# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2008
data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Min Shi'
_publ_contact_author_email       MSHI@MAIL.SIOC.AC.CN

_publ_section_title              
;
Phosphine-Catalyzed Annulation of Ethyl
(Arylimino)acetates: Synthesis of Highly Functionalized
Oxoimidazolidines
;
loop_
_publ_author_name
'Min Shi'
'Jun Gao'
'Guang-Ning Ma'
'Fei-Jun Wang'

# Attachment 'cd26131-revised.cif'

data_cd26131
_database_code_depnum_ccdc_archive 'CCDC 612928'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24.25 H20.50 Br3 Cl0.50 N3 O3'
_chemical_formula_weight         659.39

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'
N N 0.0061 0.0033 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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                   13.9165(14)
_cell_length_b                   19.129(2)
_cell_length_c                   19.595(2)
_cell_angle_alpha                90.901(3)
_cell_angle_beta                 98.503(2)
_cell_angle_gamma                90.942(2)
_cell_volume                     5157.5(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1949
_cell_measurement_theta_min      4.377
_cell_measurement_theta_max      32.637

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.044
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2596
_exptl_absorpt_coefficient_mu    4.776
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.78936
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27508
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_sigmaI/netI    0.3395
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.50
_reflns_number_total             17002
_reflns_number_gt                5177
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         18902
_refine_ls_number_parameters     1205
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.2301
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1505
_refine_ls_wR_factor_gt          0.1005
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_restrained_S_all      0.862
_refine_ls_shift/su_max          0.002
_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
Br1 Br 1.37547(10) 0.55926(8) 0.12361(8) 0.1114(5) Uani 1 1 d . . .
Br2 Br 1.29062(10) 1.03828(7) 0.08644(8) 0.1084(6) Uani 1 1 d . . .
Br3 Br 0.36667(9) 0.77226(8) 0.03276(9) 0.1148(6) Uani 1 1 d . . .
Br4 Br -0.46869(12) 0.53670(12) 0.30127(10) 0.1293(9) Uani 1 1 d . . .
Br5 Br -0.33229(10) 1.02331(8) 0.43586(9) 0.1265(6) Uani 1 1 d . . .
Br6 Br 0.55536(11) 0.72893(11) 0.43721(10) 0.1477(7) Uani 1 1 d . . .
Br7 Br -0.41649(10) 0.03601(8) 0.11109(9) 0.1255(6) Uani 1 1 d . . .
Br8 Br -0.36550(9) 0.52965(7) 0.06274(8) 0.1001(5) Uani 1 1 d . . .
Br9 Br 0.56715(10) 0.29622(10) 0.15596(10) 0.1420(7) Uani 1 1 d . . .
Br10 Br 1.42272(11) 0.05835(10) 0.32879(13) 0.1358(9) Uani 1 1 d . . .
Br11 Br 1.36345(10) 0.50952(8) 0.46870(8) 0.1037(5) Uani 1 1 d . . .
Br12 Br 0.42065(10) 0.28218(12) 0.33617(10) 0.1355(8) Uani 1 1 d . . .
O1 O 0.8478(5) 0.6709(4) 0.0687(4) 0.083(3) Uani 1 1 d . . .
O2 O 0.8318(7) 0.8347(5) 0.2215(5) 0.107(3) Uani 1 1 d . . .
O3 O 0.8390(6) 0.9428(5) 0.1828(4) 0.082(3) Uani 1 1 d . . .
O4 O 0.0695(6) 0.6382(5) 0.4295(5) 0.094(3) Uani 1 1 d . . .
O5 O 0.0616(6) 0.8208(4) 0.2935(4) 0.094(3) Uani 1 1 d . . .
O6 O 0.1384(6) 0.9095(5) 0.3526(4) 0.093(3) Uani 1 1 d . . .
O7 O 0.0893(6) 0.1794(5) 0.0660(4) 0.085(3) Uani 1 1 d . . .
O8 O 0.0973(6) 0.3439(5) 0.2249(5) 0.091(3) Uani 1 1 d . . .
O9 O 0.1422(6) 0.4433(5) 0.1862(4) 0.097(3) Uani 1 1 d . . .
O10 O 0.8889(6) 0.1543(4) 0.4145(4) 0.089(3) Uani 1 1 d . . .
O11 O 0.8965(6) 0.3309(5) 0.2738(4) 0.095(3) Uani 1 1 d . . .
O12 O 0.8661(6) 0.4301(5) 0.3273(4) 0.088(3) Uani 1 1 d . . .
N1 N 1.0255(6) 0.7287(5) 0.1635(4) 0.061(3) Uani 1 1 d . . .
H1 H 1.0100 0.7378 0.2036 0.074 Uiso 1 1 calc R . .
N2 N 0.9605(7) 0.8336(5) 0.1117(4) 0.065(3) Uani 1 1 d . . .
N3 N 0.8086(6) 0.7845(5) 0.0853(4) 0.053(2) Uani 1 1 d . . .
N4 N -0.0996(7) 0.7123(5) 0.3400(5) 0.071(3) Uani 1 1 d . . .
H4 H -0.0779 0.7277 0.3041 0.085 Uiso 1 1 calc R . .
N5 N -0.0270(7) 0.8061(5) 0.4171(4) 0.062(3) Uani 1 1 d . . .
N6 N 0.1189(8) 0.7535(5) 0.4242(4) 0.066(3) Uani 1 1 d . . .
N7 N -0.0694(6) 0.2331(4) 0.1456(5) 0.060(3) Uani 1 1 d . . .
H7 H -0.0440 0.2478 0.1861 0.072 Uiso 1 1 calc R . .
N8 N -0.0239(7) 0.3368(5) 0.0888(4) 0.064(3) Uani 1 1 d . . .
N9 N 0.1300(7) 0.2942(4) 0.0906(4) 0.055(3) Uani 1 1 d . . .
N10 N 1.0530(6) 0.2140(5) 0.3402(5) 0.065(3) Uani 1 1 d . . .
H10 H 1.0204 0.2255 0.3014 0.078 Uiso 1 1 calc R . .
N11 N 1.0151(7) 0.3115(5) 0.4098(4) 0.065(3) Uani 1 1 d . . .
N12 N 0.8589(6) 0.2692(5) 0.4013(4) 0.060(3) Uani 1 1 d . . .
Cl1 Cl 0.5566(5) 0.9035(4) 0.2599(4) 0.277(3) Uani 1 1 d D . .
Cl2 Cl 0.4643(5) 0.7780(4) 0.2363(4) 0.263(3) Uani 1 1 d D . .
C1 C 0.8691(8) 0.7317(7) 0.0832(5) 0.055(3) Uani 1 1 d . . .
C2 C 0.9709(8) 0.7595(6) 0.1028(6) 0.057(3) Uani 1 1 d . . .
H2 H 1.0063 0.7515 0.0638 0.069 Uiso 1 1 calc R . .
C3 C 0.8605(8) 0.8498(6) 0.1062(6) 0.054(3) Uani 1 1 d . . .
H3 H 0.8442 0.8849 0.0707 0.065 Uiso 1 1 calc R . .
C4 C 1.0998(8) 0.6864(5) 0.1578(6) 0.049(3) Uani 1 1 d . . .
C5 C 1.0992(9) 0.6371(7) 0.1049(6) 0.072(4) Uani 1 1 d . . .
H5 H 1.0419 0.6293 0.0746 0.086 Uiso 1 1 calc R . .
C6 C 1.1805(11) 0.5988(6) 0.0951(6) 0.073(4) Uani 1 1 d . . .
H6 H 1.1770 0.5671 0.0582 0.088 Uiso 1 1 calc R . .
C7 C 1.2641(9) 0.6075(7) 0.1390(7) 0.069(4) Uani 1 1 d . . .
C8 C 1.2695(8) 0.6513(7) 0.1951(7) 0.083(4) Uani 1 1 d . . .
H8 H 1.3259 0.6552 0.2272 0.100 Uiso 1 1 calc R . .
C9 C 1.1885(10) 0.6896(6) 0.2028(6) 0.075(4) Uani 1 1 d . . .
H9 H 1.1929 0.7200 0.2407 0.090 Uiso 1 1 calc R . .
C10 C 1.0373(8) 0.8805(6) 0.1032(5) 0.052(3) Uani 1 1 d . . .
C11 C 1.1271(8) 0.8584(6) 0.1032(5) 0.055(3) Uani 1 1 d . . .
H11 H 1.1393 0.8108 0.1066 0.066 Uiso 1 1 calc R . .
C12 C 1.2036(8) 0.9051(7) 0.0980(6) 0.070(4) Uani 1 1 d . . .
H12 H 1.2666 0.8897 0.0978 0.084 Uiso 1 1 calc R . .
C13 C 1.1812(9) 0.9770(7) 0.0929(6) 0.067(3) Uani 1 1 d . . .
C14 C 1.0906(10) 0.9995(6) 0.0906(6) 0.072(4) Uani 1 1 d . . .
H14 H 1.0776 1.0468 0.0846 0.086 Uiso 1 1 calc R . .
C15 C 1.0156(7) 0.9520(6) 0.0970(5) 0.063(3) Uani 1 1 d . . .
H15 H 0.9525 0.9672 0.0972 0.076 Uiso 1 1 calc R . .
C16 C 0.7036(8) 0.7837(6) 0.0728(5) 0.055(3) Uani 1 1 d . . .
C17 C 0.6506(10) 0.7206(6) 0.0728(6) 0.083(4) Uani 1 1 d . . .
H17 H 0.6848 0.6796 0.0816 0.100 Uiso 1 1 calc R . .
C18 C 0.5545(10) 0.7165(8) 0.0610(8) 0.108(5) Uani 1 1 d . . .
H18 H 0.5218 0.6738 0.0615 0.130 Uiso 1 1 calc R . .
C19 C 0.5050(9) 0.7770(8) 0.0480(6) 0.077(4) Uani 1 1 d . . .
C20 C 0.5497(9) 0.8405(7) 0.0462(6) 0.090(4) Uani 1 1 d . . .
H20 H 0.5143 0.8809 0.0367 0.107 Uiso 1 1 calc R . .
C21 C 0.6485(9) 0.8422(6) 0.0592(6) 0.071(4) Uani 1 1 d . . .
