# Electronic Supplementary Material (ESI) for ChemComm.
# 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_ccx073t1
_database_code_depnum_ccdc_archive 'CCDC 1528553'
_audit_update_record             
;
2017-01-19 deposited with the CCDC.
2018-05-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H13 N3 O'
_chemical_formula_weight         251.28

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   12.9903(2)
_cell_length_b                   7.8379(1)
_cell_length_c                   13.2745(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.935(8)
_cell_angle_gamma                90.00
_cell_volume                     1225.58(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    1888
_cell_measurement_theta_min      6.70
_cell_measurement_theta_max      68.24

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             528
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8708
_exptl_absorpt_correction_T_max  0.9195
_exptl_absorpt_process_details   'CrystalClear Expert 2.1 43b(Rigaku, 2013)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  'Rigaku RAXIS Rapid'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9942
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         6.70
_diffrn_reflns_theta_max         68.24
_reflns_number_total             2216
_reflns_number_gt                1888
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear Expert 2.1 43b(Rigaku, 2013)'
_computing_cell_refinement       'CrystalClear Expert 2.1 43b(Rigaku, 2013)'
_computing_data_reduction        'CrystalClear Expert 2.1 43b(Rigaku, 2013)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_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)+(0.0722P)²+0.1973P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0079(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2216
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.1084
_refine_ls_wR_factor_gt          0.1015
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.004
_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 0.34278(9) 0.41506(15) 0.70333(10) 0.0235(3) Uani 1 1 d . . .
C2 C 0.30283(10) 0.27234(15) 0.62443(10) 0.0235(3) Uani 1 1 d . . .
N3 N 0.18851(8) 0.23715(13) 0.57781(8) 0.0249(3) Uani 1 1 d . . .
C4 C 0.11114(10) 0.32544(15) 0.60618(10) 0.0235(3) Uani 1 1 d . . .
N5 N 0.00327(8) 0.27447(13) 0.55673(9) 0.0285(3) Uani 1 1 d . . .
C6 C -0.07183(10) 0.35770(17) 0.58289(11) 0.0306(3) Uani 1 1 d . . .
H6 H -0.1492 0.3238 0.5478 0.037 Uiso 1 1 calc R . .
C7 C -0.04301(10) 0.49083(17) 0.65852(11) 0.0308(3) Uani 1 1 d . . .
H7 H -0.0991 0.5455 0.6753 0.037 Uiso 1 1 calc R . .
C8 C 0.06881(10) 0.54233(16) 0.70885(11) 0.0275(3) Uani 1 1 d . . .
H8 H 0.0904 0.6335 0.7608 0.033 Uiso 1 1 calc R . .
C9 C 0.15055(10) 0.46029(15) 0.68338(10) 0.0233(3) Uani 1 1 d . . .
C10 C 0.26855(10) 0.50721(15) 0.73056(10) 0.0232(3) Uani 1 1 d . . .
N11 N 0.45644(9) 0.44406(15) 0.74360(10) 0.0312(3) Uani 1 1 d . . .
O12 O 0.37015(7) 0.18916(11) 0.59999(7) 0.0299(3) Uani 1 1 d . . .
C13 C 0.14628(11) 0.10084(17) 0.49411(11) 0.0361(3) Uani 1 1 d . . .
H13A H 0.2102 0.0485 0.4848 0.054 Uiso 1 1 calc R . .
H13B H 0.0930 0.1491 0.4231 0.054 Uiso 1 1 calc R . .
H13C H 0.1075 0.0141 0.5186 0.054 Uiso 1 1 calc R . .
C14 C 0.30686(9) 0.65755(15) 0.80642(10) 0.0231(3) Uani 1 1 d . . .
C15 C 0.28264(10) 0.82163(16) 0.76268(11) 0.0283(3) Uani 1 1 d . . .
H15 H 0.2449 0.8373 0.6845 0.034 Uiso 1 1 calc R . .
C16 C 0.31339(10) 0.96276(16) 0.83255(11) 0.0308(3) Uani 1 1 d . . .
H16 H 0.2970 1.0744 0.8021 0.037 Uiso 1 1 calc R . .
C17 C 0.36777(10) 0.94086(17) 0.94638(11) 0.0310(3) Uani 1 1 d . . .
H17 H 0.3875 1.0373 0.9942 0.037 Uiso 1 1 calc R . .
C18 C 0.39332(10) 0.77863(18) 0.99047(11) 0.0319(3) Uani 1 1 d . . .
H18 H 0.4315 0.7638 1.0686 0.038 Uiso 1 1 calc R . .
C19 C 0.36347(10) 0.63679(17) 0.92110(10) 0.0274(3) Uani 1 1 d . . .
H19 H 0.3817 0.5255 0.9520 0.033 Uiso 1 1 calc R . .
H11A H 0.4881(13) 0.526(2) 0.7910(13) 0.037(4) Uiso 1 1 d . . .
H11B H 0.4957(14) 0.379(2) 0.7127(13) 0.048(5) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N11 1.3609(15) . ?
C1 C10 1.3696(16) . ?
C1 C2 1.4695(17) . ?
C2 O12 1.2386(14) . ?
C2 N3 1.3747(15) . ?
N3 C4 1.3964(15) . ?
N3 C13 1.4706(16) . ?
C4 N5 1.3337(15) . ?
C4 C9 1.4097(17) . ?
N5 C6 1.3354(16) . ?
C6 C7 1.3856(18) . ?
C7 C8 1.3787(17) . ?
C8 C9 1.3992(17) . ?
C9 C10 1.4379(16) . ?
C10 C14 1.4926(16) . ?
C14 C15 1.3914(17) . ?
C14 C19 1.3931(17) . ?
C15 C16 1.3896(18) . ?
C16 C17 1.3827(19) . ?
C17 C18 1.3805(19) . ?
C18 C19 1.3904(18) . ?

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
N11 C1 C10 125.19(11) . . ?
