# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1418019'
_audit_update_record             
;
2015-12-11 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;
_audit_creation_date             2015-12-11
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C17 H16 F3 N O5, C2 H6 O S'
_chemical_formula_sum            'C19 H22 F3 N O6 S'
_chemical_formula_weight         449.43
_chemical_melting_point          ?
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'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1681(14)
_cell_length_b                   11.800(2)
_cell_length_c                   12.478(2)
_cell_angle_alpha                114.931(3)
_cell_angle_beta                 91.661(3)
_cell_angle_gamma                99.121(3)
_cell_volume                     1070.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1183
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.328
_cell_measurement_theta_min      3.173
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.132742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0390 before and 0.0164 after correction.
The Ratio of minimum to maximum transmission is 0.1327.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5630
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.810
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2291
_reflns_number_total             3878
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3878
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0605
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0905P)²+0.3490P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1914
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.6401(5) 1.1909(3) 0.9910(2) 0.1389(13) Uani 1 1 d . . . . .
F2 F 0.5711(5) 0.9953(3) 0.8895(2) 0.1466(15) Uani 1 1 d . . . . .
F3 F 0.8111(5) 1.0850(4) 0.9002(3) 0.1608(16) Uani 1 1 d . . . . .
O1 O 0.6174(3) 1.1212(2) 0.8014(2) 0.0689(7) Uani 1 1 d . . . . .
O2 O 0.3993(3) 0.5916(2) 0.2247(2) 0.0694(7) Uani 1 1 d . . . . .
O3 O 0.1374(3) 0.8000(2) 0.61240(19) 0.0611(7) Uani 1 1 d . . . . .
O4 O -0.3051(3) 0.4811(2) 0.3816(2) 0.0678(7) Uani 1 1 d . . . . .
O5 O -0.0776(3) 0.4639(2) 0.2844(2) 0.0729(8) Uani 1 1 d . . . . .
N1 N 0.6097(3) 0.7534(3) 0.3461(2) 0.0575(8) Uani 1 1 d . . . . .
H1 H 0.6853 0.7411 0.2979 0.069 Uiso 1 1 calc R . . . .
C1 C 0.0823(4) 0.7009(3) 0.5051(3) 0.0497(8) Uani 1 1 d . . . . .
C2 C 0.4835(4) 0.8436(3) 0.5159(3) 0.0458(8) Uani 1 1 d . . . . .
C3 C 0.3627(4) 0.7368(3) 0.4286(3) 0.0460(8) Uani 1 1 d . . . . .
C4 C 0.6313(4) 0.8488(3) 0.4611(3) 0.0499(8) Uani 1 1 d . . . . .
C5 C 0.6239(4) 1.0243(3) 0.6861(3) 0.0545(9) Uani 1 1 d . . . . .
C6 C 0.4810(4) 0.9349(3) 0.6303(3) 0.0498(8) Uani 1 1 d . . . . .
H6 H 0.3851 0.9361 0.6688 0.060 Uiso 1 1 calc R . . . .
C7 C 0.2039(4) 0.6775(3) 0.4214(3) 0.0494(8) Uani 1 1 d . . . . .
H7 H 0.1666 0.6085 0.3484 0.059 Uiso 1 1 calc R . . . .
C8 C 0.4539(4) 0.6820(3) 0.3191(3) 0.0521(9) Uani 1 1 d . . . . .
C9 C -0.1443(4) 0.5195(3) 0.3713(3) 0.0571(9) Uani 1 1 d . . . . .
C10 C 0.7714(4) 0.9399(3) 0.5176(3) 0.0632(10) Uani 1 1 d . . . . .
H10 H 0.8670 0.9414 0.4791 0.076 Uiso 1 1 calc R . . . .
C11 C 0.7676(4) 1.0293(3) 0.6326(3) 0.0609(10) Uani 1 1 d . . . . .
H11 H 0.8609 1.0918 0.6731 0.073 Uiso 1 1 calc R . . . .
C12 C 0.0290(5) 0.8252(4) 0.7068(3) 0.0659(10) Uani 1 1 d . . . . .
H12A H -0.0022 0.7502 0.7208 0.079 Uiso 1 1 calc R . . . .
H12B H -0.0718 0.8478 0.6849 0.079 Uiso 1 1 calc R . . . .
C13 C -0.0730(4) 0.6304(3) 0.4812(3) 0.0579(9) Uani 1 1 d . . . . .
H13 H -0.1423 0.6552 0.5416 0.069 Uiso 1 1 calc R . . . .
C14 C 0.6559(6) 1.0990(4) 0.8927(4) 0.0781(12) Uani 1 1 d . . . . .
C15 C -0.3970(4) 0.3697(4) 0.2842(3) 0.0714(11) Uani 1 1 d . . . . .
H15A H -0.3442 0.2973 0.2700 0.086 Uiso 1 1 calc R . . . .
H15B H -0.3999 0.3828 0.2125 0.086 Uiso 1 1 calc R . . . .
C16 C 0.1221(5) 0.9319(4) 0.8152(3) 0.0902(14) Uani 1 1 d . . . . .
H16A H 0.1591 1.0037 0.7986 0.135 Uiso 1 1 calc GR . . . .
H16B H 0.2169 0.9062 0.8395 0.135 Uiso 1 1 calc GR . . . .
H16C H 0.0505 0.9549 0.8777 0.135 Uiso 1 1 calc GR . . . .
C17 C -0.5684(5) 0.3458(4) 0.3156(4) 0.0749(12) Uani 1 1 d . . . . .
H17A H -0.6309 0.2690 0.2534 0.112 Uiso 1 1 calc GR . . . .
H17B H -0.6217 0.4159 0.3250 0.112 Uiso 1 1 calc GR . . . .
H17C H -0.5638 0.3371 0.3886 0.112 Uiso 1 1 calc GR . . . .
S1 S 0.89033(14) 0.65590(12) 0.08437(9) 0.0856(4) Uani 1 1 d . . . . .
O6 O 0.8716(3) 0.7508(3) 0.2052(2) 0.0919(10) Uani 1 1 d . . . . .
C18 C 0.7843(11) 0.6945(6) -0.0141(6) 0.188(4) Uani 1 1 d . . . . .
H18A H 0.6692 0.6913 0.0003 0.283 Uiso 1 1 calc GR . . . .
H18B H 0.7921 0.6349 -0.0941 0.283 Uiso 1 1 calc GR . . . .
H18C H 0.8329 0.7788 -0.0030 0.283 Uiso 1 1 calc GR . . . .
C19 C 0.7530(6) 0.5131(4) 0.0562(4) 0.0870(13) Uiso 1 1 d . . . . .
H19A H 0.7909 0.4768 0.1060 0.130 Uiso 1 1 calc GR . . . .
H19B H 0.7500 0.4544 -0.0257 0.130 Uiso 1 1 calc GR . . . .
H19C H 0.6432 0.5303 0.0728 0.130 Uiso 1 1 calc GR . . . .


_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
F1 C14 1.277(4) . ?
F2 C14 1.291(5) . ?
F3 C14 1.310(5) . ?
O1 C5 1.421(4) . ?
O1 C14 1.311(5) . ?
O2 C8 1.218(4) . ?
O3 C1 1.357(4) . ?
O3 C12 1.452(4) . ?
O4 C9 1.348(4) . ?
O4 C15 1.434(4) . ?
O5 C9 1.204(4) . ?
N1 H1 0.8600 . ?
N1 C4 1.385(4) . ?
N1 C8 1.356(4) . ?
C1 C7 1.434(4) . ?
C1 C13 1.351(5) . ?
C2 C3 1.462(4) . ?
C2 C4 1.410(4) . ?
C2 C6 1.382(4) . ?
C3 C7 1.353(4) . ?
C3 C8 1.519(4) . ?
C4 C10 1.374(4) . ?
C5 C6 1.379(4) . ?
C5 C11 1.372(5) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C9 C13 1.460(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.383(5) . ?
C11 H11 0.9300 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C16 1.481(5) . ?
C13 H13 0.9300 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C17 1.481(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
S1 O6 1.482(3) . ?
S1 C18 1.733(6) . ?
S1 C19 1.760(4) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

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
C14 O1 C5 117.6(3) . . ?
C1 O3 C12 118.5(3) . . ?
C9 O4 C15 117.5(3) . . ?
C4 N1 H1 124.4 . . ?
C8 N1 H1 124.4 . . ?
C8 N1 C4 111.2(3) . . ?
O3 C1 C7 114.0(3) . . ?
C13 C1 O3 122.3(3) . . ?
C13 C1 C7 123.7(3) . . ?
C4 C2 C3 106.6(3) . . ?
C6 C2 C3 135.3(3) . . ?
C6 C2 C4 118.1(3) . . ?
C2 C3 C8 105.1(3) . . ?
C7 C3 C2 138.4(3) . . ?
C7 C3 C8 116.6(3) . . ?
N1 C4 C2 110.3(3) . . ?
C10 C4 N1 127.3(3) . . ?
C10 C4 C2 122.4(3) . . ?
C6 C5 O1 118.0(3) . . ?
C11 C5 O1 118.5(3) . . ?
C11 C5 C6 123.3(3) . . ?
C2 C6 H6 120.7 . . ?
C5 C6 C2 118.5(3) . . ?
C5 C6 H6 120.7 . . ?
C1 C7 H7 113.9 . . ?
C3 C7 C1 132.2(3) . . ?
C3 C7 H7 113.9 . . ?
O2 C8 N1 126.0(3) . . ?
O2 C8 C3 127.2(3) . . ?
N1 C8 C3 106.8(3) . . ?
O4 C9 C13 108.5(3) . . ?
O5 C9 O4 122.4(3) . . ?
O5 C9 C13 129.0(3) . . ?
C4 C10 H10 120.6 . . ?
C4 C10 C11 118.8(3) . . ?
C11 C10 H10 120.6 . . ?
C5 C11 C10 118.9(3) . . ?
C5 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
O3 C12 H12A 110.2 . . ?
O3 C12 H12B 110.2 . . ?
O3 C12 C16 107.6(3) . . ?
H12A C12 H12B 108.5 . . ?
C16 C12 H12A 110.2 . . ?
C16 C12 H12B 110.2 . . ?
C1 C13 C9 127.3(3) . . ?
C1 C13 H13 116.3 . . ?
C9 C13 H13 116.3 . . ?
F1 C14 F2 108.3(4) . . ?
F1 C14 F3 105.6(4) . . ?
F1 C14 O1 111.8(4) . . ?
F2 C14 F3 103.8(5) . . ?
F2 C14 O1 114.3(4) . . ?
F3 C14 O1 112.5(4) . . ?
O4 C15 H15A 110.1 . . ?
O4 C15 H15B 110.1 . . ?
O4 C15 C17 107.9(3) . . ?
H15A C15 H15B 108.4 . . ?
C17 C15 H15A 110.1 . . ?
C17 C15 H15B 110.1 . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O6 S1 C18 106.3(3) . . ?
O6 S1 C19 107.9(2) . . ?
C18 S1 C19 96.9(3) . . ?
S1 C18 H18A 109.5 . . ?
S1 C18 H18B 109.5 . . ?
S1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
S1 C19 H19A 109.5 . . ?
S1 C19 H19B 109.5 . . ?
S1 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
O1 C5 C6 C2 177.1(3) . . . . ?
O1 C5 C11 C10 -176.1(3) . . . . ?
O3 C1 C7 C3 -1.2(5) . . . . ?
O3 C1 C13 C9 -177.7(3) . . . . ?
O4 C9 C13 C1 -176.8(4) . . . . ?
O5 C9 C13 C1 5.7(7) . . . . ?
N1 C4 C10 C11 178.6(3) . . . . ?
C1 O3 C12 C16 176.6(3) . . . . ?
C2 C3 C7 C1 0.9(7) . . . . ?
C2 C3 C8 O2 -179.8(3) . . . . ?
C2 C3 C8 N1 0.1(4) . . . . ?
C2 C4 C10 C11 0.4(6) . . . . ?
C3 C2 C4 N1 0.5(4) . . . . ?
C3 C2 C4 C10 179.0(3) . . . . ?
C3 C2 C6 C5 -179.4(3) . . . . ?
C4 N1 C8 O2 -179.9(3) . . . . ?
C4 N1 C8 C3 0.1(4) . . . . ?
C4 C2 C3 C7 178.4(4) . . . . ?
C4 C2 C3 C8 -0.4(3) . . . . ?
C4 C2 C6 C5 -1.6(5) . . . . ?
C4 C10 C11 C5 -0.3(6) . . . . ?
C5 O1 C14 F1 -177.8(3) . . . . ?
C5 O1 C14 F2 -54.4(5) . . . . ?
C5 O1 C14 F3 63.5(5) . . . . ?
C6 C2 C3 C7 -3.7(7) . . . . ?
C6 C2 C3 C8 177.6(4) . . . . ?
C6 C2 C4 N1 -177.9(3) . . . . ?
C6 C2 C4 C10 0.6(5) . . . . ?
C6 C5 C11 C10 -0.8(6) . . . . ?
C7 C1 C13 C9 1.3(6) . . . . ?
C7 C3 C8 O2 1.1(5) . . . . ?
C7 C3 C8 N1 -178.9(3) . . . . ?
C8 N1 C4 C2 -0.4(4) . . . . ?
C8 N1 C4 C10 -178.8(4) . . . . ?
C8 C3 C7 C1 179.5(3) . . . . ?
C9 O4 C15 C17 179.8(3) . . . . ?
C11 C5 C6 C2 1.7(5) . . . . ?
C12 O3 C1 C7 -174.9(3) . . . . ?
C12 O3 C1 C13 4.1(5) . . . . ?
C13 C1 C7 C3 179.8(4) . . . . ?