H21 H 0.6805 0.8853 0.0588 0.085 Uiso 1 1 calc R . .
C22 C 0.8372(8) 0.8774(8) 0.1758(7) 0.075(4) Uani 1 1 d . . .
C23 C 0.8314(10) 0.9753(7) 0.2492(6) 0.106(5) Uani 1 1 d . . .
H23A H 0.7676 0.9954 0.2480 0.127 Uiso 1 1 calc R . .
H23B H 0.8392 0.9403 0.2847 0.127 Uiso 1 1 calc R . .
C24 C 0.9054(11) 1.0294(7) 0.2652(7) 0.112(6) Uani 1 1 d . . .
H24A H 0.9684 1.0095 0.2658 0.138 Uiso 1 1 calc R . .
H24B H 0.9009 1.0498 0.3097 0.138 Uiso 1 1 calc R . .
H24C H 0.8961 1.0648 0.2309 0.138 Uiso 1 1 calc R . .
C25 C 0.0567(10) 0.6996(8) 0.4235(6) 0.078(4) Uani 1 1 d . . .
C26 C -0.0476(9) 0.7309(6) 0.4068(6) 0.068(3) Uani 1 1 d . . .
H26 H -0.0862 0.7154 0.4419 0.082 Uiso 1 1 calc R . .
C27 C 0.0737(8) 0.8202(6) 0.4157(6) 0.065(3) Uani 1 1 d . . .
H27 H 0.1003 0.8525 0.4533 0.078 Uiso 1 1 calc R . .
C28 C -0.1818(8) 0.6713(6) 0.3306(7) 0.059(3) Uani 1 1 d . . .
C29 C -0.2022(9) 0.6233(7) 0.3778(6) 0.080(4) Uani 1 1 d . . .
H29 H -0.1580 0.6183 0.4179 0.096 Uiso 1 1 calc R . .
C30 C -0.2839(10) 0.5828(6) 0.3686(6) 0.077(4) Uani 1 1 d . . .
H30 H -0.2941 0.5506 0.4020 0.092 Uiso 1 1 calc R . .
C31 C -0.3511(9) 0.5885(9) 0.3114(8) 0.101(5) Uani 1 1 d . . .
C32 C -0.3329(10) 0.6332(8) 0.2620(8) 0.103(5) Uani 1 1 d . . .
H32 H -0.3755 0.6346 0.2208 0.124 Uiso 1 1 calc R . .
C33 C -0.2515(10) 0.6773(7) 0.2718(7) 0.101(5) Uani 1 1 d . . .
H33 H -0.2433 0.7109 0.2393 0.121 Uiso 1 1 calc R . .
C34 C -0.0968(8) 0.8561(6) 0.4209(5) 0.051(3) Uani 1 1 d . . .
C35 C -0.1950(9) 0.8371(7) 0.4173(5) 0.070(4) Uani 1 1 d . . .
H35 H -0.2146 0.7904 0.4110 0.083 Uiso 1 1 calc R . .
C36 C -0.2648(9) 0.8898(9) 0.4234(6) 0.081(4) Uani 1 1 d . . .
H36 H -0.3298 0.8770 0.4220 0.098 Uiso 1 1 calc R . .
C37 C -0.2387(9) 0.9560(7) 0.4310(6) 0.066(3) Uani 1 1 d . . .
C38 C -0.1415(11) 0.9772(7) 0.4351(6) 0.080(4) Uani 1 1 d . . .
H38 H -0.1240 1.0243 0.4410 0.096 Uiso 1 1 calc R . .
C39 C -0.0703(9) 0.9272(7) 0.4303(5) 0.075(4) Uani 1 1 d . . .
H39 H -0.0055 0.9410 0.4334 0.089 Uiso 1 1 calc R . .
C40 C 0.2240(11) 0.7479(8) 0.4276(6) 0.072(4) Uani 1 1 d . . .
C41 C 0.2609(12) 0.6922(8) 0.3945(6) 0.085(4) Uani 1 1 d . . .
H41 H 0.2215 0.6578 0.3699 0.102 Uiso 1 1 calc R . .
C42 C 0.3615(12) 0.6917(8) 0.4011(7) 0.089(4) Uani 1 1 d . . .
H42 H 0.3889 0.6545 0.3804 0.106 Uiso 1 1 calc R . .
C43 C 0.4215(10) 0.7388(11) 0.4338(8) 0.104(6) Uani 1 1 d . . .
C44 C 0.3835(12) 0.7988(9) 0.4651(7) 0.103(5) Uani 1 1 d . . .
H44 H 0.4236 0.8344 0.4869 0.123 Uiso 1 1 calc R . .
C45 C 0.2876(10) 0.8000(7) 0.4609(6) 0.084(4) Uani 1 1 d . . .
H45 H 0.2606 0.8377 0.4813 0.100 Uiso 1 1 calc R . .
C46 C 0.0898(8) 0.8504(7) 0.3439(7) 0.072(4) Uani 1 1 d . . .
C47 C 0.1686(12) 0.9395(9) 0.2869(9) 0.125(7) Uani 1 1 d . . .
H47A H 0.1208 0.9276 0.2471 0.134 Uiso 1 1 calc R . .
H47B H 0.1760 0.9900 0.2907 0.134 Uiso 1 1 calc R . .
C48 C 0.2652(13) 0.9059(11) 0.2811(8) 0.127(10) Uani 1 1 d . . .
H48A H 0.3075 0.9111 0.3243 0.138 Uiso 1 1 calc R . .
H48B H 0.2944 0.9281 0.2455 0.138 Uiso 1 1 calc R . .
H48C H 0.2546 0.8570 0.2699 0.138 Uiso 1 1 calc R . .
C49 C 0.0698(9) 0.2388(8) 0.0799(6) 0.064(4) Uani 1 1 d . . .
C50 C -0.0311(8) 0.2602(5) 0.0853(5) 0.054(3) Uani 1 1 d . . .
H50 H -0.0743 0.2455 0.0433 0.065 Uiso 1 1 calc R . .
C51 C 0.0788(7) 0.3567(6) 0.1030(6) 0.061(3) Uani 1 1 d . . .
H51 H 0.0936 0.3936 0.0718 0.073 Uiso 1 1 calc R . .
C52 C -0.1455(8) 0.1843(6) 0.1393(6) 0.062(3) Uani 1 1 d . . .
C53 C -0.1568(7) 0.1339(6) 0.0889(6) 0.059(3) Uani 1 1 d . . .
H53 H -0.1112 0.1297 0.0589 0.071 Uiso 1 1 calc R . .
C54 C -0.2370(10) 0.0885(6) 0.0824(7) 0.083(4) Uani 1 1 d . . .
H54 H -0.2420 0.0529 0.0492 0.100 Uiso 1 1 calc R . .
C55 C -0.3089(9) 0.0943(7) 0.1230(8) 0.077(4) Uani 1 1 d . . .
C56 C -0.2944(8) 0.1435(7) 0.1758(7) 0.077(4) Uani 1 1 d . . .
H56 H -0.3385 0.1457 0.2071 0.093 Uiso 1 1 calc R . .
C57 C -0.2148(9) 0.1904(6) 0.1834(6) 0.064(3) Uani 1 1 d . . .
H57 H -0.2085 0.2251 0.2175 0.076 Uiso 1 1 calc R . .
C58 C -0.1017(9) 0.3824(6) 0.0836(5) 0.056(3) Uani 1 1 d . . .
C59 C -0.1948(9) 0.3558(6) 0.0745(5) 0.063(3) Uani 1 1 d . . .
H59 H -0.2060 0.3077 0.0729 0.075 Uiso 1 1 calc R . .
C60 C -0.2707(8) 0.4004(7) 0.0677(5) 0.067(3) Uani 1 1 d . . .
H60 H -0.3332 0.3812 0.0622 0.081 Uiso 1 1 calc R . .
C61 C -0.2610(8) 0.4693(7) 0.0684(6) 0.066(3) Uani 1 1 d . . .
C62 C -0.1649(10) 0.4963(6) 0.0784(5) 0.074(4) Uani 1 1 d . . .
H62 H -0.1550 0.5445 0.0805 0.089 Uiso 1 1 calc R . .
C63 C -0.0862(8) 0.4543(6) 0.0852(5) 0.059(3) Uani 1 1 d . . .
H63 H -0.0235 0.4733 0.0907 0.071 Uiso 1 1 calc R . .
C64 C 0.2322(9) 0.2923(7) 0.1005(6) 0.060(3) Uani 1 1 d . . .
C65 C 0.2799(11) 0.2332(8) 0.1167(6) 0.083(4) Uani 1 1 d . . .
H65 H 0.2452 0.1917 0.1196 0.099 Uiso 1 1 calc R . .
C66 C 0.3781(13) 0.2337(7) 0.1289(7) 0.097(5) Uani 1 1 d . . .
H66 H 0.4106 0.1919 0.1364 0.117 Uiso 1 1 calc R . .
C67 C 0.4293(8) 0.2944(10) 0.1302(6) 0.084(4) Uani 1 1 d . . .
C68 C 0.3820(11) 0.3563(8) 0.1132(7) 0.102(5) Uani 1 1 d . . .
H68 H 0.4168 0.3981 0.1119 0.123 Uiso 1 1 calc R . .
C69 C 0.2821(10) 0.3545(7) 0.0982(7) 0.097(5) Uani 1 1 d . . .
H69 H 0.2485 0.3953 0.0866 0.117 Uiso 1 1 calc R . .
C70 C 0.1085(8) 0.3807(8) 0.1791(7) 0.067(4) Uani 1 1 d . . .
C71 C 0.1714(10) 0.4763(9) 0.2557(7) 0.121(7) Uani 1 1 d D . .
H71A H 0.1332 0.4579 0.2892 0.131 Uiso 1 1 calc R . .
H71B H 0.1657 0.5268 0.2542 0.131 Uiso 1 1 calc R . .
C72 C 0.2752(13) 0.4552(11) 0.2711(10) 0.131(10) Uiso 1 1 d D . .
H72A H 0.2792 0.4055 0.2647 0.141 Uiso 1 1 calc R . .
H72B H 0.3006 0.4679 0.3179 0.141 Uiso 1 1 calc R . .
H72C H 0.3124 0.4785 0.2404 0.141 Uiso 1 1 calc R . .