N11 C1 C2 113.94(11) . . ?
C10 C1 C2 120.88(10) . . ?
O12 C2 N3 121.63(11) . . ?
O12 C2 C1 120.75(11) . . ?
N3 C2 C1 117.61(10) . . ?
C2 N3 C4 122.88(10) . . ?
C2 N3 C13 118.30(10) . . ?
C4 N3 C13 118.82(10) . . ?
N5 C4 N3 116.44(11) . . ?
N5 C4 C9 124.51(11) . . ?
N3 C4 C9 119.05(10) . . ?
C4 N5 C6 117.19(11) . . ?
N5 C6 C7 123.53(11) . . ?
C8 C7 C6 118.64(12) . . ?
C7 C8 C9 120.01(12) . . ?
C8 C9 C4 116.12(11) . . ?
C8 C9 C10 123.74(11) . . ?
C4 C9 C10 120.13(11) . . ?
C1 C10 C9 119.34(11) . . ?
C1 C10 C14 121.52(10) . . ?
C9 C10 C14 119.12(10) . . ?
C15 C14 C19 119.10(11) . . ?
C15 C14 C10 119.72(11) . . ?
C19 C14 C10 121.15(11) . . ?
C14 C15 C16 120.42(12) . . ?
C17 C16 C15 120.08(12) . . ?
C18 C17 C16 119.90(12) . . ?
C17 C18 C19 120.37(12) . . ?
C14 C19 C18 120.11(12) . . ?

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
N11 C1 C2 O12 0.41(17) . . . . ?
C10 C1 C2 O12 -179.97(11) . . . . ?
N11 C1 C2 N3 -178.49(11) . . . . ?
C10 C1 C2 N3 1.14(17) . . . . ?
O12 C2 N3 C4 178.07(11) . . . . ?
C1 C2 N3 C4 -3.04(17) . . . . ?
O12 C2 N3 C13 -2.18(18) . . . . ?
C1 C2 N3 C13 176.71(10) . . . . ?
C2 N3 C4 N5 -178.11(10) . . . . ?
C13 N3 C4 N5 2.14(16) . . . . ?
C2 N3 C4 C9 2.02(17) . . . . ?
C13 N3 C4 C9 -177.73(11) . . . . ?
N3 C4 N5 C6 -179.95(10) . . . . ?
C9 C4 N5 C6 -0.08(18) . . . . ?
C4 N5 C6 C7 -0.70(18) . . . . ?
N5 C6 C7 C8 0.8(2) . . . . ?
C6 C7 C8 C9 -0.14(19) . . . . ?
C7 C8 C9 C4 -0.55(18) . . . . ?
C7 C8 C9 C10 179.02(11) . . . . ?
N5 C4 C9 C8 0.69(18) . . . . ?
N3 C4 C9 C8 -179.45(10) . . . . ?
N5 C4 C9 C10 -178.90(11) . . . . ?
N3 C4 C9 C10 0.97(17) . . . . ?
N11 C1 C10 C9 -178.73(11) . . . . ?
C2 C1 C10 C9 1.69(17) . . . . ?
N11 C1 C10 C14 2.48(19) . . . . ?
C2 C1 C10 C14 -177.10(10) . . . . ?
C8 C9 C10 C1 177.69(11) . . . . ?
C4 C9 C10 C1 -2.76(17) . . . . ?
C8 C9 C10 C14 -3.49(18) . . . . ?
C4 C9 C10 C14 176.06(10) . . . . ?
C1 C10 C14 C15 103.96(14) . . . . ?
C9 C10 C14 C15 -74.83(15) . . . . ?
C1 C10 C14 C19 -78.15(15) . . . . ?
C9 C10 C14 C19 103.06(13) . . . . ?
C19 C14 C15 C16 -0.72(18) . . . . ?
C10 C14 C15 C16 177.21(11) . . . . ?
C14 C15 C16 C17 -0.41(18) . . . . ?
C15 C16 C17 C18 1.16(18) . . . . ?
C16 C17 C18 C19 -0.77(18) . . . . ?
C15 C14 C19 C18 1.11(18) . . . . ?
C10 C14 C19 C18 -176.79(10) . . . . ?
C17 C18 C19 C14 -0.37(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        68.24
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.039
####################################################################### 
# 
# 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_ccx481t2
_database_code_depnum_ccdc_archive 'CCDC 1528554'
_audit_update_record             
;
2017-01-19 deposited with the CCDC.
2018-05-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C61.50 H53.50 Cl4.50 N12 O4'
_chemical_formula_weight         1184.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.82470(10)
_cell_length_b                   14.6849(2)
_cell_length_c                   19.4686(13)
_cell_angle_alpha                74.323(5)
_cell_angle_beta                 82.323(6)
_cell_angle_gamma                77.013(5)
_cell_volume                     2894.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    9025
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      68.25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1230
_exptl_absorpt_coefficient_mu    2.552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7008
_exptl_absorpt_correction_T_max  0.8830
_exptl_absorpt_process_details   'CrystalClear Expert 2.1 43b(Rigaku, 2013)'

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.000 271 70 ' '
_platon_squeeze_details          
;
The unit cell contains 1 disordered molecule of chloroform around the inversion 
center  and which have been treated as a diffuse contribution to the overall 
scatering without specific atom positions by SQUEEZE/PLATON.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  'Rigaku RAXIS Rapid'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44251
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         68.25
_reflns_number_total             10437
_reflns_number_gt                9025
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear Expert 2.1 43b(Rigaku, 2013)'
_computing_cell_refinement       'CrystalClear Expert 2.1 43b(Rigaku, 2013)'
_computing_data_reduction        'CrystalClear Expert 2.1 43b(Rigaku, 2013)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_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)+(0.0984P)²+2.2180P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00164(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         10437
_refine_ls_number_parameters     750
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1704
_refine_ls_wR_factor_gt          0.1556
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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 0.5771(2) 0.38507(15) 0.19109(11) 0.0295(5) Uani 1 1 d . . .