C14 O1 C5 C6 90.5(4) . . . . ?
C14 O1 C5 C11 -93.9(4) . . . . ?
C15 O4 C9 O5 0.0(5) . . . . ?
C15 O4 C9 C13 -177.7(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_A150508D_twin1_hklf5
_database_code_depnum_ccdc_archive 'CCDC 1418020'
_audit_update_record             
;
2015-08-11 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H24 Br N O6'
_chemical_formula_weight         478.33

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'
Br Br -0.6763 1.2805 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.0861(5)
_cell_length_b                   17.2584(7)
_cell_length_c                   17.3652(7)
_cell_angle_alpha                66.864(4)
_cell_angle_beta                 87.873(3)
_cell_angle_gamma                66.771(3)
_cell_volume                     4284.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_absorpt_special_details   ?
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_F_000             1968
_exptl_transmission_factor_min   0.80281
_exptl_transmission_factor_max   1.00000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    2.948
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26251
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.638
_diffrn_reflns_theta_max         74.381
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             26251
_reflns_number_gt                20886
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0928P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         26251
_refine_ls_number_parameters     1112
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1299
_refine_ls_wR_factor_gt          0.1250
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_restrained_S_all      0.960
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.94226(2) -0.13116(3) 1.26885(2) 0.02915(10) Uani 1 1 d . . . . .
O1 O 0.59705(16) 0.2173(2) 0.88359(15) 0.0317(6) Uani 1 1 d . . . . .
O2 O 0.60710(18) 0.0069(2) 1.07282(16) 0.0355(7) Uani 1 1 d . . . . .
O3 O 0.61655(15) -0.00255(19) 0.80428(14) 0.0260(5) Uani 1 1 d . . . . .
O4 O 0.79791(15) 0.15320(18) 0.87931(15) 0.0258(5) Uani 1 1 d . . . . .
N1 N 0.66077(17) 0.2023(2) 1.00597(18) 0.0239(6) Uani 1 1 d . . . . .
C1 C 0.70177(19) 0.0643(2) 0.98605(18) 0.0187(6) Uani 1 1 d . . . . .
C2 C 0.64725(19) 0.1707(2) 0.9491(2) 0.0228(7) Uani 1 1 d . . . . .
C3 C 0.7233(2) 0.1318(2) 1.0744(2) 0.0209(6) Uani 1 1 d . . . . .
C4 C 0.7564(2) 0.1376(3) 1.1428(2) 0.0248(7) Uani 1 1 d . . . . .
H4 H 0.7366 0.1931 1.1490 0.030 Uiso 1 1 calc R U . . .
C5 C 0.8206(2) 0.0571(3) 1.2017(2) 0.0245(7) Uani 1 1 d . . . . .
H5 H 0.8436 0.0582 1.2488 0.029 Uiso 1 1 calc R U . . .
C6 C 0.85047(19) -0.0244(3) 1.19057(19) 0.0220(7) Uani 1 1 d . . . . .
C7 C 0.8159(2) -0.0306(2) 1.12252(19) 0.0196(6) Uani 1 1 d . . . . .
H7 H 0.8358 -0.0861 1.1163 0.024 Uiso 1 1 calc R U . . .
C8 C 0.75121(19) 0.0488(2) 1.06485(19) 0.0183(6) Uani 1 1 d . . . . .
C9 C 0.6193(3) 0.2987(3) 0.9931(3) 0.0348(8) Uani 1 1 d . . . . .
H9A H 0.6604 0.3256 0.9798 0.052 Uiso 1 1 calc R U . . .
H9B H 0.5974 0.3026 1.0438 0.052 Uiso 1 1 calc R U . . .
H9C H 0.5728 0.3317 0.9474 0.052 Uiso 1 1 calc R U . . .
C10 C 0.6351(2) 0.0214(2) 1.00550(19) 0.0212(6) Uani 1 1 d . . . . .
C11 C 0.6067(2) 0.0011(3) 0.9408(2) 0.0224(7) Uani 1 1 d . . . . .
H11 H 0.5646 -0.0217 0.9504 0.027 Uiso 1 1 calc R U . . .
C12 C 0.6396(2) 0.0142(2) 0.86680(19) 0.0212(6) Uani 1 1 d . . . . .
C13 C 0.7092(2) 0.0478(3) 0.84628(19) 0.0244(7) Uani 1 1 d . . . . .
H13A H 0.6841 0.1139 0.8119 0.029 Uiso 1 1 calc R U . . .
H13B H 0.7472 0.0175 0.8141 0.029 Uiso 1 1 calc R U . . .
C14 C 0.7608(2) 0.0270(2) 0.92756(18) 0.0205(6) Uani 1 1 d . . . . .
H14 H 0.7891 -0.0405 0.9581 0.025 Uiso 1 1 calc R U . . .
C15 C 0.5526(2) -0.0398(3) 0.8170(2) 0.0306(8) Uani 1 1 d . . . . .
H15A H 0.5392 -0.0453 0.7667 0.046 Uiso 1 1 calc R U . . .
H15B H 0.5014 0.0008 0.8294 0.046 Uiso 1 1 calc R U . . .
H15C H 0.5745 -0.0997 0.8635 0.046 Uiso 1 1 calc R U . . .
C16 C 0.8306(2) 0.0610(2) 0.90614(18) 0.0206(6) Uani 1 1 d . . . . .
C17 C 0.8513(2) 0.2019(3) 0.8440(2) 0.0269(7) Uani 1 1 d . . . . .
H17A H 0.8773 0.1868 0.7983 0.032 Uiso 1 1 calc R U . . .
H17B H 0.8968 0.1854 0.8869 0.032 Uiso 1 1 calc R U . . .
C18 C 0.7930(3) 0.3035(3) 0.8116(3) 0.0367(9) Uani 1 1 d . . . . .
H18A H 0.7466 0.3180 0.7716 0.055 Uiso 1 1 calc R U . . .
H18B H 0.8251 0.3392 0.7845 0.055 Uiso 1 1 calc R U . . .
H18C H 0.7703 0.3180 0.8580 0.055 Uiso 1 1 calc R U . . .
C19 C 0.9142(2) 0.0074(3) 0.9078(2) 0.0259(7) Uani 1 1 d . . . . .
H19 H 0.9524 0.0354 0.8935 0.031 Uiso 1 1 calc R U . . .
C20 C 0.9478(2) -0.0924(3) 0.9308(3) 0.0356(9) Uani 1 1 d D . . . .
O5 O 0.9170(2) -0.1472(3) 0.9651(5) 0.0479(12) Uani 0.788(6) 1 d D . P A 1
O6 O 1.0266(2) -0.1171(2) 0.9014(3) 0.0316(8) Uani 0.788(6) 1 d D . P A 1
C21 C 1.0696(3) -0.2124(3) 0.9108(3) 0.0318(10) Uani 0.788(6) 1 d D . P A 1
H21A H 1.1042 -0.2153 0.8656 0.038 Uiso 0.788(6) 1 calc R U P A 1
H21B H 1.0272 -0.2356 0.9074 0.038 Uiso 0.788(6) 1 calc R U P A 1
C22 C 1.1255(5) -0.2703(4) 0.9939(4) 0.0473(17) Uani 0.788(6) 1 d D . P A 1
H22A H 1.1584 -0.3317 0.9976 0.071 Uiso 0.788(6) 1 calc R U P A 1
H22B H 1.0904 -0.2729 1.0385 0.071 Uiso 0.788(6) 1 calc R U P A 1
H22C H 1.1638 -0.2437 0.9991 0.071 Uiso 0.788(6) 1 calc R U P A 1
O5' O 0.8972(10) -0.1291(15) 0.954(3) 0.0479(12) Uani 0.212(6) 1 d D . P A 2
O6' O 1.0302(5) -0.1378(8) 0.9462(11) 0.0316(8) Uani 0.212(6) 1 d D . P A 2
C21' C 1.0627(10) -0.2378(9) 0.9782(12) 0.0318(10) Uani 0.212(6) 1 d D . P A 2
H21C H 1.0313 -0.2546 0.9467 0.038 Uiso 0.212(6) 1 calc R U P A 2
H21D H 1.0556 -0.2637 1.0373 0.038 Uiso 0.212(6) 1 calc R U P A 2
C22' C 1.1555(11) -0.2746(14) 0.9686(17) 0.0473(17) Uani 0.212(6) 1 d D . P A 2
H22D H 1.1616 -0.2529 0.9096 0.071 Uiso 0.212(6) 1 calc R U P A 2
H22E H 1.1795 -0.3410 0.9937 0.071 Uiso 0.212(6) 1 calc R U P A 2
H22F H 1.1852 -0.2536 0.9963 0.071 Uiso 0.212(6) 1 calc R U P A 2
Br3 Br 0.54566(2) 0.17690(3) 0.22005(2) 0.03667(11) Uani 1 1 d . . . . .
O13 O 0.88031(16) -0.21241(19) 0.59880(15) 0.0293(6) Uani 1 1 d . . . . .
O14 O 0.87657(17) 0.0080(2) 0.42093(15) 0.0316(6) Uani 1 1 d . . . . .
O15 O 0.88935(18) -0.0300(2) 0.70503(17) 0.0381(7) Uani 1 1 d . . . . .
O16 O 0.67385(15) -0.13257(18) 0.59056(16) 0.0270(5) Uani 1 1 d . . . . .
O17 O 0.5893(2) 0.1450(2) 0.5768(3) 0.0515(8) Uani 1 1 d . . . . .
O18 O 0.4644(2) 0.1316(3) 0.6043(3) 0.0639(11) Uani 1 1 d . . . . .
N3 N 0.81896(19) -0.1784(2) 0.46736(17) 0.0234(6) Uani 1 1 d . . . . .
C02Y C 0.5468(3) 0.1006(3) 0.5891(3) 0.0346(8) Uani 1 1 d . . . . .
C45 C 0.7810(2) -0.0520(2) 0.50454(18) 0.0192(6) Uani 1 1 d . . . . .
C46 C 0.8324(2) -0.1578(2) 0.5329(2) 0.0213(6) Uani 1 1 d . . . . .
C47 C 0.7569(2) -0.1020(2) 0.4028(2) 0.0212(6) Uani 1 1 d . . . . .
C48 C 0.7300(2) -0.0255(2) 0.42242(18) 0.0194(6) Uani 1 1 d . . . . .
C49 C 0.6661(2) 0.0581(2) 0.36928(19) 0.0225(7) Uani 1 1 d . . . . .
H49 H 0.6460 0.1091 0.3827 0.027 Uiso 1 1 calc R U . . .
C50 C 0.6329(2) 0.0625(3) 0.2942(2) 0.0247(7) Uani 1 1 d . . . . .
C51 C 0.6612(2) -0.0119(3) 0.2730(2) 0.0263(7) Uani 1 1 d . . . . .
H51 H 0.6385 -0.0058 0.2220 0.032 Uiso 1 1 calc R U . . .
C52 C 0.7242(2) -0.0969(3) 0.3283(2) 0.0251(7) Uani 1 1 d . . . . .
H52 H 0.7434 -0.1483 0.3155 0.030 Uiso 1 1 calc R U . . .
C53 C 0.8602(3) -0.2698(3) 0.4688(2) 0.0344(8) Uani 1 1 d . . . . .
H53A H 0.9079 -0.3073 0.5135 0.052 Uiso 1 1 calc R U . . .
H53B H 0.8804 -0.2656 0.4156 0.052 Uiso 1 1 calc R U . . .
H53C H 0.8197 -0.2973 0.4783 0.052 Uiso 1 1 calc R U . . .
C54 C 0.8514(2) -0.0138(2) 0.4896(2) 0.0212(6) Uani 1 1 d . . . . .
C55 C 0.8872(2) -0.0091(3) 0.5610(2) 0.0238(7) Uani 1 1 d . . . . .
H55 H 0.9325 0.0088 0.5550 0.029 Uiso 1 1 calc R U . . .
C56 C 0.8571(2) -0.0298(3) 0.6358(2) 0.0267(7) Uani 1 1 d . . . . .
C57 C 0.9642(3) -0.0094(5) 0.6980(3) 0.0569(16) Uani 1 1 d . . . . .
H57A H 0.9512 0.0498 0.6521 0.085 Uiso 1 1 calc R U . . .
H57B H 1.0110 -0.0562 0.6875 0.085 Uiso 1 1 calc R U . . .
H57C H 0.9801 -0.0079 0.7497 0.085 Uiso 1 1 calc R U . . .
C58 C 0.7808(2) -0.0533(3) 0.6518(2) 0.0245(7) Uani 1 1 d . . . . .
H58A H 0.7465 -0.0243 0.6866 0.029 Uiso 1 1 calc R U . . .
H58B H 0.8001 -0.1198 0.6820 0.029 Uiso 1 1 calc R U . . .
C59 C 0.7258(2) -0.0196(2) 0.56750(19) 0.0202(6) Uani 1 1 d . . . . .
H59 H 0.7021 0.0481 0.5424 0.024 Uiso 1 1 calc R U . . .
C60 C 0.6506(2) -0.0459(2) 0.58317(18) 0.0202(6) Uani 1 1 d . . . . .
C61 C 0.6129(3) -0.1736(3) 0.6141(3) 0.0388(9) Uani 1 1 d . . . . .
H61A H 0.5632 -0.1405 0.5708 0.047 Uiso 1 1 calc R U . . .
H61B H 0.5937 -0.1722 0.6670 0.047 Uiso 1 1 calc R U . . .
C62 C 0.6603(4) -0.2725(4) 0.6235(5) 0.0721(19) Uani 1 1 d . . . . .
H62A H 0.6765 -0.2726 0.5701 0.108 Uiso 1 1 calc R U . . .