C73 C 0.9165(8) 0.2132(7) 0.4074(6) 0.061(3) Uani 1 1 d . . .
C74 C 1.0197(8) 0.2385(6) 0.4021(6) 0.066(3) Uani 1 1 d . . .
H74 H 1.0633 0.2208 0.4417 0.079 Uiso 1 1 calc R . .
C75 C 0.9178(8) 0.3340(6) 0.3971(6) 0.062(3) Uani 1 1 d . . .
H75 H 0.9056 0.3681 0.4325 0.075 Uiso 1 1 calc R . .
C76 C 1.1321(8) 0.1741(6) 0.3384(7) 0.056(3) Uani 1 1 d . . .
C77 C 1.1744(10) 0.1322(7) 0.3914(6) 0.093(4) Uani 1 1 d . . .
H77 H 1.1455 0.1283 0.4310 0.112 Uiso 1 1 calc R . .
C78 C 1.2574(12) 0.0967(7) 0.3865(8) 0.103(5) Uani 1 1 d . . .
H78 H 1.2829 0.0678 0.4222 0.123 Uiso 1 1 calc R . .
C79 C 1.3044(8) 0.1029(7) 0.3289(10) 0.089(5) Uani 1 1 d . . .
C80 C 1.2588(12) 0.1393(9) 0.2770(7) 0.107(5) Uani 1 1 d . . .
H80 H 1.2846 0.1408 0.2358 0.129 Uiso 1 1 calc R . .
C81 C 1.1753(10) 0.1748(7) 0.2818(7) 0.081(4) Uani 1 1 d . . .
H81 H 1.1475 0.2005 0.2442 0.097 Uiso 1 1 calc R . .
C82 C 1.0952(8) 0.3601(6) 0.4230(5) 0.056(3) Uani 1 1 d . . .
C83 C 1.1888(8) 0.3340(6) 0.4278(5) 0.057(3) Uani 1 1 d . . .
H83 H 1.1992 0.2866 0.4211 0.068 Uiso 1 1 calc R . .
C84 C 1.2655(8) 0.3810(7) 0.4427(5) 0.070(4) Uani 1 1 d . . .
H84 H 1.3282 0.3639 0.4467 0.084 Uiso 1 1 calc R . .
C85 C 1.2548(9) 0.4515(7) 0.4521(5) 0.067(3) Uani 1 1 d . . .
C86 C 1.1600(10) 0.4753(6) 0.4438(6) 0.075(4) Uani 1 1 d . . .
H86 H 1.1501 0.5231 0.4472 0.090 Uiso 1 1 calc R . .
C87 C 1.0793(8) 0.4306(6) 0.4308(5) 0.061(3) Uani 1 1 d . . .
H87 H 1.0167 0.4477 0.4274 0.073 Uiso 1 1 calc R . .
C88 C 0.7559(8) 0.2753(7) 0.3882(5) 0.056(3) Uani 1 1 d . . .
C89 C 0.7028(10) 0.2162(7) 0.3572(6) 0.080(4) Uani 1 1 d . . .
H89 H 0.7357 0.1766 0.3462 0.096 Uiso 1 1 calc R . .
C90 C 0.6043(12) 0.2169(9) 0.3434(7) 0.109(6) Uani 1 1 d . . .
H90 H 0.5688 0.1779 0.3245 0.131 Uiso 1 1 calc R . .
C91 C 0.5588(9) 0.2772(10) 0.3584(6) 0.091(5) Uani 1 1 d . . .
C92 C 0.6101(11) 0.3335(7) 0.3916(7) 0.091(4) Uani 1 1 d . . .
H92 H 0.5778 0.3728 0.4039 0.110 Uiso 1 1 calc R . .
C93 C 0.7066(8) 0.3306(7) 0.4058(6) 0.081(4) Uani 1 1 d . . .
H93 H 0.7409 0.3683 0.4287 0.097 Uiso 1 1 calc R . .
C94 C 0.8881(9) 0.3652(7) 0.3213(8) 0.074(4) Uani 1 1 d . . .
C95 C 0.8303(10) 0.4669(8) 0.2618(8) 0.119(6) Uiso 1 1 d D . .
H95A H 0.7707 0.4916 0.2648 0.137 Uiso 1 1 calc R . .
H95B H 0.8203 0.4349 0.2224 0.137 Uiso 1 1 calc R . .
C96 C 0.9190(14) 0.5194(13) 0.2585(12) 0.125(13) Uiso 1 1 d D . .
H96A H 0.9396 0.5401 0.3033 0.138 Uiso 1 1 calc R . .
H96B H 0.8992 0.5555 0.2261 0.138 Uiso 1 1 calc R . .
H96C H 0.9720 0.4944 0.2439 0.138 Uiso 1 1 calc R . .
C97 C 0.5824(11) 0.8159(8) 0.2505(9) 0.153(9) Uani 1 1 d D . .
H97A H 0.6205 0.7982 0.2919 0.232 Uiso 1 1 calc R . .
H97B H 0.6165 0.8078 0.2115 0.232 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.1100(11) 0.1153(13) 0.1112(13) 0.0196(10) 0.0183(9) 0.0391(9)
Br2 0.1120(11) 0.0844(11) 0.1376(14) -0.0135(10) 0.0536(10) -0.0389(9)
Br3 0.0768(10) 0.1103(13) 0.1496(15) -0.0293(11) -0.0057(9) 0.0060(8)
Br4 0.1154(13) 0.232(2) 0.1480(18) 0.0315(15) -0.0158(12) -0.0742(14)
Br5 0.1122(12) 0.0929(12) 0.1698(17) -0.0048(11) 0.0026(11) 0.0337(9)
Br6 0.0963(12) 0.183(2) 0.1676(18) 0.0518(14) 0.0250(11) 0.0293(11)
Br7 0.1123(12) 0.1142(13) 0.1454(16) 0.0103(11) 0.0089(10) -0.0488(10)
Br8 0.0874(10) 0.0786(10) 0.1356(14) 0.0076(9) 0.0179(9) 0.0191(8)
Br9 0.0757(10) 0.1801(18) 0.1783(18) 0.0806(14) 0.0355(10) 0.0154(10)
Br10 0.1024(13) 0.1282(17) 0.303(3) 0.0115(17) 0.0465(14) 0.0328(11)
Br11 0.1023(10) 0.1042(12) 0.1014(12) 0.0106(9) 0.0081(9) -0.0368(9)
Br12 0.0812(11) 0.222(2) 0.1627(18) -0.0593(16) 0.0243(10) -0.0092(12)
O1 0.100(6) 0.042(5) 0.107(7) -0.005(5) 0.015(5) -0.011(5)
O2 0.187(9) 0.068(7) 0.068(7) 0.003(5) 0.029(6) -0.005(6)
O3 0.150(7) 0.047(6) 0.057(7) 0.003(5) 0.039(5) -0.008(5)
O4 0.123(7) 0.048(6) 0.117(8) 0.004(6) 0.033(5) -0.021(5)
O5 0.123(7) 0.089(7) 0.064(7) -0.012(5) 0.000(5) -0.050(6)
O6 0.125(7) 0.094(7) 0.057(6) 0.001(5) 0.010(5) -0.043(6)
O7 0.107(7) 0.073(7) 0.077(7) 0.009(5) 0.019(5) -0.010(6)
O8 0.116(7) 0.081(7) 0.077(7) 0.015(5) 0.019(6) -0.016(5)
O9 0.133(7) 0.085(7) 0.068(7) 0.000(6) 0.006(5) -0.052(6)
O10 0.105(7) 0.056(6) 0.107(8) 0.009(5) 0.020(5) -0.015(5)
O11 0.141(8) 0.085(8) 0.064(7) -0.014(6) 0.031(6) 0.004(6)
O12 0.127(7) 0.088(7) 0.047(6) 0.008(5) 0.005(5) 0.003(6)
N1 0.073(6) 0.074(7) 0.045(7) 0.013(5) 0.033(5) 0.020(6)
N2 0.065(7) 0.065(8) 0.067(7) 0.007(6) 0.019(5) -0.019(6)
N3 0.059(7) 0.041(6) 0.064(7) 0.014(5) 0.021(5) 0.016(5)
N4 0.095(7) 0.068(7) 0.049(7) 0.007(6) 0.006(6) -0.027(6)
N5 0.063(7) 0.045(7) 0.077(8) -0.009(5) 0.010(5) 0.010(5)
N6 0.082(8) 0.042(7) 0.072(8) 0.001(5) 0.013(6) -0.001(6)
N7 0.070(6) 0.053(6) 0.054(7) 0.013(5) -0.005(5) -0.004(5)
N8 0.056(7) 0.069(8) 0.064(7) 0.011(6) 0.000(5) -0.014(6)
N9 0.056(7) 0.029(6) 0.081(8) -0.005(5) 0.012(5) 0.002(5)
N10 0.069(6) 0.073(7) 0.053(7) 0.002(6) 0.002(5) 0.031(5)
N11 0.058(7) 0.058(7) 0.074(8) -0.005(6) -0.004(5) 0.011(6)
N12 0.046(6) 0.045(6) 0.092(8) 0.000(5) 0.018(5) 0.014(5)
Cl1 0.278(8) 0.238(9) 0.311(10) 0.048(7) 0.025(6) 0.012(7)
Cl2 0.224(6) 0.278(9) 0.287(9) 0.025(6) 0.041(6) -0.063(6)
C1 0.056(8) 0.075(10) 0.035(8) 0.010(7) 0.010(6) 0.010(8)
C2 0.080(9) 0.048(8) 0.044(8) 0.006(6) 0.010(7) -0.012(6)
C3 0.073(9) 0.057(8) 0.034(8) 0.003(6) 0.014(6) -0.007(7)
C4 0.056(8) 0.035(7) 0.055(9) 0.007(6) 0.006(7) 0.020(6)
C5 0.087(10) 0.074(10) 0.054(10) 0.003(8) 0.007(7) -0.012(8)
C6 0.126(12) 0.057(9) 0.036(9) 0.002(7) 0.010(9) -0.007(9)
C7 0.081(10) 0.071(9) 0.055(9) -0.009(8) 0.010(8) 0.013(7)
C8 0.079(10) 0.074(10) 0.085(12) 0.041(9) -0.029(8) 0.023(8)
C9 0.092(10) 0.060(9) 0.070(10) -0.002(7) 0.000(8) 0.007(8)
