# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_bo4267
_database_code_depnum_ccdc_archive 'CCDC 1446037'
_audit_update_record             
;
2016-01-08 deposited with the CCDC.
2016-03-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
"(3aS,3'R,4S,6R,6aS)-Tri-tert-butyl 4-(2-bromophenyl)-1,2',3-trioxo-3a,4,6,6a-tetrahydro -1H-spiro[cyclopenta[c]pyrrole-5,3'-indoline]-1',2,6(3H)-tricarboxylate"
_chemical_name_common            ?
_chemical_melting_point          141-142
_chemical_formula_moiety         C35H39BrN2O9
_chemical_formula_sum            'C35 H39 Br N2 O9'
_chemical_formula_weight         711.59

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   12.919(2)
_cell_length_b                   15.875(3)
_cell_length_c                   17.332(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3554.7(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    14245
_cell_measurement_theta_min      2.032
_cell_measurement_theta_max      31.507

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_type   Multi-scans
_exptl_absorpt_correction_T_min  0.7128
_exptl_absorpt_correction_T_max  0.8115
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  AFC10/Saturn724+
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            35914
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.82
_diffrn_reflns_theta_max         31.50
_reflns_number_total             11767
_reflns_number_gt                9833
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0095P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_number_reflns         11767
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.0559
_refine_ls_wR_factor_gt          0.0524
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_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
Br1 Br 0.507313(16) 0.241695(13) 0.287764(10) 0.03492(5) Uani 1 1 d . . .
O1 O 0.45282(11) 0.46268(8) 0.59614(8) 0.0375(4) Uani 1 1 d . . .
O2 O 0.26530(11) 0.43623(9) 0.37396(8) 0.0387(4) Uani 1 1 d . . .
O3 O 0.56306(10) 0.17184(8) 0.46958(7) 0.0257(3) Uani 1 1 d . . .
O4 O 0.35143(11) 0.61105(8) 0.50162(8) 0.0334(3) Uani 1 1 d . . .
O5 O 0.44432(11) 0.55978(9) 0.40110(8) 0.0376(4) Uani 1 1 d . . .
O6 O 0.46073(10) 0.16085(8) 0.65076(7) 0.0286(3) Uani 1 1 d . . .
O7 O 0.37988(12) 0.27314(9) 0.70472(8) 0.0500(4) Uani 1 1 d . . .
O8 O 0.56235(10) 0.02707(8) 0.39208(7) 0.0317(3) Uani 1 1 d . . .
O9 O 0.44287(13) -0.06884(8) 0.42990(9) 0.0467(4) Uani 1 1 d . . .
N1 N 0.35783(12) 0.47026(10) 0.48349(9) 0.0260(4) Uani 1 1 d . . .
N2 N 0.43539(12) 0.06749(9) 0.47226(9) 0.0240(3) Uani 1 1 d . . .
C1 C 0.39197(16) 0.43168(12) 0.55148(11) 0.0278(4) Uani 1 1 d . . .
C2 C 0.34147(15) 0.34514(11) 0.55531(11) 0.0245(4) Uani 1 1 d . . .
H2 H 0.2867 0.3449 0.5961 0.029 Uiso 1 1 calc R . .
C3 C 0.41644(13) 0.27117(10) 0.56849(9) 0.0226(4) Uani 1 1 d . . .
H3 H 0.4882 0.2913 0.5570 0.027 Uiso 1 1 calc R . .
C4 C 0.38631(14) 0.20611(11) 0.50668(10) 0.0206(4) Uani 1 1 d . . .
C5 C 0.35768(13) 0.26406(11) 0.43660(9) 0.0209(4) Uani 1 1 d . . .
H5 H 0.4233 0.2917 0.4193 0.025 Uiso 1 1 calc R . .
C6 C 0.29149(15) 0.33284(11) 0.47557(10) 0.0237(4) Uani 1 1 d . . .
H6 H 0.2177 0.3147 0.4804 0.028 Uiso 1 1 calc R . .
C7 C 0.29967(14) 0.41665(12) 0.43577(11) 0.0265(4) Uani 1 1 d . . .
C8 C 0.30351(15) 0.14389(11) 0.52847(10) 0.0229(4) Uani 1 1 d . . .