H62B H 0.6234 -0.3044 0.6420 0.108 Uiso 1 1 calc R U . . .
H62C H 0.7108 -0.3033 0.6645 0.108 Uiso 1 1 calc R U . . .
C63 C 0.5717(2) 0.0078(3) 0.5921(2) 0.0255(7) Uani 1 1 d . . . . .
H63 H 0.5300 -0.0157 0.6008 0.031 Uiso 1 1 calc R U . . .
C64 C 0.4253(4) 0.2198(4) 0.6110(5) 0.0667(16) Uani 1 1 d . . . . .
H64A H 0.3674 0.2543 0.5804 0.080 Uiso 1 1 calc R U . . .
H64B H 0.4583 0.2559 0.5857 0.080 Uiso 1 1 calc R U . . .
C65 C 0.4223(4) 0.2052(4) 0.7003(4) 0.0621(14) Uani 1 1 d . . . . .
H65A H 0.3905 0.2635 0.7035 0.093 Uiso 1 1 calc R U . . .
H65B H 0.4798 0.1783 0.7288 0.093 Uiso 1 1 calc R U . . .
H65C H 0.3947 0.1644 0.7267 0.093 Uiso 1 1 calc R U . . .
Br2 Br 0.52445(2) 0.36585(3) 0.70145(2) 0.02745(9) Uani 1 1 d . . . . .
O7 O 0.13453(15) 0.70649(18) 0.36010(15) 0.0271(5) Uani 1 1 d . . . . .
O8 O 0.05390(14) 0.49203(19) 0.37482(14) 0.0248(5) Uani 1 1 d . . . . .
O9 O 0.33077(15) 0.4911(2) 0.37161(16) 0.0295(6) Uani 1 1 d . . . . .
O10 O 0.13967(16) 0.64392(18) 0.55539(15) 0.0254(5) Uani 1 1 d . . . . .
O11 O 0.1870(3) 0.3547(2) 0.66711(18) 0.0496(9) Uani 1 1 d . . . . .
O12 O 0.1563(2) 0.3780(2) 0.78491(17) 0.0461(8) Uani 1 1 d . . . . .
N2 N 0.26480(17) 0.6892(2) 0.41199(17) 0.0207(5) Uani 1 1 d . . . . .
C23 C 0.2031(2) 0.6590(2) 0.40576(19) 0.0201(6) Uani 1 1 d . . . . .
C24 C 0.24074(18) 0.5534(2) 0.46195(18) 0.0174(6) Uani 1 1 d . . . . .
C25 C 0.32144(18) 0.5391(2) 0.50842(18) 0.0164(6) Uani 1 1 d . . . . .
C26 C 0.37780(19) 0.4623(2) 0.57608(19) 0.0190(6) Uani 1 1 d . . . . .
H26 H 0.3690 0.4083 0.6005 0.023 Uiso 1 1 calc R U . . .
C27 C 0.44854(19) 0.4692(2) 0.60617(18) 0.0217(7) Uani 1 1 d . . . . .
C28 C 0.4637(2) 0.5481(3) 0.5701(2) 0.0226(7) Uani 1 1 d . . . . .
H28 H 0.5124 0.5496 0.5907 0.027 Uiso 1 1 calc R U . . .
C29 C 0.4057(2) 0.6258(3) 0.5028(2) 0.0222(6) Uani 1 1 d . . . . .
H29 H 0.4147 0.6795 0.4779 0.027 Uiso 1 1 calc R U . . .
C30 C 0.3345(2) 0.6201(2) 0.47451(18) 0.0189(6) Uani 1 1 d . . . . .
C31 C 0.2549(3) 0.7840(3) 0.3657(2) 0.0310(8) Uani 1 1 d . . . . .
H31A H 0.2057 0.8170 0.3228 0.046 Uiso 1 1 calc R U . . .
H31B H 0.3055 0.7842 0.3399 0.046 Uiso 1 1 calc R U . . .
H31C H 0.2468 0.8134 0.4040 0.046 Uiso 1 1 calc R U . . .
C32 C 0.26180(19) 0.5078(2) 0.39803(19) 0.0189(6) Uani 1 1 d . . . . .
C33 C 0.1948(2) 0.4900(2) 0.36910(19) 0.0202(6) Uani 1 1 d . . . . .
H33 H 0.2041 0.4676 0.3273 0.024 Uiso 1 1 calc R U . . .
C34 C 0.11918(19) 0.5046(2) 0.40065(19) 0.0192(6) Uani 1 1 d . . . . .
C35 C 0.0664(2) 0.4582(3) 0.3094(2) 0.0308(8) Uani 1 1 d . . . . .
H35A H 0.0834 0.4975 0.2619 0.046 Uiso 1 1 calc R U . . .
H35B H 0.0137 0.4583 0.2920 0.046 Uiso 1 1 calc R U . . .
H35C H 0.1105 0.3963 0.3308 0.046 Uiso 1 1 calc R U . . .
C36 C 0.09887(19) 0.5366(3) 0.4703(2) 0.0227(7) Uani 1 1 d . . . . .
H36A H 0.0673 0.5050 0.5079 0.027 Uiso 1 1 calc R U . . .
H36B H 0.0628 0.6025 0.4467 0.027 Uiso 1 1 calc R U . . .
C37 C 0.18179(19) 0.5167(2) 0.52036(18) 0.0179(6) Uani 1 1 d . . . . .
H37 H 0.2131 0.4493 0.5490 0.021 Uiso 1 1 calc R U . . .
C38 C 0.16000(18) 0.5528(2) 0.5881(2) 0.0192(6) Uani 1 1 d . . . . .
C39 C 0.1016(2) 0.6956(3) 0.6054(2) 0.0300(8) Uani 1 1 d . . . . .
H39A H 0.1436 0.6792 0.6516 0.036 Uiso 1 1 calc R U . . .
H39B H 0.0534 0.6829 0.6288 0.036 Uiso 1 1 calc R U . . .
C40 C 0.0718(3) 0.7967(3) 0.5463(3) 0.0457(10) Uani 1 1 d . . . . .
H40A H 0.0353 0.8103 0.4977 0.069 Uiso 1 1 calc R U . . .
H40B H 0.1208 0.8097 0.5285 0.069 Uiso 1 1 calc R U . . .
H40C H 0.0402 0.8343 0.5751 0.069 Uiso 1 1 calc R U . . .
C41 C 0.1574(2) 0.5023(3) 0.6696(2) 0.0253(7) Uani 1 1 d . . . . .
H41 H 0.1470 0.5308 0.7069 0.030 Uiso 1 1 calc R U . . .
C42 C 0.1698(3) 0.4053(3) 0.7029(2) 0.0316(8) Uani 1 1 d . . . . .
C43 C 0.1523(4) 0.2886(3) 0.8262(3) 0.0547(14) Uani 1 1 d . . . . .
H43A H 0.1752 0.2609 0.8856 0.066 Uiso 1 1 calc R U . . .
H43B H 0.1872 0.2478 0.8007 0.066 Uiso 1 1 calc R U . . .
C44 C 0.0614(4) 0.2997(4) 0.8176(3) 0.0564(13) Uani 1 1 d . . . . .
H44A H 0.0395 0.3251 0.7588 0.085 Uiso 1 1 calc R U . . .
H44B H 0.0269 0.3407 0.8422 0.085 Uiso 1 1 calc R U . . .
H44C H 0.0593 0.2405 0.8462 0.085 Uiso 1 1 calc R U . . .
Br4 Br -0.01959(2) 0.66622(3) -0.20167(2) 0.03422(11) Uani 1 1 d . . . . .
O19 O 0.34745(16) 0.27406(18) 0.14773(16) 0.0292(6) Uani 1 1 d . . . . .
O20 O 0.17290(15) 0.4943(2) 0.14392(16) 0.0306(6) Uani 1 1 d . . . . .
O21 O 0.46600(15) 0.4453(2) 0.15830(16) 0.0324(6) Uani 1 1 d . . . . .
O22 O 0.35804(15) 0.35096(17) -0.05587(14) 0.0243(5) Uani 1 1 d . . . . .
O23 O 0.2762(3) 0.6481(2) -0.14688(17) 0.0504(9) Uani 1 1 d . . . . .
O24 O 0.30463(18) 0.64076(18) -0.27085(15) 0.0295(5) Uani 1 1 d . . . . .
N4 N 0.21832(18) 0.3097(2) 0.07718(18) 0.0230(6) Uani 1 1 d . . . . .
C66 C 0.25598(18) 0.4352(2) 0.04820(18) 0.0178(6) Uani 1 1 d . . . . .
C68 C 0.1542(2) 0.3878(3) 0.01525(19) 0.0210(6) Uani 1 1 d . . . . .
C69 C 0.2832(2) 0.3294(2) 0.09692(19) 0.0212(6) Uani 1 1 d . . . . .
C70 C 0.2206(2) 0.2175(3) 0.1121(3) 0.0314(8) Uani 1 1 d . . . . .
H70A H 0.1660 0.2200 0.1297 0.047 Uiso 1 1 calc R U . . .
H70B H 0.2650 0.1782 0.1598 0.047 Uiso 1 1 calc R U . . .
H70C H 0.2323 0.1931 0.0698 0.047 Uiso 1 1 calc R U . . .
C71 C 0.0822(2) 0.3933(3) -0.0248(2) 0.0259(7) Uani 1 1 d . . . . .
H71 H 0.0696 0.3419 -0.0098 0.031 Uiso 1 1 calc R U . . .
C72 C 0.0293(2) 0.4784(3) -0.0881(2) 0.0271(8) Uani 1 1 d . . . . .
H72 H -0.0205 0.4849 -0.1149 0.032 Uiso 1 1 calc R U . . .
C73 C 0.0505(2) 0.5525(3) -0.11110(19) 0.0250(7) Uani 1 1 d . . . . .
C74 C 0.12305(19) 0.5475(2) -0.07013(19) 0.0205(6) Uani 1 1 d . . . . .
H74 H 0.1364 0.5985 -0.0862 0.025 Uiso 1 1 calc R U . . .
C75 C 0.17335(18) 0.4645(2) -0.00547(19) 0.0188(6) Uani 1 1 d . . . . .
C76 C 0.32091(19) 0.4661(2) -0.00475(18) 0.0178(6) Uani 1 1 d . . . . .
H76 H 0.2969 0.5338 -0.0264 0.021 Uiso 1 1 calc R U . . .
C77 C 0.40724(19) 0.4288(3) 0.0495(2) 0.0217(7) Uani 1 1 d . . . . .
H77A H 0.4362 0.3624 0.0674 0.026 Uiso 1 1 calc R U . . .
H77B H 0.4437 0.4566 0.0162 0.026 Uiso 1 1 calc R U . . .
C78 C 0.3927(2) 0.4509(2) 0.1253(2) 0.0221(7) Uani 1 1 d . . . . .
C79 C 0.3167(2) 0.4729(2) 0.1551(2) 0.0222(6) Uani 1 1 d . . . . .
H79 H 0.3117 0.4894 0.2006 0.027 Uiso 1 1 calc R U . . .
C80 C 0.2424(2) 0.4716(2) 0.11870(18) 0.0202(6) Uani 1 1 d . . . . .
C81 C 0.4642(3) 0.4588(4) 0.2350(3) 0.0488(13) Uani 1 1 d . . . . .
H81A H 0.4244 0.5208 0.2244 0.073 Uiso 1 1 calc R U . . .
H81B H 0.5206 0.4489 0.2544 0.073 Uiso 1 1 calc R U . . .
H81C H 0.4463 0.4156 0.2774 0.073 Uiso 1 1 calc R U . . .
C82 C 0.33489(19) 0.4425(2) -0.08035(19) 0.0189(6) Uani 1 1 d . . . . .
C83 C 0.3759(3) 0.3134(3) -0.1184(2) 0.0301(8) Uani 1 1 d . . . . .
H83A H 0.4243 0.3221 -0.1454 0.036 Uiso 1 1 calc R U . . .
H83B H 0.3263 0.3438 -0.1615 0.036 Uiso 1 1 calc R U . . .
C84 C 0.3965(4) 0.2116(3) -0.0725(3) 0.0451(11) Uani 1 1 d . . . . .
H84A H 0.4146 0.1823 -0.1108 0.068 Uiso 1 1 calc R U . . .
H84B H 0.3461 0.2041 -0.0510 0.068 Uiso 1 1 calc R U . . .
H84C H 0.4417 0.1838 -0.0263 0.068 Uiso 1 1 calc R U . . .
C85 C 0.3283(2) 0.5025(2) -0.1601(2) 0.0238(7) Uani 1 1 d . . . . .
H85 H 0.3421 0.4790 -0.2012 0.029 Uiso 1 1 calc R U . . .
C86 C 0.3011(2) 0.6019(3) -0.1874(2) 0.0278(7) Uani 1 1 d . . . . .
C87 C 0.2765(3) 0.7408(3) -0.3091(2) 0.0344(8) Uani 1 1 d . . . . .
H87A H 0.3087 0.7592 -0.2800 0.041 Uiso 1 1 calc R U . . .
H87B H 0.2158 0.7718 -0.3070 0.041 Uiso 1 1 calc R U . . .
C88 C 0.2940(3) 0.7643(3) -0.3993(2) 0.0369(9) Uani 1 1 d . . . . .
H88A H 0.2679 0.8302 -0.4309 0.055 Uiso 1 1 calc R U . . .
H88B H 0.2703 0.7359 -0.4240 0.055 Uiso 1 1 calc R U . . .
H88C H 0.3549 0.7416 -0.4006 0.055 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C6 1.901(3) . ?
O1 C2 1.219(4) . ?
O2 C10 1.217(4) . ?
O3 C12 1.337(4) . ?
O3 C15 1.443(4) . ?