C2 C 0.6496(2) 0.29972(16) 0.17327(12) 0.0361(5) Uani 1 1 d . . .
N3 N 0.6475(2) 0.21154(13) 0.22293(11) 0.0370(5) Uani 1 1 d . . .
C4 C 0.5698(2) 0.20429(15) 0.28588(11) 0.0287(4) Uani 1 1 d . . .
N5 N 0.57082(19) 0.11484(13) 0.32741(10) 0.0351(4) Uani 1 1 d . . .
C6 C 0.4953(2) 0.10646(16) 0.38827(12) 0.0351(5) Uani 1 1 d . . .
H6 H 0.4948 0.0436 0.4182 0.042 Uiso 1 1 calc R . .
C7 C 0.4186(2) 0.18314(16) 0.41005(12) 0.0342(5) Uani 1 1 d . . .
H7 H 0.3668 0.1733 0.4538 0.041 Uiso 1 1 calc R . .
C8 C 0.4182(2) 0.27497(16) 0.36697(12) 0.0316(5) Uani 1 1 d . . .
H8 H 0.3659 0.3293 0.3809 0.038 Uiso 1 1 calc R . .
C9 C 0.4949(2) 0.28752(15) 0.30302(11) 0.0281(4) Uani 1 1 d . . .
C10 C 0.5003(2) 0.38148(15) 0.25412(11) 0.0277(4) Uani 1 1 d . . .
N11 N 0.4278(2) 0.46114(14) 0.27069(12) 0.0361(5) Uani 1 1 d . . .
O12 O 0.7169(2) 0.29970(12) 0.11582(9) 0.0493(5) Uani 1 1 d . . .
C13 C 0.7311(3) 0.12538(19) 0.20701(17) 0.0621(9) Uani 1 1 d . . .
H13A H 0.7631 0.0816 0.2514 0.093 Uiso 1 1 calc R . .
H13B H 0.8028 0.1441 0.1738 0.093 Uiso 1 1 calc R . .
H13C H 0.6833 0.0927 0.1851 0.093 Uiso 1 1 calc R . .
C14 C 0.5883(2) 0.47897(15) 0.13880(11) 0.0309(5) Uani 1 1 d . . .
C15 C 0.6923(2) 0.52081(17) 0.13726(13) 0.0372(5) Uani 1 1 d . . .
H15 H 0.7545 0.4906 0.1708 0.045 Uiso 1 1 calc R . .
C16 C 0.7061(3) 0.60639(17) 0.08718(13) 0.0401(5) Uani 1 1 d . . .
H16 H 0.7772 0.6345 0.0868 0.048 Uiso 1 1 calc R . .
C17 C 0.6157(3) 0.65076(16) 0.03769(13) 0.0405(6) Uani 1 1 d . . .
H17 H 0.6257 0.7086 0.0029 0.049 Uiso 1 1 calc R . .
C18 C 0.5114(3) 0.61027(17) 0.03932(13) 0.0407(6) Uani 1 1 d . . .
H18 H 0.4492 0.6406 0.0058 0.049 Uiso 1 1 calc R . .
C19 C 0.4973(2) 0.52501(17) 0.09000(13) 0.0369(5) Uani 1 1 d . . .
H19 H 0.4248 0.4981 0.0912 0.044 Uiso 1 1 calc R . .
H11A H 0.444(3) 0.513(2) 0.2409(16) 0.044 Uiso 1 1 d . . .
H11B H 0.401(3) 0.460(2) 0.3112(17) 0.044 Uiso 1 1 d . . .
C21 C 0.2232(2) 0.63576(15) 0.39977(12) 0.0300(5) Uani 1 1 d . . .
C22 C 0.2481(2) 0.53599(15) 0.43890(12) 0.0322(5) Uani 1 1 d . . .
N23 N 0.18053(18) 0.50982(12) 0.50388(10) 0.0306(4) Uani 1 1 d . . .
C24 C 0.0884(2) 0.57517(15) 0.53101(12) 0.0297(5) Uani 1 1 d . . .
N25 N 0.02352(19) 0.53947(14) 0.59234(10) 0.0352(4) Uani 1 1 d . . .
C26 C -0.0646(2) 0.60186(18) 0.62057(13) 0.0367(5) Uani 1 1 d . . .
H26 H -0.1118 0.5773 0.6638 0.044 Uiso 1 1 calc R . .
C27 C -0.0908(2) 0.70041(17) 0.59014(13) 0.0371(5) Uani 1 1 d . . .
H27 H -0.1531 0.7422 0.6126 0.045 Uiso 1 1 calc R . .
C28 C -0.0249(2) 0.73670(16) 0.52663(12) 0.0328(5) Uani 1 1 d . . .
H28 H -0.0413 0.8040 0.5048 0.039 Uiso 1 1 calc R . .
C29 C 0.0654(2) 0.67425(15) 0.49487(12) 0.0299(5) Uani 1 1 d . . .
C30 C 0.1372(2) 0.70462(15) 0.42694(12) 0.0305(5) Uani 1 1 d . . .
N31 N 0.1177(2) 0.79886(14) 0.39182(12) 0.0386(5) Uani 1 1 d . . .
O32 O 0.32924(17) 0.47299(11) 0.41648(9) 0.0397(4) Uani 1 1 d . . .
C33 C 0.2087(3) 0.40875(16) 0.54503(13) 0.0412(6) Uani 1 1 d . . .
H33A H 0.2657 0.3699 0.5155 0.062 Uiso 1 1 calc R . .
H33B H 0.1294 0.3845 0.5590 0.062 Uiso 1 1 calc R . .
H33C H 0.2498 0.4044 0.5880 0.062 Uiso 1 1 calc R . .
C34 C 0.2968(2) 0.66221(15) 0.32948(12) 0.0329(5) Uani 1 1 d . . .
C35 C 0.4251(3) 0.66282(18) 0.32580(15) 0.0431(6) Uani 1 1 d . . .