C9 C 0.20914(15) 0.15510(12) 0.56518(11) 0.0291(4) Uani 1 1 d . . .
H9 H 0.1879 0.2096 0.5814 0.035 Uiso 1 1 calc R . .
C10 C 0.14620(16) 0.08566(13) 0.57790(12) 0.0360(5) Uani 1 1 d . . .
H10 H 0.0823 0.0923 0.6043 0.043 Uiso 1 1 calc R . .
C11 C 0.17603(16) 0.00699(13) 0.55246(14) 0.0412(6) Uani 1 1 d . . .
H11 H 0.1310 -0.0395 0.5604 0.049 Uiso 1 1 calc R . .
C12 C 0.27055(16) -0.00611(12) 0.51543(12) 0.0357(5) Uani 1 1 d . . .
H12 H 0.2907 -0.0606 0.4983 0.043 Uiso 1 1 calc R . .
C13 C 0.33359(15) 0.06296(11) 0.50458(11) 0.0251(4) Uani 1 1 d . . .
C14 C 0.47517(14) 0.14895(11) 0.48131(10) 0.0213(4) Uani 1 1 d . . .
C15 C 0.31188(14) 0.22122(11) 0.36672(10) 0.0239(4) Uani 1 1 d . . .
C16 C 0.20876(16) 0.19246(12) 0.36788(12) 0.0316(5) Uani 1 1 d . . .
H16 H 0.1678 0.2025 0.4125 0.038 Uiso 1 1 calc R . .
C17 C 0.16519(18) 0.15005(13) 0.30627(13) 0.0412(6) Uani 1 1 d . . .
H17 H 0.0956 0.1309 0.3092 0.049 Uiso 1 1 calc R . .
C18 C 0.22305(19) 0.13545(13) 0.24017(12) 0.0428(6) Uani 1 1 d . . .
H18 H 0.1935 0.1062 0.1977 0.051 Uiso 1 1 calc R . .
C19 C 0.32423(18) 0.16395(13) 0.23660(11) 0.0372(5) Uani 1 1 d . . .
H19 H 0.3643 0.1549 0.1914 0.045 Uiso 1 1 calc R . .
C20 C 0.36690(15) 0.20585(11) 0.29953(11) 0.0276(4) Uani 1 1 d . . .
C21 C 0.39088(15) 0.55243(12) 0.45700(11) 0.0276(4) Uani 1 1 d . . .
C22 C 0.37502(18) 0.70249(12) 0.48487(12) 0.0361(5) Uani 1 1 d . . .
C23 C 0.49054(19) 0.71721(13) 0.48968(13) 0.0528(6) Uani 1 1 d . . .
H23A H 0.5172 0.6931 0.5378 0.063 Uiso 1 1 calc R . .
H23B H 0.5046 0.7779 0.4888 0.063 Uiso 1 1 calc R . .
H23C H 0.5247 0.6902 0.4456 0.063 Uiso 1 1 calc R . .
C24 C 0.31945(17) 0.74747(14) 0.54951(12) 0.0511(6) Uani 1 1 d . . .
H24A H 0.2446 0.7394 0.5439 0.061 Uiso 1 1 calc R . .
H24B H 0.3356 0.8077 0.5474 0.061 Uiso 1 1 calc R . .
H24C H 0.3421 0.7244 0.5992 0.061 Uiso 1 1 calc R . .
C25 C 0.32915(17) 0.72472(13) 0.40676(12) 0.0493(6) Uani 1 1 d . . .
H25A H 0.3660 0.6939 0.3662 0.059 Uiso 1 1 calc R . .
H25B H 0.3361 0.7854 0.3978 0.059 Uiso 1 1 calc R . .
H25C H 0.2557 0.7092 0.4059 0.059 Uiso 1 1 calc R . .
C26 C 0.41537(15) 0.23627(13) 0.65048(11) 0.0298(4) Uani 1 1 d . . .
C27 C 0.46834(16) 0.10835(12) 0.72245(11) 0.0337(5) Uani 1 1 d . . .
C28 C 0.51169(17) 0.02639(12) 0.69180(11) 0.0428(5) Uani 1 1 d . . .