O4 C16 1.340(4) . ?
O4 C17 1.440(4) . ?
N1 C2 1.366(5) . ?
N1 C3 1.402(4) . ?
N1 C9 1.454(5) . ?
C1 C8 1.509(4) . ?
C1 C14 1.546(5) . ?
C1 C10 1.549(5) . ?
C1 C2 1.555(5) . ?
C3 C4 1.390(5) . ?
C3 C8 1.395(5) . ?
C4 C5 1.394(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.385(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.399(4) . ?
C7 C8 1.383(4) . ?
C7 H7 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.451(4) . ?
C11 C12 1.355(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.492(5) . ?
C13 C14 1.531(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C16 1.501(5) . ?
C14 H14 0.9800 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C19 1.355(5) . ?
C17 C18 1.507(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.467(5) . ?
C19 H19 0.9300 . ?
C20 O5 1.205(6) . ?
C20 O5' 1.230(11) . ?
C20 O6' 1.288(8) . ?
C20 O6 1.387(5) . ?
O6 C21 1.455(5) . ?
C21 C22 1.486(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
O6' C21' 1.453(11) . ?
C21' C22' 1.488(12) . ?
C21' H21C 0.9700 . ?
C21' H21D 0.9700 . ?
C22' H22D 0.9600 . ?
C22' H22E 0.9600 . ?
C22' H22F 0.9600 . ?
Br3 C50 1.898(3) . ?
O13 C46 1.218(4) . ?
O14 C54 1.219(4) . ?
O15 C56 1.339(4) . ?
O15 C57 1.446(5) . ?
O16 C60 1.340(4) . ?
O16 C61 1.440(5) . ?
O17 C02Y 1.209(6) . ?
O18 C02Y 1.352(5) . ?
O18 C64 1.452(7) . ?
N3 C46 1.369(4) . ?
N3 C47 1.394(4) . ?
N3 C53 1.442(5) . ?
C02Y C63 1.466(6) . ?
C45 C48 1.506(4) . ?
C45 C59 1.545(5) . ?
C45 C46 1.551(5) . ?
C45 C54 1.554(5) . ?
C47 C52 1.386(4) . ?
C47 C48 1.390(5) . ?
C48 C49 1.382(4) . ?
C49 C50 1.404(5) . ?
C49 H49 0.9300 . ?
C50 C51 1.374(6) . ?
C51 C52 1.398(5) . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 C55 1.446(5) . ?
C55 C56 1.345(5) . ?
C55 H55 0.9300 . ?
C56 C58 1.498(5) . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C58 C59 1.538(4) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 C60 1.506(5) . ?
C59 H59 0.9800 . ?
C60 C63 1.345(5) . ?
C61 C62 1.516(7) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C63 H63 0.9300 . ?
C64 C65 1.472(9) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
Br2 C27 1.902(3) . ?
O7 C23 1.214(4) . ?
O8 C34 1.341(4) . ?
O8 C35 1.443(4) . ?
O9 C32 1.216(4) . ?
O10 C38 1.340(4) . ?
O10 C39 1.443(4) . ?
O11 C42 1.203(5) . ?
O12 C42 1.355(4) . ?
O12 C43 1.453(6) . ?
N2 C23 1.371(4) . ?
N2 C30 1.407(4) . ?
N2 C31 1.452(5) . ?
C23 C24 1.553(4) . ?
C24 C25 1.507(4) . ?
C24 C37 1.539(4) . ?
C24 C32 1.555(4) . ?
C25 C26 1.385(4) . ?
C25 C30 1.394(5) . ?
C26 C27 1.399(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.383(5) . ?
C28 C29 1.397(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.380(4) . ?
C29 H29 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.449(4) . ?
C33 C34 1.353(5) . ?
C33 H33 0.9300 . ?
C34 C36 1.493(4) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.535(4) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.507(4) . ?
C37 H37 0.9800 . ?
C38 C41 1.349(5) . ?
C39 C40 1.512(6) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.466(6) . ?
C41 H41 0.9300 . ?
C43 C44 1.494(9) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
Br4 C73 1.903(3) . ?
O19 C69 1.216(4) . ?
O20 C80 1.218(4) . ?
O21 C78 1.349(4) . ?
O21 C81 1.436(5) . ?
O22 C82 1.351(4) . ?
O22 C83 1.438(4) . ?
O23 C86 1.209(5) . ?
O24 C86 1.347(4) . ?
O24 C87 1.457(5) . ?
N4 C69 1.371(4) . ?
N4 C68 1.399(4) . ?
N4 C70 1.448(5) . ?
C66 C75 1.510(4) . ?
C66 C76 1.539(4) . ?
C66 C69 1.552(5) . ?
C66 C80 1.555(4) . ?
C68 C71 1.389(4) . ?
C68 C75 1.394(5) . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C71 C72 1.393(5) . ?
C71 H71 0.9300 . ?
C72 C73 1.372(6) . ?
C72 H72 0.9300 . ?
C73 C74 1.408(4) . ?
C74 C75 1.374(4) . ?
C74 H74 0.9300 . ?
C76 C82 1.505(4) . ?
C76 C77 1.534(4) . ?
C76 H76 0.9800 . ?
C77 C78 1.495(4) . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
C78 C79 1.347(5) . ?
C79 C80 1.451(4) . ?
C79 H79 0.9300 . ?
C81 H81A 0.9600 . ?
C81 H81B 0.9600 . ?
C81 H81C 0.9600 . ?
C82 C85 1.340(5) . ?
C83 C84 1.509(6) . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C84 H84A 0.9600 . ?
C84 H84B 0.9600 . ?
C84 H84C 0.9600 . ?
C85 C86 1.461(5) . ?
C85 H85 0.9300 . ?
C87 C88 1.506(5) . ?
C87 H87A 0.9700 . ?
C87 H87B 0.9700 . ?
C88 H88A 0.9600 . ?
C88 H88B 0.9600 . ?
C88 H88C 0.9600 . ?

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
C12 O3 C15 117.5(3) . . ?
C16 O4 C17 119.8(3) . . ?
C2 N1 C3 111.7(3) . . ?
C2 N1 C9 123.4(3) . . ?
C3 N1 C9 124.8(3) . . ?
C8 C1 C14 112.8(2) . . ?
C8 C1 C10 112.9(3) . . ?
C14 C1 C10 108.4(3) . . ?
C8 C1 C2 101.3(3) . . ?
C14 C1 C2 116.2(3) . . ?
C10 C1 C2 105.0(2) . . ?
O1 C2 N1 125.5(3) . . ?
O1 C2 C1 126.5(3) . . ?
N1 C2 C1 107.9(2) . . ?
C4 C3 C8 122.0(3) . . ?
C4 C3 N1 128.6(3) . . ?
C8 C3 N1 109.4(3) . . ?
C3 C4 C5 117.4(3) . . ?
C3 C4 H4 121.3 . . ?
C5 C4 H4 121.3 . . ?
C6 C5 C4 120.5(3) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 122.0(3) . . ?
C5 C6 Br1 119.4(2) . . ?
C7 C6 Br1 118.6(3) . . ?
C8 C7 C6 117.5(3) . . ?
C8 C7 H7 121.3 . . ?
C6 C7 H7 121.3 . . ?
C7 C8 C3 120.5(3) . . ?
C7 C8 C1 130.1(3) . . ?
C3 C8 C1 109.4(3) . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C10 C11 121.8(3) . . ?
O2 C10 C1 120.2(3) . . ?
C11 C10 C1 117.9(3) . . ?
C12 C11 C10 122.2(3) . . ?
C12 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
O3 C12 C11 125.6(3) . . ?
O3 C12 C13 111.3(3) . . ?
C11 C12 C13 123.1(3) . . ?
C12 C13 C14 110.3(3) . . ?
C12 C13 H13A 109.6 . . ?
C14 C13 H13A 109.6 . . ?
C12 C13 H13B 109.6 . . ?
C14 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C16 C14 C13 109.9(3) . . ?
C16 C14 C1 113.8(3) . . ?
C13 C14 C1 111.7(3) . . ?
C16 C14 H14 107.1 . . ?
C13 C14 H14 107.1 . . ?
C1 C14 H14 107.1 . . ?
O3 C15 H15A 109.5 . . ?
O3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O4 C16 C19 124.3(3) . . ?
O4 C16 C14 110.6(3) . . ?
C19 C16 C14 125.0(3) . . ?
O4 C17 C18 106.2(3) . . ?
O4 C17 H17A 110.5 . . ?
C18 C17 H17A 110.5 . . ?
O4 C17 H17B 110.5 . . ?
C18 C17 H17B 110.5 . . ?
H17A C17 H17B 108.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 C20 123.7(4) . . ?
C16 C19 H19 118.1 . . ?
C20 C19 H19 118.1 . . ?
O5' C20 O6' 123.6(11) . . ?
O5 C20 O6 122.4(5) . . ?
O5 C20 C19 131.0(4) . . ?
O5' C20 C19 117.1(13) . . ?
O6' C20 C19 116.9(6) . . ?
O6 C20 C19 106.5(3) . . ?
C20 O6 C21 116.7(4) . . ?
O6 C21 C22 109.5(4) . . ?
O6 C21 H21A 109.8 . . ?
C22 C21 H21A 109.8 . . ?
O6 C21 H21B 109.8 . . ?
C22 C21 H21B 109.8 . . ?
H21A C21 H21B 108.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 O6' C21' 116.5(11) . . ?
O6' C21' C22' 108.0(11) . . ?
O6' C21' H21C 110.1 . . ?
C22' C21' H21C 110.1 . . ?
O6' C21' H21D 110.1 . . ?
C22' C21' H21D 110.1 . . ?
H21C C21' H21D 108.4 . . ?
C21' C22' H22D 109.5 . . ?
C21' C22' H22E 109.5 . . ?
H22D C22' H22E 109.5 . . ?
C21' C22' H22F 109.5 . . ?
H22D C22' H22F 109.5 . . ?
H22E C22' H22F 109.5 . . ?
C56 O15 C57 116.2(3) . . ?
C60 O16 C61 118.6(3) . . ?
C02Y O18 C64 119.7(4) . . ?
C46 N3 C47 111.5(3) . . ?
C46 N3 C53 123.4(3) . . ?
C47 N3 C53 125.0(3) . . ?
O17 C02Y O18 122.9(4) . . ?
O17 C02Y C63 128.9(4) . . ?
O18 C02Y C63 108.2(4) . . ?
C48 C45 C59 114.0(3) . . ?
C48 C45 C46 101.6(3) . . ?
C59 C45 C46 117.2(3) . . ?
C48 C45 C54 111.5(3) . . ?
C59 C45 C54 108.1(3) . . ?
C46 C45 C54 104.1(2) . . ?
O13 C46 N3 125.5(3) . . ?
O13 C46 C45 127.0(3) . . ?
N3 C46 C45 107.4(3) . . ?
C52 C47 C48 122.0(3) . . ?
C52 C47 N3 128.3(3) . . ?
C48 C47 N3 109.8(3) . . ?
C49 C48 C47 120.6(3) . . ?
C49 C48 C45 130.4(3) . . ?
C47 C48 C45 109.0(3) . . ?
C48 C49 C50 117.1(3) . . ?
C48 C49 H49 121.5 . . ?
C50 C49 H49 121.5 . . ?
C51 C50 C49 122.7(3) . . ?
C51 C50 Br3 119.6(2) . . ?
C49 C50 Br3 117.6(3) . . ?
C50 C51 C52 119.8(3) . . ?
C50 C51 H51 120.1 . . ?
C52 C51 H51 120.1 . . ?
C47 C52 C51 117.8(3) . . ?
C47 C52 H52 121.1 . . ?
C51 C52 H52 121.1 . . ?
N3 C53 H53A 109.5 . . ?
N3 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
N3 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O14 C54 C55 122.3(3) . . ?
O14 C54 C45 120.5(3) . . ?
C55 C54 C45 117.2(3) . . ?
C56 C55 C54 122.3(3) . . ?
C56 C55 H55 118.9 . . ?
C54 C55 H55 118.9 . . ?
O15 C56 C55 125.1(3) . . ?
O15 C56 C58 110.9(3) . . ?
C55 C56 C58 124.0(3) . . ?
O15 C57 H57A 109.5 . . ?
O15 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
O15 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 C59 110.1(3) . . ?
C56 C58 H58A 109.6 . . ?
C59 C58 H58A 109.6 . . ?
C56 C58 H58B 109.6 . . ?
C59 C58 H58B 109.6 . . ?
H58A C58 H58B 108.1 . . ?
C60 C59 C58 110.3(3) . . ?
C60 C59 C45 114.0(3) . . ?
C58 C59 C45 111.5(3) . . ?
C60 C59 H59 106.9 . . ?
C58 C59 H59 106.9 . . ?
C45 C59 H59 106.9 . . ?
O16 C60 C63 124.0(3) . . ?
O16 C60 C59 110.4(3) . . ?
C63 C60 C59 125.5(3) . . ?
O16 C61 C62 105.8(4) . . ?
O16 C61 H61A 110.6 . . ?
C62 C61 H61A 110.6 . . ?
O16 C61 H61B 110.6 . . ?
C62 C61 H61B 110.6 . . ?
H61A C61 H61B 108.7 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C60 C63 C02Y 124.6(4) . . ?
C60 C63 H63 117.7 . . ?
C02Y C63 H63 117.7 . . ?
O18 C64 C65 110.3(5) . . ?
O18 C64 H64A 109.6 . . ?
C65 C64 H64A 109.6 . . ?
O18 C64 H64B 109.6 . . ?
C65 C64 H64B 109.6 . . ?
H64A C64 H64B 108.1 . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C34 O8 C35 117.1(3) . . ?
C38 O10 C39 119.4(3) . . ?
