.1928 0.4091 0.037 Uiso 1 1 calc R . .
C99 C 0.46786(16) 0.3518(2) 0.22973(12) 0.0498(6) Uani 1 1 d . . .
H51 H 0.4786 0.3103 0.2025 0.060 Uiso 1 1 calc R . .
C101 C 1.07701(18) 0.45409(16) 0.08004(13) 0.0510(6) Uani 1 1 d . . .
H52 H 1.0049 0.4622 0.0848 0.061 Uiso 1 1 calc R . .
C102 C 0.43312(16) 0.47167(16) 0.30999(13) 0.0463(6) Uani 1 1 d . . .
H53 H 0.4215 0.5121 0.3383 0.056 Uiso 1 1 calc R . .
C104 C 0.36591(17) 0.4082(2) 0.24073(13) 0.0635(8) Uani 1 1 d . . .
H54 H 0.3077 0.4045 0.2214 0.076 Uiso 1 1 calc R . .
C105 C 1.00733(13) 0.20409(12) 0.04498(9) 0.0210(4) Uani 1 1 d . . .
H55 H 0.9737 0.2204 0.0004 0.025 Uiso 1 1 calc R . .
C106 C 1.11327(13) 0.15097(12) 0.06285(8) 0.0187(3) Uani 1 1 d . . .
C107 C 0.95829(13) 0.22966(12) 0.10403(8) 0.0207(4) Uani 1 1 d . . .
H56 H 0.8856 0.2668 0.1066 0.025 Uiso 1 1 calc R . .
C108 C 1.22403(13) -0.09100(13) 0.24302(9) 0.0249(4) Uani 1 1 d . . .
H57 H 1.1615 -0.0369 0.2249 0.030 Uiso 1 1 calc R . .
C109 C 1.22021(14) -0.17812(14) 0.26616(10) 0.0294(4) Uani 1 1 d . . .
H58 H 1.1550 -0.1844 0.2641 0.035 Uiso 1 1 calc R . .
C110 C 1.31199(15) -0.25830(14) 0.29293(11) 0.0329(4) Uani 1 1 d . . .
H59 H 1.3085 -0.3186 0.3083 0.039 Uiso 1 1 calc R . .
C111 C 1.40657(14) -0.25089(13) 0.29724(10) 0.0293(4) Uani 1 1 d . . .
H60 H 1.4682 -0.3057 0.3157 0.035 Uiso 1 1 calc R . .
C112 C 0.05478(15) 0.77017(15) 0.16142(9) 0.0312(4) Uani 1 1 d . . .
C113 C -0.02601(14) 0.82446(14) 0.19503(9) 0.0291(4) Uani 1 1 d . . .
H61 H -0.0641 0.7954 0.2294 0.035 Uiso 1 1 calc R . .
C114 C -0.05207(15) 0.91995(15) 0.17946(10) 0.0326(5) Uani 1 1 d . . .
H62 H -0.1069 0.9557 0.2036 0.039 Uiso 1 1 calc R . .
C115 C 0.00129(16) 0.96348(16) 0.12900(10) 0.0367(5) Uani 1 1 d . . .
H63 H -0.0173 1.0293 0.1175 0.044 Uiso 1 1 calc R . .
C116 C 0.10875(15) 0.81507(17) 0.11151(10) 0.0365(5) Uani 1 1 d . . .
H64 H 0.1650 0.7793 0.0882 0.044 Uiso 1 1 calc R . .
C117 C 0.08221(16) 0.91024(17) 0.09528(10) 0.0391(5) Uani 1 1 d . . .
H65 H 0.1197 0.9396 0.0607 0.047 Uiso 1 1 calc R . .
C118 C 0.08159(19) 0.66645(17) 0.17868(13) 0.0501(6) Uani 1 1 d . . .
H66 H 0.0348 0.6483 0.2147 0.075 Uiso 1 1 calc R . .
H67 H 0.1552 0.6315 0.1966 0.075 Uiso 1 1 calc R . .
H68 H 0.0723 0.6520 0.1360 0.075 Uiso 1 1 calc R . .
C120 C 0.5615(3) 0.3351(2) -0.0764(2) 0.0476(18) Uani 0.530(6) 1 d PGU A 1
C121 C 0.5843(4) 0.2430(3) -0.0748(2) 0.051(2) Uani 0.530(6) 1 d PGU A 1
H85 H 0.5532 0.2310 -0.1096 0.061 Uiso 0.530(6) 1 calc PR A 1
C124 C 0.6527(3) 0.1685(2) -0.0223(2) 0.0477(15) Uani 0.530(6) 1 d PGU A 1
H86 H 0.6683 0.1056 -0.0213 0.057 Uiso 0.530(6) 1 calc PR A 1
C122 C 0.6983(3) 0.1861(3) 0.0286(2) 0.062(3) Uani 0.530(6) 1 d PGU A 1
H87 H 0.7450 0.1352 0.0645 0.074 Uiso 0.530(6) 1 calc PR A 1
C119 C 0.6755(4) 0.2782(3) 0.0270(2) 0.077(4) Uani 0.530(6) 1 d PGU A 1
H88 H 0.7066 0.2902 0.0618 0.092 Uiso 0.530(6) 1 calc PR A 1
C123 C 0.6071(4) 0.3527(3) -0.0255(2) 0.0598(19) Uani 0.530(6) 1 d PGU A 1
H89 H 0.5915 0.4156 -0.0266 0.072 Uiso 0.530(6) 1 calc PR A 1
C125 C 0.4910(5) 0.4085(5) -0.1360(4) 0.104(3) Uani 0.530(6) 1 d PU A 1
H74 H 0.4653 0.3790 -0.1628 0.156 Uiso 0.530(6) 1 calc PR A 1
H75 H 0.5300 0.4433 -0.1670 0.156 Uiso 0.530(6) 1 calc PR A 1
H76 H 0.4307 0.4519 -0.1178 0.156 Uiso 0.530(6) 1 calc PR A 1
C131 C 0.5804(10) 0.1907(9) -0.1038(5) 0.186(6) Uani 0.470(6) 1 d PDU A 2
H77 H 0.5300 0.2389 -0.1417 0.279 Uiso 0.470(6) 1 calc PR A 2
H78 H 0.5490 0.1470 -0.0758 0.279 Uiso 0.470(6) 1 calc PR A 2
H79 H 0.6450 0.1561 -0.1244 0.279 Uiso 0.470(6) 1 calc PR A 2
C1 C 0.6056(6) 0.2348(7) -0.0593(4) 0.082(4) Uani 0.470(6) 1 d PGU A 2
C126 C 0.6719(5) 0.2059(6) -0.0005(3) 0.081(3) Uani 0.470(6) 1 d PGDU A 2
H80 H 0.7158 0.1413 0.0188 0.098 Uiso 0.470(6) 1 calc PR A 2
C127 C 0.6739(7) 0.2716(7) 0.0301(4) 0.089(5) Uani 0.470(6) 1 d PGU A 2
H81 H 0.7192 0.2519 0.0703 0.107 Uiso 0.470(6) 1 calc PR A 2
C128 C 0.6097(8) 0.3661(7) 0.0019(5) 0.142(5) Uani 0.470(6) 1 d PGU A 2
H82 H 0.6111 0.4110 0.0228 0.170 Uiso 0.470(6) 1 calc PR A 2
C129 C 0.5434(7) 0.3950(6) -0.0569(5) 0.143(5) Uani 0.470(6) 1 d PGU A 2
H90 H 0.4995 0.4596 -0.0762 0.171 Uiso 0.470(6) 1 calc PR A 2
C130 C 0.5413(6) 0.3293(8) -0.0875(4) 0.119(5) Uani 0.470(6) 1 d PGDU A 2
H84 H 0.4960 0.3490 -0.1277 0.143 Uiso 0.470(6) 1 calc PR 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
N9 C20 1.320(2) . ?
N9 C13 1.369(2) . ?
N1 C21 1.321(2) . ?
N1 C22 1.368(2) . ?
N5 C34 1.369(2) . ?
N5 C29 1.372(2) . ?
N5 H1 0.8800 . ?
N6 C67 1.368(2) . ?
N6 C36 1.373(2) . ?
N6 H2 0.8800 . ?
N7 C32 1.323(2) . ?
N7 C49 1.367(2) . ?
N3 C37 1.372(2) . ?
N3 C15 1.379(2) . ?
N3 H3 0.8800 . ?
N8 C30 1.322(2) . ?
N8 C64 1.369(2) . ?
N11 C106 1.366(2) . ?
N11 C23 1.377(2) . ?
N11 H4 0.8800 . ?
N2 C14 1.324(2) . ?
N2 C28 1.371(2) . ?
N12 C59 1.364(2) . ?
N12 C16 1.374(2) . ?
N12 H5 0.8800 . ?
N10 C24 1.328(2) . ?
N10 C18 1.366(2) . ?
N4 C45 1.371(2) . ?
N4 C27 1.381(2) . ?
N4 H6 0.8800 . ?
C13 C51 1.409(2) . ?
C13 C18 1.410(2) . ?
C14 C21 1.453(2) . ?
C14 C15 1.459(2) . ?
C15 C35 1.384(2) . ?
C16 C75 1.381(2) . ?
C16 C20 1.460(2) . ?
C17 C61 1.381(2) . ?
C17 C26 1.395(2) . ?
C17 H7 0.9500 . ?
C18 C47 1.409(2) . ?
C19 C27 1.380(2) . ?
C19 C63 1.397(2) . ?
C19 H8 0.9500 . ?
C20 C24 1.450(2) . ?
C21 C27 1.454(2) . ?
C22 C111 1.408(3) . ?
C22 C28 1.410(2) . ?
C23 C107 1.390(2) . ?
C23 C24 1.457(2) . ?
C26 C46 1.397(2) . ?
C26 C106 1.466(2) . ?
C28 C108 1.407(2) . ?
C29 C60 1.386(2) . ?
C29 C30 1.459(2) . ?
C30 C32 1.445(2) . ?
C32 C36 1.458(2) . ?
C34 C50 1.383(2) . ?
C34 C65 1.458(2) . ?
C35 C70 1.401(2) . ?
C35 H9 0.9500 . ?
C36 C72 1.375(2) . ?
C37 C70 1.379(2) . ?
C37 C56 1.462(2) . ?
C39 C73 1.383(3) . ?
C39 C65 1.399(2) . ?
C39 H10 0.9500 . ?
C40 C48 1.385(3) . ?
C40 C53 1.397(2) . ?
C40 C45 1.465(2) . ?
C41 C59 1.383(3) . ?
C41 C75 1.403(2) . ?
C41 H11 0.9500 . ?
C42 C51 1.365(2) . ?
C42 C55 1.404(3) . ?
C42 H12 0.9500 . ?
C44 C83 1.383(3) . ?
C44 C52 1.394(3) . ?
C44 H13 0.9500 . ?
C45 C63 1.378(2) . ?
C46 C58 1.385(2) . ?
C46 H14 0.9500 . ?
C47 C55 1.363(2) . ?
C47 H15 0.9500 . ?
C48 C88 1.387(3) . ?
C48 H16 0.9500 . ?
C49 C87 1.407(3) . ?
C49 C64 1.410(3) . ?
C50 C60 1.398(3) . ?
C50 H17 0.9500 . ?
C51 H18 0.9500 . ?
C52 C76 1.394(2) . ?
C52 C67 1.460(2) . ?
C53 C98 1.379(2) . ?
C53 H19 0.9500 . ?
C55 H20 0.9500 . ?
C56 C86 1.386(3) . ?
C56 C89 1.390(3) . ?
C57 C80 1.382(3) . ?
C57 C76 1.385(3) . ?
C57 H21 0.9500 . ?
C58 C68 1.384(2) . ?
C58 H22 0.9500 . ?
C59 C85 1.467(2) . ?
C60 H23 0.9500 . ?
C61 C68 1.382(2) . ?
C61 H24 0.9500 . ?
C62 C67 1.380(3) . ?
C62 C72 1.398(3) . ?
C62 H25 0.9500 . ?
C63 H26 0.9500 . ?
C64 C78 1.409(2) . ?
C65 C71 1.395(2) . ?
C68 H27 0.9500 . ?
C70 H28 0.9500 . ?
C71 C74 1.383(3) . ?
C71 H29 0.9500 . ?
C72 H30 0.9500 . ?
C73 C81 1.379(3) . ?
C73 H31 0.9500 . ?
C74 C81 1.383(3) . ?
C74 H32 0.9500 . ?
C75 H33 0.9500 . ?
C76 H34 0.9500 . ?
C78 C79 1.368(3) . ?
C78 H35 0.9500 . ?
C79 C90 1.403(3) . ?
C79 H36 0.9500 . ?
C80 C83 1.383(3) . ?
C80 H37 0.9500 . ?
C81 H38 0.9500 . ?
C82 C98 1.374(3) . ?
C82 C88 1.383(3) . ?
C82 H39 0.9500 . ?
C83 H40 0.9500 . ?
C85 C99 1.377(3) . ?
C85 C97 1.401(3) . ?
C86 C91 1.381(3) . ?
C86 H41 0.9500 . ?
C87 C90 1.364(3) . ?
C87 H42 0.9500 . ?
C88 H43 0.9500 . ?
C89 C101 1.381(3) . ?
C89 H44 0.9500 . ?
C90 H45 0.9500 . ?
C91 C92 1.359(3) . ?
C91 H46 0.9500 . ?
C92 C101 1.383(3) . ?
C92 H47 0.9500 . ?
C96 C104 1.369(4) . ?
C96 C102 1.387(3) . ?
C96 H48 0.9500 . ?
C97 C102 1.382(3) . ?
C97 H49 0.9500 . ?
C98 H50 0.9500 . ?
C99 C104 1.384(3) . ?
C99 H51 0.9500 . ?
C101 H52 0.9500 . ?
C102 H53 0.9500 . ?
C104 H54 0.9500 . ?
C105 C106 1.381(2) . ?
C105 C107 1.399(2) . ?
C105 H55 0.9500 . ?
C107 H56 0.9500 . ?
C108 C109 1.366(3) . ?
C108 H57 0.9500 . ?
C109 C110 1.402(3) . ?
C109 H58 0.9500 . ?
C110 C111 1.368(3) . ?
C110 H59 0.9500 . ?
C111 H60 0.9500 . ?
C112 C113 1.388(3) . ?
C112 C116 1.390(3) . ?
C112 C118 1.503(3) . ?
C113 C114 1.381(3) . ?
C113 H61 0.9500 . ?
C114 C115 1.378(3) . ?
C114 H62 0.9500 . ?
C115 C117 1.382(3) . ?
C115 H63 0.9500 . ?
C116 C117 1.374(3) . ?
C116 H64 0.9500 . ?
C117 H65 0.9500 . ?
C118 H66 0.9800 . ?
C118 H67 0.9800 . ?
C118 H68 0.9800 . ?
C120 C121 1.3900 . ?
C120 C123 1.3900 . ?
C120 C125 1.478(7) . ?
C121 C124 1.3900 . ?
C121 H85 0.9500 . ?
C124 C122 1.3900 . ?
C124 H86 0.9500 . ?
C122 C119 1.3900 . ?
C122 H87 0.9500 . ?
C119 C123 1.3900 . ?
C119 H88 0.9500 . ?
C123 H89 0.9500 . ?
C125 H74 0.9800 . ?
C125 H75 0.9800 . ?
C125 H76 0.9800 . ?
C131 C1 1.434(9) . ?
C131 H77 0.9800 . ?
C131 H78 0.9800 . ?
C131 H79 0.9800 . ?
C1 C126 1.3900 . ?
C1 C130 1.3900 . ?
C126 C127 1.3900 . ?
C126 H80 0.9500 . ?
C127 C128 1.3900 . ?
C127 H81 0.9500 . ?
C128 C129 1.3900 . ?
C128 H82 0.9500 . ?
C129 C130 1.3900 . ?
C129 H90 0.9500 . ?
C130 H84 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C20 N9 C13 118.81(14) . . ?
C21 N1 C22 118.79(14) . . ?
C34 N5 C29 110.30(14) . . ?
C34 N5 H1 124.8 . . ?
C29 N5 H1 124.8 . . ?
C67 N6 C36 109.83(14) . . ?
C67 N6 H2 125.1 . . ?
C36 N6 H2 125.1 . . ?
C32 N7 C49 117.96(15) . . ?
C37 N3 C15 109.91(13) . . ?
C37 N3 H3 125.0 . . ?
C15 N3 H3 125.0 . . ?
C30 N8 C64 118.54(15) . . ?
C106 N11 C23 110.27(13) . . ?
C106 N11 H4 124.9 . . ?
C23 N11 H4 124.9 . . ?
C14 N2 C28 118.80(14) . . ?
C59 N12 C16 110.22(14) . . ?
C59 N12 H5 124.9 . . ?
C16 N12 H5 124.9 . . ?
C24 N10 C18 118.69(14) . . ?
C45 N4 C27 109.75(14) . . ?
C45 N4 H6 125.1 . . ?
C27 N4 H6 125.1 . . ?
N9 C13 C51 120.02(15) . . ?
N9 C13 C18 120.25(15) . . ?
C51 C13 C18 119.62(15) . . ?
N2 C14 C21 120.34(15) . . ?
N2 C14 C15 115.57(14) . . ?
C21 C14 C15 124.03(14) . . ?
N3 C15 C35 106.97(15) . . ?
N3 C15 C14 119.96(14) . . ?
C35 C15 C14 131.71(15) . . ?
N12 C16 C75 107.19(14) . . ?
N12 C16 C20 119.36(14) . . ?
C75 C16 C20 133.06(16) . . ?
C61 C17 C26 120.97(16) . . ?
C61 C17 H7 119.5 . . ?
C26 C17 H7 119.5 . . ?
N10 C18 C47 120.22(15) . . ?
N10 C18 C13 120.54(15) . . ?
C47 C18 C13 119.19(15) . . ?
C27 C19 C63 107.88(15) . . ?
C27 C19 H8 126.1 . . ?
C63 C19 H8 126.1 . . ?
N9 C20 C24 120.68(14) . . ?
N9 C20 C16 115.88(14) . . ?
C24 C20 C16 123.44(14) . . ?
N1 C21 C14 120.62(14) . . ?
N1 C21 C27 116.05(14) . . ?
C14 C21 C27 123.12(15) . . ?
N1 C22 C111 120.17(15) . . ?
N1 C22 C28 120.41(16) . . ?
C111 C22 C28 119.35(15) . . ?
N11 C23 C107 106.66(14) . . ?
N11 C23 C24 119.51(14) . . ?
C107 C23 C24 132.78(15) . . ?
N10 C24 C20 120.35(14) . . ?
N10 C24 C23 115.70(14) . . ?
C20 C24 C23 123.79(14) . . ?
C17 C26 C46 118.51(15) . . ?
C17 C26 C106 120.33(15) . . ?
C46 C26 C106 120.83(15) . . ?
C19 C27 N4 106.99(14) . . ?
C19 C27 C21 131.29(15) . . ?
N4 C27 C21 120.61(15) . . ?
N2 C28 C108 120.06(15) . . ?
N2 C28 C22 120.34(15) . . ?
C108 C28 C22 119.53(16) . . ?
N5 C29 C60 107.06(15) . . ?
N5 C29 C30 119.74(14) . . ?
C60 C29 C30 132.62(16) . . ?
N8 C30 C32 120.79(15) . . ?
N8 C30 C29 116.09(15) . . ?
C32 C30 C29 123.07(14) . . ?
N7 C32 C30 121.23(15) . . ?
N7 C32 C36 116.67(15) . . ?
C30 C32 C36 122.09(15) . . ?
N5 C34 C50 106.79(15) . . ?
N5 C34 C65 122.24(15) . . ?
C50 C34 C65 130.91(15) . . ?
C15 C35 C70 107.77(15) . . ?
C15 C35 H9 126.1 . . ?
C70 C35 H9 126.1 . . ?
N6 C36 C72 107.39(15) . . ?
N6 C36 C32 120.28(15) . . ?
C72 C36 C32 132.29(16) . . ?
N3 C37 C70 107.24(15) . . ?
N3 C37 C56 122.60(14) . . ?
C70 C37 C56 130.15(15) . . ?
C73 C39 C65 120.75(17) . . ?
C73 C39 H10 119.6 . . ?
C65 C39 H10 119.6 . . ?
C48 C40 C53 118.18(16) . . ?
C48 C40 C45 123.23(15) . . ?
C53 C40 C45 118.58(16) . . ?
C59 C41 C75 107.94(15) . . ?
C59 C41 H11 126.0 . . ?
C75 C41 H11 126.0 . . ?
C51 C42 C55 120.57(16) . . ?
C51 C42 H12 119.7 . . ?
C55 C42 H12 119.7 . . ?
C83 C44 C52 120.45(17) . . ?
C83 C44 H13 119.8 . . ?
C52 C44 H13 119.8 . . ?
N4 C45 C63 107.18(14) . . ?
N4 C45 C40 124.32(15) . . ?
C63 C45 C40 128.48(15) . . ?
C58 C46 C26 120.08(16) . . ?
C58 C46 H14 120.0 . . ?
C26 C46 H14 120.0 . . ?
C55 C47 C18 120.00(16) . . ?
C55 C47 H15 120.0 . . ?
C18 C47 H15 120.0 . . ?
C40 C48 C88 120.42(17) . . ?
C40 C48 H16 119.8 . . ?
C88 C48 H16 119.8 . . ?
N7 C49 C87 119.65(17) . . ?
N7 C49 C64 121.09(15) . . ?
C87 C49 C64 119.25(16) . . ?
C34 C50 C60 108.34(15) . . ?
C34 C50 H17 125.8 . . ?
C60 C50 H17 125.8 . . ?
C42 C51 C13 119.83(16) . . ?
C42 C51 H18 120.1 . . ?
C13 C51 H18 120.1 . . ?
C76 C52 C44 118.58(16) . . ?
C76 C52 C67 119.85(16) . . ?
C44 C52 C67 121.57(15) . . ?
C98 C53 C40 121.16(18) . . ?
C98 C53 H19 119.4 . . ?
C40 C53 H19 119.4 . . ?
C47 C55 C42 120.75(16) . . ?
C47 C55 H20 119.6 . . ?
C42 C55 H20 119.6 . . ?
C86 C56 C89 117.56(17) . . ?
C86 C56 C37 121.05(16) . . ?
C89 C56 C37 121.34(16) . . ?
C80 C57 C76 120.37(17) . . ?
C80 C57 H21 119.8 . . ?
C76 C57 H21 119.8 . . ?
C68 C58 C46 120.77(16) . . ?
C68 C58 H22 119.6 . . ?
C46 C58 H22 119.6 . . ?
N12 C59 C41 107.10(15) . . ?
N12 C59 C85 122.08(16) . . ?
C41 C59 C85 130.81(16) . . ?
C29 C60 C50 107.48(16) . . ?
C29 C60 H23 126.3 . . ?
C50 C60 H23 126.3 . . ?
C17 C61 C68 120.17(16) . . ?
C17 C61 H24 119.9 . . ?
C68 C61 H24 119.9 . . ?
C67 C62 C72 108.05(15) . . ?
C67 C62 H25 126.0 . . ?
C72 C62 H25 126.0 . . ?
C45 C63 C19 108.19(15) . . ?
C45 C63 H26 125.9 . . ?
C19 C63 H26 125.9 . . ?
N8 C64 C78 120.18(16) . . ?
N8 C64 C49 120.35(15) . . ?
C78 C64 C49 119.44(16) . . ?
C71 C65 C39 118.31(16) . . ?
C71 C65 C34 121.69(15) . . ?
C39 C65 C34 119.98(16) . . ?
N6 C67 C62 107.02(15) . . ?
N6 C67 C52 122.18(15) . . ?
C62 C67 C52 130.73(16) . . ?
C61 C68 C58 119.49(16) . . ?
C61 C68 H27 120.3 . . ?
C58 C68 H27 120.3 . . ?
C37 C70 C35 108.11(15) . . ?
C37 C70 H28 125.9 . . ?
C35 C70 H28 125.9 . . ?
C74 C71 C65 120.58(17) . . ?
C74 C71 H29 119.7 . . ?
C65 C71 H29 119.7 . . ?
C36 C72 C62 107.65(16) . . ?
C36 C72 H30 126.2 . . ?
C62 C72 H30 126.2 . . ?
C81 C73 C39 120.16(18) . . ?
C81 C73 H31 119.9 . . ?
C39 C73 H31 119.9 . . ?
C81 C74 C71 120.35(18) . . ?
C81 C74 H32 119.8 . . ?
C71 C74 H32 119.8 . . ?
C16 C75 C41 107.54(16) . . ?
C16 C75 H33 126.2 . . ?
C41 C75 H33 126.2 . . ?
C57 C76 C52 120.60(18) . . ?
C57 C76 H34 119.7 . . ?
C52 C76 H34 119.7 . . ?
C79 C78 C64 120.05(18) . . ?
C79 C78 H35 120.0 . . ?
C64 C78 H35 120.0 . . ?
C78 C79 C90 120.35(18) . . ?
C78 C79 H36 119.8 . . ?
C90 C79 H36 119.8 . . ?
C57 C80 C83 119.45(17) . . ?
C57 C80 H37 120.3 . . ?
C83 C80 H37 120.3 . . ?
C73 C81 C74 119.85(18) . . ?
C73 C81 H38 120.1 . . ?
C74 C81 H38 120.1 . . ?
C98 C82 C88 119.51(17) . . ?
C98 C82 H39 120.2 . . ?
C88 C82 H39 120.2 . . ?
C44 C83 C80 120.53(18) . . ?
C44 C83 H40 119.7 . . ?
C80 C83 H40 119.7 . . ?
C99 C85 C97 117.81(17) . . ?
C99 C85 C59 121.19(17) . . ?
C97 C85 C59 120.93(16) . . ?
C91 C86 C56 121.02(19) . . ?
C91 C86 H41 119.5 . . ?
C56 C86 H41 119.5 . . ?
C90 C87 C49 120.20(19) . . ?
C90 C87 H42 119.9 . . ?
C49 C87 H42 119.9 . . ?
C82 C88 C48 120.57(19) . . ?
C82 C88 H43 119.7 . . ?
C48 C88 H43 119.7 . . ?
C101 C89 C56 120.9(2) . . ?
C101 C89 H44 119.5 . . ?
C56 C89 H44 119.5 . . ?
C87 C90 C79 120.68(18) . . ?
C87 C90 H45 119.7 . . ?
C79 C90 H45 119.7 . . ?
C92 C91 C86 120.99(19) . . ?
C92 C91 H46 119.5 . . ?
C86 C91 H46 119.5 . . ?
C91 C92 C101 119.1(2) . . ?
C91 C92 H47 120.5 . . ?
C101 C92 H47 120.5 . . ?
C104 C96 C102 119.4(2) . . ?
C104 C96 H48 120.3 . . ?
C102 C96 H48 120.3 . . ?
C102 C97 C85 121.1(2) . . ?
C102 C97 H49 119.5 . . ?
C85 C97 H49 119.5 . . ?
C82 C98 C53 120.14(17) . . ?
C82 C98 H50 119.9 . . ?
C53 C98 H50 119.9 . . ?
C85 C99 C104 121.1(2) . . ?
C85 C99 H51 119.5 . . ?
C104 C99 H51 119.5 . . ?
C89 C101 C92 120.4(2) . . ?
C89 C101 H52 119.8 . . ?
C92 C101 H52 119.8 . . ?
C97 C102 C96 119.8(2) . . ?
C97 C102 H53 120.1 . . ?
C96 C102 H53 120.1 . . ?
C96 C104 C99 120.7(2) . . ?
C96 C104 H54 119.6 . . ?
C99 C104 H54 119.6 . . ?
C106 C105 C107 108.04(14) . . ?
C106 C105 H55 126.0 . . ?
C107 C105 H55 126.0 . . ?
N11 C106 C105 107.25(14) . . ?
N11 C106 C26 122.06(14) . . ?
C105 C106 C26 130.34(15) . . ?
C23 C107 C105 107.78(14) . . ?
C23 C107 H56 126.1 . . ?
C105 C107 H56 126.1 . . ?
C109 C108 C28 120.05(17) . . ?
C109 C108 H57 120.0 . . ?
C28 C108 H57 120.0 . . ?
C108 C109 C110 120.38(16) . . ?
C108 C109 H58 119.8 . . ?
C110 C109 H58 119.8 . . ?
C111 C110 C109 120.85(18) . . ?
C111 C110 H59 119.6 . . ?
C109 C110 H59 119.6 . . ?
C110 C111 C22 119.82(17) . . ?
C110 C111 H60 120.1 . . ?
C22 C111 H60 120.1 . . ?
C113 C112 C116 117.77(19) . . ?
C113 C112 C118 120.49(19) . . ?
C116 C112 C118 121.74(19) . . ?
C114 C113 C112 121.21(18) . . ?
C114 C113 H61 119.4 . . ?
C112 C113 H61 119.4 . . ?
C115 C114 C113 120.16(19) . . ?
C115 C114 H62 119.9 . . ?
C113 C114 H62 119.9 . . ?
C114 C115 C117 119.3(2) . . ?
C114 C115 H63 120.4 . . ?
C117 C115 H63 120.4 . . ?
C117 C116 C112 121.17(19) . . ?
C117 C116 H64 119.4 . . ?
C112 C116 H64 119.4 . . ?
C116 C117 C115 120.41(19) . . ?
C116 C117 H65 119.8 . . ?
C115 C117 H65 119.8 . . ?
C112 C118 H66 109.5 . . ?
C112 C118 H67 109.5 . . ?
H66 C118 H67 109.5 . . ?
C112 C118 H68 109.5 . . ?
H66 C118 H68 109.5 . . ?
H67 C118 H68 109.5 . . ?
C121 C120 C123 120.0 . . ?
C121 C120 C125 115.3(4) . . ?
C123 C120 C125 124.7(4) . . ?
C120 C121 C124 120.0 . . ?
C120 C121 H85 120.0 . . ?
C124 C121 H85 120.0 . . ?
C122 C124 C121 120.0 . . ?
C122 C124 H86 120.0 . . ?
C121 C124 H86 120.0 . . ?
C124 C122 C119 120.0 . . ?
C124 C122 H87 120.0 . . ?
C119 C122 H87 120.0 . . ?
C123 C119 C122 120.0 . . ?
C123 C119 H88 120.0 . . ?
C122 C119 H88 120.0 . . ?
C119 C123 C120 120.0 . . ?
C119 C123 H89 120.0 . . ?
C120 C123 H89 120.0 . . ?
C120 C125 H74 109.5 . . ?
C120 C125 H75 109.5 . . ?
H74 C125 H75 109.5 . . ?
C120 C125 H76 109.5 . . ?
H74 C125 H76 109.5 . . ?
H75 C125 H76 109.5 . . ?
C1 C131 H77 109.5 . . ?
C1 C131 H78 109.5 . . ?
H77 C131 H78 109.5 . . ?
C1 C131 H79 109.5 . . ?
H77 C131 H79 109.5 . . ?
H78 C131 H79 109.5 . . ?
C126 C1 C130 120.0 . . ?
C126 C1 C131 136.6(8) . . ?
C130 C1 C131 103.4(8) . . ?
C1 C126 C127 120.0 . . ?
C1 C126 H80 120.0 . . ?
C127 C126 H80 120.0 . . ?
C126 C127 C128 120.0 . . ?
C126 C127 H81 120.0 . . ?
C128 C127 H81 120.0 . . ?
C129 C128 C127 120.0 . . ?
C129 C128 H82 120.0 . . ?
C127 C128 H82 120.0 . . ?
C128 C129 C130 120.0 . . ?
C128 C129 H90 120.0 . . ?
C130 C129 H90 120.0 . . ?
C129 C130 C1 120.0 . . ?
C129 C130 H84 120.0 . . ?
C1 C130 H84 120.0 . . ?