H35 H 0.4667 0.6471 0.3687 0.052 Uiso 1 1 calc R . .
C36 C 0.4937(3) 0.6861(2) 0.26023(18) 0.0543(7) Uani 1 1 d . . .
H36 H 0.5821 0.6852 0.2584 0.065 Uiso 1 1 calc R . .
C37 C 0.4338(3) 0.71044(18) 0.19755(16) 0.0533(8) Uani 1 1 d . . .
H37 H 0.4806 0.7274 0.1527 0.064 Uiso 1 1 calc R . .
C38 C 0.3070(3) 0.71009(19) 0.20023(14) 0.0506(7) Uani 1 1 d . . .
H38 H 0.2660 0.7260 0.1571 0.061 Uiso 1 1 calc R . .
C39 C 0.2375(3) 0.68638(18) 0.26602(13) 0.0413(6) Uani 1 1 d . . .
H39 H 0.1493 0.6867 0.2675 0.050 Uiso 1 1 calc R . .
H31A H 0.163(3) 0.816(2) 0.3543(18) 0.050 Uiso 1 1 d . . .
H31B H 0.070(3) 0.845(2) 0.4109(16) 0.050 Uiso 1 1 d . . .
C41 C -0.0329(2) 0.10920(15) 0.34338(12) 0.0320(5) Uani 1 1 d . . .
C42 C -0.0873(2) 0.05282(15) 0.40804(12) 0.0318(5) Uani 1 1 d . . .
N43 N -0.18715(18) 0.09995(13) 0.44628(10) 0.0321(4) Uani 1 1 d . . .
C44 C -0.2326(2) 0.19843(15) 0.42548(11) 0.0284(4) Uani 1 1 d . . .
N45 N -0.32795(18) 0.23507(13) 0.46859(10) 0.0324(4) Uani 1 1 d . . .
C46 C -0.3728(2) 0.32980(16) 0.44958(13) 0.0340(5) Uani 1 1 d . . .
H46 H -0.4401 0.3565 0.4793 0.041 Uiso 1 1 calc R . .
C47 C -0.3276(2) 0.39197(15) 0.38905(12) 0.0325(5) Uani 1 1 d . . .
H47 H -0.3627 0.4591 0.3780 0.039 Uiso 1 1 calc R . .
C48 C -0.2305(2) 0.35390(15) 0.34539(12) 0.0305(5) Uani 1 1 d . . .
H48 H -0.1975 0.3949 0.3037 0.037 Uiso 1 1 calc R . .
C49 C -0.1804(2) 0.25466(15) 0.36255(11) 0.0284(4) Uani 1 1 d . . .
C50 C -0.0770(2) 0.20748(15) 0.32050(12) 0.0303(5) Uani 1 1 d . . .
N51 N -0.0276(2) 0.26051(15) 0.25921(11) 0.0402(5) Uani 1 1 d . . .
O52 O -0.04862(17) -0.03520(11) 0.43076(9) 0.0424(4) Uani 1 1 d . . .
C53 C -0.2422(3) 0.04223(18) 0.51208(14) 0.0431(6) Uani 1 1 d . . .
H53A H -0.1974 -0.0252 0.5199 0.065 Uiso 1 1 calc R . .
H53B H -0.3325 0.0462 0.5076 0.065 Uiso 1 1 calc R . .
H53C H -0.2335 0.0671 0.5527 0.065 Uiso 1 1 calc R . .
C54 C 0.0760(2) 0.05806(15) 0.30395(12) 0.0334(5) Uani 1 1 d . . .
C55 C 0.2002(2) 0.06702(16) 0.30826(12) 0.0358(5) Uani 1 1 d . . .
H55 H 0.2146 0.1086 0.3349 0.043 Uiso 1 1 calc R . .
C56 C 0.3029(2) 0.01639(18) 0.27434(13) 0.0418(6) Uani 1 1 d . . .
H56 H 0.3868 0.0227 0.2786 0.050 Uiso 1 1 calc R . .
C57 C 0.2837(3) -0.04331(18) 0.23427(13) 0.0435(6) Uani 1 1 d . . .
H57 H 0.3541 -0.0785 0.2114 0.052 Uiso 1 1 calc R . .
C58 C 0.1619(3) -0.05119(18) 0.22795(14) 0.0442(6) Uani 1 1 d . . .
H58 H 0.1481 -0.0910 0.1997 0.053 Uiso 1 1 calc R . .
C59 C 0.0580(3) -0.00111(17) 0.26270(13) 0.0398(5) Uani 1 1 d . . .
H59 H -0.0256 -0.0076 0.2581 0.048 Uiso 1 1 calc R . .
H51A H -0.040(3) 0.321(2) 0.2502(16) 0.048 Uiso 1 1 d . . .
H51B H 0.042(3) 0.228(2) 0.2341(16) 0.048 Uiso 1 1 d . . .
C61 C 0.9061(2) 0.48975(15) 0.87942(11) 0.0297(5) Uani 1 1 d . . .
C62 C 0.9928(2) 0.46898(16) 0.82057(12) 0.0318(5) Uani 1 1 d . . .
N63 N 1.02982(19) 0.37360(14) 0.81622(10) 0.0367(4) Uani 1 1 d . . .
C64 C 0.9908(2) 0.29885(17) 0.86873(13) 0.0371(5) Uani 1 1 d . . .
N65 N 1.0330(2) 0.20998(15) 0.85857(12) 0.0494(6) Uani 1 1 d . . .
C66 C 0.9961(3) 0.13700(19) 0.90781(16) 0.0582(8) Uani 1 1 d . . .
H66 H 1.0253 0.0738 0.9009 0.070 Uiso 1 1 calc R . .
C67 C 0.9178(3) 0.14735(19) 0.96844(16) 0.0564(8) Uani 1 1 d . . .
H67 H 0.8946 0.0927 1.0023 0.068 Uiso 1 1 calc R . .