C42 O12 C43 117.5(4) . . ?
C23 N2 C30 111.9(3) . . ?
C23 N2 C31 123.7(3) . . ?
C30 N2 C31 124.1(3) . . ?
O7 C23 N2 125.1(3) . . ?
O7 C23 C24 127.5(3) . . ?
N2 C23 C24 107.2(2) . . ?
C25 C24 C37 113.9(2) . . ?
C25 C24 C23 101.5(3) . . ?
C37 C24 C23 116.9(3) . . ?
C25 C24 C32 111.4(2) . . ?
C37 C24 C32 108.2(3) . . ?
C23 C24 C32 104.5(2) . . ?
C26 C25 C30 120.4(3) . . ?
C26 C25 C24 130.1(3) . . ?
C30 C25 C24 109.6(3) . . ?
C25 C26 C27 117.2(3) . . ?
C25 C26 H26 121.4 . . ?
C27 C26 H26 121.4 . . ?
C28 C27 C26 122.5(3) . . ?
C28 C27 Br2 119.7(2) . . ?
C26 C27 Br2 117.8(3) . . ?
C27 C28 C29 119.8(3) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C30 C29 C28 117.9(3) . . ?
C30 C29 H29 121.0 . . ?
C28 C29 H29 121.0 . . ?
C29 C30 C25 122.1(3) . . ?
C29 C30 N2 129.0(3) . . ?
C25 C30 N2 108.8(3) . . ?
N2 C31 H31A 109.5 . . ?
N2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O9 C32 C33 122.0(3) . . ?
O9 C32 C24 120.7(3) . . ?
C33 C32 C24 117.2(3) . . ?
C34 C33 C32 122.5(3) . . ?
C34 C33 H33 118.8 . . ?
C32 C33 H33 118.8 . . ?
O8 C34 C33 125.3(3) . . ?
O8 C34 C36 111.5(3) . . ?
C33 C34 C36 123.3(3) . . ?
O8 C35 H35A 109.5 . . ?
O8 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O8 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 C37 110.5(3) . . ?
C34 C36 H36A 109.5 . . ?
C37 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C37 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C38 C37 C36 109.8(3) . . ?
C38 C37 C24 113.2(3) . . ?
C36 C37 C24 111.8(2) . . ?
C38 C37 H37 107.2 . . ?
C36 C37 H37 107.2 . . ?
C24 C37 H37 107.2 . . ?
O10 C38 C41 124.2(3) . . ?
O10 C38 C37 110.4(3) . . ?
C41 C38 C37 125.3(3) . . ?
O10 C39 C40 106.3(3) . . ?
O10 C39 H39A 110.5 . . ?
C40 C39 H39A 110.5 . . ?
O10 C39 H39B 110.5 . . ?
C40 C39 H39B 110.5 . . ?
H39A C39 H39B 108.7 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 C42 124.0(3) . . ?
C38 C41 H41 118.0 . . ?
C42 C41 H41 118.0 . . ?
O11 C42 O12 122.3(4) . . ?
O11 C42 C41 129.0(3) . . ?
O12 C42 C41 108.8(3) . . ?
O12 C43 C44 110.2(4) . . ?
O12 C43 H43A 109.6 . . ?
C44 C43 H43A 109.6 . . ?
O12 C43 H43B 109.6 . . ?
C44 C43 H43B 109.6 . . ?
H43A C43 H43B 108.1 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C78 O21 C81 117.0(3) . . ?
C82 O22 C83 119.2(3) . . ?
C86 O24 C87 116.4(3) . . ?
C69 N4 C68 111.5(3) . . ?
C69 N4 C70 123.3(3) . . ?
C68 N4 C70 125.1(3) . . ?
C75 C66 C76 112.4(2) . . ?
C75 C66 C69 101.9(3) . . ?
C76 C66 C69 116.9(3) . . ?
C75 C66 C80 113.4(3) . . ?
C76 C66 C80 107.8(3) . . ?
C69 C66 C80 104.2(2) . . ?
C71 C68 C75 121.9(3) . . ?
C71 C68 N4 128.0(4) . . ?
C75 C68 N4 110.0(3) . . ?
O19 C69 N4 125.3(3) . . ?
O19 C69 C66 126.9(3) . . ?
N4 C69 C66 107.6(2) . . ?
N4 C70 H70A 109.5 . . ?
N4 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
N4 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C68 C71 C72 117.8(4) . . ?
C68 C71 H71 121.1 . . ?
C72 C71 H71 121.1 . . ?
C73 C72 C71 120.1(3) . . ?
C73 C72 H72 119.9 . . ?
C71 C72 H72 119.9 . . ?
C72 C73 C74 122.3(3) . . ?
C72 C73 Br4 119.3(2) . . ?
C74 C73 Br4 118.4(3) . . ?
C75 C74 C73 117.5(3) . . ?
C75 C74 H74 121.2 . . ?
C73 C74 H74 121.2 . . ?
C74 C75 C68 120.3(3) . . ?
C74 C75 C66 130.8(3) . . ?
C68 C75 C66 108.7(3) . . ?
C82 C76 C77 110.3(3) . . ?
C82 C76 C66 113.8(3) . . ?
C77 C76 C66 111.7(2) . . ?
C82 C76 H76 106.9 . . ?
C77 C76 H76 106.9 . . ?
C66 C76 H76 106.9 . . ?
C78 C77 C76 110.0(3) . . ?
C78 C77 H77A 109.7 . . ?
C76 C77 H77A 109.7 . . ?
C78 C77 H77B 109.7 . . ?
C76 C77 H77B 109.7 . . ?
H77A C77 H77B 108.2 . . ?
C79 C78 O21 126.0(3) . . ?
C79 C78 C77 123.8(3) . . ?
O21 C78 C77 110.2(3) . . ?
C78 C79 C80 122.2(3) . . ?
C78 C79 H79 118.9 . . ?
C80 C79 H79 118.9 . . ?
O20 C80 C79 122.2(3) . . ?
O20 C80 C66 120.7(3) . . ?
C79 C80 C66 117.0(3) . . ?
O21 C81 H81A 109.5 . . ?
O21 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
O21 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C85 C82 O22 124.5(3) . . ?
C85 C82 C76 125.4(3) . . ?
O22 C82 C76 110.1(3) . . ?
O22 C83 C84 106.6(3) . . ?
O22 C83 H83A 110.4 . . ?
C84 C83 H83A 110.4 . . ?
O22 C83 H83B 110.4 . . ?
C84 C83 H83B 110.4 . . ?
H83A C83 H83B 108.6 . . ?
C83 C84 H84A 109.5 . . ?
C83 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C83 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C82 C85 C86 124.8(3) . . ?
C82 C85 H85 117.6 . . ?
C86 C85 H85 117.6 . . ?
O23 C86 O24 121.4(4) . . ?
O23 C86 C85 129.4(3) . . ?
O24 C86 C85 109.2(3) . . ?
O24 C87 C88 105.2(3) . . ?
O24 C87 H87A 110.7 . . ?
C88 C87 H87A 110.7 . . ?
O24 C87 H87B 110.7 . . ?
C88 C87 H87B 110.7 . . ?
H87A C87 H87B 108.8 . . ?
C87 C88 H88A 109.5 . . ?
C87 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C87 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 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
C3 N1 C2 O1 -179.3(3) . . . . ?
C9 N1 C2 O1 -3.4(6) . . . . ?
C3 N1 C2 C1 4.8(4) . . . . ?
C9 N1 C2 C1 -179.2(3) . . . . ?
C8 C1 C2 O1 178.7(3) . . . . ?
C14 C1 C2 O1 56.0(5) . . . . ?
C10 C1 C2 O1 -63.7(4) . . . . ?
C8 C1 C2 N1 -5.5(3) . . . . ?
C14 C1 C2 N1 -128.2(3) . . . . ?
C10 C1 C2 N1 112.1(3) . . . . ?
C2 N1 C3 C4 177.5(4) . . . . ?
C9 N1 C3 C4 1.6(6) . . . . ?
C2 N1 C3 C8 -1.9(4) . . . . ?
C9 N1 C3 C8 -177.8(3) . . . . ?
C8 C3 C4 C5 1.2(5) . . . . ?
N1 C3 C4 C5 -178.1(3) . . . . ?
C3 C4 C5 C6 1.1(5) . . . . ?
C4 C5 C6 C7 -2.4(5) . . . . ?
C4 C5 C6 Br1 176.7(3) . . . . ?
C5 C6 C7 C8 1.3(5) . . . . ?
Br1 C6 C7 C8 -177.8(2) . . . . ?
C6 C7 C8 C3 1.1(5) . . . . ?
C6 C7 C8 C1 180.0(3) . . . . ?
C4 C3 C8 C7 -2.4(5) . . . . ?
N1 C3 C8 C7 177.1(3) . . . . ?
C4 C3 C8 C1 178.6(3) . . . . ?
N1 C3 C8 C1 -2.0(4) . . . . ?
C14 C1 C8 C7 -49.5(5) . . . . ?
C10 C1 C8 C7 73.8(4) . . . . ?
C2 C1 C8 C7 -174.5(3) . . . . ?
C14 C1 C8 C3 129.4(3) . . . . ?
C10 C1 C8 C3 -107.2(3) . . . . ?
C2 C1 C8 C3 4.5(3) . . . . ?
C8 C1 C10 O2 23.2(5) . . . . ?
C14 C1 C10 O2 149.0(3) . . . . ?
C2 C1 C10 O2 -86.2(4) . . . . ?
C8 C1 C10 C11 -157.8(3) . . . . ?
C14 C1 C10 C11 -32.1(4) . . . . ?
C2 C1 C10 C11 92.7(3) . . . . ?
O2 C10 C11 C12 -177.8(4) . . . . ?
C1 C10 C11 C12 3.3(5) . . . . ?
C15 O3 C12 C11 -1.5(5) . . . . ?
C15 O3 C12 C13 177.0(3) . . . . ?
C10 C11 C12 O3 -179.8(3) . . . . ?
C10 C11 C12 C13 1.9(5) . . . . ?
O3 C12 C13 C14 -155.5(3) . . . . ?
C11 C12 C13 C14 23.1(5) . . . . ?
C12 C13 C14 C16 180.0(3) . . . . ?
C12 C13 C14 C1 -52.8(4) . . . . ?
C8 C1 C14 C16 -52.3(4) . . . . ?
C10 C1 C14 C16 -178.1(2) . . . . ?
C2 C1 C14 C16 64.1(3) . . . . ?
C8 C1 C14 C13 -177.3(3) . . . . ?
C10 C1 C14 C13 56.9(4) . . . . ?
C2 C1 C14 C13 -60.9(4) . . . . ?
C17 O4 C16 C19 4.5(5) . . . . ?
C17 O4 C16 C14 -171.2(3) . . . . ?
C13 C14 C16 O4 76.2(4) . . . . ?
C1 C14 C16 O4 -49.8(3) . . . . ?
C13 C14 C16 C19 -99.4(4) . . . . ?
C1 C14 C16 C19 134.6(3) . . . . ?
C16 O4 C17 C18 173.7(3) . . . . ?
O4 C16 C19 C20 -174.9(3) . . . . ?
C14 C16 C19 C20 0.2(5) . . . . ?
C16 C19 C20 O5 -14.6(9) . . . . ?
C16 C19 C20 O5' -4(2) . . . . ?
C16 C19 C20 O6' -166.4(9) . . . . ?
C16 C19 C20 O6 162.5(3) . . . . ?
O5 C20 O6 C21 2.3(8) . . . . ?
O5' C20 O6 C21 -12(3) . . . . ?
O6' C20 O6 C21 69.8(12) . . . . ?
C19 C20 O6 C21 -175.1(4) . . . . ?
C20 O6 C21 C22 -89.6(6) . . . . ?
O5 C20 O6' C21' 15.1(17) . . . . ?
O5' C20 O6' C21' 12(3) . . . . ?
O6 C20 O6' C21' -110(2) . . . . ?
C19 C20 O6' C21' 173.2(12) . . . . ?
C20 O6' C21' C22' 164.1(17) . . . . ?
C64 O18 C02Y O17 -3.4(8) . . . . ?
C64 O18 C02Y C63 175.7(5) . . . . ?
C47 N3 C46 O13 176.8(3) . . . . ?
C53 N3 C46 O13 0.8(6) . . . . ?
C47 N3 C46 C45 -7.4(4) . . . . ?
C53 N3 C46 C45 176.6(3) . . . . ?
C48 C45 C46 O13 -175.9(3) . . . . ?
C59 C45 C46 O13 -51.1(5) . . . . ?
C54 C45 C46 O13 68.2(4) . . . . ?
C48 C45 C46 N3 8.3(3) . . . . ?
C59 C45 C46 N3 133.1(3) . . . . ?
C54 C45 C46 N3 -107.6(3) . . . . ?
C46 N3 C47 C52 -177.6(3) . . . . ?
C53 N3 C47 C52 -1.6(6) . . . . ?
C46 N3 C47 C48 3.1(4) . . . . ?
C53 N3 C47 C48 179.1(4) . . . . ?
C52 C47 C48 C49 3.1(5) . . . . ?
N3 C47 C48 C49 -177.6(3) . . . . ?
C52 C47 C48 C45 -176.7(3) . . . . ?
N3 C47 C48 C45 2.7(4) . . . . ?
C59 C45 C48 C49 46.8(5) . . . . ?
C46 C45 C48 C49 173.7(3) . . . . ?
C54 C45 C48 C49 -75.9(4) . . . . ?
C59 C45 C48 C47 -133.5(3) . . . . ?
C46 C45 C48 C47 -6.5(3) . . . . ?
C54 C45 C48 C47 103.8(3) . . . . ?
C47 C48 C49 C50 -2.5(5) . . . . ?