H28A H 0.4652 0.0038 0.6522 0.051 Uiso 1 1 calc R . .
H28B H 0.5179 -0.0142 0.7341 0.051 Uiso 1 1 calc R . .
H28C H 0.5801 0.0365 0.6692 0.051 Uiso 1 1 calc R . .
C29 C 0.5424(2) 0.15023(15) 0.77734(13) 0.0642(9) Uani 1 1 d . . .
H29A H 0.6069 0.1636 0.7502 0.077 Uiso 1 1 calc R . .
H29B H 0.5571 0.1121 0.8204 0.077 Uiso 1 1 calc R . .
H29C H 0.5113 0.2023 0.7971 0.077 Uiso 1 1 calc R . .
C30 C 0.36085(19) 0.09549(15) 0.75621(13) 0.0519(7) Uani 1 1 d . . .
H30A H 0.3347 0.1492 0.7761 0.062 Uiso 1 1 calc R . .
H30B H 0.3644 0.0544 0.7983 0.062 Uiso 1 1 calc R . .
H30C H 0.3142 0.0745 0.7160 0.062 Uiso 1 1 calc R . .
C31 C 0.48054(16) 0.00023(12) 0.42932(11) 0.0305(5) Uani 1 1 d . . .
C32 C 0.60209(16) -0.02243(13) 0.32429(11) 0.0324(5) Uani 1 1 d . . .
C33 C 0.68884(16) 0.03346(13) 0.29469(12) 0.0440(6) Uani 1 1 d . . .
H33A H 0.6635 0.0914 0.2894 0.053 Uiso 1 1 calc R . .
H33B H 0.7123 0.0128 0.2443 0.053 Uiso 1 1 calc R . .
H33C H 0.7467 0.0322 0.3312 0.053 Uiso 1 1 calc R . .
C34 C 0.51543(18) -0.02967(13) 0.26584(10) 0.0388(5) Uani 1 1 d . . .
H34A H 0.4596 -0.0642 0.2873 0.047 Uiso 1 1 calc R . .
H34B H 0.5418 -0.0561 0.2187 0.047 Uiso 1 1 calc R . .
H34C H 0.4888 0.0266 0.2537 0.047 Uiso 1 1 calc R . .
C35 C 0.64381(18) -0.10638(13) 0.35080(13) 0.0454(6) Uani 1 1 d . . .
H35A H 0.6925 -0.0976 0.3934 0.055 Uiso 1 1 calc R . .
H35B H 0.6796 -0.1341 0.3079 0.055 Uiso 1 1 calc R . .
H35C H 0.5865 -0.1420 0.3683 0.055 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C20 1.9121(19) . ?
O1 C1 1.208(2) . ?
O2 C7 1.201(2) . ?
O3 C14 1.209(2) . ?
O4 C21 1.313(2) . ?
O4 C22 1.511(2) . ?
O5 C21 1.195(2) . ?
O6 C26 1.333(2) . ?
O6 C27 1.499(2) . ?
O7 C26 1.199(2) . ?
O8 C31 1.310(2) . ?
O8 C32 1.504(2) . ?
O9 C31 1.200(2) . ?
N1 C1 1.399(2) . ?
N1 C7 1.404(2) . ?
N1 C21 1.447(2) . ?
N2 C14 1.400(2) . ?
N2 C31 1.426(2) . ?
N2 C13 1.431(2) . ?
C1 C2 1.522(2) . ?
C2 C6 1.538(2) . ?
C2 C3 1.539(2) . ?
C2 H2 1.0000 . ?
C3 C26 1.525(2) . ?
C3 C4 1.538(2) . ?
C3 H3 1.0000 . ?
C4 C8 1.504(2) . ?
C4 C14 1.528(2) . ?
C4 C5 1.568(2) . ?
C5 C15 1.510(2) . ?
C5 C6 1.543(2) . ?
C5 H5 1.0000 . ?
C6 C7 1.502(2) . ?
C6 H6 1.0000 . ?
C8 C9 1.387(3) . ?
C8 C13 1.405(2) . ?
C9 C10 1.387(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.395(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.379(2) . ?
C12 H12 0.9500 . ?