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
C20 N9 C13 C51 -179.32(16) . . . . ?
C20 N9 C13 C18 -3.1(2) . . . . ?
C28 N2 C14 C21 -4.9(2) . . . . ?
C28 N2 C14 C15 172.46(14) . . . . ?
C37 N3 C15 C35 -0.19(18) . . . . ?
C37 N3 C15 C14 -168.39(14) . . . . ?
N2 C14 C15 N3 24.8(2) . . . . ?
C21 C14 C15 N3 -157.96(15) . . . . ?
N2 C14 C15 C35 -139.99(18) . . . . ?
C21 C14 C15 C35 37.2(3) . . . . ?
C59 N12 C16 C75 -1.35(19) . . . . ?
C59 N12 C16 C20 -175.11(14) . . . . ?
C24 N10 C18 C47 178.15(16) . . . . ?
C24 N10 C18 C13 -4.1(2) . . . . ?
N9 C13 C18 N10 7.7(2) . . . . ?
C51 C13 C18 N10 -176.05(15) . . . . ?
N9 C13 C18 C47 -174.58(15) . . . . ?
C51 C13 C18 C47 1.7(2) . . . . ?
C13 N9 C20 C24 -4.5(2) . . . . ?
C13 N9 C20 C16 175.04(14) . . . . ?
N12 C16 C20 N9 29.8(2) . . . . ?
C75 C16 C20 N9 -142.00(19) . . . . ?
N12 C16 C20 C24 -150.63(16) . . . . ?
C75 C16 C20 C24 37.5(3) . . . . ?
C22 N1 C21 C14 -2.8(2) . . . . ?
C22 N1 C21 C27 172.11(14) . . . . ?
N2 C14 C21 N1 7.9(2) . . . . ?
C15 C14 C21 N1 -169.19(15) . . . . ?
N2 C14 C21 C27 -166.63(14) . . . . ?
C15 C14 C21 C27 16.3(2) . . . . ?
C21 N1 C22 C111 178.21(16) . . . . ?
C21 N1 C22 C28 -4.7(2) . . . . ?
C106 N11 C23 C107 -0.60(19) . . . . ?
C106 N11 C23 C24 -170.38(14) . . . . ?
C18 N10 C24 C20 -3.4(2) . . . . ?
C18 N10 C24 C23 172.28(14) . . . . ?
N9 C20 C24 N10 8.1(2) . . . . ?
C16 C20 C24 N10 -171.44(15) . . . . ?
N9 C20 C24 C23 -167.29(15) . . . . ?
C16 C20 C24 C23 13.2(3) . . . . ?
N11 C23 C24 N10 16.5(2) . . . . ?
C107 C23 C24 N10 -150.14(18) . . . . ?
N11 C23 C24 C20 -167.96(15) . . . . ?
C107 C23 C24 C20 25.4(3) . . . . ?
C61 C17 C26 C46 1.3(3) . . . . ?
C61 C17 C26 C106 -172.14(16) . . . . ?
C63 C19 C27 N4 0.03(18) . . . . ?
C63 C19 C27 C21 167.70(16) . . . . ?
C45 N4 C27 C19 0.00(17) . . . . ?
C45 N4 C27 C21 -169.25(14) . . . . ?
N1 C21 C27 C19 -151.22(17) . . . . ?
C14 C21 C27 C19 23.5(3) . . . . ?
N1 C21 C27 N4 15.0(2) . . . . ?
C14 C21 C27 N4 -170.19(14) . . . . ?
C14 N2 C28 C108 -179.59(15) . . . . ?
C14 N2 C28 C22 -2.6(2) . . . . ?
N1 C22 C28 N2 7.8(2) . . . . ?
C111 C22 C28 N2 -175.17(16) . . . . ?
N1 C22 C28 C108 -175.28(15) . . . . ?
C111 C22 C28 C108 1.8(2) . . . . ?
C34 N5 C29 C60 -1.43(18) . . . . ?
C34 N5 C29 C30 -173.73(14) . . . . ?
C64 N8 C30 C32 -0.8(2) . . . . ?
C64 N8 C30 C29 176.62(14) . . . . ?
N5 C29 C30 N8 28.7(2) . . . . ?
C60 C29 C30 N8 -141.23(19) . . . . ?
N5 C29 C30 C32 -153.89(15) . . . . ?
C60 C29 C30 C32 36.1(3) . . . . ?
C49 N7 C32 C30 -1.8(2) . . . . ?
C49 N7 C32 C36 179.23(14) . . . . ?
N8 C30 C32 N7 2.3(2) . . . . ?
C29 C30 C32 N7 -174.97(15) . . . . ?
N8 C30 C32 C36 -178.75(15) . . . . ?
C29 C30 C32 C36 4.0(2) . . . . ?
C29 N5 C34 C50 1.73(18) . . . . ?
C29 N5 C34 C65 -175.53(15) . . . . ?
N3 C15 C35 C70 -0.05(18) . . . . ?
C14 C15 C35 C70 166.22(16) . . . . ?
C67 N6 C36 C72 -2.18(19) . . . . ?
C67 N6 C36 C32 179.93(15) . . . . ?
N7 C32 C36 N6 41.2(2) . . . . ?
C30 C32 C36 N6 -137.85(16) . . . . ?
N7 C32 C36 C72 -136.1(2) . . . . ?
C30 C32 C36 C72 44.9(3) . . . . ?
C15 N3 C37 C70 0.36(18) . . . . ?
C15 N3 C37 C56 178.90(14) . . . . ?
C27 N4 C45 C63 -0.03(17) . . . . ?
C27 N4 C45 C40 178.58(14) . . . . ?
C48 C40 C45 N4 -12.6(3) . . . . ?
C53 C40 C45 N4 167.93(15) . . . . ?
C48 C40 C45 C63 165.71(17) . . . . ?
C53 C40 C45 C63 -13.8(3) . . . . ?
C17 C26 C46 C58 -0.6(3) . . . . ?
C106 C26 C46 C58 172.84(16) . . . . ?
N10 C18 C47 C55 177.29(16) . . . . ?
C13 C18 C47 C55 -0.5(3) . . . . ?
C53 C40 C48 C88 -0.7(3) . . . . ?
C45 C40 C48 C88 179.85(17) . . . . ?
C32 N7 C49 C87 -179.19(16) . . . . ?
C32 N7 C49 C64 0.0(2) . . . . ?
N5 C34 C50 C60 -1.34(19) . . . . ?
C65 C34 C50 C60 175.58(17) . . . . ?
C55 C42 C51 C13 0.1(3) . . . . ?
N9 C13 C51 C42 174.77(16) . . . . ?
C18 C13 C51 C42 -1.5(3) . . . . ?
C83 C44 C52 C76 -1.3(2) . . . . ?
C83 C44 C52 C67 178.47(16) . . . . ?
C48 C40 C53 C98 0.0(3) . . . . ?
C45 C40 C53 C98 179.48(16) . . . . ?
C18 C47 C55 C42 -1.0(3) . . . . ?
C51 C42 C55 C47 1.2(3) . . . . ?
N3 C37 C56 C86 162.94(17) . . . . ?
C70 C37 C56 C86 -18.9(3) . . . . ?
N3 C37 C56 C89 -19.5(3) . . . . ?
C70 C37 C56 C89 158.62(19) . . . . ?
C26 C46 C58 C68 -0.5(3) . . . . ?
C16 N12 C59 C41 1.40(19) . . . . ?
C16 N12 C59 C85 -179.65(15) . . . . ?
C75 C41 C59 N12 -0.89(19) . . . . ?
C75 C41 C59 C85 -179.71(18) . . . . ?
N5 C29 C60 C50 0.56(19) . . . . ?
C30 C29 C60 C50 171.47(17) . . . . ?
C34 C50 C60 C29 0.5(2) . . . . ?
C26 C17 C61 C68 -0.9(3) . . . . ?
N4 C45 C63 C19 0.05(18) . . . . ?
C40 C45 C63 C19 -178.48(15) . . . . ?
C27 C19 C63 C45 -0.05(19) . . . . ?
C30 N8 C64 C78 -178.89(16) . . . . ?
C30 N8 C64 C49 -1.0(2) . . . . ?
N7 C49 C64 N8 1.5(2) . . . . ?
C87 C49 C64 N8 -179.38(16) . . . . ?
N7 C49 C64 C78 179.41(16) . . . . ?
C87 C49 C64 C78 -1.4(3) . . . . ?
C73 C39 C65 C71 0.4(3) . . . . ?
C73 C39 C65 C34 -177.90(16) . . . . ?
N5 C34 C65 C71 -19.2(2) . . . . ?
C50 C34 C65 C71 164.26(18) . . . . ?
N5 C34 C65 C39 158.98(15) . . . . ?
C50 C34 C65 C39 -17.5(3) . . . . ?
C36 N6 C67 C62 2.23(19) . . . . ?
C36 N6 C67 C52 -175.24(15) . . . . ?
C72 C62 C67 N6 -1.4(2) . . . . ?
C72 C62 C67 C52 175.76(17) . . . . ?
C76 C52 C67 N6 149.38(16) . . . . ?
C44 C52 C67 N6 -30.4(2) . . . . ?
C76 C52 C67 C62 -27.4(3) . . . . ?
C44 C52 C67 C62 152.75(19) . . . . ?
C17 C61 C68 C58 -0.2(3) . . . . ?
C46 C58 C68 C61 0.9(3) . . . . ?
N3 C37 C70 C35 -0.38(18) . . . . ?
C56 C37 C70 C35 -178.77(16) . . . . ?
C15 C35 C70 C37 0.27(19) . . . . ?
C39 C65 C71 C74 -0.8(3) . . . . ?
C34 C65 C71 C74 177.43(16) . . . . ?
N6 C36 C72 C62 1.3(2) . . . . ?
C32 C36 C72 C62 178.78(18) . . . . ?
C67 C62 C72 C36 0.1(2) . . . . ?
C65 C39 C73 C81 0.1(3) . . . . ?
C65 C71 C74 C81 0.8(3) . . . . ?
N12 C16 C75 C41 0.76(19) . . . . ?
C20 C16 C75 C41 173.31(17) . . . . ?
C59 C41 C75 C16 0.1(2) . . . . ?
C80 C57 C76 C52 0.1(3) . . . . ?
C44 C52 C76 C57 0.8(3) . . . . ?
C67 C52 C76 C57 -179.05(16) . . . . ?
N8 C64 C78 C79 178.19(17) . . . . ?
C49 C64 C78 C79 0.2(3) . . . . ?
C64 C78 C79 C90 1.1(3) . . . . ?
C76 C57 C80 C83 -0.4(3) . . . . ?
C39 C73 C81 C74 -0.1(3) . . . . ?
C71 C74 C81 C73 -0.3(3) . . . . ?
C52 C44 C83 C80 1.1(3) . . . . ?
C57 C80 C83 C44 -0.2(3) . . . . ?
N12 C59 C85 C99 167.47(19) . . . . ?
C41 C59 C85 C99 -13.9(3) . . . . ?
N12 C59 C85 C97 -15.9(3) . . . . ?
C41 C59 C85 C97 162.8(2) . . . . ?
C89 C56 C86 C91 1.5(3) . . . . ?
C37 C56 C86 C91 179.11(18) . . . . ?
N7 C49 C87 C90 -179.53(18) . . . . ?
C64 C49 C87 C90 1.3(3) . . . . ?
C98 C82 C88 C48 -0.2(3) . . . . ?
C40 C48 C88 C82 0.8(3) . . . . ?
C86 C56 C89 C101 -1.8(3) . . . . ?
C37 C56 C89 C101 -179.4(2) . . . . ?
C49 C87 C90 C79 0.0(3) . . . . ?
C78 C79 C90 C87 -1.2(3) . . . . ?
C56 C86 C91 C92 0.1(3) . . . . ?
C86 C91 C92 C101 -1.5(3) . . . . ?
C99 C85 C97 C102 -2.2(3) . . . . ?
C59 C85 C97 C102 -179.0(2) . . . . ?
C88 C82 C98 C53 -0.5(3) . . . . ?
C40 C53 C98 C82 0.6(3) . . . . ?
C97 C85 C99 C104 1.9(4) . . . . ?
C59 C85 C99 C104 178.7(2) . . . . ?
C56 C89 C101 C92 0.5(4) . . . . ?
C91 C92 C101 C89 1.2(4) . . . . ?
C85 C97 C102 C96 0.1(4) . . . . ?
C104 C96 C102 C97 2.5(4) . . . . ?
C102 C96 C104 C99 -2.8(4) . . . . ?
C85 C99 C104 C96 0.6(4) . . . . ?
C23 N11 C106 C105 0.29(19) . . . . ?
C23 N11 C106 C26 174.16(15) . . . . ?
C107 C105 C106 N11 0.13(19) . . . . ?
C107 C105 C106 C26 -173.05(17) . . . . ?
C17 C26 C106 N11 -28.9(2) . . . . ?
C46 C26 C106 N11 157.81(16) . . . . ?
C17 C26 C106 C105 143.40(19) . . . . ?
C46 C26 C106 C105 -29.9(3) . . . . ?
N11 C23 C107 C105 0.66(19) . . . . ?
C24 C23 C107 C105 168.53(17) . . . . ?
C106 C105 C107 C23 -0.5(2) . . . . ?
N2 C28 C108 C109 175.68(16) . . . . ?
C22 C28 C108 C109 -1.3(3) . . . . ?
C28 C108 C109 C110 0.0(3) . . . . ?
C108 C109 C110 C111 0.8(3) . . . . ?
C109 C110 C111 C22 -0.3(3) . . . . ?
N1 C22 C111 C110 176.07(17) . . . . ?
C28 C22 C111 C110 -1.0(3) . . . . ?
C116 C112 C113 C114 0.0(3) . . . . ?
C118 C112 C113 C114 -179.59(18) . . . . ?
C112 C113 C114 C115 1.0(3) . . . . ?
C113 C114 C115 C117 -1.2(3) . . . . ?
C113 C112 C116 C117 -0.8(3) . . . . ?
C118 C112 C116 C117 178.80(19) . . . . ?
C112 C116 C117 C115 0.6(3) . . . . ?
C114 C115 C117 C116 0.4(3) . . . . ?
C123 C120 C121 C124 0.0 . . . . ?
C125 C120 C121 C124 177.9(5) . . . . ?
C120 C121 C124 C122 0.0 . . . . ?
C121 C124 C122 C119 0.0 . . . . ?
C124 C122 C119 C123 0.0 . . . . ?
C122 C119 C123 C120 0.0 . . . . ?
C121 C120 C123 C119 0.0 . . . . ?
C125 C120 C123 C119 -177.7(6) . . . . ?
C130 C1 C126 C127 0.0 . . . . ?
C131 C1 C126 C127 -179.1(9) . . . . ?
C1 C126 C127 C128 0.0 . . . . ?
C126 C127 C128 C129 0.0 . . . . ?
C127 C128 C129 C130 0.0 . . . . ?
C128 C129 C130 C1 0.0 . . . . ?
C126 C1 C130 C129 0.0 . . . . ?
C131 C1 C130 C129 179.3(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H1 N9 0.88 2.18 3.0502(19) 171.8 1_645
N6 H2 N1 0.88 2.17 3.045(2) 175.4 .
N3 H3 N10 0.88 2.16 3.0379(19) 172.3 .
N11 H4 N2 0.88 2.15 3.001(2) 163.0 .
N11 H4 N3 0.88 2.65 3.2657(19) 127.5 .
N12 H5 N8 0.88 2.13 2.984(2) 163.7 1_465
N12 H5 N5 0.88 2.67 3.2526(19) 124.7 1_465
N4 H6 N7 0.88 2.31 3.190(2) 177.5 .