C10 0.041(7) 0.056(8) 0.057(8) -0.004(6) 0.003(6) 0.031(6)
C11 0.061(8) 0.053(8) 0.047(8) 0.008(6) -0.001(6) -0.007(7)
C12 0.053(8) 0.081(10) 0.082(10) -0.009(8) 0.024(7) 0.033(7)
C13 0.065(9) 0.078(10) 0.058(9) -0.001(7) 0.005(7) -0.015(8)
C14 0.086(10) 0.061(9) 0.070(10) 0.000(7) 0.015(8) 0.001(8)
C15 0.046(7) 0.055(8) 0.092(10) 0.002(7) 0.021(6) 0.019(6)
C16 0.058(8) 0.066(9) 0.044(8) -0.002(7) 0.016(6) 0.011(7)
C17 0.090(10) 0.030(8) 0.129(13) -0.005(7) 0.016(9) 0.001(7)
C18 0.064(10) 0.075(12) 0.189(17) -0.021(11) 0.032(10) -0.020(9)
C19 0.083(10) 0.067(10) 0.083(10) -0.030(8) 0.020(8) -0.010(9)
C20 0.067(10) 0.095(12) 0.106(12) 0.031(9) 0.002(8) 0.025(8)
C21 0.076(9) 0.038(8) 0.103(11) 0.021(7) 0.020(8) 0.018(7)
C22 0.077(9) 0.077(11) 0.064(12) 0.033(10) -0.012(8) -0.020(8)
C23 0.116(14) 0.080(11) 0.054(10) -0.016(9) 0.025(9) 0.013(10)
C24 0.142(17) 0.056(10) 0.088(12) -0.008(9) -0.008(11) -0.019(11)
C25 0.106(12) 0.076(11) 0.052(9) -0.011(8) 0.013(8) -0.050(11)
C26 0.102(11) 0.052(9) 0.049(9) 0.001(7) 0.010(8) -0.025(8)
C27 0.070(9) 0.057(9) 0.065(10) -0.021(7) 0.001(7) -0.016(7)
C28 0.062(8) 0.043(7) 0.075(11) 0.017(7) 0.021(8) 0.014(6)
C29 0.082(10) 0.096(11) 0.055(10) 0.006(8) -0.011(7) -0.026(8)
C30 0.099(10) 0.079(10) 0.053(10) 0.007(7) 0.014(8) -0.012(8)
C31 0.076(10) 0.158(15) 0.062(11) 0.034(10) -0.012(9) -0.024(9)
C32 0.109(12) 0.109(13) 0.077(12) 0.010(10) -0.031(9) -0.020(10)
C33 0.113(11) 0.097(11) 0.080(11) 0.046(9) -0.028(9) -0.011(9)
C34 0.049(8) 0.064(9) 0.038(7) 0.000(6) 0.000(6) 0.008(7)
C35 0.072(9) 0.080(10) 0.056(9) 0.004(7) 0.007(7) -0.023(8)
C36 0.084(10) 0.097(12) 0.061(10) 0.004(9) 0.004(7) -0.007(10)
C37 0.073(9) 0.064(10) 0.058(9) 0.000(7) -0.001(7) 0.012(7)
C38 0.118(12) 0.066(10) 0.058(9) 0.004(7) 0.017(8) 0.012(9)
C39 0.103(10) 0.061(10) 0.055(9) 0.006(7) 0.001(7) -0.022(9)
C40 0.102(12) 0.087(11) 0.027(8) 0.018(8) 0.005(8) -0.012(10)
C41 0.130(14) 0.076(11) 0.046(9) 0.003(8) -0.001(9) 0.004(10)
C42 0.081(11) 0.093(12) 0.096(12) 0.029(9) 0.015(9) 0.054(9)
C43 0.084(12) 0.147(17) 0.073(12) 0.055(11) -0.014(9) -0.043(12)
C44 0.090(13) 0.119(15) 0.099(13) 0.001(11) 0.016(10) -0.022(11)
C45 0.069(10) 0.102(12) 0.078(11) 0.006(9) 0.007(8) -0.015(9)
C46 0.088(9) 0.073(10) 0.045(10) -0.008(8) -0.013(8) -0.045(8)
C47 0.117(16) 0.108(16) 0.104(18) 0.017(13) 0.043(14) -0.038(14)
C48 0.12(2) 0.17(3) 0.049(13) 0.017(14) 0.051(14) -0.06(2)
C49 0.072(10) 0.060(10) 0.061(9) 0.018(8) 0.009(7) 0.029(9)
C50 0.087(9) 0.035(7) 0.036(8) 0.002(6) -0.002(6) 0.000(6)
C51 0.047(8) 0.068(9) 0.066(10) 0.016(7) -0.003(6) 0.022(6)
C52 0.065(9) 0.058(9) 0.060(9) 0.003(7) 0.000(7) -0.011(7)
C53 0.064(8) 0.049(8) 0.064(9) 0.001(7) 0.006(6) -0.001(6)
C54 0.111(11) 0.032(8) 0.096(12) -0.026(7) -0.017(9) 0.001(8)
C55 0.073(10) 0.060(9) 0.094(12) 0.002(8) 0.003(8) 0.013(7)
C56 0.056(8) 0.086(10) 0.092(11) -0.002(9) 0.024(7) -0.007(7)
C57 0.064(8) 0.055(8) 0.070(10) -0.001(7) 0.002(7) 0.027(7)
C58 0.066(9) 0.057(9) 0.044(8) 0.012(7) 0.008(6) -0.001(7)
C59 0.064(8) 0.047(8) 0.073(9) 0.007(6) -0.003(7) -0.020(7)
C60 0.078(9) 0.054(9) 0.066(9) 0.007(7) 0.000(7) -0.001(8)
C61 0.074(9) 0.063(10) 0.064(9) -0.001(7) 0.022(7) -0.006(7)
C62 0.100(10) 0.065(9) 0.057(9) 0.010(7) 0.008(8) 0.008(9)
C63 0.054(8) 0.067(9) 0.058(9) 0.020(7) 0.013(6) 0.000(7)
C64 0.056(9) 0.052(9) 0.069(9) 0.004(7) 0.001(7) 0.001(8)
C65 0.079(10) 0.099(13) 0.072(10) 0.008(9) 0.020(8) -0.021(10)
C66 0.129(14) 0.071(11) 0.097(12) 0.019(9) 0.033(10) -0.001(10)
C67 0.055(8) 0.127(14) 0.082(11) 0.035(10) 0.043(7) 0.011(9)
C68 0.110(13) 0.087(12) 0.118(13) 0.043(10) 0.040(10) -0.005(10)
C69 0.059(9) 0.105(13) 0.127(13) 0.029(9) 0.014(8) -0.024(8)
C70 0.060(8) 0.080(11) 0.061(11) 0.033(9) 0.004(7) -0.006(7)
C71 0.135(16) 0.150(19) 0.081(13) -0.001(13) 0.007(11) -0.083(14)
C73 0.058(9) 0.071(10) 0.052(9) -0.005(8) 0.003(6) 0.018(8)
C74 0.082(10) 0.053(9) 0.061(9) -0.015(7) 0.009(7) 0.004(7)
C75 0.072(9) 0.052(8) 0.065(10) -0.019(7) 0.021(7) 0.011(7)
C76 0.054(8) 0.055(8) 0.062(10) -0.003(7) 0.012(7) 0.030(6)
C77 0.119(12) 0.099(11) 0.064(11) 0.013(9) 0.016(9) 0.045(9)
C78 0.128(14) 0.096(12) 0.078(12) 0.000(10) -0.009(10) 0.046(10)
C79 0.059(9) 0.084(10) 0.126(15) 0.009(11) 0.016(10) 0.037(7)
C80 0.122(14) 0.128(14) 0.082(13) 0.037(10) 0.045(10) 0.016(11)
C81 0.078(10) 0.085(10) 0.083(12) 0.016(9) 0.022(9) 0.018(8)
C82 0.070(9) 0.048(8) 0.050(8) -0.001(6) 0.010(6) 0.016(7)
C83 0.060(8) 0.046(7) 0.068(9) 0.004(6) 0.017(6) 0.030(7)
C84 0.060(8) 0.085(11) 0.063(9) -0.010(8) 0.009(6) -0.002(8)
C85 0.094(10) 0.068(10) 0.037(8) 0.002(7) 0.011(7) -0.020(8)
C86 0.088(10) 0.069(9) 0.070(10) 0.017(7) 0.018(8) -0.004(9)
C87 0.059(8) 0.069(9) 0.054(9) 0.009(7) 0.003(6) 0.003(7)
C88 0.043(8) 0.081(10) 0.046(8) 0.012(7) 0.012(6) 0.028(7)
C89 0.079(10) 0.099(11) 0.068(10) -0.019(8) 0.037(8) -0.019(9)
C90 0.101(13) 0.131(15) 0.107(13) -0.062(11) 0.061(10) -0.024(11)
C91 0.080(10) 0.150(15) 0.045(9) -0.017(10) 0.028(7) -0.037(11)
C92 0.095(12) 0.096(12) 0.086(11) -0.006(9) 0.021(9) 0.004(9)
C93 0.030(8) 0.106(12) 0.106(11) 0.000(9) 0.005(7) 0.015(7)
C94 0.092(10) 0.035(9) 0.095(15) -0.005(9) 0.017(9) -0.018(8)
C97 0.24(2) 0.16(2) 0.161(19) -0.031(15) -0.018(15) 0.073(18)

_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
Br1 C7 1.876(11) . ?
Br2 C13 1.927(11) . ?
Br3 C19 1.905(12) . ?
Br4 C31 1.882(13) . ?
Br5 C37 1.857(11) . ?
Br6 C43 1.867(15) . ?
Br7 C55 1.836(12) . ?
Br8 C61 1.863(12) . ?
Br9 C67 1.909(11) . ?
Br10 C79 1.868(12) . ?
Br11 C85 1.847(11) . ?
Br12 C91 1.912(13) . ?
O1 C1 1.215(12) . ?
O2 C22 1.231(13) . ?
O3 C22 1.255(14) . ?
O3 C23 1.451(12) . ?
O4 C25 1.197(15) . ?