C68 C 0.8741(3) 0.23863(18) 0.97875(14) 0.0443(6) Uani 1 1 d . . .
H68 H 0.8198 0.2477 1.0199 0.053 Uiso 1 1 calc R . .
C69 C 0.9100(2) 0.31795(16) 0.92832(12) 0.0340(5) Uani 1 1 d . . .
C70 C 0.8668(2) 0.41710(15) 0.93344(11) 0.0301(5) Uani 1 1 d . . .
N71 N 0.78809(19) 0.43647(15) 0.98990(10) 0.0351(4) Uani 1 1 d . . .
O72 O 1.03639(16) 0.53195(12) 0.77353(9) 0.0394(4) Uani 1 1 d . . .
C73 C 1.1148(3) 0.3542(2) 0.75419(15) 0.0520(7) Uani 1 1 d . . .
H73A H 1.2020 0.3562 0.7614 0.078 Uiso 1 1 calc R . .
H73B H 1.0872 0.4032 0.7109 0.078 Uiso 1 1 calc R . .
H73C H 1.1121 0.2902 0.7488 0.078 Uiso 1 1 calc R . .
C74 C 0.8609(2) 0.59322(15) 0.87934(11) 0.0307(5) Uani 1 1 d . . .
C75 C 0.9209(3) 0.63821(18) 0.91563(13) 0.0405(6) Uani 1 1 d . . .
H75 H 0.9917 0.6025 0.9419 0.049 Uiso 1 1 calc R . .
C76 C 0.8775(3) 0.73575(19) 0.91364(14) 0.0471(6) Uani 1 1 d . . .
H76 H 0.9186 0.7660 0.9390 0.057 Uiso 1 1 calc R . .
C77 C 0.7758(3) 0.78852(17) 0.87536(14) 0.0443(6) Uani 1 1 d . . .
H77 H 0.7475 0.8551 0.8737 0.053 Uiso 1 1 calc R . .
C78 C 0.7150(2) 0.74438(17) 0.83934(14) 0.0426(6) Uani 1 1 d . . .
H78 H 0.6443 0.7805 0.8132 0.051 Uiso 1 1 calc R . .
C79 C 0.7570(2) 0.64711(17) 0.84137(13) 0.0368(5) Uani 1 1 d . . .
H79 H 0.7146 0.6171 0.8166 0.044 Uiso 1 1 calc R . .
H71A H 0.768(3) 0.394(2) 1.0274(16) 0.044 Uiso 1 1 d . . .
H71B H 0.759(3) 0.496(2) 0.9938(15) 0.044 Uiso 1 1 d . . .
C91 C 0.6602(3) 0.88991(18) 0.33175(16) 0.0514(7) Uani 1 1 d . . .
H91 H 0.6447 0.9597 0.3316 0.062 Uiso 1 1 calc R . .
Cl1 Cl 0.54551(7) 0.83575(5) 0.39349(4) 0.0564(2) Uani 1 1 d . . .
Cl2 Cl 0.81492(9) 0.83623(7) 0.35614(6) 0.0774(3) Uani 1 1 d . . .
Cl3 Cl 0.64606(8) 0.88175(5) 0.24467(4) 0.0588(2) 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 C10 1.382(3) . ?
C1 C2 1.424(3) . ?
C1 C14 1.495(3) . ?
C2 O12 1.251(3) . ?
C2 N3 1.394(3) . ?
N3 C4 1.384(3) . ?
N3 C13 1.462(3) . ?
C4 N5 1.342(3) . ?
C4 C9 1.402(3) . ?
N5 C6 1.340(3) . ?
C6 C7 1.372(3) . ?
C7 C8 1.382(3) . ?
C8 C9 1.394(3) . ?
C9 C10 1.458(3) . ?
C10 N11 1.346(3) . ?
C14 C19 1.390(3) . ?
C14 C15 1.392(3) . ?
C15 C16 1.391(3) . ?
C16 C17 1.391(4) . ?
C17 C18 1.383(4) . ?
C18 C19 1.394(3) . ?
C21 C30 1.380(3) . ?
C21 C22 1.440(3) . ?
C21 C34 1.489(3) . ?
C22 O32 1.253(3) . ?
C22 N23 1.378(3) . ?
N23 C24 1.377(3) . ?
N23 C33 1.469(3) . ?
C24 N25 1.341(3) . ?
C24 C29 1.416(3) . ?
N25 C26 1.338(3) . ?
C26 C27 1.387(3) . ?
C27 C28 1.379(3) . ?
C28 C29 1.386(3) . ?
C29 C30 1.454(3) . ?
C30 N31 1.350(3) . ?
C34 C35 1.383(4) . ?
C34 C39 1.392(3) . ?
C35 C36 1.386(4) . ?
C36 C37 1.381(5) . ?
C37 C38 1.368(5) . ?
C38 C39 1.395(4) . ?
C41 C50 1.382(3) . ?
C41 C42 1.440(3) . ?
C41 C54 1.488(3) . ?
C42 O52 1.241(3) . ?
C42 N43 1.389(3) . ?
N43 C44 1.384(3) . ?
N43 C53 1.467(3) . ?
C44 N45 1.350(3) . ?
C44 C49 1.407(3) . ?
N45 C46 1.332(3) . ?
C46 C47 1.388(3) . ?
C47 C48 1.376(3) . ?
C48 C49 1.400(3) . ?
C49 C50 1.455(3) . ?
C50 N51 1.353(3) . ?
C54 C59 1.390(3) . ?
C54 C55 1.395(3) . ?
C55 C56 1.387(3) . ?
C56 C57 1.384(4) . ?
C57 C58 1.374(4) . ?
C58 C59 1.399(4) . ?
C61 C70 1.380(3) . ?
C61 C62 1.435(3) . ?
C61 C74 1.488(3) . ?
C62 O72 1.241(3) . ?
C62 N63 1.390(3) . ?
N63 C64 1.384(3) . ?
N63 C73 1.469(3) . ?