C45 C48 C49 C50 177.2(3) . . . . ?
C48 C49 C50 C51 0.3(5) . . . . ?
C48 C49 C50 Br3 -179.6(2) . . . . ?
C49 C50 C51 C52 1.5(5) . . . . ?
Br3 C50 C51 C52 -178.6(3) . . . . ?
C48 C47 C52 C51 -1.2(5) . . . . ?
N3 C47 C52 C51 179.6(3) . . . . ?
C50 C51 C52 C47 -1.0(5) . . . . ?
C48 C45 C54 O14 -20.6(5) . . . . ?
C59 C45 C54 O14 -146.6(3) . . . . ?
C46 C45 C54 O14 88.1(4) . . . . ?
C48 C45 C54 C55 161.7(3) . . . . ?
C59 C45 C54 C55 35.7(4) . . . . ?
C46 C45 C54 C55 -89.6(3) . . . . ?
O14 C54 C55 C56 177.3(4) . . . . ?
C45 C54 C55 C56 -5.0(5) . . . . ?
C57 O15 C56 C55 -2.2(7) . . . . ?
C57 O15 C56 C58 179.2(4) . . . . ?
C54 C55 C56 O15 177.4(4) . . . . ?
C54 C55 C56 C58 -4.2(6) . . . . ?
O15 C56 C58 C59 159.7(3) . . . . ?
C55 C56 C58 C59 -18.9(5) . . . . ?
C56 C58 C59 C60 178.2(3) . . . . ?
C56 C58 C59 C45 50.5(4) . . . . ?
C48 C45 C59 C60 51.3(4) . . . . ?
C46 C45 C59 C60 -67.1(3) . . . . ?
C54 C45 C59 C60 175.8(2) . . . . ?
C48 C45 C59 C58 176.9(3) . . . . ?
C46 C45 C59 C58 58.6(4) . . . . ?
C54 C45 C59 C58 -58.6(4) . . . . ?
C61 O16 C60 C63 -3.6(5) . . . . ?
C61 O16 C60 C59 173.9(3) . . . . ?
C58 C59 C60 O16 -84.6(3) . . . . ?
C45 C59 C60 O16 41.7(3) . . . . ?
C58 C59 C60 C63 92.9(4) . . . . ?
C45 C59 C60 C63 -140.8(3) . . . . ?
C60 O16 C61 C62 -175.8(4) . . . . ?
O16 C60 C63 C02Y 176.3(3) . . . . ?
C59 C60 C63 C02Y -0.9(5) . . . . ?
O17 C02Y C63 C60 1.8(7) . . . . ?
O18 C02Y C63 C60 -177.2(4) . . . . ?
C02Y O18 C64 C65 -102.5(6) . . . . ?
C30 N2 C23 O7 175.8(3) . . . . ?
C31 N2 C23 O7 1.8(5) . . . . ?
C30 N2 C23 C24 -8.4(4) . . . . ?
C31 N2 C23 C24 177.6(3) . . . . ?
O7 C23 C24 C25 -174.5(3) . . . . ?
N2 C23 C24 C25 9.8(3) . . . . ?
O7 C23 C24 C37 -50.1(4) . . . . ?
N2 C23 C24 C37 134.3(3) . . . . ?
O7 C23 C24 C32 69.5(4) . . . . ?
N2 C23 C24 C32 -106.2(3) . . . . ?
C37 C24 C25 C26 43.9(5) . . . . ?
C23 C24 C25 C26 170.4(3) . . . . ?
C32 C24 C25 C26 -78.8(4) . . . . ?
C37 C24 C25 C30 -134.5(3) . . . . ?
C23 C24 C25 C30 -8.1(3) . . . . ?
C32 C24 C25 C30 102.7(3) . . . . ?
C30 C25 C26 C27 -1.9(5) . . . . ?
C24 C25 C26 C27 179.8(3) . . . . ?
C25 C26 C27 C28 -1.0(5) . . . . ?
C25 C26 C27 Br2 177.9(2) . . . . ?
C26 C27 C28 C29 2.1(5) . . . . ?
Br2 C27 C28 C29 -176.8(2) . . . . ?
C27 C28 C29 C30 -0.2(5) . . . . ?
C28 C29 C30 C25 -2.8(5) . . . . ?
C28 C29 C30 N2 175.9(3) . . . . ?
C26 C25 C30 C29 3.9(5) . . . . ?
C24 C25 C30 C29 -177.5(3) . . . . ?
C26 C25 C30 N2 -175.0(3) . . . . ?
C24 C25 C30 N2 3.7(4) . . . . ?
C23 N2 C30 C29 -175.5(3) . . . . ?
C31 N2 C30 C29 -1.6(6) . . . . ?
C23 N2 C30 C25 3.2(4) . . . . ?
C31 N2 C30 C25 177.2(3) . . . . ?
C25 C24 C32 O9 -21.7(4) . . . . ?
C37 C24 C32 O9 -147.6(3) . . . . ?
C23 C24 C32 O9 87.1(3) . . . . ?
C25 C24 C32 C33 160.8(3) . . . . ?
C37 C24 C32 C33 34.9(3) . . . . ?
C23 C24 C32 C33 -90.3(3) . . . . ?
O9 C32 C33 C34 177.2(3) . . . . ?
C24 C32 C33 C34 -5.4(5) . . . . ?
C35 O8 C34 C33 1.4(5) . . . . ?
C35 O8 C34 C36 -178.0(3) . . . . ?
C32 C33 C34 O8 178.0(3) . . . . ?
C32 C33 C34 C36 -2.6(5) . . . . ?
O8 C34 C36 C37 159.2(3) . . . . ?
C33 C34 C36 C37 -20.3(5) . . . . ?
C34 C36 C37 C38 177.7(3) . . . . ?
C34 C36 C37 C24 51.1(4) . . . . ?
C25 C24 C37 C38 52.9(4) . . . . ?
C23 C24 C37 C38 -65.1(3) . . . . ?
C32 C24 C37 C38 177.4(2) . . . . ?
C25 C24 C37 C36 177.6(3) . . . . ?
C23 C24 C37 C36 59.7(4) . . . . ?
C32 C24 C37 C36 -57.9(3) . . . . ?
C39 O10 C38 C41 -8.6(5) . . . . ?
C39 O10 C38 C37 168.7(3) . . . . ?
C36 C37 C38 O10 -81.4(3) . . . . ?
C24 C37 C38 O10 44.4(3) . . . . ?
C36 C37 C38 C41 95.9(4) . . . . ?
C24 C37 C38 C41 -138.3(3) . . . . ?
C38 O10 C39 C40 -169.8(3) . . . . ?
O10 C38 C41 C42 172.5(3) . . . . ?
C37 C38 C41 C42 -4.4(5) . . . . ?
C43 O12 C42 O11 -7.9(7) . . . . ?
C43 O12 C42 C41 170.7(4) . . . . ?
C38 C41 C42 O11 3.2(7) . . . . ?
C38 C41 C42 O12 -175.2(3) . . . . ?
C42 O12 C43 C44 -91.9(5) . . . . ?
C69 N4 C68 C71 175.0(3) . . . . ?
C70 N4 C68 C71 -0.4(6) . . . . ?
C69 N4 C68 C75 -2.9(4) . . . . ?
C70 N4 C68 C75 -178.3(3) . . . . ?
C68 N4 C69 O19 -178.9(3) . . . . ?
C70 N4 C69 O19 -3.4(6) . . . . ?
C68 N4 C69 C66 5.4(4) . . . . ?
C70 N4 C69 C66 -179.1(3) . . . . ?
C75 C66 C69 O19 178.8(3) . . . . ?
C76 C66 C69 O19 55.9(4) . . . . ?
C80 C66 C69 O19 -63.0(4) . . . . ?
C75 C66 C69 N4 -5.6(3) . . . . ?
C76 C66 C69 N4 -128.5(3) . . . . ?
C80 C66 C69 N4 112.6(3) . . . . ?
C75 C68 C71 C72 1.0(5) . . . . ?
N4 C68 C71 C72 -176.7(3) . . . . ?
C68 C71 C72 C73 2.1(5) . . . . ?
C71 C72 C73 C74 -2.9(5) . . . . ?
C71 C72 C73 Br4 176.8(3) . . . . ?
C72 C73 C74 C75 0.4(5) . . . . ?
Br4 C73 C74 C75 -179.3(2) . . . . ?
C73 C74 C75 C68 2.7(5) . . . . ?
C73 C74 C75 C66 177.3(3) . . . . ?
C71 C68 C75 C74 -3.5(5) . . . . ?
N4 C68 C75 C74 174.5(3) . . . . ?
C71 C68 C75 C66 -179.1(3) . . . . ?
N4 C68 C75 C66 -1.1(4) . . . . ?
C76 C66 C75 C74 -45.1(5) . . . . ?
C69 C66 C75 C74 -171.0(3) . . . . ?
C80 C66 C75 C74 77.6(4) . . . . ?
C76 C66 C75 C68 130.0(3) . . . . ?
C69 C66 C75 C68 4.0(3) . . . . ?
C80 C66 C75 C68 -107.4(3) . . . . ?
C75 C66 C76 C82 -49.4(4) . . . . ?
C69 C66 C76 C82 68.0(3) . . . . ?
C80 C66 C76 C82 -175.1(2) . . . . ?
C75 C66 C76 C77 -175.1(3) . . . . ?
C69 C66 C76 C77 -57.8(4) . . . . ?
C80 C66 C76 C77 59.1(3) . . . . ?
C82 C76 C77 C78 -178.9(3) . . . . ?
C66 C76 C77 C78 -51.2(4) . . . . ?
C81 O21 C78 C79 3.8(6) . . . . ?
C81 O21 C78 C77 -176.1(4) . . . . ?
C76 C77 C78 C79 19.2(5) . . . . ?
C76 C77 C78 O21 -160.8(3) . . . . ?
O21 C78 C79 C80 -176.1(3) . . . . ?
C77 C78 C79 C80 3.8(6) . . . . ?
C78 C79 C80 O20 -177.6(4) . . . . ?
C78 C79 C80 C66 5.4(5) . . . . ?
C75 C66 C80 O20 21.9(5) . . . . ?
C76 C66 C80 O20 147.0(3) . . . . ?
C69 C66 C80 O20 -88.1(4) . . . . ?
C75 C66 C80 C79 -161.0(3) . . . . ?
C76 C66 C80 C79 -35.9(4) . . . . ?
C69 C66 C80 C79 89.0(3) . . . . ?
C83 O22 C82 C85 -1.1(5) . . . . ?
C83 O22 C82 C76 -179.0(3) . . . . ?
C77 C76 C82 C85 -106.2(4) . . . . ?
C66 C76 C82 C85 127.3(3) . . . . ?
C77 C76 C82 O22 71.7(3) . . . . ?
C66 C76 C82 O22 -54.8(3) . . . . ?
C82 O22 C83 C84 -178.0(3) . . . . ?
O22 C82 C85 C86 178.3(3) . . . . ?
C76 C82 C85 C86 -4.1(5) . . . . ?
C87 O24 C86 O23 -0.2(6) . . . . ?
C87 O24 C86 C85 177.9(3) . . . . ?
C82 C85 C86 O23 -4.2(7) . . . . ?
C82 C85 C86 O24 177.9(3) . . . . ?
C86 O24 C87 C88 175.4(3) . . . . ?

_refine_diff_density_max         1.054
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.107

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_n141127b
_database_code_depnum_ccdc_archive 'CCDC 1418021'
_audit_update_record             
;
2015-08-11 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H23 N O6'
_chemical_formula_weight         385.40

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'

_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                   10.0957(6)
_cell_length_b                   10.7765(6)
_cell_length_c                   18.4533(11)
_cell_angle_alpha                95.1770(10)
_cell_angle_beta                 90.5100(10)
_cell_angle_gamma                94.5590(10)
_cell_volume                     1992.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3624
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      28.27

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9832
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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            11611
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         25.01
_reflns_number_total             7003
_reflns_number_gt                5466
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 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)+(0.0364P)²+0.8978P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7003
_refine_ls_number_parameters     519
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0982
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.98088(12) 0.66436(12) 0.04730(7) 0.0211(3) Uani 1 1 d . . .
O2 O 0.94146(13) 0.61753(12) 0.24161(7) 0.0259(3) Uani 1 1 d . . .
O3 O 0.89115(14) 1.02670(12) 0.17942(8) 0.0293(3) Uani 1 1 d . . .
O4 O 0.69527(12) 0.62092(12) 0.00034(6) 0.0211(3) Uani 1 1 d . . .
O5 O 0.31445(13) 0.82642(14) 0.05662(8) 0.0323(4) Uani 1 1 d D . .
O6 O 0.46226(15) 0.84123(15) 0.14837(8) 0.0415(4) Uani 1 1 d . . .
O7 O 0.32155(12) 0.47998(11) 0.47247(7) 0.0206(3) Uani 1 1 d . . .
O8 O 0.27914(14) 0.38187(14) 0.27541(8) 0.0350(4) Uani 1 1 d . . .
O9 O -0.10586(12) 0.40155(12) 0.41800(7) 0.0214(3) Uani 1 1 d . . .
O10 O 0.28398(13) 0.22055(11) 0.53976(7) 0.0211(3) Uani 1 1 d . . .
O11 O 0.21471(14) -0.18748(12) 0.43318(8) 0.0297(4) Uani 1 1 d . . .
O12 O 0.10004(14) -0.05527(12) 0.37550(7) 0.0281(3) Uani 1 1 d . . .
N1 N 0.89744(14) 0.46766(14) 0.07098(8) 0.0186(3) Uani 1 1 d . . .
H1 H 0.9504 0.4238 0.0432 0.022 Uiso 1 1 calc R . .