C15 C20 1.386(2) . ?
C15 C16 1.408(2) . ?
C16 C17 1.382(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.391(3) . ?
C19 H19 0.9500 . ?
C22 C24 1.510(3) . ?
C22 C23 1.513(3) . ?
C22 C25 1.519(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C27 C29 1.504(3) . ?
C27 C28 1.513(3) . ?
C27 C30 1.521(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C32 C35 1.509(3) . ?
C32 C34 1.514(3) . ?
C32 C33 1.519(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 O4 C22 119.30(15) . . ?
C26 O6 C27 122.08(15) . . ?
C31 O8 C32 119.37(15) . . ?
C1 N1 C7 113.54(16) . . ?
C1 N1 C21 124.64(16) . . ?
C7 N1 C21 121.15(16) . . ?
C14 N2 C31 126.85(16) . . ?
C14 N2 C13 109.86(15) . . ?
C31 N2 C13 122.85(16) . . ?
O1 C1 N1 124.51(18) . . ?
O1 C1 C2 128.21(18) . . ?
N1 C1 C2 107.25(17) . . ?
C1 C2 C6 104.80(15) . . ?
C1 C2 C3 115.18(16) . . ?
C6 C2 C3 107.49(14) . . ?
C1 C2 H2 109.7 . . ?
C6 C2 H2 109.7 . . ?
C3 C2 H2 109.7 . . ?
C26 C3 C4 113.75(15) . . ?
C26 C3 C2 114.19(15) . . ?
C4 C3 C2 104.46(14) . . ?
C26 C3 H3 108.1 . . ?
C4 C3 H3 108.1 . . ?
C2 C3 H3 108.1 . . ?
C8 C4 C14 102.51(14) . . ?
C8 C4 C3 116.48(15) . . ?
C14 C4 C3 114.15(15) . . ?
C8 C4 C5 114.33(15) . . ?
C14 C4 C5 107.62(14) . . ?
C3 C4 C5 101.85(13) . . ?
C15 C5 C6 116.93(14) . . ?
C15 C5 C4 116.71(14) . . ?
C6 C5 C4 101.94(13) . . ?
C15 C5 H5 106.8 . . ?
C6 C5 H5 106.8 . . ?
C4 C5 H5 106.8 . . ?
C7 C6 C2 105.70(15) . . ?
C7 C6 C5 112.76(15) . . ?
C2 C6 C5 104.52(14) . . ?
C7 C6 H6 111.2 . . ?
C2 C6 H6 111.2 . . ?
C5 C6 H6 111.2 . . ?
O2 C7 N1 124.49(18) . . ?
O2 C7 C6 127.80(19) . . ?
N1 C7 C6 107.69(16) . . ?
C9 C8 C13 119.73(18) . . ?
C9 C8 C4 131.01(17) . . ?
C13 C8 C4 109.26(16) . . ?
C8 C9 C10 119.09(19) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C11 C10 C9 120.3(2) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 121.8(2) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C13 C12 C11 117.46(19) . . ?
C13 C12 H12 121.3 . . ?
C11 C12 H12 121.3 . . ?
C12 C13 C8 121.59(19) . . ?
C12 C13 N2 129.50(18) . . ?
C8 C13 N2 108.89(16) . . ?
O3 C14 N2 127.10(17) . . ?
O3 C14 C4 125.12(17) . . ?
N2 C14 C4 107.76(15) . . ?
C20 C15 C16 116.11(17) . . ?
C20 C15 C5 123.53(16) . . ?
C16 C15 C5 120.35(16) . . ?
C17 C16 C15 122.1(2) . . ?
C17 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
C16 C17 C18 120.0(2) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 119.4(2) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 119.7(2) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C15 C20 C19 122.66(19) . . ?
C15 C20 Br1 121.59(14) . . ?
C19 C20 Br1 115.75(15) . . ?
O5 C21 O4 129.23(19) . . ?
O5 C21 N1 121.02(18) . . ?
O4 C21 N1 109.73(16) . . ?
C24 C22 O4 102.46(16) . . ?
C24 C22 C23 110.80(19) . . ?
O4 C22 C23 109.68(16) . . ?