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        68.37
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.043
####################################################################### 
# 
# 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_ydkr_a
_database_code_depnum_ccdc_archive 'CCDC 1871612'
_audit_update_record             
;
2018-10-05 deposited with the CCDC.
2018-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44.46 H55.93 Cl0.93 N5'
_chemical_formula_sum            'C44.46 H55.93 Cl0.93 N5'
_chemical_formula_weight         693.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0016 '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 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1459 0.1553 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   22.064(3)
_cell_length_b                   8.4746(9)
_cell_length_c                   21.388(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3999.2(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30130
_cell_measurement_theta_min      1.820
_cell_measurement_theta_max      27.065

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_F_000             1494
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.121
_shelx_estimated_absorpt_T_min   0.995
_shelx_estimated_absorpt_T_max   0.999
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7007
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL02B1'
_diffrn_radiation_monochromator  'Si 311'
_diffrn_measurement_device_type  'Rigaku MercuryCCD2'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30130
_diffrn_reflns_av_unetI/netI     0.2189
_diffrn_reflns_av_R_equivalents  0.1661
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.820
_diffrn_reflns_theta_max         27.065
_diffrn_reflns_theta_full        24.861
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_point_group_measured_fraction_full 0.962
_reflns_number_total             8664
_reflns_number_gt                3329
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_max     0.918
_reflns_Friedel_fraction_full    0.939

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

_computing_data_collection       RAPID-AUTO
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        RAPID-AUTO
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0426P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1011 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.24(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8664
_refine_ls_number_parameters     474
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1890
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1431
_refine_ls_wR_factor_gt          0.1140
_refine_ls_goodness_of_fit_ref   0.812
_refine_ls_restrained_S_all      0.812
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7305(2) 0.5873(7) 0.6375(3) 0.0454(17) Uani 1 1 d . . . . .
H1 H 0.7341 0.5611 0.5945 0.055 Uiso 1 1 calc R U . . .
C2 C 0.7786(3) 0.5561(8) 0.6778(3) 0.054(2) Uani 1 1 d . . . . .
H2 H 0.8151 0.5112 0.6624 0.065 Uiso 1 1 calc R U . . .
C3 C 0.7724(3) 0.5919(8) 0.7412(3) 0.056(2) Uani 1 1 d . . . . .
H3 H 0.8050 0.5708 0.7690 0.067 Uiso 1 1 calc R U . . .
C4 C 0.7209(3) 0.6558(8) 0.7635(3) 0.0497(18) Uani 1 1 d . . . . .
H4 H 0.7172 0.6789 0.8068 0.060 Uiso 1 1 calc R U . . .
C5 C 0.6736(3) 0.6874(7) 0.7237(3) 0.0438(16) Uani 1 1 d . . . . .
H5 H 0.6374 0.7317 0.7401 0.053 Uiso 1 1 calc R U . . .
C6 C 0.6776(2) 0.6557(7) 0.6590(3) 0.0391(16) Uani 1 1 d . . . . .
C7 C 0.6265(2) 0.6900(7) 0.6182(3) 0.0383(15) Uani 1 1 d . . . . .
C8 C 0.5665(2) 0.7183(7) 0.6345(3) 0.0389(15) Uani 1 1 d . . . . .
H6 H 0.5505 0.7244 0.6756 0.047 Uiso 1 1 calc R U . . .
C9 C 0.5345(2) 0.7362(7) 0.5789(3) 0.0386(15) Uani 1 1 d . . . . .
H7 H 0.4923 0.7559 0.5745 0.046 Uiso 1 1 calc R U . . .
C10 C 0.5765(2) 0.7192(6) 0.5314(3) 0.0330(14) Uani 1 1 d . . . . .
C11 C 0.5613(2) 0.7093(6) 0.4647(3) 0.0366(15) Uani 1 1 d . . . . .
C12 C 0.6009(2) 0.7328(7) 0.4124(3) 0.0369(15) Uani 1 1 d . . . . .
C13 C 0.6606(2) 0.8048(6) 0.4131(3) 0.0382(15) Uani 1 1 d . . . . .
C14 C 0.6927(3) 0.8643(7) 0.3631(3) 0.0447(17) Uani 1 1 d . . . . .
H8 H 0.6804 0.8628 0.3206 0.054 Uiso 1 1 calc R U . . .
C15 C 0.7468(3) 0.9273(7) 0.3862(3) 0.0502(18) Uani 1 1 d . . . . .
H9 H 0.7772 0.9779 0.3621 0.060 Uiso 1 1 calc R U . . .
C16 C 0.7485(2) 0.9036(7) 0.4501(3) 0.0383(15) Uani 1 1 d . . . . .
C17 C 0.7919(2) 0.9548(7) 0.4957(3) 0.0395(16) Uani 1 1 d . . . . .
C18 C 0.8407(3) 1.0444(8) 0.4790(3) 0.0521(18) Uani 1 1 d . . . . .
H10 H 0.8465 1.0695 0.4362 0.063 Uiso 1 1 calc R U . . .
C19 C 0.8813(3) 1.0992(8) 0.5220(4) 0.062(2) Uani 1 1 d . . . . .
H11 H 0.9147 1.1616 0.5088 0.074 Uiso 1 1 calc R U . . .
C20 C 0.8742(3) 1.0641(7) 0.5850(4) 0.061(2) Uani 1 1 d . . . . .
H12 H 0.9017 1.1033 0.6154 0.074 Uiso 1 1 calc R U . . .
C21 C 0.8259(3) 0.9709(8) 0.6020(3) 0.057(2) Uani 1 1 d . . . . .
H13 H 0.8211 0.9415 0.6446 0.069 Uiso 1 1 calc R U . . .
C22 C 0.7848(3) 0.9199(7) 0.5588(3) 0.0529(19) Uani 1 1 d . . . . .
H14 H 0.7509 0.8597 0.5721 0.063 Uiso 1 1 calc R U . . .
C23 C 0.4839(2) 0.6507(7) 0.3946(3) 0.0430(16) Uani 1 1 d . . . . .
C24 C 0.4224(3) 0.6185(7) 0.3836(3) 0.0480(17) Uani 1 1 d . . . . .
H15 H 0.3946 0.6151 0.4175 0.058 Uiso 1 1 calc R U . . .
C25 C 0.4026(3) 0.5922(8) 0.3244(4) 0.061(2) Uani 1 1 d . . . . .
H16 H 0.3610 0.5705 0.3168 0.074 Uiso 1 1 calc R U . . .
C26 C 0.4430(3) 0.5972(8) 0.2755(4) 0.068(2) Uani 1 1 d . . . . .
H17 H 0.4285 0.5777 0.2344 0.081 Uiso 1 1 calc R U . . .
C27 C 0.5035(3) 0.6291(8) 0.2835(3) 0.064(2) Uani 1 1 d . . . . .
H18 H 0.5306 0.6319 0.2490 0.077 Uiso 1 1 calc R U . . .
C28 C 0.5240(3) 0.6578(7) 0.3455(3) 0.0474(17) Uani 1 1 d . . . . .
C29 C 0.6120(3) 1.1258(7) 0.5669(3) 0.0501(18) Uani 1 1 d . . . . .
H21 H 0.5812 1.0623 0.5892 0.060 Uiso 1 1 calc R U . . .
H22 H 0.6386 1.0513 0.5440 0.060 Uiso 1 1 calc R U . . .
C30 C 0.6502(3) 1.2108(7) 0.6153(3) 0.0498(18) Uani 1 1 d . . . . .
H23 H 0.6274 1.3019 0.6322 0.060 Uiso 1 1 calc R U . . .
H24 H 0.6878 1.2509 0.5957 0.060 Uiso 1 1 calc R U . . .
C31 C 0.6660(3) 1.0965(8) 0.6681(3) 0.0572(19) Uani 1 1 d . . . . .
H25 H 0.6283 1.0642 0.6897 0.069 Uiso 1 1 calc R U . . .
H26 H 0.6848 1.0007 0.6501 0.069 Uiso 1 1 calc R U . . .
C32 C 0.7087(3) 1.1689(9) 0.7149(3) 0.076(2) Uani 1 1 d . . . . .
H47 H 0.6885 1.2565 0.7363 0.114 Uiso 1 1 calc R U . . .
H48 H 0.7448 1.2084 0.6932 0.114 Uiso 1 1 calc R U . . .
H49 H 0.7208 1.0890 0.7456 0.114 Uiso 1 1 calc R U . . .
C33 C 0.6246(3) 1.3334(7) 0.4853(3) 0.0467(17) Uani 1 1 d . . . . .
H27 H 0.6446 1.4029 0.5163 0.056 Uiso 1 1 calc R U . . .
H28 H 0.6019 1.4018 0.4559 0.056 Uiso 1 1 calc R U . . .
C34 C 0.6736(3) 1.2454(8) 0.4487(3) 0.063(2) Uani 1 1 d . . . . .
H29 H 0.6543 1.1708 0.4191 0.075 Uiso 1 1 calc R U . . .
H30 H 0.6991 1.1838 0.4780 0.075 Uiso 1 1 calc R U . . .
C35 C 0.7133(3) 1.3628(8) 0.4124(3) 0.063(2) Uani 1 1 d . . . . .
H31 H 0.7372 1.3048 0.3806 0.075 Uiso 1 1 calc R U . . .
H32 H 0.6869 1.4389 0.3902 0.075 Uiso 1 1 calc R U . . .
C36 C 0.7558(3) 1.4515(8) 0.4543(4) 0.068(2) Uani 1 1 d . . . . .
H50 H 0.7800 1.3765 0.4786 0.102 Uiso 1 1 calc R U . . .
H51 H 0.7324 1.5184 0.4829 0.102 Uiso 1 1 calc R U . . .
H52 H 0.7826 1.5176 0.4289 0.102 Uiso 1 1 calc R U . . .
C37 C 0.5356(2) 1.3392(7) 0.5513(3) 0.0384(15) Uani 1 1 d . . . . .
H33 H 0.5148 1.4024 0.5189 0.046 Uiso 1 1 calc R U . . .
H34 H 0.5589 1.4131 0.5779 0.046 Uiso 1 1 calc R U . . .
C38 C 0.4877(3) 1.2591(7) 0.5917(3) 0.0525(17) Uani 1 1 d . . . . .
H35 H 0.4696 1.1697 0.5685 0.063 Uiso 1 1 calc R U . . .
H36 H 0.5068 1.2170 0.6301 0.063 Uiso 1 1 calc R U . . .
C39 C 0.4386(3) 1.3758(8) 0.6091(3) 0.0535(19) Uani 1 1 d . . . . .
H37 H 0.4578 1.4692 0.6286 0.064 Uiso 1 1 calc R U . . .
H38 H 0.4119 1.3267 0.6407 0.064 Uiso 1 1 calc R U . . .
C40 C 0.4000(3) 1.4305(9) 0.5544(3) 0.076(2) Uani 1 1 d . . . . .
H53 H 0.3832 1.3385 0.5327 0.114 Uiso 1 1 calc R U . . .
H54 H 0.4251 1.4917 0.5253 0.114 Uiso 1 1 calc R U . . .
H55 H 0.3668 1.4967 0.5699 0.114 Uiso 1 1 calc R U . . .
C41 C 0.5480(3) 1.1171(7) 0.4757(3) 0.0459(17) Uani 1 1 d . . . . .
H39 H 0.5228 1.0442 0.5008 0.055 Uiso 1 1 calc R U . . .
H40 H 0.5789 1.0530 0.4537 0.055 Uiso 1 1 calc R U . . .
C42 C 0.5078(3) 1.1961(8) 0.4269(3) 0.060(2) Uani 1 1 d . . . . .
H41 H 0.4738 1.2511 0.4477 0.072 Uiso 1 1 calc R U . . .
H42 H 0.5315 1.2749 0.4031 0.072 Uiso 1 1 calc R U . . .
C43 C 0.4839(3) 1.0715(8) 0.3835(3) 0.067(2) Uani 1 1 d . . . . .
H43 H 0.4633 0.9892 0.4086 0.081 Uiso 1 1 calc R U . . .
H44 H 0.5185 1.0211 0.3618 0.081 Uiso 1 1 calc R U . . .
C44 C 0.4397(4) 1.1346(10) 0.3348(4) 0.104(3) Uani 1 1 d . . . . .
H56 H 0.4587 1.2216 0.3118 0.156 Uiso 1 1 calc R U . . .
H57 H 0.4030 1.1727 0.3556 0.156 Uiso 1 1 calc R U . . .
H58 H 0.4291 1.0500 0.3055 0.156 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5887(3) 0.3159(9) 0.2754(4) 0.160(3) Uani 0.463(5) 1 d . . P . .
Cl2 Cl 0.5626(4) 0.0072(7) 0.2343(3) 0.174(4) Uani 0.463(5) 1 d . . P . .
C45 C 0.6180(8) 0.149(3) 0.2625(9) 0.123(9) Uani 0.463(5) 1 d . . P . .
H45 H 0.6364 0.1088 0.3017 0.148 Uiso 0.463(5) 1 calc R U P . .
H46 H 0.6507 0.1604 0.2312 0.148 Uiso 0.463(5) 1 calc R U P . .
N1 N 0.63314(18) 0.6896(5) 0.5544(2) 0.0335(12) Uani 1 1 d . . . . .
N2 N 0.69527(19) 0.8300(5) 0.4652(2) 0.0400(13) Uani 1 1 d . . . . .
H59 H 0.6848 0.8025 0.5034 0.048 Uiso 1 1 calc R U . . .
N3 N 0.50389(19) 0.6725(5) 0.4547(2) 0.0386(13) Uani 1 1 d . . . . .
N4 N 0.5829(2) 0.7005(6) 0.3551(2) 0.0486(15) Uani 1 1 d . . . . .
N5 N 0.5798(2) 1.2286(5) 0.5193(2) 0.0429(13) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.381(8) . ?
C1 C2 1.394(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.395(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.348(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.413(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.455(7) . ?
C7 N1 1.373(7) . ?
C7 C8 1.389(7) . ?
C8 C9 1.392(7) . ?
C8 H6 0.9500 . ?
C9 C10 1.383(7) . ?
C9 H7 0.9500 . ?
C10 N1 1.366(6) . ?
C10 C11 1.468(8) . ?
C11 N3 1.321(6) . ?
C11 C12 1.434(8) . ?
C12 N4 1.317(7) . ?
C12 C13 1.451(7) . ?
C13 N2 1.370(7) . ?
C13 C14 1.378(7) . ?
C14 C15 1.396(8) . ?
C14 H8 0.9500 . ?
C15 C16 1.381(8) . ?
C15 H9 0.9500 . ?
C16 N2 1.368(7) . ?
C16 C17 1.436(8) . ?
C17 C18 1.364(7) . ?
C17 C22 1.390(8) . ?
C18 C19 1.366(8) . ?
C18 H10 0.9500 . ?
C19 C20 1.388(8) . ?
C19 H11 0.9500 . ?
C20 C21 1.374(8) . ?
C20 H12 0.9500 . ?
C21 C22 1.365(8) . ?
C21 H13 0.9500 . ?
C22 H14 0.9500 . ?
C23 N3 1.373(7) . ?
C23 C28 1.374(8) . ?
C23 C24 1.404(7) . ?
C24 C25 1.358(8) . ?
C24 H15 0.9500 . ?
C25 C26 1.374(9) . ?
C25 H16 0.9500 . ?
C26 C27 1.372(8) . ?
C26 H17 0.9500 . ?
C27 C28 1.422(9) . ?
C27 H18 0.9500 . ?
C28 N4 1.363(7) . ?
C29 C30 1.516(8) . ?
C29 N5 1.516(7) . ?
C29 H21 0.9900 . ?
C29 H22 0.9900 . ?
C30 C31 1.528(8) . ?
C30 H23 0.9900 . ?
C30 H24 0.9900 . ?
C31 C32 1.507(8) . ?
C31 H25 0.9900 . ?
C31 H26 0.9900 . ?
C32 H47 0.9800 . ?
C32 H48 0.9800 . ?
C32 H49 0.9800 . ?
C33 N5 1.515(7) . ?
C33 C34 1.528(8) . ?
C33 H27 0.9900 . ?
C33 H28 0.9900 . ?
C34 C35 1.537(9) . ?
C34 H29 0.9900 . ?
C34 H30 0.9900 . ?
C35 C36 1.498(9) . ?
C35 H31 0.9900 . ?
C35 H32 0.9900 . ?
C36 H50 0.9800 . ?
C36 H51 0.9800 . ?
C36 H52 0.9800 . ?
C37 N5 1.516(7) . ?
C37 C38 1.524(7) . ?
C37 H33 0.9900 . ?
C37 H34 0.9900 . ?
C38 C39 1.513(8) . ?
C38 H35 0.9900 . ?
C38 H36 0.9900 . ?
C39 C40 1.520(8) . ?
C39 H37 0.9900 . ?
C39 H38 0.9900 . ?
C40 H53 0.9800 . ?
C40 H54 0.9800 . ?
C40 H55 0.9800 . ?
C41 N5 1.502(7) . ?
C41 C42 1.523(8) . ?
C41 H39 0.9900 . ?
C41 H40 0.9900 . ?
C42 C43 1.502(8) . ?
C42 H41 0.9900 . ?
C42 H42 0.9900 . ?
C43 C44 1.525(9) . ?
C43 H43 0.9900 . ?
C43 H44 0.9900 . ?
C44 H56 0.9800 . ?
C44 H57 0.9800 . ?
C44 H58 0.9800 . ?
Cl1 C45 1.578(19) . ?
Cl2 C45 1.82(2) . ?
C45 H45 0.9900 . ?
C45 H46 0.9900 . ?
N2 H59 0.8800 . ?