N2 N 0.49216(14) 0.35922(14) 0.43853(8) 0.0186(3) Uani 1 1 d . . .
H2 H 0.5563 0.4016 0.4650 0.022 Uiso 1 1 calc R . .
C1 C 0.79616(17) 0.41498(17) 0.11270(10) 0.0178(4) Uani 1 1 d . . .
C2 C 0.73357(17) 0.50963(17) 0.15192(9) 0.0168(4) Uani 1 1 d . . .
C3 C 0.62836(17) 0.47884(18) 0.19566(10) 0.0198(4) Uani 1 1 d . . .
H3 H 0.5837 0.5425 0.2220 0.024 Uiso 1 1 calc R . .
C4 C 0.58816(18) 0.35335(18) 0.20089(10) 0.0225(4) Uani 1 1 d . . .
H4 H 0.5157 0.3312 0.2309 0.027 Uiso 1 1 calc R . .
C5 C 0.65345(19) 0.26063(19) 0.16249(10) 0.0236(4) Uani 1 1 d . . .
H5 H 0.6258 0.1754 0.1671 0.028 Uiso 1 1 calc R . .
C6 C 0.75864(19) 0.28998(18) 0.11728(10) 0.0215(4) Uani 1 1 d . . .
H6 H 0.8029 0.2265 0.0906 0.026 Uiso 1 1 calc R . .
C7 C 0.90405(17) 0.59400(17) 0.07858(10) 0.0175(4) Uani 1 1 d . . .
C8 C 0.80344(17) 0.63380(17) 0.13725(10) 0.0170(4) Uani 1 1 d . . .
C9 C 0.89147(17) 0.68915(18) 0.20407(10) 0.0185(4) Uani 1 1 d . . .
C10 C 0.91531(18) 0.82315(18) 0.21796(10) 0.0211(4) Uani 1 1 d . . .
H10 H 0.9657 0.8568 0.2599 0.025 Uiso 1 1 calc R . .
C11 C 0.86832(18) 0.90122(18) 0.17340(10) 0.0215(4) Uani 1 1 d . . .
C12 C 0.78271(19) 0.85826(17) 0.10807(10) 0.0218(4) Uani 1 1 d . . .
H12A H 0.8386 0.8525 0.0643 0.026 Uiso 1 1 calc R . .
H12B H 0.7174 0.9203 0.1013 0.026 Uiso 1 1 calc R . .
C13 C 0.70894(18) 0.73069(17) 0.11619(10) 0.0188(4) Uani 1 1 d . . .
H13 H 0.6456 0.7426 0.1571 0.023 Uiso 1 1 calc R . .
C14 C 0.9757(2) 1.0836(2) 0.23819(12) 0.0341(5) Uani 1 1 d . . .
H14A H 0.9378 1.0624 0.2846 0.041 Uiso 1 1 calc R . .
H14B H 0.9830 1.1745 0.2367 0.041 Uiso 1 1 calc R . .
H14C H 1.0642 1.0526 0.2333 0.041 Uiso 1 1 calc R . .
C15 C 0.62639(18) 0.69107(17) 0.04815(10) 0.0182(4) Uani 1 1 d . A .
C16 C 0.63955(19) 0.58405(18) -0.07171(10) 0.0224(4) Uani 1 1 d . . .
H16A H 0.6266 0.6587 -0.0977 0.027 Uiso 1 1 calc R . .
H16B H 0.5525 0.5358 -0.0684 0.027 Uiso 1 1 calc R . .
C17 C 0.7367(2) 0.5050(2) -0.11114(11) 0.0310(5) Uani 1 1 d . . .
H17A H 0.8214 0.5548 -0.1154 0.037 Uiso 1 1 calc R . .
H17B H 0.7014 0.4756 -0.1598 0.037 Uiso 1 1 calc R . .
H17C H 0.7508 0.4330 -0.0840 0.037 Uiso 1 1 calc R . .
C18 C 0.50491(18) 0.72655(18) 0.03481(10) 0.0218(4) Uani 1 1 d . . .
H18 H 0.4648 0.7004 -0.0114 0.026 Uiso 1 1 calc R A .
C19 C 0.43039(19) 0.80264(19) 0.08658(11) 0.0261(5) Uani 1 1 d . A .
C20 C 0.2289(7) 0.9034(7) 0.1000(2) 0.0379(6) Uani 0.797(4) 1 d PD A 1
H20A H 0.2321 0.8826 0.1511 0.046 Uiso 0.797(4) 1 calc PR A 1
H20B H 0.1361 0.8861 0.0818 0.046 Uiso 0.797(4) 1 calc PR A 1
C21 C 0.2716(3) 1.0401(3) 0.09680(17) 0.0461(8) Uani 0.797(4) 1 d PD A 1
H21A H 0.3600 1.0590 0.1193 0.055 Uiso 0.797(4) 1 calc PR A 1
H21B H 0.2080 1.0909 0.1231 0.055 Uiso 0.797(4) 1 calc PR A 1
H21C H 0.2745 1.0594 0.0459 0.055 Uiso 0.797(4) 1 calc PR A 1
C20' C 0.233(3) 0.901(3) 0.1053(8) 0.0379(6) Uani 0.203(4) 1 d PD A 2
H20C H 0.2896 0.9642 0.1360 0.046 Uiso 0.203(4) 1 calc PR A 2
H20D H 0.1817 0.8464 0.1374 0.046 Uiso 0.203(4) 1 calc PR A 2
C21' C 0.1398(11) 0.9632(11) 0.0577(7) 0.0461(8) Uani 0.203(4) 1 d PD A 2
H21D H 0.1919 1.0155 0.0258 0.055 Uiso 0.203(4) 1 calc PR A 2
H21E H 0.0837 1.0154 0.0886 0.055 Uiso 0.203(4) 1 calc PR A 2
H21F H 0.0836 0.8992 0.0281 0.055 Uiso 0.203(4) 1 calc PR A 2
C22 C 0.38889(18) 0.20893(16) 0.35796(9) 0.0167(4) Uani 1 1 d . . .
C23 C 0.51030(18) 0.25317(16) 0.39059(10) 0.0167(4) Uani 1 1 d . . .
C24 C 0.62655(18) 0.19835(17) 0.37426(10) 0.0196(4) Uani 1 1 d . . .
H24 H 0.7085 0.2287 0.3976 0.024 Uiso 1 1 calc R . .
C25 C 0.61823(19) 0.09639(17) 0.32187(10) 0.0215(4) Uani 1 1 d . . .
H25 H 0.6968 0.0578 0.3083 0.026 Uiso 1 1 calc R . .
C26 C 0.49857(19) 0.05007(17) 0.28923(10) 0.0223(4) Uani 1 1 d . . .
H26 H 0.4956 -0.0204 0.2542 0.027 Uiso 1 1 calc R . .
C27 C 0.38250(19) 0.10605(17) 0.30736(10) 0.0194(4) Uani 1 1 d . . .
H27 H 0.3000 0.0740 0.2852 0.023 Uiso 1 1 calc R . .
C28 C 0.36408(17) 0.38829(16) 0.43908(10) 0.0168(4) Uani 1 1 d . . .
C29 C 0.28264(17) 0.28834(16) 0.38765(9) 0.0156(4) Uani 1 1 d . . .
C30 C 0.21610(18) 0.35638(17) 0.32879(10) 0.0186(4) Uani 1 1 d . . .
C31 C 0.08187(17) 0.39138(16) 0.34026(10) 0.0175(4) Uani 1 1 d . . .
H31 H 0.0399 0.4333 0.3043 0.021 Uiso 1 1 calc R . .
C32 C 0.01516(17) 0.36583(16) 0.40065(10) 0.0169(4) Uani 1 1 d . . .
C33 C -0.16999(19) 0.47454(19) 0.36855(11) 0.0258(5) Uani 1 1 d . . .
H33A H -0.1138 0.5512 0.3626 0.031 Uiso 1 1 calc R . .
H33B H -0.2559 0.4962 0.3881 0.031 Uiso 1 1 calc R . .
H33C H -0.1839 0.4259 0.3212 0.031 Uiso 1 1 calc R . .
C34 C 0.06741(17) 0.29376(17) 0.45806(10) 0.0179(4) Uani 1 1 d . . .
H34A H -0.0063 0.2410 0.4775 0.022 Uiso 1 1 calc R . .
H34B H 0.1060 0.3523 0.4986 0.022 Uiso 1 1 calc R . .
C35 C 0.17329(17) 0.21142(16) 0.42756(9) 0.0160(4) Uani 1 1 d . . .
H35 H 0.1284 0.1486 0.3902 0.019 Uiso 1 1 calc R . .
C36 C 0.23115(17) 0.13957(17) 0.48452(9) 0.0175(4) Uani 1 1 d . . .
C37 C 0.3435(2) 0.16913(18) 0.60062(10) 0.0272(5) Uani 1 1 d . . .
H37A H 0.4238 0.1276 0.5851 0.033 Uiso 1 1 calc R . .
H37B H 0.2799 0.1066 0.6205 0.033 Uiso 1 1 calc R . .
C38 C 0.3794(2) 0.27534(19) 0.65714(11) 0.0288(5) Uani 1 1 d . . .
H38A H 0.4394 0.3381 0.6362 0.035 Uiso 1 1 calc R . .
H38B H 0.4237 0.2441 0.6985 0.035 Uiso 1 1 calc R . .
H38C H 0.2986 0.3133 0.6737 0.035 Uiso 1 1 calc R . .
C39 C 0.23326(19) 0.01558(17) 0.48236(10) 0.0217(4) Uani 1 1 d . . .
H39 H 0.2761 -0.0170 0.5217 0.026 Uiso 1 1 calc R . .
C40 C 0.17510(19) -0.07409(17) 0.42437(10) 0.0210(4) Uani 1 1 d . . .
C41 C 0.1651(2) -0.28866(18) 0.37965(11) 0.0301(5) Uani 1 1 d . . .
H41A H 0.0709 -0.2787 0.3677 0.036 Uiso 1 1 calc R . .
H41B H 0.1692 -0.3696 0.4007 0.036 Uiso 1 1 calc R . .
C42 C 0.2446(2) -0.2896(2) 0.31153(14) 0.0461(7) Uani 1 1 d . . .
H42A H 0.2368 -0.2113 0.2892 0.069 Uiso 1 1 calc R . .
H42B H 0.2109 -0.3603 0.2774 0.069 Uiso 1 1 calc R . .
H42C H 0.3381 -0.2979 0.3234 0.069 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
O1 C7 1.226(2) . ?
O2 C9 1.218(2) . ?
O3 C11 1.348(2) . ?
O3 C14 1.436(2) . ?
O4 C15 1.344(2) . ?
O4 C16 1.448(2) . ?
O5 C19 1.343(2) . ?
O5 C20 1.443(4) . ?
O5 C20' 1.452(10) . ?
O6 C19 1.210(2) . ?
O7 C28 1.226(2) . ?
O8 C30 1.218(2) . ?
O9 C32 1.343(2) . ?
O9 C33 1.439(2) . ?
O10 C36 1.357(2) . ?
O10 C37 1.443(2) . ?
O11 C40 1.339(2) . ?
O11 C41 1.458(2) . ?
O12 C40 1.214(2) . ?
N1 C7 1.352(2) . ?
N1 C1 1.400(2) . ?
N1 H1 0.8800 . ?
N2 C28 1.354(2) . ?
N2 C23 1.406(2) . ?
N2 H2 0.8800 . ?
C1 C6 1.380(3) . ?
C1 C2 1.393(3) . ?
C2 C3 1.377(3) . ?
C2 C8 1.510(3) . ?
C3 C4 1.393(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.547(3) . ?
C8 C13 1.541(2) . ?
C8 C9 1.559(2) . ?
C9 C10 1.444(3) . ?
C10 C11 1.338(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.494(2) . ?
C12 C13 1.531(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C15 1.510(2) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C18 1.341(3) . ?
C16 C17 1.500(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.456(3) . ?
C18 H18 0.9500 . ?
C20 C21 1.508(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C20' C21' 1.518(10) . ?
C20' H20C 0.9900 . ?
C20' H20D 0.9900 . ?
C21' H21D 0.9800 . ?
C21' H21E 0.9800 . ?
C21' H21F 0.9800 . ?
C22 C27 1.381(2) . ?
C22 C23 1.391(2) . ?
C22 C29 1.502(2) . ?
C23 C24 1.379(3) . ?
C24 C25 1.393(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.381(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.390(3) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.548(2) . ?
C29 C30 1.542(2) . ?
C29 C35 1.558(2) . ?
C30 C31 1.448(3) . ?
C31 C32 1.346(3) . ?
C31 H31 0.9500 . ?
C32 C34 1.486(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.522(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.501(2) . ?
C35 H35 1.0000 . ?
C36 C39 1.335(3) . ?
C37 C38 1.497(3) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.461(3) . ?
C39 H39 0.9500 . ?
C41 C42 1.497(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 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
C11 O3 C14 117.77(15) . . ?
C15 O4 C16 119.26(13) . . ?
C19 O5 C20 117.8(3) . . ?
C19 O5 C20' 113.8(9) . . ?
C20 O5 C20' 4.5(7) . . ?
C32 O9 C33 117.73(15) . . ?
C36 O10 C37 117.87(14) . . ?
C40 O11 C41 116.42(14) . . ?
C7 N1 C1 111.89(15) . . ?
C7 N1 H1 124.1 . . ?
C1 N1 H1 124.1 . . ?
C28 N2 C23 111.89(14) . . ?
C28 N2 H2 124.1 . . ?
C23 N2 H2 124.1 . . ?
C6 C1 C2 122.29(18) . . ?
C6 C1 N1 128.07(17) . . ?