O5 C46 1.144(11) . ?
O6 C46 1.305(12) . ?
O6 C47 1.529(16) . ?
O7 C49 1.209(12) . ?
O8 C70 1.177(12) . ?
O9 C70 1.276(13) . ?
O9 C71 1.490(14) . ?
O10 C73 1.201(13) . ?
O11 C94 1.151(13) . ?
O12 C94 1.290(13) . ?
O12 C95 1.499(15) . ?
N1 C4 1.341(11) . ?
N1 C2 1.452(12) . ?
N1 H1 0.8600 . ?
N2 C10 1.413(12) . ?
N2 C3 1.421(12) . ?
N2 C2 1.439(12) . ?
N3 C1 1.330(12) . ?
N3 C16 1.444(11) . ?
N3 C3 1.455(12) . ?
N4 C28 1.364(11) . ?
N4 C26 1.436(11) . ?
N4 H4 0.8600 . ?
N5 C34 1.382(12) . ?
N5 C27 1.428(11) . ?
N5 C26 1.467(12) . ?
N6 C25 1.334(13) . ?
N6 C27 1.433(13) . ?
N6 C40 1.460(14) . ?
N7 C52 1.391(12) . ?
N7 C50 1.464(11) . ?
N7 H7 0.8600 . ?
N8 C58 1.396(12) . ?
N8 C51 1.458(11) . ?
N8 C50 1.465(12) . ?
N9 C49 1.334(14) . ?
N9 C64 1.408(12) . ?
N9 C51 1.438(11) . ?
N10 C76 1.355(11) . ?
N10 C74 1.435(12) . ?
N10 H10 0.8600 . ?
N11 C74 1.406(13) . ?
N11 C75 1.416(11) . ?
N11 C82 1.430(12) . ?
N12 C73 1.345(13) . ?
N12 C88 1.426(12) . ?
N12 C75 1.484(12) . ?
Cl1 C97 1.734(13) . ?
Cl2 C97 1.767(14) . ?
C1 C2 1.498(13) . ?
C2 H2 0.9800 . ?
C3 C22 1.535(16) . ?
C3 H3 0.9800 . ?
C4 C5 1.389(13) . ?
C4 C9 1.407(13) . ?
C5 C6 1.393(15) . ?
C5 H5 0.9300 . ?
C6 C7 1.348(13) . ?
C6 H6 0.9300 . ?
C7 C8 1.364(14) . ?
C8 C9 1.381(14) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.326(12) . ?
C10 C15 1.410(13) . ?
C11 C12 1.395(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.418(14) . ?
C12 H12 0.9300 . ?
C13 C14 1.333(13) . ?
C14 C15 1.395(13) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C21 1.376(13) . ?
C16 C17 1.403(14) . ?
C17 C18 1.324(13) . ?
C17 H17 0.9300 . ?
C18 C19 1.366(16) . ?
C18 H18 0.9300 . ?
C19 C20 1.358(15) . ?
C20 C21 1.361(13) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C23 C24 1.445(14) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.570(16) . ?
C26 H26 0.9800 . ?
C27 C46 1.574(15) . ?
C27 H27 0.9800 . ?
C28 C29 1.369(14) . ?
C28 C33 1.400(14) . ?
C29 C30 1.353(13) . ?
C29 H29 0.9300 . ?
C30 C31 1.357(14) . ?
C30 H30 0.9300 . ?
C31 C32 1.351(16) . ?
C32 C33 1.389(15) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 C35 1.400(12) . ?
C34 C39 1.405(14) . ?
C35 C36 1.428(15) . ?
C35 H35 0.9300 . ?
C36 C37 1.313(15) . ?
C36 H36 0.9300 . ?
C37 C38 1.396(14) . ?
C38 C39 1.400(14) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C41 1.384(15) . ?
C40 C45 1.408(15) . ?
C41 C42 1.386(15) . ?
C41 H41 0.9300 . ?
C42 C43 1.311(16) . ?
C42 H42 0.9300 . ?
C43 C44 1.437(19) . ?
C44 C45 1.325(15) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C47 C48 1.52(2) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 C50 1.489(14) . ?
C50 H50 0.9800 . ?
C51 C70 1.547(14) . ?
C51 H51 0.9800 . ?
C52 C53 1.360(13) . ?
C52 C57 1.392(13) . ?
C53 C54 1.391(13) . ?
C53 H53 0.9300 . ?
C54 C55 1.373(15) . ?
C54 H54 0.9300 . ?
C55 C56 1.378(15) . ?
C56 C57 1.402(13) . ?
C56 H56 0.9300 . ?
C57 H57 0.9300 . ?
C58 C59 1.369(12) . ?
C58 C63 1.388(14) . ?
C59 C60 1.361(13) . ?
C59 H59 0.9300 . ?
C60 C61 1.322(14) . ?
C60 H60 0.9300 . ?
C61 C62 1.411(13) . ?
C62 C63 1.361(13) . ?
C62 H62 0.9300 . ?
C63 H63 0.9300 . ?
C64 C65 1.338(15) . ?
C64 C69 1.372(14) . ?
C65 C66 1.352(14) . ?
C65 H65 0.9300 . ?
C66 C67 1.350(16) . ?
C66 H66 0.9300 . ?
C67 C68 1.387(16) . ?
C68 C69 1.377(14) . ?
C68 H68 0.9300 . ?
C69 H69 0.9300 . ?
C71 C72 1.495(14) . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C73 C74 1.527(14) . ?
C74 H74 0.9800 . ?
C75 C94 1.608(16) . ?
C75 H75 0.9800 . ?
C76 C81 1.339(14) . ?
C76 C77 1.386(15) . ?
C77 C78 1.365(15) . ?
C77 H77 0.9300 . ?
C78 C79 1.391(16) . ?
C78 H78 0.9300 . ?
C79 C80 1.330(16) . ?
C80 C81 1.370(17) . ?
C80 H80 0.9300 . ?
C81 H81 0.9300 . ?
C82 C87 1.379(13) . ?
C82 C83 1.394(12) . ?
C83 C84 1.379(13) . ?
C83 H83 0.9300 . ?
C84 C85 1.372(14) . ?
C84 H84 0.9300 . ?
C85 C86 1.390(14) . ?
C86 C87 1.390(13) . ?
C86 H86 0.9300 . ?
C87 H87 0.9300 . ?
C88 C93 1.338(14) . ?
C88 C89 1.417(14) . ?
C89 C90 1.358(14) . ?
C89 H89 0.9300 . ?
C90 C91 1.373(17) . ?
C90 H90 0.9300 . ?
C91 C92 1.381(15) . ?
C92 C93 1.333(13) . ?
C92 H92 0.9300 . ?
C93 H93 0.9300 . ?
C95 C96 1.589(15) . ?
C95 H95A 0.9700 . ?
C95 H95B 0.9700 . ?
C96 H96A 0.9600 . ?
C96 H96B 0.9600 . ?
C96 H96C 0.9600 . ?
C97 H97A 0.9700 . ?
C97 H97B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 O3 C23 120.5(11) . . ?
C46 O6 C47 114.8(10) . . ?
C70 O9 C71 121.6(11) . . ?
C94 O12 C95 116.5(11) . . ?
C4 N1 C2 120.6(9) . . ?
C4 N1 H1 119.7 . . ?
C2 N1 H1 119.7 . . ?
C10 N2 C3 126.4(10) . . ?
C10 N2 C2 120.6(10) . . ?
C3 N2 C2 109.8(8) . . ?
C1 N3 C16 129.1(10) . . ?
C1 N3 C3 111.7(9) . . ?
C16 N3 C3 119.2(9) . . ?
C28 N4 C26 123.2(10) . . ?
C28 N4 H4 118.4 . . ?
C26 N4 H4 118.4 . . ?
C34 N5 C27 125.3(9) . . ?
C34 N5 C26 124.6(10) . . ?
C27 N5 C26 109.8(9) . . ?
C25 N6 C27 114.3(11) . . ?
C25 N6 C40 125.1(12) . . ?
C27 N6 C40 120.4(10) . . ?
C52 N7 C50 122.0(9) . . ?
C52 N7 H7 119.0 . . ?
C50 N7 H7 119.0 . . ?
C58 N8 C51 126.0(9) . . ?
C58 N8 C50 125.9(9) . . ?
C51 N8 C50 108.0(9) . . ?
C49 N9 C64 125.8(10) . . ?
C49 N9 C51 111.4(10) . . ?
C64 N9 C51 121.9(9) . . ?
C76 N10 C74 124.8(10) . . ?
C76 N10 H10 117.6 . . ?
C74 N10 H10 117.6 . . ?
C74 N11 C75 111.0(9) . . ?
C74 N11 C82 127.1(10) . . ?
C75 N11 C82 121.7(10) . . ?
C73 N12 C88 131.8(10) . . ?
C73 N12 C75 110.3(9) . . ?
C88 N12 C75 117.1(10) . . ?
O1 C1 N3 127.2(11) . . ?
O1 C1 C2 124.5(11) . . ?
N3 C1 C2 108.3(11) . . ?
N2 C2 N1 111.8(9) . . ?
N2 C2 C1 104.6(10) . . ?
N1 C2 C1 115.3(9) . . ?
N2 C2 H2 108.3 . . ?
N1 C2 H2 108.3 . . ?
C1 C2 H2 108.3 . . ?
N2 C3 N3 105.2(9) . . ?
N2 C3 C22 110.2(9) . . ?
N3 C3 C22 111.8(10) . . ?
N2 C3 H3 109.8 . . ?
N3 C3 H3 109.8 . . ?
C22 C3 H3 109.8 . . ?
N1 C4 C5 123.7(12) . . ?
N1 C4 C9 123.4(12) . . ?
C5 C4 C9 112.8(10) . . ?
C4 C5 C6 123.2(11) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C7 C6 C5 120.0(12) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.9(11) . . ?
C6 C7 Br1 120.2(12) . . ?
C8 C7 Br1 118.9(11) . . ?
C7 C8 C9 117.7(11) . . ?
C7 C8 H8 121.1 . . ?
C9 C8 H8 121.1 . . ?
C8 C9 C4 125.2(11) . . ?
C8 C9 H9 117.4 . . ?
C4 C9 H9 117.4 . . ?
C11 C10 C15 121.0(11) . . ?