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
C6 C1 C2 121.2(6) . . ?
C6 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
C1 C2 C3 119.0(6) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 120.9(6) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 120.0(6) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 121.5(6) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C5 117.3(6) . . ?
C1 C6 C7 122.7(6) . . ?
C5 C6 C7 120.0(5) . . ?
N1 C7 C8 110.6(5) . . ?
N1 C7 C6 120.8(5) . . ?
C8 C7 C6 128.5(6) . . ?
C7 C8 C9 106.8(5) . . ?
C7 C8 H6 126.6 . . ?
C9 C8 H6 126.6 . . ?
C10 C9 C8 106.0(5) . . ?
C10 C9 H7 127.0 . . ?
C8 C9 H7 127.0 . . ?
N1 C10 C9 111.6(5) . . ?
N1 C10 C11 123.3(5) . . ?
C9 C10 C11 124.5(5) . . ?
N3 C11 C12 119.4(5) . . ?
N3 C11 C10 112.9(5) . . ?
C12 C11 C10 127.6(5) . . ?
N4 C12 C11 120.9(5) . . ?
N4 C12 C13 111.8(5) . . ?
C11 C12 C13 127.1(6) . . ?
N2 C13 C14 106.6(5) . . ?
N2 C13 C12 125.5(6) . . ?
C14 C13 C12 127.8(6) . . ?
C13 C14 C15 107.8(6) . . ?
C13 C14 H8 126.1 . . ?
C15 C14 H8 126.1 . . ?
C16 C15 C14 108.5(6) . . ?
C16 C15 H9 125.7 . . ?
C14 C15 H9 125.7 . . ?
N2 C16 C15 106.1(6) . . ?
N2 C16 C17 123.3(6) . . ?
C15 C16 C17 130.3(6) . . ?
C18 C17 C22 117.5(6) . . ?
C18 C17 C16 121.1(6) . . ?
C22 C17 C16 121.4(6) . . ?
C17 C18 C19 122.1(6) . . ?
C17 C18 H10 119.0 . . ?
C19 C18 H10 119.0 . . ?
C18 C19 C20 120.4(6) . . ?
C18 C19 H11 119.8 . . ?
C20 C19 H11 119.8 . . ?
C21 C20 C19 117.9(7) . . ?
C21 C20 H12 121.0 . . ?
C19 C20 H12 121.0 . . ?
C22 C21 C20 121.2(7) . . ?
C22 C21 H13 119.4 . . ?
C20 C21 H13 119.4 . . ?
C21 C22 C17 121.0(6) . . ?
C21 C22 H14 119.5 . . ?
C17 C22 H14 119.5 . . ?
N3 C23 C28 120.1(5) . . ?
N3 C23 C24 119.6(6) . . ?
C28 C23 C24 120.3(6) . . ?
C25 C24 C23 119.9(6) . . ?
C25 C24 H15 120.1 . . ?
C23 C24 H15 120.1 . . ?
C24 C25 C26 119.7(6) . . ?
C24 C25 H16 120.1 . . ?
C26 C25 H16 120.1 . . ?
C27 C26 C25 122.8(7) . . ?
C27 C26 H17 118.6 . . ?
C25 C26 H17 118.6 . . ?
C26 C27 C28 117.4(7) . . ?
C26 C27 H18 121.3 . . ?
C28 C27 H18 121.3 . . ?
N4 C28 C23 120.8(6) . . ?
N4 C28 C27 119.3(6) . . ?
C23 C28 C27 119.9(6) . . ?
C30 C29 N5 116.4(5) . . ?
C30 C29 H21 108.2 . . ?
N5 C29 H21 108.2 . . ?
C30 C29 H22 108.2 . . ?
N5 C29 H22 108.2 . . ?
H21 C29 H22 107.3 . . ?
C29 C30 C31 109.2(5) . . ?
C29 C30 H23 109.8 . . ?
C31 C30 H23 109.8 . . ?
C29 C30 H24 109.8 . . ?
C31 C30 H24 109.8 . . ?
H23 C30 H24 108.3 . . ?
C32 C31 C30 112.0(6) . . ?
C32 C31 H25 109.2 . . ?
C30 C31 H25 109.2 . . ?
C32 C31 H26 109.2 . . ?
C30 C31 H26 109.2 . . ?
H25 C31 H26 107.9 . . ?
C31 C32 H47 109.5 . . ?
C31 C32 H48 109.5 . . ?
H47 C32 H48 109.5 . . ?
C31 C32 H49 109.5 . . ?
H47 C32 H49 109.5 . . ?
H48 C32 H49 109.5 . . ?
N5 C33 C34 114.9(5) . . ?
N5 C33 H27 108.6 . . ?
C34 C33 H27 108.6 . . ?
N5 C33 H28 108.6 . . ?
C34 C33 H28 108.6 . . ?
H27 C33 H28 107.5 . . ?
C33 C34 C35 110.2(5) . . ?
C33 C34 H29 109.6 . . ?
C35 C34 H29 109.6 . . ?
C33 C34 H30 109.6 . . ?
C35 C34 H30 109.6 . . ?
H29 C34 H30 108.1 . . ?
C36 C35 C34 112.3(6) . . ?
C36 C35 H31 109.1 . . ?
C34 C35 H31 109.1 . . ?
C36 C35 H32 109.1 . . ?
C34 C35 H32 109.1 . . ?
H31 C35 H32 107.9 . . ?
C35 C36 H50 109.5 . . ?
C35 C36 H51 109.5 . . ?
H50 C36 H51 109.5 . . ?
C35 C36 H52 109.5 . . ?
H50 C36 H52 109.5 . . ?
H51 C36 H52 109.5 . . ?
N5 C37 C38 115.3(5) . . ?
N5 C37 H33 108.5 . . ?
C38 C37 H33 108.5 . . ?
N5 C37 H34 108.5 . . ?
C38 C37 H34 108.5 . . ?
H33 C37 H34 107.5 . . ?
C39 C38 C37 110.2(5) . . ?
C39 C38 H35 109.6 . . ?
C37 C38 H35 109.6 . . ?
C39 C38 H36 109.6 . . ?
C37 C38 H36 109.6 . . ?
H35 C38 H36 108.1 . . ?
C38 C39 C40 114.3(6) . . ?
C38 C39 H37 108.7 . . ?
C40 C39 H37 108.7 . . ?
C38 C39 H38 108.7 . . ?
C40 C39 H38 108.7 . . ?
H37 C39 H38 107.6 . . ?
C39 C40 H53 109.5 . . ?
C39 C40 H54 109.5 . . ?
H53 C40 H54 109.5 . . ?
C39 C40 H55 109.5 . . ?
H53 C40 H55 109.5 . . ?
H54 C40 H55 109.5 . . ?
N5 C41 C42 114.9(5) . . ?
N5 C41 H39 108.5 . . ?
C42 C41 H39 108.5 . . ?
N5 C41 H40 108.5 . . ?
C42 C41 H40 108.5 . . ?
H39 C41 H40 107.5 . . ?
C43 C42 C41 108.6(5) . . ?
C43 C42 H41 110.0 . . ?
C41 C42 H41 110.0 . . ?
C43 C42 H42 110.0 . . ?
C41 C42 H42 110.0 . . ?
H41 C42 H42 108.4 . . ?
C42 C43 C44 113.7(6) . . ?
C42 C43 H43 108.8 . . ?
C44 C43 H43 108.8 . . ?
C42 C43 H44 108.8 . . ?
C44 C43 H44 108.8 . . ?
H43 C43 H44 107.7 . . ?
C43 C44 H56 109.5 . . ?
C43 C44 H57 109.5 . . ?
H56 C44 H57 109.5 . . ?
C43 C44 H58 109.5 . . ?
H56 C44 H58 109.5 . . ?
H57 C44 H58 109.5 . . ?
Cl1 C45 Cl2 112.0(10) . . ?
Cl1 C45 H45 109.2 . . ?
Cl2 C45 H45 109.2 . . ?
Cl1 C45 H46 109.2 . . ?
Cl2 C45 H46 109.2 . . ?
H45 C45 H46 107.9 . . ?
C10 N1 C7 105.0(4) . . ?
C16 N2 C13 110.9(5) . . ?
C16 N2 H59 124.5 . . ?
C13 N2 H59 124.5 . . ?
C11 N3 C23 119.4(5) . . ?
C12 N4 C28 118.8(5) . . ?
C41 N5 C33 112.0(5) . . ?
C41 N5 C37 111.6(4) . . ?
C33 N5 C37 105.9(4) . . ?
C41 N5 C29 106.0(4) . . ?
C33 N5 C29 110.7(4) . . ?
C37 N5 C29 110.7(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.4(10) . . . . ?
C1 C2 C3 C4 -0.1(10) . . . . ?
C2 C3 C4 C5 -0.3(10) . . . . ?
C3 C4 C5 C6 -0.5(10) . . . . ?
C2 C1 C6 C5 -2.2(9) . . . . ?
C2 C1 C6 C7 180.0(6) . . . . ?
C4 C5 C6 C1 1.7(9) . . . . ?
C4 C5 C6 C7 179.7(5) . . . . ?
C1 C6 C7 N1 -15.1(9) . . . . ?
C5 C6 C7 N1 167.1(5) . . . . ?
C1 C6 C7 C8 161.4(6) . . . . ?
C5 C6 C7 C8 -16.4(9) . . . . ?
N1 C7 C8 C9 0.1(7) . . . . ?
C6 C7 C8 C9 -176.7(6) . . . . ?
C7 C8 C9 C10 -0.5(6) . . . . ?
C8 C9 C10 N1 0.8(6) . . . . ?
C8 C9 C10 C11 171.8(5) . . . . ?
N1 C10 C11 N3 151.6(5) . . . . ?
C9 C10 C11 N3 -18.4(8) . . . . ?
N1 C10 C11 C12 -27.7(9) . . . . ?
C9 C10 C11 C12 162.3(5) . . . . ?
N3 C11 C12 N4 -8.0(8) . . . . ?
C10 C11 C12 N4 171.3(6) . . . . ?
N3 C11 C12 C13 166.0(5) . . . . ?
C10 C11 C12 C13 -14.8(9) . . . . ?
N4 C12 C13 N2 -169.6(5) . . . . ?
C11 C12 C13 N2 16.0(9) . . . . ?
N4 C12 C13 C14 12.2(8) . . . . ?
C11 C12 C13 C14 -162.2(6) . . . . ?
N2 C13 C14 C15 -0.8(6) . . . . ?
C12 C13 C14 C15 177.7(5) . . . . ?
C13 C14 C15 C16 1.2(7) . . . . ?
C14 C15 C16 N2 -1.2(7) . . . . ?
C14 C15 C16 C17 -175.5(6) . . . . ?
N2 C16 C17 C18 -172.0(6) . . . . ?
C15 C16 C17 C18 1.4(10) . . . . ?
N2 C16 C17 C22 5.7(9) . . . . ?
C15 C16 C17 C22 179.1(6) . . . . ?
C22 C17 C18 C19 -0.2(9) . . . . ?
C16 C17 C18 C19 177.6(6) . . . . ?
C17 C18 C19 C20 0.2(10) . . . . ?
C18 C19 C20 C21 1.2(10) . . . . ?
C19 C20 C21 C22 -2.8(10) . . . . ?
C20 C21 C22 C17 2.9(10) . . . . ?
C18 C17 C22 C21 -1.3(9) . . . . ?
C16 C17 C22 C21 -179.1(6) . . . . ?
N3 C23 C24 C25 -178.1(6) . . . . ?
C28 C23 C24 C25 0.9(9) . . . . ?
C23 C24 C25 C26 0.1(10) . . . . ?
C24 C25 C26 C27 -0.5(11) . . . . ?
C25 C26 C27 C28 0.0(11) . . . . ?
N3 C23 C28 N4 -6.0(9) . . . . ?
C24 C23 C28 N4 175.1(6) . . . . ?
N3 C23 C28 C27 177.6(6) . . . . ?
C24 C23 C28 C27 -1.4(9) . . . . ?
C26 C27 C28 N4 -175.6(6) . . . . ?
C26 C27 C28 C23 0.9(10) . . . . ?
N5 C29 C30 C31 165.9(5) . . . . ?
C29 C30 C31 C32 174.6(5) . . . . ?
N5 C33 C34 C35 175.9(5) . . . . ?
C33 C34 C35 C36 73.9(7) . . . . ?
N5 C37 C38 C39 -167.4(5) . . . . ?
C37 C38 C39 C40 67.7(7) . . . . ?
N5 C41 C42 C43 174.9(5) . . . . ?
C41 C42 C43 C44 176.4(6) . . . . ?
C9 C10 N1 C7 -0.8(6) . . . . ?
C11 C10 N1 C7 -171.9(5) . . . . ?
C8 C7 N1 C10 0.4(6) . . . . ?
C6 C7 N1 C10 177.5(5) . . . . ?
C15 C16 N2 C13 0.7(7) . . . . ?
C17 C16 N2 C13 175.5(5) . . . . ?
C14 C13 N2 C16 0.0(6) . . . . ?
C12 C13 N2 C16 -178.5(5) . . . . ?
C12 C11 N3 C23 2.8(7) . . . . ?
C10 C11 N3 C23 -176.5(5) . . . . ?
C28 C23 N3 C11 3.9(8) . . . . ?
C24 C23 N3 C11 -177.2(5) . . . . ?
C11 C12 N4 C28 5.9(9) . . . . ?
C13 C12 N4 C28 -168.9(5) . . . . ?
C23 C28 N4 C12 0.9(9) . . . . ?
C27 C28 N4 C12 177.4(6) . . . . ?
C42 C41 N5 C33 -64.3(7) . . . . ?
C42 C41 N5 C37 54.3(7) . . . . ?
C42 C41 N5 C29 174.9(5) . . . . ?
C34 C33 N5 C41 -57.4(7) . . . . ?
C34 C33 N5 C37 -179.4(5) . . . . ?
C34 C33 N5 C29 60.6(7) . . . . ?
C38 C37 N5 C41 60.9(7) . . . . ?
C38 C37 N5 C33 -177.0(5) . . . . ?
C38 C37 N5 C29 -56.9(6) . . . . ?
C30 C29 N5 C41 177.5(5) . . . . ?
C30 C29 N5 C33 55.8(7) . . . . ?
C30 C29 N5 C37 -61.3(6) . . . . ?

_refine_diff_density_max         0.194
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.045

####################################################################### 
# 
# 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_40719m2
_database_code_depnum_ccdc_archive 'CCDC 1871608'
_audit_update_record             
;
2018-10-05 deposited with the CCDC.
2018-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H10 N2'
_chemical_formula_sum            'C14 H10 N2'
_chemical_formula_weight         206.24

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_Int_Tables_number      60

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

_cell_length_a                   23.909(11)
_cell_length_b                   11.079(5)
_cell_length_c                   7.591(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2010.8(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    2281
_cell_measurement_theta_min      25.2
_cell_measurement_theta_max      68.2

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6281
_exptl_absorpt_correction_T_max  0.8825
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.8140
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6714
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         6.84
_diffrn_reflns_theta_max         66.00
_reflns_number_total             1728
_reflns_number_gt                1632
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0850P)²+0.4145P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1728
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1150
_refine_ls_wR_factor_gt          0.1121
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.72511(5) 0.47364(11) -0.05319(16) 0.0190(3) Uani 1 1 d . . .
H1 H 0.7004 0.5346 -0.0946 0.023 Uiso 1 1 calc R . .
C2 C 0.78215(5) 0.48430(12) -0.08373(16) 0.0209(3) Uani 1 1 d . . .
H2 H 0.7962 0.5528 -0.1447 0.025 Uiso 1 1 calc R . .
C3 C 0.81891(5) 0.39568(12) -0.02598(16) 0.0200(3) Uani 1 1 d . . .
H3 H 0.8580 0.4037 -0.0460 0.024 Uiso 1 1 calc R . .
C4 C 0.79787(5) 0.29493(11) 0.06160(16) 0.0192(3) Uani 1 1 d . . .
H4 H 0.8226 0.2331 0.0994 0.023 Uiso 1 1 calc R . .
C5 C 0.74081(5) 0.28437(11) 0.09399(16) 0.0177(3) Uani 1 1 d . . .
H5 H 0.7270 0.2156 0.1547 0.021 Uiso 1 1 calc R . .
C6 C 0.70350(5) 0.37418(10) 0.03794(15) 0.0160(3) Uani 1 1 d . . .
C7 C 0.64329(5) 0.36771(11) 0.07571(15) 0.0164(3) Uani 1 1 d . . .
C8 C 0.60118(5) 0.45260(11) 0.05459(16) 0.0185(3) Uani 1 1 d . . .
H6 H 0.6054 0.5313 0.0067 0.022 Uiso 1 1 calc R . .
C9 C 0.55099(5) 0.40132(11) 0.11674(16) 0.0181(3) Uani 1 1 d . . .
H7 H 0.5154 0.4394 0.1182 0.022 Uiso 1 1 calc R . .
C10 C 0.56265(5) 0.28560(11) 0.17544(16) 0.0158(3) Uani 1 1 d . . .
C11 C 0.52957(5) 0.18069(11) 0.22808(15) 0.0149(3) Uani 1 1 d . . .
C12 C 0.52962(5) -0.02835(11) 0.24387(15) 0.0160(3) Uani 1 1 d . . .
C13 C 0.55863(5) -0.13930(11) 0.24444(17) 0.0202(3) Uani 1 1 d . . .
H8 H 0.5984 -0.1400 0.2423 0.024 Uiso 1 1 calc R . .
C14 C 0.52964(6) -0.24586(11) 0.24804(16) 0.0223(3) Uani 1 1 d . . .
H9 H 0.5494 -0.3203 0.2479 0.027 Uiso 1 1 calc R . .
N1 N 0.61910(4) 0.26781(9) 0.14908(13) 0.0162(3) Uani 1 1 d . . .
H10 H 0.6372 0.2011 0.1759 0.019 Uiso 1 1 calc R . .
N2 N 0.55784(4) 0.07760(9) 0.22446(13) 0.0169(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.3884(19) . ?
C1 C6 1.3999(18) . ?
C1 H1 0.9500 . ?
C2 C3 1.3887(19) . ?
C2 H2 0.9500 . ?
C3 C4 1.3932(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.3912(18) . ?
C4 H4 0.9500 . ?
C5 C6 1.4024(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.4696(17) . ?
C7 N1 1.3674(16) . ?
C7 C8 1.3871(17) . ?
C8 C9 1.4090(18) . ?
C8 H6 0.9500 . ?
C9 C10 1.3856(18) . ?
C9 H7 0.9500 . ?
C10 N1 1.3785(16) . ?
C10 C11 1.4616(17) . ?
C11 N2 1.3276(16) . ?
C11 C11 1.453(2) 4_655 ?
C12 N2 1.3620(16) . ?
C12 C13 1.4115(17) . ?
C12 C12 1.419(2) 4_655 ?
C13 C14 1.3692(18) . ?
C13 H8 0.9500 . ?
C14 C14 1.418(3) 4_655 ?
C14 H9 0.9500 . ?
N1 H10 0.8800 . ?