C2 C1 N1 109.64(16) . . ?
C3 C2 C1 119.51(18) . . ?
C3 C2 C8 132.06(17) . . ?
C1 C2 C8 108.42(16) . . ?
C2 C3 C4 119.27(18) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 120.28(18) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.24(18) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 117.39(18) . . ?
C1 C6 H6 121.3 . . ?
C5 C6 H6 121.3 . . ?
O1 C7 N1 126.06(17) . . ?
O1 C7 C8 126.09(16) . . ?
N1 C7 C8 107.75(15) . . ?
C2 C8 C13 113.95(15) . . ?
C2 C8 C7 101.88(14) . . ?
C13 C8 C7 115.63(15) . . ?
C2 C8 C9 110.48(15) . . ?
C13 C8 C9 109.82(14) . . ?
C7 C8 C9 104.47(13) . . ?
O2 C9 C10 122.07(16) . . ?
O2 C9 C8 118.67(16) . . ?
C10 C9 C8 119.22(16) . . ?
C11 C10 C9 121.82(16) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C10 C11 O3 126.25(16) . . ?
C10 C11 C12 123.31(17) . . ?
O3 C11 C12 110.43(16) . . ?
C11 C12 C13 111.21(16) . . ?
C11 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C15 C13 C12 108.82(15) . . ?
C15 C13 C8 114.46(15) . . ?
C12 C13 C8 112.14(15) . . ?
C15 C13 H13 107.0 . . ?
C12 C13 H13 107.0 . . ?
C8 C13 H13 107.0 . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C15 O4 124.24(16) . . ?
C18 C15 C13 125.29(16) . . ?
O4 C15 C13 110.34(14) . . ?
O4 C16 C17 106.75(14) . . ?
O4 C16 H16A 110.4 . . ?
C17 C16 H16A 110.4 . . ?
O4 C16 H16B 110.4 . . ?
C17 C16 H16B 110.4 . . ?
H16A C16 H16B 108.6 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 C19 124.23(16) . . ?
C15 C18 H18 117.9 . . ?
C19 C18 H18 117.9 . . ?
O6 C19 O5 121.99(18) . . ?
O6 C19 C18 127.69(18) . . ?
O5 C19 C18 110.33(16) . . ?
O5 C20 C21 110.7(5) . . ?
O5 C20 H20A 109.5 . . ?
C21 C20 H20A 109.5 . . ?
O5 C20 H20B 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
O5 C20' C21' 106.8(9) . . ?
O5 C20' H20C 110.4 . . ?
C21' C20' H20C 110.4 . . ?
O5 C20' H20D 110.4 . . ?
C21' C20' H20D 110.4 . . ?
H20C C20' H20D 108.6 . . ?
C20' C21' H21D 109.5 . . ?
C20' C21' H21E 109.5 . . ?
H21D C21' H21E 109.5 . . ?
C20' C21' H21F 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
C27 C22 C23 119.60(17) . . ?
C27 C22 C29 131.10(16) . . ?
C23 C22 C29 109.30(15) . . ?
C24 C23 C22 122.51(16) . . ?
C24 C23 N2 128.37(16) . . ?
C22 C23 N2 109.10(15) . . ?
C23 C24 C25 116.89(16) . . ?
C23 C24 H24 121.6 . . ?
C25 C24 H24 121.6 . . ?
C26 C25 C24 121.62(18) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C25 C26 C27 120.34(17) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C22 C27 C26 119.02(17) . . ?
C22 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
O7 C28 N2 125.84(16) . . ?
O7 C28 C29 126.27(15) . . ?
N2 C28 C29 107.85(14) . . ?
C22 C29 C30 112.93(15) . . ?
C22 C29 C28 101.76(13) . . ?
C30 C29 C28 107.74(14) . . ?
C22 C29 C35 112.08(14) . . ?
C30 C29 C35 109.00(14) . . ?
C28 C29 C35 113.17(14) . . ?
O8 C30 C31 122.29(17) . . ?
O8 C30 C29 119.12(16) . . ?
C31 C30 C29 118.56(16) . . ?
C32 C31 C30 121.49(17) . . ?
C32 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
O9 C32 C31 125.56(16) . . ?
O9 C32 C34 110.55(15) . . ?
C31 C32 C34 123.89(16) . . ?
O9 C33 H33A 109.5 . . ?
O9 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O9 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 C35 110.65(15) . . ?
C32 C34 H34A 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
C36 C35 C34 112.23(15) . . ?
C36 C35 C29 112.05(14) . . ?
C34 C35 C29 111.31(14) . . ?
C36 C35 H35 107.0 . . ?
C34 C35 H35 107.0 . . ?
C29 C35 H35 107.0 . . ?
C39 C36 O10 124.04(16) . . ?
C39 C36 C35 126.52(16) . . ?
O10 C36 C35 109.44(14) . . ?
O10 C37 C38 107.33(15) . . ?
O10 C37 H37A 110.2 . . ?
C38 C37 H37A 110.2 . . ?
O10 C37 H37B 110.2 . . ?
C38 C37 H37B 110.2 . . ?
H37A C37 H37B 108.5 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 C40 125.32(17) . . ?
C36 C39 H39 117.3 . . ?
C40 C39 H39 117.3 . . ?
O12 C40 O11 122.60(17) . . ?
O12 C40 C39 128.08(17) . . ?
O11 C40 C39 109.29(15) . . ?
O11 C41 C42 111.40(17) . . ?
O11 C41 H41A 109.3 . . ?
C42 C41 H41A 109.3 . . ?
O11 C41 H41B 109.3 . . ?
C42 C41 H41B 109.3 . . ?
H41A C41 H41B 108.0 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 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 C6 178.50(17) . . . . ?
C7 N1 C1 C2 -1.7(2) . . . . ?
C6 C1 C2 C3 -1.6(3) . . . . ?
N1 C1 C2 C3 178.58(15) . . . . ?
C6 C1 C2 C8 177.11(16) . . . . ?
N1 C1 C2 C8 -2.70(19) . . . . ?
C1 C2 C3 C4 1.2(2) . . . . ?
C8 C2 C3 C4 -177.16(17) . . . . ?
C2 C3 C4 C5 0.0(3) . . . . ?
C3 C4 C5 C6 -1.0(3) . . . . ?
C2 C1 C6 C5 0.7(3) . . . . ?
N1 C1 C6 C5 -179.53(17) . . . . ?
C4 C5 C6 C1 0.6(3) . . . . ?
C1 N1 C7 O1 -178.22(16) . . . . ?
C1 N1 C7 C8 5.22(19) . . . . ?
C3 C2 C8 C13 -50.9(3) . . . . ?
C1 C2 C8 C13 130.62(16) . . . . ?
C3 C2 C8 C7 -176.14(17) . . . . ?
C1 C2 C8 C7 5.37(17) . . . . ?
C3 C2 C8 C9 73.3(2) . . . . ?
C1 C2 C8 C9 -105.19(16) . . . . ?
O1 C7 C8 C2 177.09(16) . . . . ?
N1 C7 C8 C2 -6.35(17) . . . . ?
O1 C7 C8 C13 53.0(2) . . . . ?
N1 C7 C8 C13 -130.48(16) . . . . ?
O1 C7 C8 C9 -67.9(2) . . . . ?
N1 C7 C8 C9 108.71(16) . . . . ?
C2 C8 C9 O2 31.5(2) . . . . ?
C13 C8 C9 O2 157.99(17) . . . . ?
C7 C8 C9 O2 -77.4(2) . . . . ?
C2 C8 C9 C10 -150.83(16) . . . . ?
C13 C8 C9 C10 -24.3(2) . . . . ?
C7 C8 C9 C10 100.30(18) . . . . ?
O2 C9 C10 C11 174.88(18) . . . . ?
C8 C9 C10 C11 -2.7(3) . . . . ?
C9 C10 C11 O3 -176.11(18) . . . . ?
C9 C10 C11 C12 3.0(3) . . . . ?
C14 O3 C11 C10 1.2(3) . . . . ?
C14 O3 C11 C12 -177.98(17) . . . . ?
C10 C11 C12 C13 24.3(3) . . . . ?
O3 C11 C12 C13 -156.43(16) . . . . ?
C11 C12 C13 C15 -178.91(15) . . . . ?
C11 C12 C13 C8 -51.3(2) . . . . ?
C2 C8 C13 C15 -60.2(2) . . . . ?
C7 C8 C13 C15 57.4(2) . . . . ?
C9 C8 C13 C15 175.26(15) . . . . ?
C2 C8 C13 C12 175.22(15) . . . . ?
C7 C8 C13 C12 -67.20(19) . . . . ?
C9 C8 C13 C12 50.7(2) . . . . ?
C16 O4 C15 C18 2.6(3) . . . . ?
C16 O4 C15 C13 -173.57(16) . . . . ?
C12 C13 C15 C18 -83.5(2) . . . . ?
C8 C13 C15 C18 150.16(19) . . . . ?
C12 C13 C15 O4 92.62(18) . . . . ?
C8 C13 C15 O4 -33.7(2) . . . . ?
C15 O4 C16 C17 -178.66(16) . . . . ?
O4 C15 C18 C19 -179.93(18) . . . . ?
C13 C15 C18 C19 -4.3(3) . . . . ?
C20 O5 C19 O6 1.7(5) . . . . ?
C20' O5 C19 O6 -0.5(16) . . . . ?
C20 O5 C19 C18 -178.6(4) . . . . ?
C20' O5 C19 C18 179.1(16) . . . . ?
C15 C18 C19 O6 -2.7(4) . . . . ?
C15 C18 C19 O5 177.74(19) . . . . ?
C19 O5 C20 C21 82.3(4) . . . . ?
C20' O5 C20 C21 110(26) . . . . ?
C19 O5 C20' C21' 157.0(16) . . . . ?
C20 O5 C20' C21' 3(23) . . . . ?
C27 C22 C23 C24 0.2(3) . . . . ?
C29 C22 C23 C24 179.76(17) . . . . ?
C27 C22 C23 N2 178.77(16) . . . . ?
C29 C22 C23 N2 -1.7(2) . . . . ?
C28 N2 C23 C24 178.06(19) . . . . ?
C28 N2 C23 C22 -0.4(2) . . . . ?
C22 C23 C24 C25 1.2(3) . . . . ?
N2 C23 C24 C25 -177.08(18) . . . . ?
C23 C24 C25 C26 -1.8(3) . . . . ?
C24 C25 C26 C27 1.0(3) . . . . ?
C23 C22 C27 C26 -1.1(3) . . . . ?
C29 C22 C27 C26 179.54(18) . . . . ?
C25 C26 C27 C22 0.5(3) . . . . ?
C23 N2 C28 O7 -175.49(17) . . . . ?
C23 N2 C28 C29 2.2(2) . . . . ?
C27 C22 C29 C30 -62.5(3) . . . . ?
C23 C22 C29 C30 118.01(16) . . . . ?
C27 C22 C29 C28 -177.75(19) . . . . ?
C23 C22 C29 C28 2.80(18) . . . . ?
C27 C22 C29 C35 61.0(2) . . . . ?
C23 C22 C29 C35 -118.42(16) . . . . ?
O7 C28 C29 C22 174.68(18) . . . . ?
N2 C28 C29 C22 -2.99(18) . . . . ?
O7 C28 C29 C30 55.7(2) . . . . ?
N2 C28 C29 C30 -121.96(16) . . . . ?
O7 C28 C29 C35 -64.9(2) . . . . ?
N2 C28 C29 C35 117.46(16) . . . . ?
C22 C29 C30 O8 -27.6(2) . . . . ?
C28 C29 C30 O8 83.9(2) . . . . ?
C35 C29 C30 O8 -152.88(17) . . . . ?
C22 C29 C30 C31 154.39(15) . . . . ?
C28 C29 C30 C31 -94.04(18) . . . . ?
C35 C29 C30 C31 29.1(2) . . . . ?
O8 C30 C31 C32 -177.92(18) . . . . ?
C29 C30 C31 C32 0.0(3) . . . . ?
C33 O9 C32 C31 -0.7(3) . . . . ?
C33 O9 C32 C34 178.91(14) . . . . ?
C30 C31 C32 O9 175.53(16) . . . . ?
C30 C31 C32 C34 -4.0(3) . . . . ?
O9 C32 C34 C35 157.72(14) . . . . ?
C31 C32 C34 C35 -22.7(2) . . . . ?
C32 C34 C35 C36 178.48(14) . . . . ?
C32 C34 C35 C29 51.98(18) . . . . ?
C22 C29 C35 C36 52.70(19) . . . . ?
C30 C29 C35 C36 178.45(14) . . . . ?
C28 C29 C35 C36 -61.69(19) . . . . ?
C22 C29 C35 C34 179.30(14) . . . . ?
C30 C29 C35 C34 -54.95(18) . . . . ?
C28 C29 C35 C34 64.91(18) . . . . ?
C37 O10 C36 C39 -1.4(3) . . . . ?
C37 O10 C36 C35 179.28(16) . . . . ?
C34 C35 C36 C39 122.7(2) . . . . ?
C29 C35 C36 C39 -111.2(2) . . . . ?
C34 C35 C36 O10 -58.00(19) . . . . ?
C29 C35 C36 O10 68.11(18) . . . . ?
C36 O10 C37 C38 -173.57(16) . . . . ?
O10 C36 C39 C40 178.78(18) . . . . ?
C35 C36 C39 C40 -2.0(3) . . . . ?
C41 O11 C40 O12 1.3(3) . . . . ?
C41 O11 C40 C39 179.85(17) . . . . ?
C36 C39 C40 O12 -12.0(3) . . . . ?
C36 C39 C40 O11 169.51(19) . . . . ?
C40 O11 C41 C42 81.3(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.044