C64 N65 1.341(3) . ?
C64 C69 1.409(3) . ?
N65 C66 1.327(4) . ?
C66 C67 1.380(4) . ?
C67 C68 1.377(4) . ?
C68 C69 1.398(3) . ?
C69 C70 1.452(3) . ?
C70 N71 1.351(3) . ?
C74 C75 1.387(3) . ?
C74 C79 1.394(3) . ?
C75 C76 1.395(4) . ?
C76 C77 1.375(4) . ?
C77 C78 1.381(4) . ?
C78 C79 1.390(3) . ?
C91 Cl2 1.752(3) . ?
C91 Cl3 1.760(3) . ?
C91 Cl1 1.774(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C10 C1 C2 121.57(19) . . ?
C10 C1 C14 121.39(19) . . ?
C2 C1 C14 117.04(19) . . ?
O12 C2 N3 118.1(2) . . ?
O12 C2 C1 123.5(2) . . ?
N3 C2 C1 118.4(2) . . ?
C4 N3 C2 121.85(19) . . ?
C4 N3 C13 120.12(19) . . ?
C2 N3 C13 118.0(2) . . ?
N5 C4 N3 116.27(19) . . ?
N5 C4 C9 123.6(2) . . ?
N3 C4 C9 120.14(19) . . ?
C6 N5 C4 117.04(19) . . ?
N5 C6 C7 124.0(2) . . ?
C6 C7 C8 118.6(2) . . ?
C7 C8 C9 119.7(2) . . ?
C8 C9 C4 117.15(19) . . ?
C8 C9 C10 123.5(2) . . ?
C4 C9 C10 119.3(2) . . ?
N11 C10 C1 122.4(2) . . ?
N11 C10 C9 119.1(2) . . ?
C1 C10 C9 118.51(19) . . ?
C19 C14 C15 118.8(2) . . ?
C19 C14 C1 121.0(2) . . ?
C15 C14 C1 120.1(2) . . ?
C14 C15 C16 120.7(2) . . ?
C15 C16 C17 120.0(2) . . ?
C18 C17 C16 119.7(2) . . ?
C17 C18 C19 120.2(2) . . ?
C14 C19 C18 120.6(2) . . ?
C30 C21 C22 121.5(2) . . ?
C30 C21 C34 121.21(19) . . ?
C22 C21 C34 117.27(19) . . ?
O32 C22 N23 119.22(19) . . ?
O32 C22 C21 122.5(2) . . ?
N23 C22 C21 118.24(19) . . ?
C24 N23 C22 122.14(18) . . ?
C24 N23 C33 119.51(19) . . ?
C22 N23 C33 118.35(19) . . ?
N25 C24 N23 116.37(19) . . ?
N25 C24 C29 122.9(2) . . ?
N23 C24 C29 120.7(2) . . ?
C26 N25 C24 117.5(2) . . ?
N25 C26 C27 123.5(2) . . ?
C28 C27 C26 118.8(2) . . ?
C27 C28 C29 119.5(2) . . ?
C28 C29 C24 117.7(2) . . ?
C28 C29 C30 123.8(2) . . ?
C24 C29 C30 118.5(2) . . ?
N31 C30 C21 121.6(2) . . ?
N31 C30 C29 119.5(2) . . ?
C21 C30 C29 118.83(19) . . ?
C35 C34 C39 118.7(2) . . ?
C35 C34 C21 120.9(2) . . ?
C39 C34 C21 120.4(2) . . ?
C34 C35 C36 120.7(3) . . ?
C37 C36 C35 120.2(3) . . ?
C38 C37 C36 119.8(3) . . ?
C37 C38 C39 120.3(3) . . ?
C34 C39 C38 120.3(3) . . ?
C50 C41 C42 121.2(2) . . ?
C50 C41 C54 121.4(2) . . ?
C42 C41 C54 117.32(18) . . ?
O52 C42 N43 119.1(2) . . ?
O52 C42 C41 122.9(2) . . ?
N43 C42 C41 117.98(19) . . ?
C44 N43 C42 122.36(18) . . ?
C44 N43 C53 119.84(19) . . ?
C42 N43 C53 117.77(18) . . ?
N45 C44 N43 116.08(19) . . ?
N45 C44 C49 123.52(19) . . ?
N43 C44 C49 120.4(2) . . ?
C46 N45 C44 116.99(19) . . ?
N45 C46 C47 124.2(2) . . ?
C48 C47 C46 118.4(2) . . ?
C47 C48 C49 119.8(2) . . ?
C48 C49 C44 117.1(2) . . ?
C48 C49 C50 124.1(2) . . ?
C44 C49 C50 118.75(19) . . ?
N51 C50 C41 121.4(2) . . ?
N51 C50 C49 119.28(19) . . ?
C41 C50 C49 119.27(19) . . ?
C59 C54 C55 117.8(2) . . ?
C59 C54 C41 121.4(2) . . ?
C55 C54 C41 120.7(2) . . ?
C56 C55 C54 121.2(2) . . ?
C57 C56 C55 120.2(2) . . ?
C58 C57 C56 119.3(2) . . ?
C57 C58 C59 120.6(2) . . ?
C54 C59 C58 120.7(2) . . ?
C70 C61 C62 121.5(2) . . ?
C70 C61 C74 121.7(2) . . ?
C62 C61 C74 116.81(18) . . ?
O72 C62 N63 118.5(2) . . ?
O72 C62 C61 123.2(2) . . ?
N63 C62 C61 118.32(19) . . ?
C64 N63 C62 121.8(2) . . ?
C64 N63 C73 120.7(2) . . ?
C62 N63 C73 117.5(2) . . ?
N65 C64 N63 116.3(2) . . ?
N65 C64 C69 123.4(2) . . ?
N63 C64 C69 120.4(2) . . ?
C66 N65 C64 117.5(2) . . ?
N65 C66 C67 124.0(3) . . ?
C68 C67 C66 118.5(2) . . ?