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
C2 C1 C6 120.80(11) . . ?
C2 C1 H1 119.6 . . ?
C6 C1 H1 119.6 . . ?
C1 C2 C3 120.58(11) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C2 C3 C4 119.25(12) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 120.38(11) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 120.70(11) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 118.27(11) . . ?
C1 C6 C7 119.76(11) . . ?
C5 C6 C7 121.96(11) . . ?
N1 C7 C8 106.79(11) . . ?
N1 C7 C6 122.23(10) . . ?
C8 C7 C6 130.95(11) . . ?
C7 C8 C9 107.82(11) . . ?
C7 C8 H6 126.1 . . ?
C9 C8 H6 126.1 . . ?
C10 C9 C8 108.03(11) . . ?
C10 C9 H7 126.0 . . ?
C8 C9 H7 126.0 . . ?
N1 C10 C9 106.42(10) . . ?
N1 C10 C11 117.12(10) . . ?
C9 C10 C11 135.63(11) . . ?
N2 C11 C11 120.03(7) . 4_655 ?
N2 C11 C10 113.76(10) . . ?
C11 C11 C10 126.12(7) 4_655 . ?
N2 C12 C13 120.48(11) . . ?
N2 C12 C12 120.10(7) . 4_655 ?
C13 C12 C12 119.36(7) . 4_655 ?
C14 C13 C12 120.14(12) . . ?
C14 C13 H8 119.9 . . ?
C12 C13 H8 119.9 . . ?
C13 C14 C14 120.43(8) . 4_655 ?
C13 C14 H9 119.8 . . ?
C14 C14 H9 119.8 4_655 . ?
C7 N1 C10 110.95(10) . . ?
C7 N1 H10 124.5 . . ?
C10 N1 H10 124.5 . . ?
C11 N2 C12 119.14(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.68(18) . . . . ?
C1 C2 C3 C4 0.69(18) . . . . ?
C2 C3 C4 C5 -1.29(18) . . . . ?
C3 C4 C5 C6 0.54(18) . . . . ?
C2 C1 C6 C5 -1.42(18) . . . . ?
C2 C1 C6 C7 177.20(11) . . . . ?
C4 C5 C6 C1 0.81(18) . . . . ?
C4 C5 C6 C7 -177.77(11) . . . . ?
C1 C6 C7 N1 173.62(11) . . . . ?
C5 C6 C7 N1 -7.82(18) . . . . ?
C1 C6 C7 C8 -8.6(2) . . . . ?
C5 C6 C7 C8 169.93(13) . . . . ?
N1 C7 C8 C9 -0.11(14) . . . . ?
C6 C7 C8 C9 -178.12(12) . . . . ?
C7 C8 C9 C10 0.01(14) . . . . ?
C8 C9 C10 N1 0.09(14) . . . . ?
C8 C9 C10 C11 -168.62(13) . . . . ?
N1 C10 C11 N2 -7.17(16) . . . . ?
C9 C10 C11 N2 160.65(14) . . . . ?
N1 C10 C11 C11 176.35(13) . . . 4_655 ?
C9 C10 C11 C11 -15.8(3) . . . 4_655 ?
N2 C12 C13 C14 -174.11(11) . . . . ?
C12 C12 C13 C14 3.2(2) 4_655 . . . ?
C12 C13 C14 C14 -0.3(2) . . . 4_655 ?
C8 C7 N1 C10 0.17(13) . . . . ?
C6 C7 N1 C10 178.39(10) . . . . ?
C9 C10 N1 C7 -0.16(13) . . . . ?
C11 C10 N1 C7 170.99(10) . . . . ?
C11 C11 N2 C12 6.9(2) 4_655 . . . ?
C10 C11 N2 C12 -169.85(10) . . . . ?
C13 C12 N2 C11 -178.62(11) . . . . ?
C12 C12 N2 C11 4.10(19) 4_655 . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        66.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.068
####################################################################### 
# 
# 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_40705m
_database_code_depnum_ccdc_archive 'CCDC 1871609'
_audit_update_record             
;
2018-10-05 deposited with the CCDC.
2018-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'3(C28 H20 N4, 0.12(C H Cl3), 0.22(C H2 Cl2), 0.7(Cl), 0.31(C), 0.79(H))'
_chemical_formula_sum            'C85.97 H62.41 Cl4.45 N12'
_chemical_formula_weight         1421.11

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.613(5)
_cell_length_b                   16.033(8)
_cell_length_c                   19.015(7)
_cell_angle_alpha                107.164(13)
_cell_angle_beta                 91.906(6)
_cell_angle_gamma                110.482(11)
_cell_volume                     3671(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    3395
_cell_measurement_theta_min      25.4
_cell_measurement_theta_max      68.2