C11 C10 N2 121.4(11) . . ?
C15 C10 N2 117.6(9) . . ?
C10 C11 C12 121.3(11) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C13 117.1(9) . . ?
C11 C12 H12 121.4 . . ?
C13 C12 H12 121.4 . . ?
C14 C13 C12 122.1(11) . . ?
C14 C13 Br2 123.2(11) . . ?
C12 C13 Br2 114.7(10) . . ?
C13 C14 C15 119.7(12) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C14 C15 C10 118.6(10) . . ?
C14 C15 H15 120.7 . . ?
C10 C15 H15 120.7 . . ?
C21 C16 C17 115.2(10) . . ?
C21 C16 N3 124.1(11) . . ?
C17 C16 N3 120.7(11) . . ?
C18 C17 C16 123.5(12) . . ?
C18 C17 H17 118.3 . . ?
C16 C17 H17 118.3 . . ?
C17 C18 C19 117.8(12) . . ?
C17 C18 H18 121.1 . . ?
C19 C18 H18 121.1 . . ?
C20 C19 C18 123.2(12) . . ?
C20 C19 Br3 118.5(12) . . ?
C18 C19 Br3 118.3(11) . . ?
C19 C20 C21 116.9(12) . . ?
C19 C20 H20 121.5 . . ?
C21 C20 H20 121.5 . . ?
C20 C21 C16 123.4(11) . . ?
C20 C21 H21 118.3 . . ?
C16 C21 H21 118.3 . . ?
O2 C22 O3 126.4(14) . . ?
O2 C22 C3 117.6(14) . . ?
O3 C22 C3 115.2(12) . . ?
C24 C23 O3 110.0(12) . . ?
C24 C23 H23A 109.7 . . ?
O3 C23 H23A 109.7 . . ?
C24 C23 H23B 109.7 . . ?
O3 C23 H23B 109.7 . . ?
H23A C23 H23B 108.2 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O4 C25 N6 131.5(15) . . ?
O4 C25 C26 122.3(11) . . ?
N6 C25 C26 106.0(13) . . ?
N4 C26 N5 114.1(9) . . ?
N4 C26 C25 115.2(10) . . ?
N5 C26 C25 101.9(10) . . ?
N4 C26 H26 108.5 . . ?
N5 C26 H26 108.5 . . ?
C25 C26 H26 108.5 . . ?
N5 C27 N6 104.9(9) . . ?
N5 C27 C46 110.7(9) . . ?
N6 C27 C46 109.0(10) . . ?
N5 C27 H27 110.7 . . ?
N6 C27 H27 110.7 . . ?
C46 C27 H27 110.7 . . ?
N4 C28 C29 122.8(12) . . ?
N4 C28 C33 121.0(12) . . ?
C29 C28 C33 116.2(11) . . ?
C30 C29 C28 122.7(11) . . ?
C30 C29 H29 118.6 . . ?
C28 C29 H29 118.6 . . ?
C29 C30 C31 121.0(12) . . ?
C29 C30 H30 119.5 . . ?
C31 C30 H30 119.5 . . ?
C32 C31 C30 118.6(12) . . ?
C32 C31 Br4 120.3(11) . . ?
C30 C31 Br4 121.1(12) . . ?
C31 C32 C33 121.1(12) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C32 C33 C28 120.1(12) . . ?
C32 C33 H33 119.9 . . ?
C28 C33 H33 119.9 . . ?
N5 C34 C35 120.9(11) . . ?
N5 C34 C39 120.7(11) . . ?
C35 C34 C39 118.4(11) . . ?
C34 C35 C36 119.5(11) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
C37 C36 C35 121.1(12) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C36 C37 C38 121.2(12) . . ?
C36 C37 Br5 119.8(12) . . ?
C38 C37 Br5 119.1(11) . . ?
C37 C38 C39 119.7(12) . . ?
C37 C38 H38 120.2 . . ?
C39 C38 H38 120.2 . . ?
C38 C39 C34 120.2(12) . . ?
C38 C39 H39 119.9 . . ?
C34 C39 H39 119.9 . . ?
C41 C40 C45 119.8(14) . . ?
C41 C40 N6 119.1(13) . . ?
C45 C40 N6 121.0(14) . . ?
C40 C41 C42 114.5(13) . . ?
C40 C41 H41 122.8 . . ?
C42 C41 H41 122.8 . . ?
C43 C42 C41 126.2(15) . . ?
C43 C42 H42 116.9 . . ?
C41 C42 H42 116.9 . . ?
C42 C43 C44 119.6(16) . . ?
C42 C43 Br6 119.9(18) . . ?
C44 C43 Br6 120.5(14) . . ?
C45 C44 C43 115.6(14) . . ?
C45 C44 H44 122.2 . . ?
C43 C44 H44 122.2 . . ?
C44 C45 C40 124.2(14) . . ?
C44 C45 H45 117.9 . . ?
C40 C45 H45 117.9 . . ?
O5 C46 O6 128.8(13) . . ?
O5 C46 C27 121.0(11) . . ?
O6 C46 C27 110.3(10) . . ?
C48 C47 O6 104.6(14) . . ?
C48 C47 H47A 110.8 . . ?
O6 C47 H47A 110.8 . . ?
C48 C47 H47B 110.8 . . ?
O6 C47 H47B 110.8 . . ?
H47A C47 H47B 108.9 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O7 C49 N9 127.8(12) . . ?
O7 C49 C50 122.3(12) . . ?
N9 C49 C50 109.9(11) . . ?
N7 C50 N8 110.7(8) . . ?
N7 C50 C49 114.3(9) . . ?
N8 C50 C49 103.5(10) . . ?
N7 C50 H50 109.4 . . ?
N8 C50 H50 109.4 . . ?
C49 C50 H50 109.4 . . ?
N9 C51 N8 105.1(9) . . ?
N9 C51 C70 109.1(9) . . ?
N8 C51 C70 111.5(9) . . ?
N9 C51 H51 110.3 . . ?
N8 C51 H51 110.3 . . ?
C70 C51 H51 110.3 . . ?
C53 C52 N7 121.8(12) . . ?
C53 C52 C57 119.5(10) . . ?
N7 C52 C57 118.6(12) . . ?
C52 C53 C54 119.7(11) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C55 C54 C53 122.7(12) . . ?
C55 C54 H54 118.7 . . ?
C53 C54 H54 118.7 . . ?
C54 C55 C56 116.9(11) . . ?
C54 C55 Br7 121.9(12) . . ?
C56 C55 Br7 121.2(11) . . ?
C55 C56 C57 121.5(11) . . ?
C55 C56 H56 119.2 . . ?
C57 C56 H56 119.2 . . ?
C52 C57 C56 119.4(11) . . ?
C52 C57 H57 120.3 . . ?
C56 C57 H57 120.3 . . ?
C59 C58 C63 119.6(11) . . ?
C59 C58 N8 119.5(11) . . ?
C63 C58 N8 120.9(11) . . ?
C60 C59 C58 119.4(11) . . ?
C60 C59 H59 120.3 . . ?
C58 C59 H59 120.3 . . ?
C61 C60 C59 124.1(11) . . ?
C61 C60 H60 117.9 . . ?
C59 C60 H60 117.9 . . ?
C60 C61 C62 116.1(11) . . ?
C60 C61 Br8 123.5(10) . . ?
C62 C61 Br8 120.3(10) . . ?
C63 C62 C61 122.5(11) . . ?
C63 C62 H62 118.8 . . ?
C61 C62 H62 118.8 . . ?
C62 C63 C58 118.3(11) . . ?
C62 C63 H63 120.8 . . ?
C58 C63 H63 120.8 . . ?
C65 C64 C69 120.6(12) . . ?
C65 C64 N9 121.6(12) . . ?
C69 C64 N9 117.6(12) . . ?
C64 C65 C66 120.3(13) . . ?
C64 C65 H65 119.9 . . ?
C66 C65 H65 119.9 . . ?
C67 C66 C65 120.7(14) . . ?
C67 C66 H66 119.7 . . ?
C65 C66 H66 119.7 . . ?
C66 C67 C68 120.1(12) . . ?
C66 C67 Br9 120.7(14) . . ?
C68 C67 Br9 119.2(13) . . ?
C69 C68 C67 118.4(13) . . ?
C69 C68 H68 120.8 . . ?
C67 C68 H68 120.8 . . ?
C64 C69 C68 119.8(13) . . ?
C64 C69 H69 120.1 . . ?
C68 C69 H69 120.1 . . ?
O8 C70 O9 124.8(14) . . ?
O8 C70 C51 121.3(13) . . ?
O9 C70 C51 113.9(12) . . ?
O9 C71 C72 101.0(14) . . ?
O9 C71 H71A 111.6 . . ?
C72 C71 H71A 111.6 . . ?
O9 C71 H71B 111.6 . . ?
C72 C71 H71B 111.6 . . ?
H71A C71 H71B 109.4 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O10 C73 N12 124.7(12) . . ?
O10 C73 C74 127.6(11) . . ?
N12 C73 C74 107.7(11) . . ?
N11 C74 N10 115.6(10) . . ?
N11 C74 C73 103.6(10) . . ?
N10 C74 C73 112.7(9) . . ?
N11 C74 H74 108.2 . . ?
N10 C74 H74 108.2 . . ?
C73 C74 H74 108.2 . . ?
N11 C75 N12 104.2(9) . . ?
N11 C75 C94 113.4(9) . . ?
N12 C75 C94 107.8(9) . . ?
N11 C75 H75 110.4 . . ?
N12 C75 H75 110.4 . . ?
C94 C75 H75 110.4 . . ?
C81 C76 N10 118.5(13) . . ?
C81 C76 C77 116.0(11) . . ?
N10 C76 C77 125.5(13) . . ?
C78 C77 C76 121.5(13) . . ?
C78 C77 H77 119.3 . . ?
C76 C77 H77 119.3 . . ?
C77 C78 C79 120.9(13) . . ?
C77 C78 H78 119.5 . . ?
C79 C78 H78 119.5 . . ?
C80 C79 C78 116.3(13) . . ?
C80 C79 Br10 125.1(16) . . ?
C78 C79 Br10 118.6(14) . . ?
C79 C80 C81 122.5(14) . . ?
C79 C80 H80 118.8 . . ?