C24 C22 C25 111.45(18) . . ?
O4 C22 C25 108.40(17) . . ?
C23 C22 C25 113.45(19) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O7 C26 O6 127.15(18) . . ?
O7 C26 C3 123.84(18) . . ?
O6 C26 C3 109.00(15) . . ?
O6 C27 C29 108.68(16) . . ?
O6 C27 C28 102.20(15) . . ?
C29 C27 C28 111.52(18) . . ?
O6 C27 C30 109.50(16) . . ?
C29 C27 C30 113.37(19) . . ?
C28 C27 C30 110.96(18) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O9 C31 O8 128.97(19) . . ?
O9 C31 N2 120.93(19) . . ?
O8 C31 N2 110.10(16) . . ?
O8 C32 C35 110.21(17) . . ?
O8 C32 C34 108.06(16) . . ?
C35 C32 C34 113.62(18) . . ?
O8 C32 C33 102.16(15) . . ?
C35 C32 C33 110.80(18) . . ?
C34 C32 C33 111.35(18) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N1 C1 O1 170.91(18) . . . . ?
C21 N1 C1 O1 0.3(3) . . . . ?
C7 N1 C1 C2 -7.1(2) . . . . ?
C21 N1 C1 C2 -177.77(16) . . . . ?
O1 C1 C2 C6 -167.91(19) . . . . ?
N1 C1 C2 C6 10.02(19) . . . . ?
O1 C1 C2 C3 -50.0(3) . . . . ?
N1 C1 C2 C3 127.91(17) . . . . ?
C1 C2 C3 C26 103.87(18) . . . . ?
C6 C2 C3 C26 -139.77(16) . . . . ?
C1 C2 C3 C4 -131.25(16) . . . . ?
C6 C2 C3 C4 -14.89(18) . . . . ?
C26 C3 C4 C8 36.5(2) . . . . ?
C2 C3 C4 C8 -88.64(17) . . . . ?
C26 C3 C4 C14 -82.74(19) . . . . ?
C2 C3 C4 C14 152.11(15) . . . . ?
C26 C3 C4 C5 161.60(14) . . . . ?
C2 C3 C4 C5 36.45(17) . . . . ?
C8 C4 C5 C15 -46.7(2) . . . . ?
C14 C4 C5 C15 66.46(19) . . . . ?
C3 C4 C5 C15 -173.20(14) . . . . ?
C8 C4 C5 C6 81.96(17) . . . . ?
C14 C4 C5 C6 -164.89(14) . . . . ?
C3 C4 C5 C6 -44.54(16) . . . . ?
C1 C2 C6 C7 -9.33(19) . . . . ?
C3 C2 C6 C7 -132.33(15) . . . . ?
C1 C2 C6 C5 109.87(16) . . . . ?
C3 C2 C6 C5 -13.13(18) . . . . ?
C15 C5 C6 C7 -81.8(2) . . . . ?
C4 C5 C6 C7 149.66(15) . . . . ?
C15 C5 C6 C2 163.87(14) . . . . ?
C4 C5 C6 C2 35.35(17) . . . . ?
C1 N1 C7 O2 -177.98(18) . . . . ?
C21 N1 C7 O2 -7.0(3) . . . . ?
C1 N1 C7 C6 1.0(2) . . . . ?
C21 N1 C7 C6 171.97(16) . . . . ?
C2 C6 C7 O2 -175.60(19) . . . . ?
C5 C6 C7 O2 70.8(3) . . . . ?
C2 C6 C7 N1 5.5(2) . . . . ?
C5 C6 C7 N1 -108.08(17) . . . . ?
C14 C4 C8 C9 170.55(19) . . . . ?
C3 C4 C8 C9 45.2(3) . . . . ?
C5 C4 C8 C9 -73.3(3) . . . . ?
C14 C4 C8 C13 -10.1(2) . . . . ?
C3 C4 C8 C13 -135.46(16) . . . . ?
C5 C4 C8 C13 106.05(18) . . . . ?
C13 C8 C9 C10 0.3(3) . . . . ?
C4 C8 C9 C10 179.54(19) . . . . ?
C8 C9 C10 C11 -1.7(3) . . . . ?