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1476
_exptl_absorpt_coefficient_mu    2.048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5786
_exptl_absorpt_correction_T_max  0.9602
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.8140
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44930
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         6.52
_diffrn_reflns_theta_max         65.00
_reflns_number_total             12086
_reflns_number_gt                10332
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1600P)²+5.6883P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12086
_refine_ls_number_parameters     970
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0891
_refine_ls_wR_factor_ref         0.2724
_refine_ls_wR_factor_gt          0.2653
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 1.0749(2) 1.3641(2) 0.59915(16) 0.0327(7) Uani 1 1 d . . .
H1 H 1.1400 1.3964 0.6231 0.039 Uiso 1 1 calc R . .
N2 N 0.7353(2) 1.1855(2) 0.73658(17) 0.0327(7) Uani 1 1 d . . .
H2 H 0.7412 1.1410 0.7526 0.039 Uiso 1 1 calc R . .
N3 N 1.1115(2) 1.3129(2) 0.72158(17) 0.0330(7) Uani 1 1 d . . .
N4 N 0.9458(2) 1.2343(2) 0.79535(17) 0.0346(7) Uani 1 1 d . . .
N5 N 0.7798(2) 1.1775(2) 0.90714(16) 0.0310(7) Uani 1 1 d . . .
H3 H 0.8246 1.1919 0.8763 0.037 Uiso 1 1 calc R . .
N6 N 0.6008(2) 0.8079(2) 0.92337(16) 0.0303(6) Uani 1 1 d . . .
H4 H 0.5626 0.7630 0.8825 0.036 Uiso 1 1 calc R . .
N7 N 0.7679(2) 1.0233(2) 0.79016(17) 0.0334(7) Uani 1 1 d . . .
N8 N 0.6952(2) 0.8412(2) 0.80004(17) 0.0338(7) Uani 1 1 d . . .
N9 N 0.6548(2) 0.6467(2) 0.80059(16) 0.0296(6) Uani 1 1 d . . .
H5 H 0.6618 0.7053 0.8070 0.035 Uiso 1 1 calc R . .
N10 N 0.2991(2) 0.3305(2) 0.63958(16) 0.0333(7) Uani 1 1 d . . .
H6 H 0.2394 0.3232 0.6580 0.040 Uiso 1 1 calc R . .
N11 N 0.4590(2) 0.6622(2) 0.78234(17) 0.0318(7) Uani 1 1 d . . .
N12 N 0.2818(2) 0.5104(2) 0.69177(16) 0.0331(7) Uani 1 1 d . . .
C1 C 1.0649(4) 1.4262(4) 0.4259(3) 0.0602(13) Uani 1 1 d . . .
H7 H 0.9901 1.4076 0.4156 0.072 Uiso 1 1 calc R . .
C2 C 1.1282(4) 1.4683(5) 0.3819(3) 0.0778(18) Uani 1 1 d . . .
H8 H 1.0965 1.4756 0.3400 0.093 Uiso 1 1 calc R . .
C3 C 1.2364(4) 1.5001(5) 0.3972(3) 0.0731(17) Uani 1 1 d . . .
H9 H 1.2801 1.5315 0.3677 0.088 Uiso 1 1 calc R . .
C4 C 1.2809(4) 1.4851(6) 0.4572(3) 0.088(2) Uani 1 1 d . . .
H10 H 1.3559 1.5054 0.4679 0.105 Uiso 1 1 calc R . .
C5 C 1.2185(4) 1.4418(4) 0.5007(3) 0.0593(13) Uani 1 1 d . . .
H11 H 1.2505 1.4332 0.5418 0.071 Uiso 1 1 calc R . .
C6 C 1.1091(3) 1.4103(3) 0.4857(2) 0.0376(9) Uani 1 1 d . . .
C7 C 1.0402(3) 1.3604(3) 0.5293(2) 0.0346(8) Uani 1 1 d . . .
C8 C 0.9340(3) 1.3010(3) 0.5112(2) 0.0389(9) Uani 1 1 d . . .
H12 H 0.8893 1.2842 0.4658 0.047 Uiso 1 1 calc R . .
C9 C 0.9045(3) 1.2702(3) 0.5714(2) 0.0368(8) Uani 1 1 d . . .
H13 H 0.8359 1.2291 0.5743 0.044 Uiso 1 1 calc R . .
C10 C 0.9926(3) 1.3098(3) 0.6262(2) 0.0326(8) Uani 1 1 d . . .
C11 C 1.0112(3) 1.2958(3) 0.6972(2) 0.0316(8) Uani 1 1 d . . .
C12 C 0.9272(3) 1.2604(3) 0.7381(2) 0.0328(8) Uani 1 1 d . . .
C13 C 0.8181(3) 1.2528(3) 0.7212(2) 0.0321(8) Uani 1 1 d . . .
C14 C 0.7765(3) 1.3104(3) 0.6991(2) 0.0365(8) Uani 1 1 d . . .
H14 H 0.8153 1.3640 0.6856 0.044 Uiso 1 1 calc R . .
C15 C 0.6671(3) 1.2753(3) 0.7001(2) 0.0382(9) Uani 1 1 d . . .
H15 H 0.6183 1.3006 0.6870 0.046 Uiso 1 1 calc R . .
C16 C 0.6421(3) 1.1972(3) 0.7235(2) 0.0350(8) Uani 1 1 d . . .
C17 C 0.5392(3) 1.1351(3) 0.7335(2) 0.0375(9) Uani 1 1 d . . .
C18 C 0.4454(4) 1.1438(4) 0.7113(3) 0.0578(13) Uani 1 1 d . . .
H16 H 0.4481 1.1897 0.6885 0.069 Uiso 1 1 calc R . .
C19 C 0.3494(4) 1.0864(4) 0.7222(3) 0.0649(14) Uani 1 1 d . . .
H17 H 0.2865 1.0936 0.7071 0.078 Uiso 1 1 calc R . .
C20 C 0.3427(3) 1.0187(3) 0.7543(2) 0.0470(10) Uani 1 1 d . . .
H18 H 0.2757 0.9780 0.7601 0.056 Uiso 1 1 calc R . .
C21 C 0.4342(4) 1.0110(3) 0.7779(3) 0.0501(11) Uani 1 1 d . . .
H19 H 0.4306 0.9656 0.8014 0.060 Uiso 1 1 calc R . .
C22 C 0.5318(3) 1.0682(3) 0.7680(3) 0.0453(10) Uani 1 1 d . . .
H20 H 0.5944 1.0618 0.7849 0.054 Uiso 1 1 calc R . .
C23 C 1.1317(3) 1.2912(3) 0.7831(2) 0.0337(8) Uani 1 1 d . . .
C24 C 1.2385(3) 1.3104(3) 0.8116(2) 0.0417(9) Uani 1 1 d . . .
H21 H 1.2954 1.3408 0.7890 0.050 Uiso 1 1 calc R . .
C25 C 1.2584(3) 1.2848(3) 0.8716(2) 0.0449(10) Uani 1 1 d . . .
H22 H 1.3294 1.2972 0.8904 0.054 Uiso 1 1 calc R . .
C26 C 1.1748(4) 1.2404(3) 0.9055(2) 0.0463(10) Uani 1 1 d . . .
H23 H 1.1901 1.2232 0.9471 0.056 Uiso 1 1 calc R . .
C27 C 1.0717(3) 1.2216(3) 0.8799(2) 0.0404(9) Uani 1 1 d . . .
H24 H 1.0160 1.1914 0.9034 0.049 Uiso 1 1 calc R . .
C28 C 1.0485(3) 1.2473(3) 0.8180(2) 0.0341(8) Uani 1 1 d . . .
C29 C 0.8418(3) 1.3792(3) 0.9191(3) 0.0428(9) Uani 1 1 d . . .
H25 H 0.8385 1.3371 0.8711 0.051 Uiso 1 1 calc R . .
C30 C 0.8844(3) 1.4755(3) 0.9322(3) 0.0518(11) Uani 1 1 d . . .
H26 H 0.9109 1.4992 0.8935 0.062 Uiso 1 1 calc R . .
C31 C 0.8882(4) 1.5369(3) 1.0013(3) 0.0576(13) Uani 1 1 d . . .
H27 H 0.9163 1.6030 1.0101 0.069 Uiso 1 1 calc R . .
C32 C 0.8515(4) 1.5028(3) 1.0573(3) 0.0591(13) Uani 1 1 d . . .
H28 H 0.8552 1.5457 1.1050 0.071 Uiso 1 1 calc R . .
C33 C 0.8083(3) 1.4057(3) 1.0456(3) 0.0475(10) Uani 1 1 d . . .
H29 H 0.7827 1.3829 1.0849 0.057 Uiso 1 1 calc R . .
C34 C 0.8035(3) 1.3433(3) 0.9758(2) 0.0391(9) Uani 1 1 d . . .
C35 C 0.7558(3) 1.2416(3) 0.9618(2) 0.0342(8) Uani 1 1 d . . .
C36 C 0.6814(3) 1.1911(3) 0.9966(2) 0.0360(8) Uani 1 1 d . . .
H30 H 0.6493 1.2170 1.0366 0.043 Uiso 1 1 calc R . .
C37 C 0.6613(3) 1.0956(3) 0.9631(2) 0.0353(8) Uani 1 1 d . . .
H31 H 0.6134 1.0452 0.9763 0.042 Uiso 1 1 calc R . .
C38 C 0.7237(3) 1.0872(3) 0.9071(2) 0.0310(8) Uani 1 1 d . . .
C39 C 0.7319(3) 1.0078(3) 0.8511(2) 0.0313(8) Uani 1 1 d . . .
C40 C 0.7000(3) 0.9136(3) 0.8575(2) 0.0306(8) Uani 1 1 d . . .
C41 C 0.6734(3) 0.8945(3) 0.9259(2) 0.0315(8) Uani 1 1 d . . .
C42 C 0.7180(3) 0.9432(3) 1.0000(2) 0.0356(8) Uani 1 1 d . . .
H32 H 0.7717 1.0046 1.0188 0.043 Uiso 1 1 calc R . .
C43 C 0.6704(3) 0.8861(3) 1.0423(2) 0.0368(8) Uani 1 1 d . . .
H33 H 0.6855 0.9021 1.0948 0.044 Uiso 1 1 calc R . .
C44 C 0.5969(3) 0.8020(3) 0.9937(2) 0.0329(8) Uani 1 1 d . . .
C45 C 0.5255(3) 0.7184(3) 1.0087(2) 0.0346(8) Uani 1 1 d . . .
C46 C 0.4922(3) 0.6286(3) 0.9561(2) 0.0375(8) Uani 1 1 d . . .
H34 H 0.5145 0.6210 0.9086 0.045 Uiso 1 1 calc R . .
C47 C 0.4269(3) 0.5505(3) 0.9721(2) 0.0439(9) Uani 1 1 d . . .
H35 H 0.4034 0.4898 0.9355 0.053 Uiso 1 1 calc R . .
C48 C 0.3958(3) 0.5616(3) 1.0423(3) 0.0456(10) Uani 1 1 d . . .
H36 H 0.3521 0.5081 1.0539 0.055 Uiso 1 1 calc R . .
C49 C 0.4285(3) 0.6497(3) 1.0945(2) 0.0423(9) Uani 1 1 d . . .
H37 H 0.4070 0.6566 1.1423 0.051 Uiso 1 1 calc R . .
C50 C 0.4921(3) 0.7283(3) 1.0787(2) 0.0369(8) Uani 1 1 d . . .
H38 H 0.5131 0.7891 1.1151 0.044 Uiso 1 1 calc R . .
C51 C 0.7716(3) 0.9491(3) 0.7333(2) 0.0356(8) Uani 1 1 d . . .
C52 C 0.8154(4) 0.9642(3) 0.6697(2) 0.0451(10) Uani 1 1 d . . .
H39 H 0.8441 1.0261 0.6669 0.054 Uiso 1 1 calc R . .
C53 C 0.8163(4) 0.8889(3) 0.6117(2) 0.0509(11) Uani 1 1 d . . .
H40 H 0.8473 0.8995 0.5695 0.061 Uiso 1 1 calc R . .
C54 C 0.7723(4) 0.7972(3) 0.6144(2) 0.0482(10) Uani 1 1 d . . .
H41 H 0.7724 0.7459 0.5736 0.058 Uiso 1 1 calc R . .
C55 C 0.7288(3) 0.7806(3) 0.6754(2) 0.0435(9) Uani 1 1 d . . .
H42 H 0.6980 0.7179 0.6764 0.052 Uiso 1 1 calc R . .
C56 C 0.7301(3) 0.8567(3) 0.7365(2) 0.0354(8) Uani 1 1 d . . .
C57 C 0.9253(3) 0.6592(3) 0.8545(2) 0.0377(8) Uani 1 1 d . . .
H43 H 0.9166 0.5991 0.8210 0.045 Uiso 1 1 calc R . .
C58 C 1.0243(3) 0.7185(3) 0.8974(2) 0.0437(10) Uani 1 1 d . . .
H44 H 1.0818 0.6978 0.8940 0.052 Uiso 1 1 calc R . .
C59 C 1.0382(3) 0.8062(3) 0.9439(2) 0.0466(10) Uani 1 1 d . . .
H45 H 1.1057 0.8464 0.9727 0.056 Uiso 1 1 calc R . .
C60 C 0.9542(4) 0.8366(3) 0.9494(3) 0.0493(10) Uani 1 1 d . . .
H46 H 0.9646 0.8979 0.9817 0.059 Uiso 1 1 calc R . .
C61 C 0.8545(3) 0.7777(3) 0.9078(2) 0.0384(9) Uani 1 1 d . . .
H47 H 0.7973 0.7989 0.9116 0.046 Uiso 1 1 calc R . .
C62 C 0.8390(3) 0.6876(3) 0.8607(2) 0.0319(8) Uani 1 1 d . . .
C63 C 0.7331(3) 0.6201(3) 0.82174(19) 0.0302(8) Uani 1 1 d . . .
C64 C 0.6910(3) 0.5231(3) 0.8033(2) 0.0316(8) Uani 1 1 d . . .
H48 H 0.7274 0.4852 0.8116 0.038 Uiso 1 1 calc R . .
C65 C 0.5850(3) 0.4906(3) 0.7701(2) 0.0317(8) Uani 1 1 d . . .
H49 H 0.5367 0.4269 0.7523 0.038 Uiso 1 1 calc R . .
C66 C 0.5634(3) 0.5687(2) 0.76778(19) 0.0293(7) Uani 1 1 d . . .
C67 C 0.4652(3) 0.5799(2) 0.74817(19) 0.0297(7) Uani 1 1 d . . .
C68 C 0.3748(3) 0.5027(3) 0.69797(19) 0.0309(8) Uani 1 1 d . . .
C69 C 0.3817(3) 0.4148(3) 0.6524(2) 0.0323(8) Uani 1 1 d . . .
C70 C 0.4584(3) 0.3971(3) 0.6114(2) 0.0405(9) Uani 1 1 d . . .
H63 H 0.5239 0.4426 0.6085 0.049 Uiso 1 1 calc R . .
C71 C 0.4217(3) 0.2997(3) 0.5748(2) 0.0438(10) Uani 1 1 d . . .
H64 H 0.4584 0.2675 0.5427 0.053 Uiso 1 1 calc R . .
C72 C 0.3239(3) 0.2587(3) 0.5933(2) 0.0383(9) Uani 1 1 d . . .
C73 C 0.2551(4) 0.1603(3) 0.5752(2) 0.0480(10) Uani 1 1 d . . .
C74 C 0.1533(5) 0.1323(4) 0.5922(4) 0.0747(18) Uani 1 1 d . . .
H50 H 0.1258 0.1784 0.6163 0.090 Uiso 1 1 calc R . .
C75 C 0.0921(6) 0.0392(4) 0.5747(5) 0.111(3) Uani 1 1 d . . .
H51 H 0.0225 0.0217 0.5873 0.133 Uiso 1 1 calc R . .
C76 C 0.1281(7) -0.0304(4) 0.5393(5) 0.108(3) Uani 1 1 d . . .
H52 H 0.0843 -0.0951 0.5272 0.130 Uiso 1 1 calc R . .
C77 C 0.2285(5) -0.0037(4) 0.5220(4) 0.0829(19) Uani 1 1 d . . .
H53 H 0.2548 -0.0506 0.4975 0.099 Uiso 1 1 calc R . .
C78 C 0.2921(4) 0.0897(4) 0.5394(3) 0.0625(14) Uani 1 1 d . . .
H54 H 0.3619 0.1067 0.5271 0.075 Uiso 1 1 calc R . .
C79 C 0.3643(3) 0.6724(3) 0.7710(2) 0.0324(8) Uani 1 1 d . . .
C80 C 0.3555(3) 0.7602(3) 0.8049(2) 0.0396(9) Uani 1 1 d . . .
H55 H 0.4158 0.8128 0.8342 0.047 Uiso 1 1 calc R . .
C81 C 0.2602(3) 0.7692(3) 0.7956(2) 0.0445(10) Uani 1 1 d . . .
H56 H 0.2545 0.8283 0.8184 0.053 Uiso 1 1 calc R . .
C82 C 0.1706(3) 0.6918(3) 0.7525(2) 0.0444(10) Uani 1 1 d . . .
H57 H 0.1050 0.6994 0.7464 0.053 Uiso 1 1 calc R . .
C83 C 0.1760(3) 0.6061(3) 0.7193(2) 0.0416(9) Uani 1 1 d . . .
H58 H 0.1146 0.5544 0.6906 0.050 Uiso 1 1 calc R . .
C84 C 0.2738(3) 0.5945(3) 0.7279(2) 0.0332(8) Uani 1 1 d . . .
C85 C 0.4156(7) 0.8640(8) 0.5866(5) 0.121(4) Uani 0.94(3) 1 d PU . .
H59 H 0.4055 0.9243 0.6108 0.145 Uiso 0.71(17) 1 calc PR . .
Cl1 Cl 0.39203(17) 0.8382(2) 0.49326(11) 0.0877(11) Uani 0.681(7) 1 d PU . .
Cl2 Cl 0.54558(18) 0.8789(3) 0.61936(12) 0.1328(18) Uani 0.748(8) 1 d PU . .
Cl3 Cl 0.3261(3) 0.7754(3) 0.61685(16) 0.1141(17) Uani 0.662(8) 1 d PU . .
Cl5 Cl 0.9377(6) 0.1507(5) 0.3479(4) 0.0800(16) Uani 0.353(4) 1 d PD A 1
Cl6 Cl 0.9217(3) -0.0325(3) 0.2524(2) 0.0666(13) Uani 0.353(4) 1 d PD A 1
Cl7 Cl 0.9531(4) 0.1162(3) 0.1897(3) 0.0741(14) Uani 0.353(4) 1 d PD A 1
C87 C 0.9800(12) 0.0867(11) 0.2692(8) 0.058(4) Uani 0.353(4) 1 d P A 1
H60 H 1.0585 0.1056 0.2805 0.070 Uiso 0.353(4) 1 calc PR A 1
Cl5A Cl 0.9448(3) 0.1617(2) 0.3147(2) 0.0723(8) Uani 0.647(4) 1 d P A 2
Cl4 Cl 0.9463(2) 0.01385(18) 0.18067(16) 0.0923(10) Uani 0.647(4) 1 d P A 2
C87A C 1.0028(8) 0.1360(7) 0.2327(6) 0.072(3) Uani 0.647(4) 1 d P A 2
H61 H 1.0802 0.1552 0.2465 0.087 Uiso 0.647(4) 1 calc PR A 2
H62 H 0.9917 0.1726 0.2016 0.087 Uiso 0.647(4) 1 calc PR 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
N1 C7 1.371(5) . ?
N1 C10 1.378(5) . ?
N1 H1 0.8800 . ?
N2 C13 1.370(5) . ?
N2 C16 1.371(5) . ?
N2 H2 0.8800 . ?
N3 C11 1.332(5) . ?
N3 C23 1.362(5) . ?
N4 C12 1.324(5) . ?
N4 C28 1.373(5) . ?
N5 C35 1.367(5) . ?
N5 C38 1.381(5) . ?
N5 H3 0.8800 . ?
N6 C44 1.370(5) . ?
N6 C41 1.380(5) . ?
N6 H4 0.8800 . ?
N7 C39 1.328(5) . ?
N7 C51 1.369(5) . ?
N8 C40 1.319(5) . ?
N8 C56 1.370(5) . ?
N9 C63 1.367(5) . ?
N9 C66 1.378(5) . ?
N9 H5 0.8800 . ?
N10 C69 1.369(5) . ?
N10 C72 1.382(5) . ?
N10 H6 0.8800 . ?
N11 C67 1.323(5) . ?
N11 C79 1.373(5) . ?
N12 C68 1.319(5) . ?
N12 C84 1.365(5) . ?
C1 C2 1.367(7) . ?
C1 C6 1.399(6) . ?
C1 H7 0.9500 . ?
C2 C3 1.368(8) . ?
C2 H8 0.9500 . ?
C3 C4 1.394(8) . ?
C3 H9 0.9500 . ?
C4 C5 1.365(7) . ?
C4 H10 0.9500 . ?
C5 C6 1.384(6) . ?
C5 H11 0.9500 . ?
C6 C7 1.458(6) . ?
C7 C8 1.388(6) . ?
C8 C9 1.392(6) . ?
C8 H12 0.9500 . ?
C9 C10 1.387(5) . ?
C9 H13 0.9500 . ?
C10 C11 1.460(5) . ?
C11 C12 1.448(5) . ?
C12 C13 1.463(5) . ?
C13 C14 1.390(5) . ?
C14 C15 1.399(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.464(5) . ?
C17 C22 1.391(6) . ?
C17 C18 1.397(6) . ?
C18 C19 1.373(7) . ?
C18 H16 0.9500 . ?
C19 C20 1.374(7) . ?
C19 H17 0.9500 . ?
C20 C21 1.368(6) . ?
C20 H18 0.9500 . ?
C21 C22 1.381(6) . ?
C21 H19 0.9500 . ?
C22 H20 0.9500 . ?
C23 C28 1.408(6) . ?
C23 C24 1.427(5) . ?
C24 C25 1.371(6) . ?
C24 H21 0.9500 . ?
C25 C26 1.404(6) . ?
C25 H22 0.9500 . ?
C26 C27 1.367(6) . ?
C26 H23 0.9500 . ?
C27 C28 1.418(5) . ?
C27 H24 0.9500 . ?
C29 C30 1.386(6) . ?
C29 C34 1.401(6) . ?
C29 H25 0.9500 . ?
C30 C31 1.377(7) . ?
C30 H26 0.9500 . ?
C31 C32 1.367(8) . ?
C31 H27 0.9500 . ?
C32 C33 1.402(7) . ?
C32 H28 0.9500 . ?
C33 C34 1.390(6) . ?
C33 H29 0.9500 . ?
C34 C35 1.463(6) . ?
C35 C36 1.381(6) . ?
C36 C37 1.395(6) . ?
C36 H30 0.9500 . ?
C37 C38 1.390(5) . ?
C37 H31 0.9500 . ?
C38 C39 1.441(5) . ?
C39 C40 1.461(5) . ?
C40 C41 1.452(5) . ?
C41 C42 1.388(5) . ?
C42 C43 1.399(5) . ?
C42 H32 0.9500 . ?
C43 C44 1.391(6) . ?
C43 H33 0.9500 . ?
C44 C45 1.468(5) . ?
C45 C46 1.393(6) . ?
C45 C50 1.403(5) . ?
C46 C47 1.384(6) . ?
C46 H34 0.9500 . ?
C47 C48 1.392(6) . ?
C47 H35 0.9500 . ?
C48 C49 1.372(7) . ?
C48 H36 0.9500 . ?
C49 C50 1.382(6) . ?
C49 H37 0.9500 . ?
C50 H38 0.9500 . ?
C51 C56 1.410(6) . ?
C51 C52 1.414(5) . ?
C52 C53 1.377(6) . ?
C52 H39 0.9500 . ?
C53 C54 1.398(7) . ?
C53 H40 0.9500 . ?
C54 C55 1.373(6) . ?
C54 H41 0.9500 . ?
C55 C56 1.410(6) . ?
C55 H42 0.9500 . ?
C57 C62 1.397(5) . ?
C57 C58 1.399(6) . ?
C57 H43 0.9500 . ?
C58 C59 1.365(7) . ?
C58 H44 0.9500 . ?
C59 C60 1.388(6) . ?
C59 H45 0.9500 . ?
C60 C61 1.397(6) . ?
C60 H46 0.9500 . ?
C61 C62 1.394(6) . ?
C61 H47 0.9500 . ?
C62 C63 1.471(5) . ?
C63 C64 1.382(5) . ?
C64 C65 1.404(5) . ?
C64 H48 0.9500 . ?
C65 C66 1.395(5) . ?
C65 H49 0.9500 . ?
C66 C67 1.459(5) . ?
C67 C68 1.455(5) . ?
C68 C69 1.457(5) . ?
C69 C70 1.382(5) . ?
C70 C71 1.400(6) . ?
C70 H63 0.9500 . ?
C71 C72 1.373(6) . ?
C71 H64 0.9500 . ?
C72 C73 1.451(6) . ?
C73 C74 1.380(7) . ?
C73 C78 1.402(6) . ?
C74 C75 1.360(8) . ?
C74 H50 0.9500 . ?
C75 C76 1.380(10) . ?
C75 H51 0.9500 . ?
C76 C77 1.365(10) . ?
C76 H52 0.9500 . ?
C77 C78 1.373(8) . ?
C77 H53 0.9500 . ?
C78 H54 0.9500 . ?
C79 C80 1.413(6) . ?
C79 C84 1.415(5) . ?
C80 C81 1.367(6) . ?
C80 H55 0.9500 . ?
C81 C82 1.405(6) . ?
C81 H56 0.9500 . ?
C82 C83 1.361(6) . ?
C82 H57 0.9500 . ?
C83 C84 1.417(5) . ?
C83 H58 0.9500 . ?
C85 Cl1 1.691(10) . ?
C85 Cl2 1.767(8) . ?
C85 Cl3 1.775(13) . ?
C85 H59 1.0000 . ?
Cl5 C87 1.786(17) . ?
Cl6 C87 1.716(15) . ?
Cl7 C87 1.774(14) . ?
C87 H60 1.0000 . ?
Cl5A C87A 1.776(11) . ?
Cl4 C87A 1.777(10) . ?
C87A H61 0.9900 . ?
C87A H62 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 N1 C10 109.9(3) . . ?
C7 N1 H1 125.0 . . ?
C10 N1 H1 125.0 . . ?
C13 N2 C16 110.5(3) . . ?
C13 N2 H2 124.8 . . ?