C81 C80 H80 118.8 . . ?
C76 C81 C80 122.5(13) . . ?
C76 C81 H81 118.7 . . ?
C80 C81 H81 118.7 . . ?
C87 C82 C83 121.5(10) . . ?
C87 C82 N11 120.5(10) . . ?
C83 C82 N11 118.0(11) . . ?
C84 C83 C82 117.6(11) . . ?
C84 C83 H83 121.2 . . ?
C82 C83 H83 121.2 . . ?
C85 C84 C83 123.9(11) . . ?
C85 C84 H84 118.1 . . ?
C83 C84 H84 118.1 . . ?
C84 C85 C86 116.3(11) . . ?
C84 C85 Br11 119.7(11) . . ?
C86 C85 Br11 123.9(11) . . ?
C85 C86 C87 122.8(12) . . ?
C85 C86 H86 118.6 . . ?
C87 C86 H86 118.6 . . ?
C82 C87 C86 117.9(11) . . ?
C82 C87 H87 121.0 . . ?
C86 C87 H87 121.0 . . ?
C93 C88 C89 118.5(11) . . ?
C93 C88 N12 125.0(12) . . ?
C89 C88 N12 116.4(12) . . ?
C90 C89 C88 120.6(12) . . ?
C90 C89 H89 119.7 . . ?
C88 C89 H89 119.7 . . ?
C89 C90 C91 117.8(13) . . ?
C89 C90 H90 121.1 . . ?
C91 C90 H90 121.1 . . ?
C90 C91 C92 121.5(13) . . ?
C90 C91 Br12 119.3(13) . . ?
C92 C91 Br12 119.1(14) . . ?
C93 C92 C91 119.1(13) . . ?
C93 C92 H92 120.5 . . ?
C91 C92 H92 120.5 . . ?
C92 C93 C88 122.3(12) . . ?
C92 C93 H93 118.9 . . ?
C88 C93 H93 118.9 . . ?
O11 C94 O12 131.8(15) . . ?
O11 C94 C75 119.0(13) . . ?
O12 C94 C75 108.9(12) . . ?
O12 C95 C96 100.2(13) . . ?
O12 C95 H95A 111.7 . . ?
C96 C95 H95A 111.7 . . ?
O12 C95 H95B 111.7 . . ?
C96 C95 H95B 111.7 . . ?
H95A C95 H95B 109.5 . . ?
C95 C96 H96A 109.5 . . ?
C95 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
C95 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
Cl1 C97 Cl2 101.2(9) . . ?
Cl1 C97 H97A 111.5 . . ?
Cl2 C97 H97A 111.5 . . ?
Cl1 C97 H97B 111.5 . . ?
Cl2 C97 H97B 111.5 . . ?
H97A C97 H97B 109.4 . . ?

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
C16 N3 C1 O1 1.5(18) . . . . ?
C3 N3 C1 O1 178.7(11) . . . . ?
C16 N3 C1 C2 -177.9(9) . . . . ?
C3 N3 C1 C2 -0.6(12) . . . . ?
C10 N2 C2 N1 80.0(12) . . . . ?
C3 N2 C2 N1 -119.0(10) . . . . ?
C10 N2 C2 C1 -154.6(9) . . . . ?
C3 N2 C2 C1 6.4(11) . . . . ?
C4 N1 C2 N2 -130.7(10) . . . . ?
C4 N1 C2 C1 110.0(12) . . . . ?
O1 C1 C2 N2 177.2(10) . . . . ?
N3 C1 C2 N2 -3.5(11) . . . . ?
O1 C1 C2 N1 -59.7(15) . . . . ?
N3 C1 C2 N1 119.7(10) . . . . ?
C10 N2 C3 N3 152.9(9) . . . . ?
C2 N2 C3 N3 -6.8(11) . . . . ?
C10 N2 C3 C22 -86.4(13) . . . . ?
C2 N2 C3 C22 113.9(11) . . . . ?
C1 N3 C3 N2 4.6(12) . . . . ?
C16 N3 C3 N2 -177.9(8) . . . . ?
C1 N3 C3 C22 -115.0(11) . . . . ?
C16 N3 C3 C22 62.5(12) . . . . ?
C2 N1 C4 C5 -39.3(15) . . . . ?
C2 N1 C4 C9 137.3(10) . . . . ?
N1 C4 C5 C6 172.7(11) . . . . ?
C9 C4 C5 C6 -4.3(16) . . . . ?
C4 C5 C6 C7 1.6(18) . . . . ?
C5 C6 C7 C8 3.0(18) . . . . ?
C5 C6 C7 Br1 -177.0(9) . . . . ?
C6 C7 C8 C9 -4.2(18) . . . . ?
Br1 C7 C8 C9 175.8(9) . . . . ?
C7 C8 C9 C4 1.1(18) . . . . ?
N1 C4 C9 C8 -174.1(11) . . . . ?
C5 C4 C9 C8 2.9(16) . . . . ?
C3 N2 C10 C11 -173.7(10) . . . . ?
C2 N2 C10 C11 -16.0(15) . . . . ?
C3 N2 C10 C15 8.2(15) . . . . ?
C2 N2 C10 C15 165.9(9) . . . . ?
C15 C10 C11 C12 1.0(16) . . . . ?
N2 C10 C11 C12 -177.0(9) . . . . ?
C10 C11 C12 C13 0.1(16) . . . . ?
C11 C12 C13 C14 -2.5(17) . . . . ?
C11 C12 C13 Br2 179.7(8) . . . . ?
C12 C13 C14 C15 3.6(17) . . . . ?
Br2 C13 C14 C15 -178.7(8) . . . . ?
C13 C14 C15 C10 -2.4(17) . . . . ?
C11 C10 C15 C14 0.2(16) . . . . ?
N2 C10 C15 C14 178.2(9) . . . . ?
C1 N3 C16 C21 -162.9(11) . . . . ?
C3 N3 C16 C21 20.1(14) . . . . ?
C1 N3 C16 C17 16.1(16) . . . . ?
C3 N3 C16 C17 -160.9(10) . . . . ?
C21 C16 C17 C18 -0.2(18) . . . . ?
N3 C16 C17 C18 -179.3(11) . . . . ?
C16 C17 C18 C19 0(2) . . . . ?
C17 C18 C19 C20 0(2) . . . . ?
C17 C18 C19 Br3 -178.7(10) . . . . ?
C18 C19 C20 C21 -1(2) . . . . ?
Br3 C19 C20 C21 178.3(9) . . . . ?
C19 C20 C21 C16 0.8(19) . . . . ?
C17 C16 C21 C20 -0.3(17) . . . . ?
N3 C16 C21 C20 178.8(10) . . . . ?
C23 O3 C22 O2 -2.0(19) . . . . ?
C23 O3 C22 C3 -171.6(10) . . . . ?
N2 C3 C22 O2 -75.4(13) . . . . ?
N3 C3 C22 O2 41.2(15) . . . . ?
N2 C3 C22 O3 95.1(12) . . . . ?
N3 C3 C22 O3 -148.3(10) . . . . ?
C22 O3 C23 C24 132.6(12) . . . . ?
C27 N6 C25 O4 -179.5(14) . . . . ?
C40 N6 C25 O4 5(2) . . . . ?
C27 N6 C25 C26 4.7(13) . . . . ?
C40 N6 C25 C26 -170.6(9) . . . . ?
C28 N4 C26 N5 -129.2(11) . . . . ?
C28 N4 C26 C25 113.5(12) . . . . ?
C34 N5 C26 N4 67.5(14) . . . . ?
C27 N5 C26 N4 -106.7(11) . . . . ?
C34 N5 C26 C25 -167.8(9) . . . . ?
C27 N5 C26 C25 18.1(11) . . . . ?
O4 C25 C26 N4 -65.9(16) . . . . ?
N6 C25 C26 N4 110.4(10) . . . . ?
O4 C25 C26 N5 170.1(12) . . . . ?
N6 C25 C26 N5 -13.6(12) . . . . ?
C34 N5 C27 N6 170.0(9) . . . . ?
C26 N5 C27 N6 -16.0(12) . . . . ?
C34 N5 C27 C46 -72.5(12) . . . . ?
C26 N5 C27 C46 101.5(11) . . . . ?
C25 N6 C27 N5 6.6(13) . . . . ?
C40 N6 C27 N5 -177.9(9) . . . . ?
C25 N6 C27 C46 -112.0(11) . . . . ?
C40 N6 C27 C46 63.5(12) . . . . ?
C26 N4 C28 C29 -25.8(17) . . . . ?
C26 N4 C28 C33 152.8(12) . . . . ?
N4 C28 C29 C30 179.8(11) . . . . ?
C33 C28 C29 C30 1.0(18) . . . . ?
C28 C29 C30 C31 -1(2) . . . . ?
C29 C30 C31 C32 3(2) . . . . ?
C29 C30 C31 Br4 -175.7(10) . . . . ?
C30 C31 C32 C33 -6(2) . . . . ?
Br4 C31 C32 C33 173.0(11) . . . . ?
C31 C32 C33 C28 6(2) . . . . ?
N4 C28 C33 C32 177.5(12) . . . . ?
C29 C28 C33 C32 -3.7(19) . . . . ?
C27 N5 C34 C35 175.6(10) . . . . ?
C26 N5 C34 C35 2.4(15) . . . . ?
C27 N5 C34 C39 -6.2(16) . . . . ?
C26 N5 C34 C39 -179.4(10) . . . . ?
N5 C34 C35 C36 178.1(10) . . . . ?
C39 C34 C35 C36 -0.1(15) . . . . ?
C34 C35 C36 C37 1.3(18) . . . . ?
C35 C36 C37 C38 -1.6(19) . . . . ?
C35 C36 C37 Br5 178.0(8) . . . . ?
C36 C37 C38 C39 0.7(18) . . . . ?
Br5 C37 C38 C39 -178.9(8) . . . . ?
C37 C38 C39 C34 0.5(17) . . . . ?
N5 C34 C39 C38 -179.0(10) . . . . ?
C35 C34 C39 C38 -0.8(16) . . . . ?
C25 N6 C40 C41 34.9(16) . . . . ?
C27 N6 C40 C41 -140.0(12) . . . . ?
C25 N6 C40 C45 -148.4(12) . . . . ?