C67 C68 C69 119.7(2) . . ?
C68 C69 C64 116.9(2) . . ?
C68 C69 C70 123.9(2) . . ?
C64 C69 C70 119.2(2) . . ?
N71 C70 C61 121.5(2) . . ?
N71 C70 C69 119.8(2) . . ?
C61 C70 C69 118.7(2) . . ?
C75 C74 C79 118.8(2) . . ?
C75 C74 C61 121.5(2) . . ?
C79 C74 C61 119.7(2) . . ?
C74 C75 C76 120.2(2) . . ?
C77 C76 C75 120.6(2) . . ?
C76 C77 C78 119.8(2) . . ?
C77 C78 C79 120.0(2) . . ?
C78 C79 C74 120.6(2) . . ?
Cl2 C91 Cl3 109.47(17) . . ?
Cl2 C91 Cl1 111.30(15) . . ?
Cl3 C91 Cl1 110.82(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 C1 C2 O12 177.6(2) . . . . ?
C14 C1 C2 O12 -2.7(4) . . . . ?
C10 C1 C2 N3 -3.6(3) . . . . ?
C14 C1 C2 N3 176.0(2) . . . . ?
O12 C2 N3 C4 -176.0(2) . . . . ?
C1 C2 N3 C4 5.2(3) . . . . ?
O12 C2 N3 C13 4.2(4) . . . . ?
C1 C2 N3 C13 -174.6(3) . . . . ?
C2 N3 C4 N5 176.3(2) . . . . ?
C13 N3 C4 N5 -4.0(4) . . . . ?
C2 N3 C4 C9 -3.3(3) . . . . ?
C13 N3 C4 C9 176.5(3) . . . . ?
N3 C4 N5 C6 -179.5(2) . . . . ?
C9 C4 N5 C6 0.1(3) . . . . ?
C4 N5 C6 C7 -0.2(4) . . . . ?
N5 C6 C7 C8 0.1(4) . . . . ?
C6 C7 C8 C9 0.0(3) . . . . ?
C7 C8 C9 C4 -0.1(3) . . . . ?
C7 C8 C9 C10 179.8(2) . . . . ?
N5 C4 C9 C8 0.1(3) . . . . ?
N3 C4 C9 C8 179.6(2) . . . . ?
N5 C4 C9 C10 -179.8(2) . . . . ?
N3 C4 C9 C10 -0.3(3) . . . . ?
C2 C1 C10 N11 -177.7(2) . . . . ?
C14 C1 C10 N11 2.7(3) . . . . ?
C2 C1 C10 C9 0.2(3) . . . . ?
C14 C1 C10 C9 -179.41(19) . . . . ?
C8 C9 C10 N11 -0.2(3) . . . . ?
C4 C9 C10 N11 179.7(2) . . . . ?
C8 C9 C10 C1 -178.1(2) . . . . ?
C4 C9 C10 C1 1.8(3) . . . . ?
C10 C1 C14 C19 -81.8(3) . . . . ?
C2 C1 C14 C19 98.6(3) . . . . ?
C10 C1 C14 C15 99.6(3) . . . . ?
C2 C1 C14 C15 -80.0(3) . . . . ?
C19 C14 C15 C16 -0.9(4) . . . . ?
C1 C14 C15 C16 177.7(2) . . . . ?
C14 C15 C16 C17 -0.3(4) . . . . ?
C15 C16 C17 C18 1.0(4) . . . . ?
C16 C17 C18 C19 -0.4(4) . . . . ?
C15 C14 C19 C18 1.5(4) . . . . ?
C1 C14 C19 C18 -177.1(2) . . . . ?
C17 C18 C19 C14 -0.9(4) . . . . ?
C30 C21 C22 O32 -177.2(2) . . . . ?
C34 C21 C22 O32 1.2(3) . . . . ?
C30 C21 C22 N23 1.9(3) . . . . ?
C34 C21 C22 N23 -179.63(19) . . . . ?
O32 C22 N23 C24 -178.9(2) . . . . ?
C21 C22 N23 C24 2.0(3) . . . . ?
O32 C22 N23 C33 1.2(3) . . . . ?
C21 C22 N23 C33 -178.0(2) . . . . ?
C22 N23 C24 N25 175.56(19) . . . . ?
C33 N23 C24 N25 -4.5(3) . . . . ?
C22 N23 C24 C29 -4.3(3) . . . . ?
C33 N23 C24 C29 175.6(2) . . . . ?
N23 C24 N25 C26 178.62(19) . . . . ?
C29 C24 N25 C26 -1.5(3) . . . . ?
C24 N25 C26 C27 -0.6(3) . . . . ?
N25 C26 C27 C28 1.4(4) . . . . ?
C26 C27 C28 C29 0.0(3) . . . . ?
C27 C28 C29 C24 -1.9(3) . . . . ?
C27 C28 C29 C30 178.0(2) . . . . ?
N25 C24 C29 C28 2.8(3) . . . . ?
N23 C24 C29 C28 -177.4(2) . . . . ?
N25 C24 C29 C30 -177.1(2) . . . . ?
N23 C24 C29 C30 2.7(3) . . . . ?
C22 C21 C30 N31 177.1(2) . . . . ?
C34 C21 C30 N31 -1.3(3) . . . . ?
C22 C21 C30 C29 -3.3(3) . . . . ?
C34 C21 C30 C29 178.3(2) . . . . ?
C28 C29 C30 N31 0.7(3) . . . . ?
C24 C29 C30 N31 -179.4(2) . . . . ?
C28 C29 C30 C21 -178.9(2) . . . . ?
C24 C29 C30 C21 1.1(3) . . . . ?
C30 C21 C34 C35 107.1(3) . . . . ?
C22 C21 C34 C35 -71.3(3) . . . . ?
C30 C21 C34 C39 -73.2(3) . . . . ?
C22 C21 C34 C39 108.3(2) . . . . ?
C39 C34 C35 C36 -0.6(4) . . . . ?