C16 N2 H2 124.8 . . ?
C11 N3 C23 118.2(3) . . ?
C12 N4 C28 118.0(3) . . ?
C35 N5 C38 110.5(3) . . ?
C35 N5 H3 124.8 . . ?
C38 N5 H3 124.8 . . ?
C44 N6 C41 110.1(3) . . ?
C44 N6 H4 124.9 . . ?
C41 N6 H4 124.9 . . ?
C39 N7 C51 118.6(3) . . ?
C40 N8 C56 119.2(3) . . ?
C63 N9 C66 110.3(3) . . ?
C63 N9 H5 124.8 . . ?
C66 N9 H5 124.8 . . ?
C69 N10 C72 109.6(3) . . ?
C69 N10 H6 125.2 . . ?
C72 N10 H6 125.2 . . ?
C67 N11 C79 118.5(3) . . ?
C68 N12 C84 119.1(3) . . ?
C2 C1 C6 120.6(5) . . ?
C2 C1 H7 119.7 . . ?
C6 C1 H7 119.7 . . ?
C3 C2 C1 121.2(5) . . ?
C3 C2 H8 119.4 . . ?
C1 C2 H8 119.4 . . ?
C2 C3 C4 118.3(5) . . ?
C2 C3 H9 120.8 . . ?
C4 C3 H9 120.8 . . ?
C5 C4 C3 121.0(5) . . ?
C5 C4 H10 119.5 . . ?
C3 C4 H10 119.5 . . ?
C4 C5 C6 120.8(4) . . ?
C4 C5 H11 119.6 . . ?
C6 C5 H11 119.6 . . ?
C5 C6 C1 118.0(4) . . ?
C5 C6 C7 122.0(4) . . ?
C1 C6 C7 120.0(4) . . ?
N1 C7 C8 107.1(3) . . ?
N1 C7 C6 123.0(3) . . ?
C8 C7 C6 129.8(3) . . ?
C7 C8 C9 107.9(3) . . ?
C7 C8 H12 126.0 . . ?
C9 C8 H12 126.0 . . ?
C10 C9 C8 108.1(3) . . ?
C10 C9 H13 125.9 . . ?
C8 C9 H13 125.9 . . ?
N1 C10 C9 106.9(3) . . ?
N1 C10 C11 120.6(3) . . ?
C9 C10 C11 132.2(3) . . ?
N3 C11 C12 120.5(3) . . ?
N3 C11 C10 115.8(3) . . ?
C12 C11 C10 123.6(3) . . ?
N4 C12 C11 121.1(3) . . ?
N4 C12 C13 115.2(3) . . ?
C11 C12 C13 123.7(3) . . ?
N2 C13 C14 107.0(3) . . ?
N2 C13 C12 120.4(3) . . ?
C14 C13 C12 132.2(3) . . ?
C13 C14 C15 107.7(3) . . ?
C13 C14 H14 126.2 . . ?
C15 C14 H14 126.2 . . ?
C16 C15 C14 108.1(3) . . ?
C16 C15 H15 125.9 . . ?
C14 C15 H15 125.9 . . ?
N2 C16 C15 106.8(3) . . ?
N2 C16 C17 123.4(3) . . ?
C15 C16 C17 129.8(4) . . ?
C22 C17 C18 117.8(4) . . ?
C22 C17 C16 121.3(4) . . ?
C18 C17 C16 120.8(4) . . ?
C19 C18 C17 120.5(4) . . ?
C19 C18 H16 119.8 . . ?
C17 C18 H16 119.8 . . ?
C18 C19 C20 121.2(4) . . ?
C18 C19 H17 119.4 . . ?
C20 C19 H17 119.4 . . ?
C21 C20 C19 118.8(4) . . ?
C21 C20 H18 120.6 . . ?
C19 C20 H18 120.6 . . ?
C20 C21 C22 121.1(4) . . ?
C20 C21 H19 119.4 . . ?
C22 C21 H19 119.4 . . ?
C21 C22 C17 120.5(4) . . ?
C21 C22 H20 119.7 . . ?
C17 C22 H20 119.7 . . ?
N3 C23 C28 121.0(3) . . ?
N3 C23 C24 119.6(4) . . ?
C28 C23 C24 119.4(4) . . ?
C25 C24 C23 119.6(4) . . ?
C25 C24 H21 120.2 . . ?
C23 C24 H21 120.2 . . ?
C24 C25 C26 120.6(4) . . ?
C24 C25 H22 119.7 . . ?
C26 C25 H22 119.7 . . ?
C27 C26 C25 121.2(4) . . ?
C27 C26 H23 119.4 . . ?
C25 C26 H23 119.4 . . ?
C26 C27 C28 119.5(4) . . ?
C26 C27 H24 120.2 . . ?
C28 C27 H24 120.2 . . ?
N4 C28 C23 120.6(3) . . ?
N4 C28 C27 119.6(4) . . ?
C23 C28 C27 119.7(4) . . ?
C30 C29 C34 120.6(4) . . ?
C30 C29 H25 119.7 . . ?
C34 C29 H25 119.7 . . ?
C31 C30 C29 120.0(5) . . ?
C31 C30 H26 120.0 . . ?
C29 C30 H26 120.0 . . ?
C32 C31 C30 119.9(4) . . ?
C32 C31 H27 120.0 . . ?
C30 C31 H27 120.0 . . ?
C31 C32 C33 121.3(5) . . ?
C31 C32 H28 119.4 . . ?
C33 C32 H28 119.4 . . ?
C34 C33 C32 119.1(5) . . ?
C34 C33 H29 120.4 . . ?
C32 C33 H29 120.4 . . ?
C33 C34 C29 119.0(4) . . ?
C33 C34 C35 120.0(4) . . ?
C29 C34 C35 120.9(4) . . ?
N5 C35 C36 106.9(3) . . ?
N5 C35 C34 123.1(3) . . ?
C36 C35 C34 130.0(4) . . ?
C35 C36 C37 108.4(3) . . ?
C35 C36 H30 125.8 . . ?
C37 C36 H30 125.8 . . ?
C38 C37 C36 107.9(3) . . ?
C38 C37 H31 126.0 . . ?
C36 C37 H31 126.0 . . ?
N5 C38 C37 106.3(3) . . ?
N5 C38 C39 120.0(3) . . ?
C37 C38 C39 133.5(3) . . ?
N7 C39 C38 116.2(3) . . ?
N7 C39 C40 120.2(3) . . ?
C38 C39 C40 123.5(3) . . ?
N8 C40 C41 116.7(3) . . ?
N8 C40 C39 120.4(3) . . ?
C41 C40 C39 122.9(3) . . ?
N6 C41 C42 106.7(3) . . ?
N6 C41 C40 120.3(3) . . ?
C42 C41 C40 132.3(3) . . ?
C41 C42 C43 108.2(3) . . ?
C41 C42 H32 125.9 . . ?
C43 C42 H32 125.9 . . ?
C44 C43 C42 107.6(3) . . ?
C44 C43 H33 126.2 . . ?
C42 C43 H33 126.2 . . ?
N6 C44 C43 107.2(3) . . ?
N6 C44 C45 122.6(3) . . ?
C43 C44 C45 130.1(3) . . ?
C46 C45 C50 118.8(4) . . ?
C46 C45 C44 121.9(3) . . ?
C50 C45 C44 119.4(4) . . ?
C47 C46 C45 120.9(4) . . ?
C47 C46 H34 119.6 . . ?
C45 C46 H34 119.6 . . ?
C46 C47 C48 119.5(4) . . ?
C46 C47 H35 120.2 . . ?
C48 C47 H35 120.2 . . ?
C49 C48 C47 120.0(4) . . ?
C49 C48 H36 120.0 . . ?
C47 C48 H36 120.0 . . ?
C48 C49 C50 120.9(4) . . ?
C48 C49 H37 119.6 . . ?
C50 C49 H37 119.6 . . ?
C49 C50 C45 119.9(4) . . ?
C49 C50 H38 120.1 . . ?
C45 C50 H38 120.1 . . ?
N7 C51 C56 120.8(3) . . ?
N7 C51 C52 120.1(4) . . ?
C56 C51 C52 119.1(4) . . ?
C53 C52 C51 119.8(4) . . ?
C53 C52 H39 120.1 . . ?
C51 C52 H39 120.1 . . ?
C52 C53 C54 120.7(4) . . ?
C52 C53 H40 119.7 . . ?
C54 C53 H40 119.7 . . ?
C55 C54 C53 120.6(4) . . ?
C55 C54 H41 119.7 . . ?
C53 C54 H41 119.7 . . ?
C54 C55 C56 119.8(4) . . ?
C54 C55 H42 120.1 . . ?
C56 C55 H42 120.1 . . ?
N8 C56 C55 120.0(4) . . ?
N8 C56 C51 120.1(3) . . ?
C55 C56 C51 119.8(4) . . ?
C62 C57 C58 120.6(4) . . ?
C62 C57 H43 119.7 . . ?
C58 C57 H43 119.7 . . ?
C59 C58 C57 120.1(4) . . ?
C59 C58 H44 120.0 . . ?
C57 C58 H44 120.0 . . ?
C58 C59 C60 120.2(4) . . ?
C58 C59 H45 119.9 . . ?
C60 C59 H45 119.9 . . ?
C59 C60 C61 120.3(4) . . ?
C59 C60 H46 119.8 . . ?
C61 C60 H46 119.8 . . ?
C62 C61 C60 120.0(4) . . ?
C62 C61 H47 120.0 . . ?
C60 C61 H47 120.0 . . ?
C61 C62 C57 118.8(3) . . ?
C61 C62 C63 121.5(3) . . ?
C57 C62 C63 119.6(3) . . ?
N9 C63 C64 107.4(3) . . ?
N9 C63 C62 123.4(3) . . ?
C64 C63 C62 129.1(3) . . ?
C63 C64 C65 107.9(3) . . ?
C63 C64 H48 126.1 . . ?
C65 C64 H48 126.1 . . ?
C66 C65 C64 107.7(3) . . ?
C66 C65 H49 126.1 . . ?
C64 C65 H49 126.1 . . ?
N9 C66 C65 106.6(3) . . ?
N9 C66 C67 120.4(3) . . ?
C65 C66 C67 132.3(3) . . ?
N11 C67 C68 120.8(3) . . ?
N11 C67 C66 116.7(3) . . ?
C68 C67 C66 122.3(3) . . ?
N12 C68 C67 120.4(3) . . ?
N12 C68 C69 117.0(3) . . ?
C67 C68 C69 122.6(3) . . ?
N10 C69 C70 107.6(3) . . ?
N10 C69 C68 120.8(3) . . ?
C70 C69 C68 131.5(4) . . ?
C69 C70 C71 107.4(4) . . ?
C69 C70 H63 126.3 . . ?
C71 C70 H63 126.3 . . ?
C72 C71 C70 108.4(3) . . ?
C72 C71 H64 125.8 . . ?
C70 C71 H64 125.8 . . ?
C71 C72 N10 107.0(4) . . ?
C71 C72 C73 130.9(4) . . ?
N10 C72 C73 122.0(4) . . ?
C74 C73 C78 117.7(5) . . ?
C74 C73 C72 122.7(4) . . ?
C78 C73 C72 119.7(4) . . ?
C75 C74 C73 120.6(5) . . ?
C75 C74 H50 119.7 . . ?
C73 C74 H50 119.7 . . ?
C74 C75 C76 121.9(7) . . ?
C74 C75 H51 119.0 . . ?
C76 C75 H51 119.0 . . ?
C77 C76 C75 118.1(6) . . ?
C77 C76 H52 120.9 . . ?
C75 C76 H52 120.9 . . ?
C76 C77 C78 121.1(6) . . ?
C76 C77 H53 119.4 . . ?
C78 C77 H53 119.4 . . ?
C77 C78 C73 120.6(5) . . ?
C77 C78 H54 119.7 . . ?
C73 C78 H54 119.7 . . ?
N11 C79 C80 120.0(3) . . ?
N11 C79 C84 120.5(3) . . ?
C80 C79 C84 119.4(3) . . ?
C81 C80 C79 119.9(4) . . ?
C81 C80 H55 120.1 . . ?
C79 C80 H55 120.1 . . ?
C80 C81 C82 120.5(4) . . ?
C80 C81 H56 119.7 . . ?
C82 C81 H56 119.7 . . ?
C83 C82 C81 121.2(4) . . ?
C83 C82 H57 119.4 . . ?
C81 C82 H57 119.4 . . ?
C82 C83 C84 119.7(4) . . ?
C82 C83 H58 120.2 . . ?
C84 C83 H58 120.2 . . ?
N12 C84 C79 120.3(3) . . ?
N12 C84 C83 120.3(3) . . ?
C79 C84 C83 119.3(4) . . ?
Cl1 C85 Cl2 113.2(5) . . ?
Cl1 C85 Cl3 111.9(6) . . ?
Cl2 C85 Cl3 107.5(6) . . ?
Cl1 C85 H59 108.1 . . ?
Cl2 C85 H59 108.1 . . ?
Cl3 C85 H59 108.1 . . ?
Cl6 C87 Cl7 111.1(9) . . ?
Cl6 C87 Cl5 111.2(8) . . ?
Cl7 C87 Cl5 110.3(9) . . ?
Cl6 C87 H60 108.0 . . ?
Cl7 C87 H60 108.0 . . ?
Cl5 C87 H60 108.0 . . ?
Cl5A C87A Cl4 111.1(6) . . ?
Cl5A C87A H61 109.4 . . ?
Cl4 C87A H61 109.4 . . ?
Cl5A C87A H62 109.4 . . ?
Cl4 C87A H62 109.4 . . ?
H61 C87A H62 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -3.2(10) . . . . ?
C1 C2 C3 C4 2.6(11) . . . . ?
C2 C3 C4 C5 -1.5(12) . . . . ?
C3 C4 C5 C6 1.0(11) . . . . ?
C4 C5 C6 C1 -1.5(8) . . . . ?
C4 C5 C6 C7 177.4(6) . . . . ?
C2 C1 C6 C5 2.6(8) . . . . ?
C2 C1 C6 C7 -176.4(5) . . . . ?
C10 N1 C7 C8 -1.1(4) . . . . ?
C10 N1 C7 C6 -179.7(3) . . . . ?
C5 C6 C7 N1 19.4(6) . . . . ?
C1 C6 C7 N1 -161.8(4) . . . . ?
C5 C6 C7 C8 -158.8(5) . . . . ?
C1 C6 C7 C8 20.0(7) . . . . ?
N1 C7 C8 C9 1.0(4) . . . . ?
C6 C7 C8 C9 179.4(4) . . . . ?
C7 C8 C9 C10 -0.6(5) . . . . ?
C7 N1 C10 C9 0.8(4) . . . . ?
C7 N1 C10 C11 175.0(3) . . . . ?
C8 C9 C10 N1 -0.1(4) . . . . ?
C8 C9 C10 C11 -173.4(4) . . . . ?
C23 N3 C11 C12 3.7(5) . . . . ?
C23 N3 C11 C10 -172.9(3) . . . . ?
N1 C10 C11 N3 -19.4(5) . . . . ?
C9 C10 C11 N3 153.1(4) . . . . ?
N1 C10 C11 C12 164.1(3) . . . . ?
C9 C10 C11 C12 -23.4(6) . . . . ?
C28 N4 C12 C11 4.1(5) . . . . ?
C28 N4 C12 C13 -174.5(3) . . . . ?
N3 C11 C12 N4 -7.7(5) . . . . ?
C10 C11 C12 N4 168.6(3) . . . . ?
N3 C11 C12 C13 170.8(3) . . . . ?
C10 C11 C12 C13 -12.9(6) . . . . ?
C16 N2 C13 C14 1.2(4) . . . . ?
C16 N2 C13 C12 173.9(3) . . . . ?
N4 C12 C13 N2 -29.9(5) . . . . ?
C11 C12 C13 N2 151.5(3) . . . . ?
N4 C12 C13 C14 140.6(4) . . . . ?
C11 C12 C13 C14 -38.0(6) . . . . ?
N2 C13 C14 C15 -1.1(4) . . . . ?
C12 C13 C14 C15 -172.5(4) . . . . ?
C13 C14 C15 C16 0.6(4) . . . . ?
C13 N2 C16 C15 -0.9(4) . . . . ?
C13 N2 C16 C17 178.9(3) . . . . ?
C14 C15 C16 N2 0.2(4) . . . . ?
C14 C15 C16 C17 -179.6(4) . . . . ?
N2 C16 C17 C22 9.9(6) . . . . ?
C15 C16 C17 C22 -170.4(4) . . . . ?
N2 C16 C17 C18 -172.6(4) . . . . ?
C15 C16 C17 C18 7.1(7) . . . . ?
C22 C17 C18 C19 -1.2(8) . . . . ?
C16 C17 C18 C19 -178.8(5) . . . . ?
C17 C18 C19 C20 -0.6(9) . . . . ?
C18 C19 C20 C21 2.1(8) . . . . ?
C19 C20 C21 C22 -1.7(7) . . . . ?
C20 C21 C22 C17 -0.1(7) . . . . ?
C18 C17 C22 C21 1.6(7) . . . . ?
C16 C17 C22 C21 179.2(4) . . . . ?
C11 N3 C23 C28 3.2(5) . . . . ?
C11 N3 C23 C24 -178.7(3) . . . . ?
N3 C23 C24 C25 -177.2(4) . . . . ?
C28 C23 C24 C25 0.9(6) . . . . ?
C23 C24 C25 C26 -0.4(6) . . . . ?
C24 C25 C26 C27 0.0(7) . . . . ?
C25 C26 C27 C28 -0.1(6) . . . . ?
C12 N4 C28 C23 2.8(5) . . . . ?
C12 N4 C28 C27 179.0(3) . . . . ?
N3 C23 C28 N4 -6.8(5) . . . . ?
C24 C23 C28 N4 175.2(3) . . . . ?
N3 C23 C28 C27 177.1(3) . . . . ?
C24 C23 C28 C27 -1.0(6) . . . . ?
C26 C27 C28 N4 -175.6(4) . . . . ?
C26 C27 C28 C23 0.6(6) . . . . ?
C34 C29 C30 C31 -0.8(6) . . . . ?
C29 C30 C31 C32 1.0(7) . . . . ?
C30 C31 C32 C33 -0.8(7) . . . . ?
C31 C32 C33 C34 0.3(7) . . . . ?
C32 C33 C34 C29 -0.1(6) . . . . ?
C32 C33 C34 C35 -178.1(4) . . . . ?
C30 C29 C34 C33 0.3(6) . . . . ?
C30 C29 C34 C35 178.3(4) . . . . ?
C38 N5 C35 C36 -1.1(4) . . . . ?
C38 N5 C35 C34 179.5(3) . . . . ?
C33 C34 C35 N5 -156.2(4) . . . . ?
C29 C34 C35 N5 25.8(5) . . . . ?
C33 C34 C35 C36 24.6(6) . . . . ?
C29 C34 C35 C36 -153.4(4) . . . . ?
N5 C35 C36 C37 0.7(4) . . . . ?
C34 C35 C36 C37 -180.0(4) . . . . ?
C35 C36 C37 C38 -0.1(4) . . . . ?
C35 N5 C38 C37 1.0(4) . . . . ?
C35 N5 C38 C39 176.3(3) . . . . ?
C36 C37 C38 N5 -0.5(4) . . . . ?
C36 C37 C38 C39 -174.9(4) . . . . ?
C51 N7 C39 C38 -176.4(3) . . . . ?
C51 N7 C39 C40 1.7(5) . . . . ?
N5 C38 C39 N7 -19.1(5) . . . . ?
C37 C38 C39 N7 154.7(4) . . . . ?
N5 C38 C39 C40 162.9(3) . . . . ?
C37 C38 C39 C40 -23.3(6) . . . . ?
C56 N8 C40 C41 -173.3(3) . . . . ?
C56 N8 C40 C39 6.2(5) . . . . ?
N7 C39 C40 N8 -7.6(5) . . . . ?
C38 C39 C40 N8 170.2(3) . . . . ?
N7 C39 C40 C41 171.7(3) . . . . ?
C38 C39 C40 C41 -10.4(5) . . . . ?
C44 N6 C41 C42 1.5(4) . . . . ?
C44 N6 C41 C40 173.2(3) . . . . ?
N8 C40 C41 N6 -30.6(5) . . . . ?
C39 C40 C41 N6 150.0(3) . . . . ?
N8 C40 C41 C42 138.7(4) . . . . ?
C39 C40 C41 C42 -40.8(6) . . . . ?
N6 C41 C42 C43 -1.2(4) . . . . ?
C40 C41 C42 C43 -171.5(4) . . . . ?
C41 C42 C43 C44 0.5(4) . . . . ?
C41 N6 C44 C43 -1.2(4) . . . . ?
C41 N6 C44 C45 179.0(3) . . . . ?
C42 C43 C44 N6 0.4(4) . . . . ?
C42 C43 C44 C45 -179.8(4) . . . . ?
N6 C44 C45 C46 28.1(5) . . . . ?
C43 C44 C45 C46 -151.6(4) . . . . ?
N6 C44 C45 C50 -153.7(3) . . . . ?
C43 C44 C45 C50 26.6(6) . . . . ?
C50 C45 C46 C47 0.3(6) . . . . ?
C44 C45 C46 C47 178.4(4) . . . . ?
C45 C46 C47 C48 -1.3(6) . . . . ?
C46 C47 C48 C49 1.1(6) . . . . ?
C47 C48 C49 C50 0.1(6) . . . . ?
C48 C49 C50 C45 -1.1(6) . . . . ?
C46 C45 C50 C49 0.9(5) . . . . ?
C44 C45 C50 C49 -177.3(3) . . . . ?
C39 N7 C51 C56 5.3(5) . . . . ?
C39 N7 C51 C52 -176.1(4) . . . . ?
N7 C51 C52 C53 -178.2(4) . . . . ?
C56 C51 C52 C53 0.4(6) . . . . ?
C51 C52 C53 C54 1.4(7) . . . . ?
C52 C53 C54 C55 -1.1(7) . . . . ?
C53 C54 C55 C56 -1.0(7) . . . . ?
C40 N8 C56 C55 177.9(4) . . . . ?
C40 N8 C56 C51 0.7(5) . . . . ?
C54 C55 C56 N8 -174.3(4) . . . . ?
C54 C55 C56 C51 2.9(6) . . . . ?
N7 C51 C56 N8 -6.7(6) . . . . ?
C52 C51 C56 N8 174.6(4) . . . . ?
N7 C51 C56 C55 176.1(4) . . . . ?
C52 C51 C56 C55 -2.6(6) . . . . ?
C62 C57 C58 C59 -2.1(6) . . . . ?
C57 C58 C59 C60 0.4(6) . . . . ?
C58 C59 C60 C61 0.5(7) . . . . ?
C59 C60 C61 C62 0.3(6) . . . . ?
C60 C61 C62 C57 -1.9(6) . . . . ?
C60 C61 C62 C63 173.9(4) . . . . ?
C58 C57 C62 C61 2.9(6) . . . . ?
C58 C57 C62 C63 -173.0(3) . . . . ?
C66 N9 C63 C64 -0.9(4) . . . . ?
C66 N9 C63 C62 -177.8(3) . . . . ?
C61 C62 C63 N9 29.8(5) . . . . ?
C57 C62 C63 N9 -154.5(3) . . . . ?
C61 C62 C63 C64 -146.4(4) . . . . ?
C57 C62 C63 C64 29.4(6) . . . . ?
N9 C63 C64 C65 0.2(4) . . . . ?
C62 C63 C64 C65 176.8(3) . . . . ?
C63 C64 C65 C66 0.6(4) . . . . ?
C63 N9 C66 C65 1.3(4) . . . . ?
C63 N9 C66 C67 173.1(3) . . . . ?
C64 C65 C66 N9 -1.2(4) . . . . ?
C64 C65 C66 C67 -171.5(4) . . . . ?
C79 N11 C67 C68 1.8(5) . . . . ?
C79 N11 C67 C66 -173.6(3) . . . . ?
N9 C66 C67 N11 -19.9(5) . . . . ?
C65 C66 C67 N11 149.3(4) . . . . ?
N9 C66 C67 C68 164.7(3) . . . . ?
C65 C66 C67 C68 -26.0(6) . . . . ?
C84 N12 C68 C67 5.8(5) . . . . ?
C84 N12 C68 C69 -173.8(3) . . . . ?
N11 C67 C68 N12 -7.1(5) . . . . ?
C66 C67 C68 N12 168.1(3) . . . . ?
N11 C67 C68 C69 172.4(3) . . . . ?
C66 C67 C68 C69 -12.4(5) . . . . ?
C72 N10 C69 C70 2.4(4) . . . . ?
C72 N10 C69 C68 178.2(3) . . . . ?
N12 C68 C69 N10 -37.1(5) . . . . ?
C67 C68 C69 N10 143.3(3) . . . . ?
N12 C68 C69 C70 137.5(4) . . . . ?
C67 C68 C69 C70 -42.1(6) . . . . ?
N10 C69 C70 C71 -1.6(4) . . . . ?
C68 C69 C70 C71 -176.7(4) . . . . ?
C69 C70 C71 C72 0.1(5) . . . . ?
C70 C71 C72 N10 1.3(4) . . . . ?
C70 C71 C72 C73 -175.1(4) . . . . ?
C69 N10 C72 C71 -2.3(4) . . . . ?
C69 N10 C72 C73 174.5(4) . . . . ?
C71 C72 C73 C74 -172.9(5) . . . . ?
N10 C72 C73 C74 11.1(7) . . . . ?
C71 C72 C73 C78 7.6(7) . . . . ?
N10 C72 C73 C78 -168.5(4) . . . . ?
C78 C73 C74 C75 0.2(10) . . . . ?
C72 C73 C74 C75 -179.4(7) . . . . ?
C73 C74 C75 C76 -0.4(14) . . . . ?
C74 C75 C76 C77 0.3(15) . . . . ?
C75 C76 C77 C78 0.1(13) . . . . ?
C76 C77 C78 C73 -0.3(11) . . . . ?
C74 C73 C78 C77 0.2(8) . . . . ?
C72 C73 C78 C77 179.8(5) . . . . ?
C67 N11 C79 C80 -178.2(3) . . . . ?
C67 N11 C79 C84 4.3(5) . . . . ?
N11 C79 C80 C81 -177.8(4) . . . . ?
C84 C79 C80 C81 -0.3(6) . . . . ?
C79 C80 C81 C82 0.1(6) . . . . ?
C80 C81 C82 C83 0.3(7) . . . . ?
C81 C82 C83 C84 -0.4(7) . . . . ?
C68 N12 C84 C79 0.3(5) . . . . ?
C68 N12 C84 C83 177.0(3) . . . . ?
N11 C79 C84 N12 -5.6(5) . . . . ?
C80 C79 C84 N12 176.9(3) . . . . ?
N11 C79 C84 C83 177.7(3) . . . . ?
C80 C79 C84 C83 0.2(5) . . . . ?
C82 C83 C84 N12 -176.5(4) . . . . ?
C82 C83 C84 C79 0.2(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 N12 0.88 2.17 3.024(4) 162.3 1_665
N2 H2 N7 0.88 2.34 3.215(5) 175.6 .
N5 H3 N4 0.88 2.36 3.237(4) 178.6 .
N6 H4 N11 0.88 2.15 3.029(4) 173.8 .
N9 H5 N8 0.88 2.11 2.975(5) 166.7 .
N9 H5 N6 0.88 2.69 3.248(4) 122.7 .
N10 H6 N3 0.88 2.14 3.009(4) 169.7 1_445