C27 N6 C40 C45 36.7(15) . . . . ?
C45 C40 C41 C42 3.4(17) . . . . ?
N6 C40 C41 C42 -179.9(9) . . . . ?
C40 C41 C42 C43 -1(2) . . . . ?
C41 C42 C43 C44 -2(2) . . . . ?
C41 C42 C43 Br6 179.8(10) . . . . ?
C42 C43 C44 C45 3(2) . . . . ?
Br6 C43 C44 C45 -178.7(9) . . . . ?
C43 C44 C45 C40 -1(2) . . . . ?
C41 C40 C45 C44 -2.3(19) . . . . ?
N6 C40 C45 C44 -179.0(12) . . . . ?
C47 O6 C46 O5 -6(2) . . . . ?
C47 O6 C46 C27 173.2(11) . . . . ?
N5 C27 C46 O5 -55.0(16) . . . . ?
N6 C27 C46 O5 59.9(15) . . . . ?
N5 C27 C46 O6 125.9(10) . . . . ?
N6 C27 C46 O6 -119.2(11) . . . . ?
C46 O6 C47 C48 -87.1(15) . . . . ?
C64 N9 C49 O7 -13(2) . . . . ?
C51 N9 C49 O7 177.4(11) . . . . ?
C64 N9 C49 C50 169.2(9) . . . . ?
C51 N9 C49 C50 -0.6(13) . . . . ?
C52 N7 C50 N8 130.8(10) . . . . ?
C52 N7 C50 C49 -112.8(12) . . . . ?
C58 N8 C50 N7 -67.6(12) . . . . ?
C51 N8 C50 N7 108.8(10) . . . . ?
C58 N8 C50 C49 169.5(10) . . . . ?
C51 N8 C50 C49 -14.1(11) . . . . ?
O7 C49 C50 N7 70.5(14) . . . . ?
N9 C49 C50 N7 -111.3(10) . . . . ?
O7 C49 C50 N8 -169.0(11) . . . . ?
N9 C49 C50 N8 9.2(12) . . . . ?
C49 N9 C51 N8 -8.3(12) . . . . ?
C64 N9 C51 N8 -178.6(9) . . . . ?
C49 N9 C51 C70 111.3(10) . . . . ?
C64 N9 C51 C70 -58.9(13) . . . . ?
C58 N8 C51 N9 -169.6(9) . . . . ?
C50 N8 C51 N9 14.0(11) . . . . ?
C58 N8 C51 C70 72.3(13) . . . . ?
C50 N8 C51 C70 -104.1(10) . . . . ?
C50 N7 C52 C53 34.3(15) . . . . ?
C50 N7 C52 C57 -141.7(10) . . . . ?
N7 C52 C53 C54 -176.6(10) . . . . ?
C57 C52 C53 C54 -0.6(16) . . . . ?
C52 C53 C54 C55 3.1(18) . . . . ?
C53 C54 C55 C56 -5.8(19) . . . . ?
C53 C54 C55 Br7 177.4(8) . . . . ?
C54 C55 C56 C57 6.2(19) . . . . ?
Br7 C55 C56 C57 -177.0(8) . . . . ?
C53 C52 C57 C56 1.1(17) . . . . ?
N7 C52 C57 C56 177.2(9) . . . . ?
C55 C56 C57 C52 -4.0(17) . . . . ?
C51 N8 C58 C59 -175.7(10) . . . . ?
C50 N8 C58 C59 0.1(16) . . . . ?
C51 N8 C58 C63 6.5(16) . . . . ?
C50 N8 C58 C63 -177.7(10) . . . . ?
C63 C58 C59 C60 -0.6(16) . . . . ?
N8 C58 C59 C60 -178.4(10) . . . . ?
C58 C59 C60 C61 0.9(18) . . . . ?
C59 C60 C61 C62 -1.4(18) . . . . ?
C59 C60 C61 Br8 -177.4(9) . . . . ?
C60 C61 C62 C63 1.7(17) . . . . ?
Br8 C61 C62 C63 177.8(8) . . . . ?
C61 C62 C63 C58 -1.4(17) . . . . ?
C59 C58 C63 C62 0.9(16) . . . . ?
N8 C58 C63 C62 178.6(9) . . . . ?
C49 N9 C64 C65 -16.5(18) . . . . ?
C51 N9 C64 C65 152.3(11) . . . . ?
C49 N9 C64 C69 168.5(12) . . . . ?
C51 N9 C64 C69 -22.8(16) . . . . ?
C69 C64 C65 C66 -2(2) . . . . ?
N9 C64 C65 C66 -177.1(11) . . . . ?
C64 C65 C66 C67 5(2) . . . . ?
C65 C66 C67 C68 -6(2) . . . . ?
C65 C66 C67 Br9 174.1(9) . . . . ?
C66 C67 C68 C69 3(2) . . . . ?
Br9 C67 C68 C69 -176.7(10) . . . . ?
C65 C64 C69 C68 0(2) . . . . ?
N9 C64 C69 C68 174.7(11) . . . . ?
C67 C68 C69 C64 0(2) . . . . ?
C71 O9 C70 O8 0(2) . . . . ?
C71 O9 C70 C51 177.9(10) . . . . ?
N9 C51 C70 O8 -58.2(15) . . . . ?
N8 C51 C70 O8 57.5(15) . . . . ?
N9 C51 C70 O9 123.8(11) . . . . ?
N8 C51 C70 O9 -120.5(11) . . . . ?
C70 O9 C71 C72 88.7(16) . . . . ?
C88 N12 C73 O10 -14(2) . . . . ?
C75 N12 C73 O10 177.1(12) . . . . ?
C88 N12 C73 C74 165.0(10) . . . . ?
C75 N12 C73 C74 -4.2(12) . . . . ?
C75 N11 C74 N10 105.0(11) . . . . ?
C82 N11 C74 N10 -69.9(14) . . . . ?
C75 N11 C74 C73 -18.7(12) . . . . ?
C82 N11 C74 C73 166.3(10) . . . . ?
C76 N10 C74 N11 120.8(12) . . . . ?
C76 N10 C74 C73 -120.4(12) . . . . ?
O10 C73 C74 N11 -167.5(12) . . . . ?
N12 C73 C74 N11 13.8(12) . . . . ?
O10 C73 C74 N10 66.8(16) . . . . ?
N12 C73 C74 N10 -111.9(11) . . . . ?
C74 N11 C75 N12 16.5(12) . . . . ?
C82 N11 C75 N12 -168.2(9) . . . . ?
C74 N11 C75 C94 -100.4(11) . . . . ?
C82 N11 C75 C94 74.9(12) . . . . ?
C73 N12 C75 N11 -7.0(12) . . . . ?
C88 N12 C75 N11 -177.9(8) . . . . ?
C73 N12 C75 C94 113.7(10) . . . . ?
C88 N12 C75 C94 -57.2(12) . . . . ?
C74 N10 C76 C81 -156.9(11) . . . . ?
C74 N10 C76 C77 22.2(18) . . . . ?
C81 C76 C77 C78 2.8(19) . . . . ?
N10 C76 C77 C78 -176.3(12) . . . . ?
C76 C77 C78 C79 2(2) . . . . ?
C77 C78 C79 C80 -7(2) . . . . ?
C77 C78 C79 Br10 175.3(10) . . . . ?
C78 C79 C80 C81 6(2) . . . . ?
Br10 C79 C80 C81 -175.5(10) . . . . ?
N10 C76 C81 C80 176.1(12) . . . . ?
C77 C76 C81 C80 -3(2) . . . . ?
C79 C80 C81 C76 -2(2) . . . . ?
C74 N11 C82 C87 -178.7(10) . . . . ?
C75 N11 C82 C87 6.8(15) . . . . ?
C74 N11 C82 C83 1.2(16) . . . . ?
C75 N11 C82 C83 -173.3(9) . . . . ?
C87 C82 C83 C84 1.9(15) . . . . ?
N11 C82 C83 C84 -177.9(10) . . . . ?
C82 C83 C84 C85 -0.9(17) . . . . ?
C83 C84 C85 C86 -1.7(17) . . . . ?
C83 C84 C85 Br11 -177.7(9) . . . . ?
C84 C85 C86 C87 3.6(17) . . . . ?
Br11 C85 C86 C87 179.4(8) . . . . ?
C83 C82 C87 C86 -0.2(16) . . . . ?
N11 C82 C87 C86 179.6(10) . . . . ?
C85 C86 C87 C82 -2.7(17) . . . . ?
C73 N12 C88 C93 156.1(12) . . . . ?
C75 N12 C88 C93 -35.3(15) . . . . ?
C73 N12 C88 C89 -20.5(16) . . . . ?
C75 N12 C88 C89 148.1(10) . . . . ?
C93 C88 C89 C90 2.5(18) . . . . ?
N12 C88 C89 C90 179.3(11) . . . . ?
C88 C89 C90 C91 2(2) . . . . ?
C89 C90 C91 C92 -5(2) . . . . ?
C89 C90 C91 Br12 177.2(9) . . . . ?
C90 C91 C92 C93 4(2) . . . . ?
Br12 C91 C92 C93 -178.6(9) . . . . ?
C91 C92 C93 C88 1(2) . . . . ?
C89 C88 C93 C92 -4.0(18) . . . . ?
N12 C88 C93 C92 179.5(11) . . . . ?
C95 O12 C94 O11 10(2) . . . . ?
C95 O12 C94 C75 -176.3(9) . . . . ?
N11 C75 C94 O11 56.9(15) . . . . ?
N12 C75 C94 O11 -57.9(14) . . . . ?
N11 C75 C94 O12 -117.5(11) . . . . ?
N12 C75 C94 O12 127.7(10) . . . . ?
C94 O12 C95 C96 -111.2(14) . . . . ?

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 O5 0.86 2.38 3.048(12) 135.4 1_655
N4 H4 O5 0.86 2.65 3.268(11) 130.3 .
N7 H7 O8 0.86 2.69 3.310(11) 130.4 .
N1 H1 O2 0.86 3.18 3.698(12) 121.3 .
N4 H4 O5 0.86 2.65 3.268(11) 130.3 .
N10 H10 O11 0.86 2.68 3.295(13) 129.1 .
N7 H7 O11 0.86 2.56 3.206(12) 132.7 1_455

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.107