C9 C10 C11 C12 1.8(4) . . . . ?
C10 C11 C12 C13 -0.4(3) . . . . ?
C11 C12 C13 C8 -1.1(3) . . . . ?
C11 C12 C13 N2 176.63(19) . . . . ?
C9 C8 C13 C12 1.2(3) . . . . ?
C4 C8 C13 C12 -178.22(18) . . . . ?
C9 C8 C13 N2 -176.97(16) . . . . ?
C4 C8 C13 N2 3.6(2) . . . . ?
C14 N2 C13 C12 -172.7(2) . . . . ?
C31 N2 C13 C12 14.5(3) . . . . ?
C14 N2 C13 C8 5.3(2) . . . . ?
C31 N2 C13 C8 -167.53(16) . . . . ?
C31 N2 C14 O3 -17.6(3) . . . . ?
C13 N2 C14 O3 169.93(18) . . . . ?
C31 N2 C14 C4 160.68(16) . . . . ?
C13 N2 C14 C4 -11.8(2) . . . . ?
C8 C4 C14 O3 -168.53(18) . . . . ?
C3 C4 C14 O3 -41.7(2) . . . . ?
C5 C4 C14 O3 70.6(2) . . . . ?
C8 C4 C14 N2 13.17(19) . . . . ?
C3 C4 C14 N2 140.04(15) . . . . ?
C5 C4 C14 N2 -107.72(16) . . . . ?
C6 C5 C15 C20 135.12(18) . . . . ?
C4 C5 C15 C20 -103.9(2) . . . . ?
C6 C5 C15 C16 -46.5(2) . . . . ?
C4 C5 C15 C16 74.6(2) . . . . ?
C20 C15 C16 C17 1.1(3) . . . . ?
C5 C15 C16 C17 -177.43(17) . . . . ?
C15 C16 C17 C18 -0.8(3) . . . . ?
C16 C17 C18 C19 -0.2(3) . . . . ?
C17 C18 C19 C20 0.8(3) . . . . ?
C16 C15 C20 C19 -0.5(3) . . . . ?
C5 C15 C20 C19 177.97(17) . . . . ?
C16 C15 C20 Br1 179.32(13) . . . . ?
C5 C15 C20 Br1 -2.2(2) . . . . ?
C18 C19 C20 C15 -0.4(3) . . . . ?
C18 C19 C20 Br1 179.75(16) . . . . ?
C22 O4 C21 O5 -1.4(3) . . . . ?
C22 O4 C21 N1 -179.75(16) . . . . ?
C1 N1 C21 O5 110.8(2) . . . . ?
C7 N1 C21 O5 -59.2(3) . . . . ?
C1 N1 C21 O4 -70.7(2) . . . . ?
C7 N1 C21 O4 119.28(19) . . . . ?
C21 O4 C22 C24 -178.11(17) . . . . ?
C21 O4 C22 C23 -60.4(2) . . . . ?
C21 O4 C22 C25 64.0(2) . . . . ?
C27 O6 C26 O7 3.3(3) . . . . ?
C27 O6 C26 C3 -177.58(14) . . . . ?
C4 C3 C26 O7 -136.7(2) . . . . ?
C2 C3 C26 O7 -16.9(3) . . . . ?
C4 C3 C26 O6 44.2(2) . . . . ?
C2 C3 C26 O6 163.98(15) . . . . ?
C26 O6 C27 C29 -69.2(2) . . . . ?
C26 O6 C27 C28 172.83(16) . . . . ?
C26 O6 C27 C30 55.1(2) . . . . ?
C32 O8 C31 O9 18.9(3) . . . . ?
C32 O8 C31 N2 -160.18(15) . . . . ?
C14 N2 C31 O9 174.91(19) . . . . ?
C13 N2 C31 O9 -13.5(3) . . . . ?
C14 N2 C31 O8 -5.9(3) . . . . ?
C13 N2 C31 O8 165.66(16) . . . . ?
C31 O8 C32 C35 -67.1(2) . . . . ?
C31 O8 C32 C34 57.6(2) . . . . ?
C31 O8 C32 C33 175.13(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        31.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.051
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_chemical_properties_physical    Light-sensitive