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        65.00
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.082
####################################################################### 
# 
# 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_ydkr_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1871611'
_audit_update_record             
;
2018-10-05 deposited with the CCDC.
2018-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H36 N4 O2'
_chemical_formula_sum            'C36 H36 N4 O2'
_chemical_formula_weight         556.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0041 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0135 0.0075 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0078 0.0041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   10.3008(4)
_cell_length_b                   16.7186(6)
_cell_length_c                   17.2236(7)
_cell_angle_alpha                90
_cell_angle_beta                 101.837(3)
_cell_angle_gamma                90
_cell_volume                     2903.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    15697
_cell_measurement_theta_min      1.887
_cell_measurement_theta_max      27.943

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.097
_shelx_estimated_absorpt_T_min   0.998
_shelx_estimated_absorpt_T_max   0.999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.78192
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_detector_area_resol_mean 29
_diffrn_reflns_number            15697
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.887
_diffrn_reflns_theta_max         27.943
_diffrn_reflns_theta_full        27.943
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5209
_reflns_number_gt                3095
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1711P)²+0.0790P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5209
_refine_ls_number_parameters     410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.0841
_refine_ls_wR_factor_ref         0.2823
_refine_ls_wR_factor_gt          0.2127
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6814(3) 0.3529(2) 0.1124(2) 0.0373(9) Uani 1 1 d . . . . .
H1 H 0.6082 0.3208 0.1189 0.045 Uiso 1 1 calc R U . . .
C2 C 0.7251(4) 0.3495(2) 0.0416(2) 0.0401(9) Uani 1 1 d . . . . .
H2 H 0.6823 0.3154 0.0001 0.048 Uiso 1 1 calc R U . . .
C3 C 0.8310(3) 0.3959(2) 0.0315(2) 0.0396(9) Uani 1 1 d . . . . .
C4 C 0.8921(4) 0.4472(2) 0.0928(2) 0.0425(10) Uani 1 1 d . . . . .
H3 H 0.9638 0.4803 0.0859 0.051 Uiso 1 1 calc R U . . .
C5 C 0.8485(3) 0.4494(2) 0.1625(2) 0.0388(9) Uani 1 1 d . . . . .
H4 H 0.8917 0.4839 0.2036 0.047 Uiso 1 1 calc R U . . .
C6 C 0.7431(3) 0.4030(2) 0.1752(2) 0.0342(8) Uani 1 1 d . . . . .
C7 C 0.6947(3) 0.4047(2) 0.2486(2) 0.0343(8) Uani 1 1 d . . . . .
C8 C 0.5828(3) 0.3712(2) 0.2688(2) 0.0359(9) Uani 1 1 d . . . . .
H5 H 0.5185 0.3392 0.2352 0.043 Uiso 1 1 calc R U . . .
C9 C 0.5806(3) 0.3926(2) 0.3475(2) 0.0367(9) Uani 1 1 d . . . . .
H6 H 0.5148 0.3779 0.3763 0.044 Uiso 1 1 calc R U . . .
C10 C 0.6921(3) 0.4394(2) 0.3757(2) 0.0354(8) Uani 1 1 d . . . . .
C11 C 0.7433(3) 0.4847(2) 0.4476(2) 0.0349(8) Uani 1 1 d . . . . .
C12 C 0.8857(3) 0.5887(2) 0.5006(2) 0.0349(8) Uani 1 1 d . . . . .
C13 C 0.9898(3) 0.6413(2) 0.4956(2) 0.0376(9) Uani 1 1 d . . . . .
H7 H 1.0302 0.6400 0.4507 0.045 Uiso 1 1 calc R U . . .
C14 C 1.0326(4) 0.6945(2) 0.5560(2) 0.0435(9) Uani 1 1 d . . . . .
H8 H 1.1040 0.7296 0.5531 0.052 Uiso 1 1 calc R U . . .
C15 C 0.9727(4) 0.6980(2) 0.6214(2) 0.0458(10) Uani 1 1 d . . . . .
H9 H 1.0028 0.7361 0.6621 0.055 Uiso 1 1 calc R U . . .
C16 C 0.8713(4) 0.6474(2) 0.6281(2) 0.0458(10) Uani 1 1 d . . . . .
H10 H 0.8309 0.6504 0.6728 0.055 Uiso 1 1 calc R U . . .
C17 C 0.8270(3) 0.5904(2) 0.5673(2) 0.0367(9) Uani 1 1 d . . . . .
C18 C 0.6974(3) 0.4809(2) 0.5203(2) 0.0332(8) Uani 1 1 d . . . . .
C19 C 0.6130(3) 0.4180(2) 0.5438(2) 0.0348(8) Uani 1 1 d . . . . .
C20 C 0.5829(3) 0.3380(2) 0.5232(2) 0.0385(9) Uani 1 1 d . . . . .
H11 H 0.6070 0.3094 0.4806 0.046 Uiso 1 1 calc R U . . .
C21 C 0.5101(3) 0.3081(2) 0.5777(2) 0.0377(9) Uani 1 1 d . . . . .
H12 H 0.4747 0.2556 0.5775 0.045 Uiso 1 1 calc R U . . .
C22 C 0.4985(3) 0.36776(19) 0.6317(2) 0.0346(8) Uani 1 1 d . . . . .
C23 C 0.4387(3) 0.3693(2) 0.7005(2) 0.0345(8) Uani 1 1 d . . . . .
C24 C 0.3270(3) 0.3218(2) 0.7042(2) 0.0355(8) Uani 1 1 d . . . . .
H13 H 0.2887 0.2900 0.6597 0.043 Uiso 1 1 calc R U . . .
C25 C 0.2724(3) 0.3205(2) 0.7702(2) 0.0373(9) Uani 1 1 d . . . . .
H14 H 0.1983 0.2870 0.7714 0.045 Uiso 1 1 calc R U . . .
C26 C 0.3248(3) 0.3680(2) 0.8360(2) 0.0321(8) Uani 1 1 d . . . . .
C27 C 0.4338(3) 0.4164(2) 0.8332(2) 0.0378(9) Uani 1 1 d . . . . .
H15 H 0.4704 0.4492 0.8773 0.045 Uiso 1 1 calc R U . . .
C28 C 0.4886(3) 0.41698(19) 0.7666(2) 0.0338(8) Uani 1 1 d . . . . .
H16 H 0.5625 0.4507 0.7656 0.041 Uiso 1 1 calc R U . . .
C29 C 0.8279(4) 0.3433(3) -0.0977(2) 0.0560(12) Uani 1 1 d . . . . .
H55 H 0.7299 0.3474 -0.1109 0.067 Uiso 0.799(9) 1 calc R U P A 1
H56 H 0.8527 0.2876 -0.0818 0.067 Uiso 0.799(9) 1 calc R U P A 1
H57 H 0.7418 0.3656 -0.1255 0.067 Uiso 0.201(9) 1 calc R U P A 2
H58 H 0.8083 0.2928 -0.0724 0.067 Uiso 0.201(9) 1 calc R U P A 2
C30 C 0.8875(5) 0.3683(4) -0.1690(4) 0.0397(15) Uani 0.799(9) 1 d . . P A 1
H39 H 0.8602 0.4236 -0.1853 0.048 Uiso 0.799(9) 1 calc R U P A 1
H40 H 0.9856 0.3665 -0.1544 0.048 Uiso 0.799(9) 1 calc R U P A 1
C31 C 0.8382(5) 0.3111(3) -0.2364(3) 0.0421(15) Uani 0.799(9) 1 d . . P A 1
H41 H 0.8689 0.2564 -0.2200 0.051 Uiso 0.799(9) 1 calc R U P A 1
H42 H 0.7400 0.3109 -0.2480 0.051 Uiso 0.799(9) 1 calc R U P A 1
C32 C 0.8859(5) 0.3332(4) -0.3105(3) 0.0465(15) Uani 0.799(9) 1 d . . P A 1
H49 H 0.8496 0.3854 -0.3295 0.070 Uiso 0.799(9) 1 calc R U P A 1
H50 H 0.8562 0.2927 -0.3515 0.070 Uiso 0.799(9) 1 calc R U P A 1
H51 H 0.9830 0.3357 -0.2988 0.070 Uiso 0.799(9) 1 calc R U P A 1
C33 C 0.3266(3) 0.4012(2) 0.9706(2) 0.0393(9) Uani 1 1 d . . . . .
H28 H 0.3247 0.4598 0.9619 0.047 Uiso 1 1 calc R U . . .
H29 H 0.4202 0.3841 0.9869 0.047 Uiso 1 1 calc R U . . .
C34 C 0.2508(4) 0.3801(2) 1.0344(2) 0.0396(9) Uani 1 1 d . . . . .
H30 H 0.1556 0.3921 1.0150 0.047 Uiso 1 1 calc R U . . .
H31 H 0.2595 0.3220 1.0455 0.047 Uiso 1 1 calc R U . . .
C35 C 0.3006(4) 0.4256(2) 1.1099(2) 0.0412(9) Uani 1 1 d . . . . .
H32 H 0.2801 0.4831 1.1003 0.049 Uiso 1 1 calc R U . . .
H33 H 0.3983 0.4201 1.1248 0.049 Uiso 1 1 calc R U . . .
C36 C 0.2406(4) 0.3974(2) 1.1787(2) 0.0456(10) Uani 1 1 d . . . . .
H34 H 0.1446 0.4066 1.1662 0.068 Uiso 1 1 calc R U . . .
H35 H 0.2803 0.4272 1.2267 0.068 Uiso 1 1 calc R U . . .
H36 H 0.2581 0.3401 1.1876 0.068 Uiso 1 1 calc R U . . .
O1 O 0.8818(2) 0.39755(16) -0.03559(15) 0.0467(7) Uani 1 1 d . . . . .
O2 O 0.2649(2) 0.36106(14) 0.89929(14) 0.0380(6) Uani 1 1 d . . . . .
N1 N 0.7584(3) 0.44540(17) 0.31417(17) 0.0361(7) Uani 1 1 d . . . . .
H17 H 0.8328 0.4722 0.3168 0.043 Uiso 1 1 calc R U . . .
N2 N 0.8393(3) 0.53630(17) 0.43975(17) 0.0370(7) Uani 1 1 d . . . . .
N3 N 0.7346(3) 0.53532(18) 0.57657(17) 0.0398(8) Uani 1 1 d . . . . .
N4 N 0.5623(3) 0.43291(16) 0.60985(16) 0.0344(7) Uani 1 1 d . . . . .
H18 H 0.5700 0.4789 0.6352 0.041 Uiso 1 1 calc R U . . .
C37 C 0.921(2) 0.3907(17) -0.2890(17) 0.064(8) Uani 0.201(9) 1 d . . P A 2
H52 H 1.0141 0.4072 -0.2759 0.095 Uiso 0.201(9) 1 calc R U P A 2
H53 H 0.8716 0.4263 -0.3297 0.095 Uiso 0.201(9) 1 calc R U P A 2
H54 H 0.9150 0.3356 -0.3090 0.095 Uiso 0.201(9) 1 calc R U P A 2
C38 C 0.866(3) 0.3948(15) -0.2197(18) 0.065(8) Uani 0.201(9) 1 d . . P A 2
H43 H 0.7679 0.3963 -0.2358 0.078 Uiso 0.201(9) 1 calc R U P A 2
H44 H 0.8951 0.4450 -0.1910 0.078 Uiso 0.201(9) 1 calc R U P A 2
C39 C 0.907(2) 0.3216(15) -0.1616(11) 0.041(6) Uani 0.201(9) 1 d . . P A 2
H45 H 0.8789 0.2698 -0.1875 0.049 Uiso 0.201(9) 1 calc R U P A 2
H46 H 1.0042 0.3205 -0.1399 0.049 Uiso 0.201(9) 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
C1 C2 1.386(5) . ?
C1 C6 1.412(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.378(5) . ?
C2 H2 0.9500 . ?
C3 O1 1.363(4) . ?
C3 C4 1.405(5) . ?
C4 C5 1.365(5) . ?
C4 H3 0.9500 . ?
C5 C6 1.387(5) . ?
C5 H4 0.9500 . ?
C6 C7 1.452(5) . ?
C7 N1 1.365(4) . ?
C7 C8 1.389(5) . ?
C8 C9 1.406(5) . ?
C8 H5 0.9500 . ?
C9 C10 1.392(5) . ?
C9 H6 0.9500 . ?
C10 N1 1.377(4) . ?
C10 C11 1.455(5) . ?
C11 N2 1.341(4) . ?
C11 C18 1.429(5) . ?
C12 N2 1.373(4) . ?
C12 C13 1.403(5) . ?
C12 C17 1.404(5) . ?
C13 C14 1.372(5) . ?
C13 H7 0.9500 . ?
C14 C15 1.393(5) . ?
C14 H8 0.9500 . ?
C15 C16 1.367(5) . ?
C15 H9 0.9500 . ?
C16 C17 1.420(5) . ?
C16 H10 0.9500 . ?
C17 N3 1.358(4) . ?
C18 N3 1.327(4) . ?
C18 C19 1.472(5) . ?
C19 N4 1.369(4) . ?
C19 C20 1.403(5) . ?
C20 C21 1.409(5) . ?
C20 H11 0.9500 . ?
C21 C22 1.385(5) . ?
C21 H12 0.9500 . ?
C22 N4 1.364(4) . ?
C22 C23 1.444(5) . ?
C23 C28 1.398(5) . ?
C23 C24 1.410(5) . ?
C24 C25 1.369(5) . ?
C24 H13 0.9500 . ?
C25 C26 1.399(5) . ?
C25 H14 0.9500 . ?
C26 O2 1.363(4) . ?
C26 C27 1.392(5) . ?
C27 C28 1.379(5) . ?
C27 H15 0.9500 . ?
C28 H16 0.9500 . ?
C29 O1 1.425(5) . ?
C29 C30 1.540(7) . ?
C29 C39 1.55(2) . ?
C29 H55 0.9900 . ?
C29 H56 0.9900 . ?
C29 H57 0.9900 . ?
C29 H58 0.9900 . ?
C30 C31 1.509(7) . ?
C30 H39 0.9900 . ?
C30 H40 0.9900 . ?
C31 C32 1.504(7) . ?
C31 H41 0.9900 . ?
C31 H42 0.9900 . ?
C32 H49 0.9800 . ?
C32 H50 0.9800 . ?
C32 H51 0.9800 . ?
C33 O2 1.429(4) . ?
C33 C34 1.515(5) . ?
C33 H28 0.9900 . ?
C33 H29 0.9900 . ?
C34 C35 1.503(5) . ?
C34 H30 0.9900 . ?
C34 H31 0.9900 . ?
C35 C36 1.520(5) . ?
C35 H32 0.9900 . ?
C35 H33 0.9900 . ?
C36 H34 0.9800 . ?
C36 H35 0.9800 . ?
C36 H36 0.9800 . ?
N1 H17 0.8800 . ?
N4 H18 0.8800 . ?
C37 C38 1.42(3) . ?
C37 H52 0.9800 . ?
C37 H53 0.9800 . ?
C37 H54 0.9800 . ?
C38 C39 1.58(3) . ?
C38 H43 0.9900 . ?
C38 H44 0.9900 . ?
C39 H45 0.9900 . ?
C39 H46 0.9900 . ?

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
C2 C1 C6 121.4(3) . . ?
C2 C1 H1 119.3 . . ?
C6 C1 H1 119.3 . . ?
C3 C2 C1 119.8(4) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
O1 C3 C2 124.7(4) . . ?
O1 C3 C4 115.7(3) . . ?
C2 C3 C4 119.5(3) . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H3 120.0 . . ?
C3 C4 H3 120.0 . . ?
C4 C5 C6 122.2(4) . . ?
C4 C5 H4 118.9 . . ?
C6 C5 H4 118.9 . . ?
C5 C6 C1 117.1(3) . . ?
C5 C6 C7 123.1(3) . . ?
C1 C6 C7 119.8(3) . . ?
N1 C7 C8 106.1(3) . . ?
N1 C7 C6 122.5(3) . . ?
C8 C7 C6 131.4(3) . . ?
C7 C8 C9 108.5(3) . . ?
C7 C8 H5 125.8 . . ?
C9 C8 H5 125.8 . . ?
C10 C9 C8 107.7(3) . . ?
C10 C9 H6 126.2 . . ?
C8 C9 H6 126.2 . . ?
N1 C10 C9 106.1(3) . . ?
N1 C10 C11 117.8(3) . . ?
C9 C10 C11 135.9(3) . . ?
N2 C11 C18 120.0(3) . . ?
N2 C11 C10 113.3(3) . . ?
C18 C11 C10 126.6(3) . . ?
N2 C12 C13 120.2(3) . . ?
N2 C12 C17 119.8(3) . . ?
C13 C12 C17 120.0(3) . . ?
C14 C13 C12 119.4(3) . . ?
C14 C13 H7 120.3 . . ?
C12 C13 H7 120.3 . . ?
C13 C14 C15 120.9(3) . . ?
C13 C14 H8 119.5 . . ?
C15 C14 H8 119.5 . . ?
C16 C15 C14 121.0(4) . . ?
C16 C15 H9 119.5 . . ?
C14 C15 H9 119.5 . . ?
C15 C16 C17 119.3(4) . . ?
C15 C16 H10 120.4 . . ?
C17 C16 H10 120.4 . . ?
N3 C17 C12 120.8(3) . . ?
N3 C17 C16 119.7(3) . . ?
C12 C17 C16 119.4(3) . . ?
N3 C18 C11 120.8(3) . . ?
N3 C18 C19 112.8(3) . . ?
C11 C18 C19 126.3(3) . . ?
N4 C19 C20 106.3(3) . . ?
N4 C19 C18 116.5(3) . . ?
C20 C19 C18 136.4(3) . . ?
C19 C20 C21 106.9(3) . . ?
C19 C20 H11 126.6 . . ?
C21 C20 H11 126.6 . . ?
C22 C21 C20 108.8(3) . . ?
C22 C21 H12 125.6 . . ?
C20 C21 H12 125.6 . . ?
N4 C22 C21 106.1(3) . . ?
N4 C22 C23 121.5(3) . . ?
C21 C22 C23 132.3(3) . . ?
C28 C23 C24 116.8(3) . . ?
C28 C23 C22 122.1(3) . . ?
C24 C23 C22 121.1(3) . . ?
C25 C24 C23 121.7(3) . . ?
C25 C24 H13 119.2 . . ?
C23 C24 H13 119.2 . . ?
C24 C25 C26 120.5(3) . . ?
C24 C25 H14 119.7 . . ?
C26 C25 H14 119.7 . . ?
O2 C26 C27 125.3(3) . . ?
O2 C26 C25 115.9(3) . . ?
C27 C26 C25 118.8(3) . . ?
C28 C27 C26 120.2(3) . . ?
C28 C27 H15 119.9 . . ?
C26 C27 H15 119.9 . . ?
C27 C28 C23 121.9(3) . . ?
C27 C28 H16 119.0 . . ?
C23 C28 H16 119.0 . . ?
O1 C29 C30 105.6(4) . . ?
O1 C29 C39 120.1(9) . . ?
O1 C29 H55 110.6 . . ?
C30 C29 H55 110.6 . . ?
O1 C29 H56 110.6 . . ?
C30 C29 H56 110.6 . . ?
H55 C29 H56 108.8 . . ?
O1 C29 H57 107.3 . . ?
C39 C29 H57 107.3 . . ?
O1 C29 H58 107.3 . . ?
C39 C29 H58 107.3 . . ?
H57 C29 H58 106.9 . . ?
C31 C30 C29 108.4(4) . . ?
C31 C30 H39 110.0 . . ?
C29 C30 H39 110.0 . . ?
C31 C30 H40 110.0 . . ?
C29 C30 H40 110.0 . . ?
H39 C30 H40 108.4 . . ?
C32 C31 C30 112.4(4) . . ?
C32 C31 H41 109.1 . . ?
C30 C31 H41 109.1 . . ?
C32 C31 H42 109.1 . . ?
C30 C31 H42 109.1 . . ?
H41 C31 H42 107.9 . . ?
C31 C32 H49 109.5 . . ?
C31 C32 H50 109.5 . . ?
H49 C32 H50 109.5 . . ?
C31 C32 H51 109.5 . . ?
H49 C32 H51 109.5 . . ?
H50 C32 H51 109.5 . . ?
O2 C33 C34 108.1(3) . . ?
O2 C33 H28 110.1 . . ?
C34 C33 H28 110.1 . . ?
O2 C33 H29 110.1 . . ?
C34 C33 H29 110.1 . . ?
H28 C33 H29 108.4 . . ?
C35 C34 C33 112.0(3) . . ?
C35 C34 H30 109.2 . . ?
C33 C34 H30 109.2 . . ?
C35 C34 H31 109.2 . . ?
C33 C34 H31 109.2 . . ?
H30 C34 H31 107.9 . . ?
C34 C35 C36 113.3(3) . . ?
C34 C35 H32 108.9 . . ?
C36 C35 H32 108.9 . . ?
C34 C35 H33 108.9 . . ?
C36 C35 H33 108.9 . . ?
H32 C35 H33 107.7 . . ?
C35 C36 H34 109.5 . . ?
C35 C36 H35 109.5 . . ?
H34 C36 H35 109.5 . . ?
C35 C36 H36 109.5 . . ?
H34 C36 H36 109.5 . . ?
H35 C36 H36 109.5 . . ?
C3 O1 C29 117.7(3) . . ?
C26 O2 C33 116.9(3) . . ?
C7 N1 C10 111.7(3) . . ?
C7 N1 H17 124.2 . . ?
C10 N1 H17 124.2 . . ?
C11 N2 C12 118.8(3) . . ?
C18 N3 C17 118.9(3) . . ?
C22 N4 C19 111.8(3) . . ?
C22 N4 H18 124.1 . . ?
C19 N4 H18 124.1 . . ?
C38 C37 H52 109.5 . . ?
C38 C37 H53 109.5 . . ?
H52 C37 H53 109.5 . . ?
C38 C37 H54 109.5 . . ?
H52 C37 H54 109.5 . . ?
H53 C37 H54 109.5 . . ?
C37 C38 C39 112.9(19) . . ?
C37 C38 H43 109.0 . . ?
C39 C38 H43 109.0 . . ?
C37 C38 H44 109.0 . . ?
C39 C38 H44 109.0 . . ?
H43 C38 H44 107.8 . . ?
C29 C39 C38 98.8(16) . . ?
C29 C39 H45 112.0 . . ?
C38 C39 H45 112.0 . . ?
C29 C39 H46 112.0 . . ?
C38 C39 H46 112.0 . . ?
H45 C39 H46 109.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.1(5) . . . . ?
C1 C2 C3 O1 -179.7(3) . . . . ?
C1 C2 C3 C4 -1.0(5) . . . . ?
O1 C3 C4 C5 -179.7(3) . . . . ?
C2 C3 C4 C5 1.5(5) . . . . ?
C3 C4 C5 C6 -0.8(5) . . . . ?
C4 C5 C6 C1 -0.3(5) . . . . ?
C4 C5 C6 C7 -179.7(3) . . . . ?
C2 C1 C6 C5 0.8(5) . . . . ?
C2 C1 C6 C7 -179.8(3) . . . . ?
C5 C6 C7 N1 -7.5(5) . . . . ?
C1 C6 C7 N1 173.1(3) . . . . ?
C5 C6 C7 C8 170.9(3) . . . . ?
C1 C6 C7 C8 -8.6(5) . . . . ?
N1 C7 C8 C9 0.1(4) . . . . ?
C6 C7 C8 C9 -178.5(3) . . . . ?
C7 C8 C9 C10 -0.2(4) . . . . ?
C8 C9 C10 N1 0.2(4) . . . . ?
C8 C9 C10 C11 174.4(4) . . . . ?
N1 C10 C11 N2 9.3(4) . . . . ?
C9 C10 C11 N2 -164.4(4) . . . . ?
N1 C10 C11 C18 -173.6(3) . . . . ?
C9 C10 C11 C18 12.7(6) . . . . ?
N2 C12 C13 C14 178.4(3) . . . . ?
C17 C12 C13 C14 -0.5(5) . . . . ?
C12 C13 C14 C15 -1.1(5) . . . . ?
C13 C14 C15 C16 1.2(6) . . . . ?
C14 C15 C16 C17 0.2(6) . . . . ?
N2 C12 C17 N3 7.1(5) . . . . ?
C13 C12 C17 N3 -174.0(3) . . . . ?
N2 C12 C17 C16 -177.0(3) . . . . ?
C13 C12 C17 C16 1.9(5) . . . . ?
C15 C16 C17 N3 174.2(4) . . . . ?
C15 C16 C17 C12 -1.8(6) . . . . ?
N2 C11 C18 N3 9.7(5) . . . . ?
C10 C11 C18 N3 -167.3(3) . . . . ?
N2 C11 C18 C19 -167.3(3) . . . . ?
C10 C11 C18 C19 15.7(5) . . . . ?
N3 C18 C19 N4 13.6(4) . . . . ?
C11 C18 C19 N4 -169.3(3) . . . . ?
N3 C18 C19 C20 -154.5(4) . . . . ?
C11 C18 C19 C20 22.6(6) . . . . ?
N4 C19 C20 C21 1.8(4) . . . . ?
C18 C19 C20 C21 170.7(4) . . . . ?
C19 C20 C21 C22 -1.4(4) . . . . ?
C20 C21 C22 N4 0.4(4) . . . . ?
C20 C21 C22 C23 -177.7(3) . . . . ?
N4 C22 C23 C28 -30.0(5) . . . . ?
C21 C22 C23 C28 148.0(4) . . . . ?
N4 C22 C23 C24 150.6(3) . . . . ?
C21 C22 C23 C24 -31.5(6) . . . . ?
C28 C23 C24 C25 -2.0(5) . . . . ?
C22 C23 C24 C25 177.5(3) . . . . ?
C23 C24 C25 C26 1.3(5) . . . . ?
C24 C25 C26 O2 -178.7(3) . . . . ?
C24 C25 C26 C27 -0.2(5) . . . . ?
O2 C26 C27 C28 178.1(3) . . . . ?
C25 C26 C27 C28 -0.2(5) . . . . ?
C26 C27 C28 C23 -0.5(5) . . . . ?
C24 C23 C28 C27 1.5(5) . . . . ?
C22 C23 C28 C27 -177.9(3) . . . . ?
O1 C29 C30 C31 178.0(4) . . . . ?
C29 C30 C31 C32 177.1(4) . . . . ?
O2 C33 C34 C35 -174.7(3) . . . . ?
C33 C34 C35 C36 -171.7(3) . . . . ?
C2 C3 O1 C29 -4.7(5) . . . . ?
C4 C3 O1 C29 176.6(3) . . . . ?
C30 C29 O1 C3 171.1(3) . . . . ?
C39 C29 O1 C3 -159.7(10) . . . . ?
C27 C26 O2 C33 -6.0(5) . . . . ?
C25 C26 O2 C33 172.5(3) . . . . ?
C34 C33 O2 C26 -175.4(3) . . . . ?
C8 C7 N1 C10 0.0(4) . . . . ?
C6 C7 N1 C10 178.8(3) . . . . ?
C9 C10 N1 C7 -0.2(4) . . . . ?
C11 C10 N1 C7 -175.6(3) . . . . ?
C18 C11 N2 C12 -4.3(5) . . . . ?
C10 C11 N2 C12 173.0(3) . . . . ?
C13 C12 N2 C11 177.4(3) . . . . ?
C17 C12 N2 C11 -3.7(5) . . . . ?
C11 C18 N3 C17 -6.2(5) . . . . ?
C19 C18 N3 C17 171.1(3) . . . . ?
C12 C17 N3 C18 -2.0(5) . . . . ?
C16 C17 N3 C18 -177.9(3) . . . . ?
C21 C22 N4 C19 0.7(4) . . . . ?
C23 C22 N4 C19 179.1(3) . . . . ?
C20 C19 N4 C22 -1.6(4) . . . . ?
C18 C19 N4 C22 -173.0(3) . . . . ?
O1 C29 C39 C38 -84.5(15) . . . . ?
C37 C38 C39 C29 -178(2) . . . . ?

_refine_diff_density_max         0.586
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.084