C21 C34 C35 C36 179.0(2) . . . . ?
C34 C35 C36 C37 1.0(4) . . . . ?
C35 C36 C37 C38 -1.1(4) . . . . ?
C36 C37 C38 C39 0.8(4) . . . . ?
C35 C34 C39 C38 0.4(4) . . . . ?
C21 C34 C39 C38 -179.3(2) . . . . ?
C37 C38 C39 C34 -0.5(4) . . . . ?
C50 C41 C42 O52 -178.7(2) . . . . ?
C54 C41 C42 O52 -1.2(3) . . . . ?
C50 C41 C42 N43 1.0(3) . . . . ?
C54 C41 C42 N43 178.6(2) . . . . ?
O52 C42 N43 C44 177.9(2) . . . . ?
C41 C42 N43 C44 -1.9(3) . . . . ?
O52 C42 N43 C53 -0.2(3) . . . . ?
C41 C42 N43 C53 -180.0(2) . . . . ?
C42 N43 C44 N45 -178.4(2) . . . . ?
C53 N43 C44 N45 -0.4(3) . . . . ?
C42 N43 C44 C49 1.8(3) . . . . ?
C53 N43 C44 C49 179.9(2) . . . . ?
N43 C44 N45 C46 179.83(19) . . . . ?
C49 C44 N45 C46 -0.4(3) . . . . ?
C44 N45 C46 C47 -0.2(3) . . . . ?
N45 C46 C47 C48 0.3(3) . . . . ?
C46 C47 C48 C49 0.2(3) . . . . ?
C47 C48 C49 C44 -0.8(3) . . . . ?
C47 C48 C49 C50 -179.3(2) . . . . ?
N45 C44 C49 C48 0.9(3) . . . . ?
N43 C44 C49 C48 -179.37(19) . . . . ?
N45 C44 C49 C50 179.5(2) . . . . ?
N43 C44 C49 C50 -0.8(3) . . . . ?
C42 C41 C50 N51 -178.9(2) . . . . ?
C54 C41 C50 N51 3.6(4) . . . . ?
C42 C41 C50 C49 -0.1(3) . . . . ?
C54 C41 C50 C49 -177.5(2) . . . . ?
C48 C49 C50 N51 -2.7(3) . . . . ?
C44 C49 C50 N51 178.8(2) . . . . ?
C48 C49 C50 C41 178.4(2) . . . . ?
C44 C49 C50 C41 -0.1(3) . . . . ?
C50 C41 C54 C59 -106.5(3) . . . . ?
C42 C41 C54 C59 76.0(3) . . . . ?
C50 C41 C54 C55 74.5(3) . . . . ?
C42 C41 C54 C55 -103.0(3) . . . . ?
C59 C54 C55 C56 -1.9(3) . . . . ?
C41 C54 C55 C56 177.1(2) . . . . ?
C54 C55 C56 C57 1.1(4) . . . . ?
C55 C56 C57 C58 0.6(4) . . . . ?
C56 C57 C58 C59 -1.3(4) . . . . ?
C55 C54 C59 C58 1.2(3) . . . . ?
C41 C54 C59 C58 -177.8(2) . . . . ?
C57 C58 C59 C54 0.4(4) . . . . ?
C70 C61 C62 O72 -175.3(2) . . . . ?
C74 C61 C62 O72 4.7(3) . . . . ?
C70 C61 C62 N63 4.6(3) . . . . ?
C74 C61 C62 N63 -175.44(19) . . . . ?
O72 C62 N63 C64 176.4(2) . . . . ?
C61 C62 N63 C64 -3.5(3) . . . . ?
O72 C62 N63 C73 -2.3(3) . . . . ?
C61 C62 N63 C73 177.8(2) . . . . ?
C62 N63 C64 N65 -179.9(2) . . . . ?
C73 N63 C64 N65 -1.3(4) . . . . ?
C62 N63 C64 C69 0.9(4) . . . . ?
C73 N63 C64 C69 179.5(2) . . . . ?
N63 C64 N65 C66 -179.4(3) . . . . ?
C69 C64 N65 C66 -0.2(4) . . . . ?
C64 N65 C66 C67 -0.2(5) . . . . ?
N65 C66 C67 C68 0.5(5) . . . . ?
C66 C67 C68 C69 -0.3(5) . . . . ?
C67 C68 C69 C64 -0.1(4) . . . . ?
C67 C68 C69 C70 178.5(3) . . . . ?
N65 C64 C69 C68 0.4(4) . . . . ?
N63 C64 C69 C68 179.5(2) . . . . ?
N65 C64 C69 C70 -178.3(2) . . . . ?
N63 C64 C69 C70 0.9(4) . . . . ?
C62 C61 C70 N71 178.1(2) . . . . ?
C74 C61 C70 N71 -1.9(3) . . . . ?
C62 C61 C70 C69 -2.9(3) . . . . ?
C74 C61 C70 C69 177.1(2) . . . . ?
C68 C69 C70 N71 0.7(4) . . . . ?
C64 C69 C70 N71 179.2(2) . . . . ?
C68 C69 C70 C61 -178.4(2) . . . . ?
C64 C69 C70 C61 0.2(3) . . . . ?
C70 C61 C74 C75 85.8(3) . . . . ?
C62 C61 C74 C75 -94.2(3) . . . . ?
C70 C61 C74 C79 -95.1(3) . . . . ?
C62 C61 C74 C79 84.9(3) . . . . ?
C79 C74 C75 C76 -0.2(4) . . . . ?
C61 C74 C75 C76 179.0(2) . . . . ?
C74 C75 C76 C77 -0.5(4) . . . . ?
C75 C76 C77 C78 0.9(4) . . . . ?
C76 C77 C78 C79 -0.5(4) . . . . ?
C77 C78 C79 C74 -0.2(4) . . . . ?
C75 C74 C79 C78 0.6(4) . . . . ?
C61 C74 C79 C78 -178.6(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        68.25
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.071
