# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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data_1c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C51 H38 F2 N4 O4'
_chemical_formula_sum            'C51 H38 F2 N4 O4'
_chemical_formula_weight         808.85

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   12.3870(16)
_cell_length_b                   14.2715(19)
_cell_length_c                   14.5968(19)
_cell_angle_alpha                72.050(4)
_cell_angle_beta                 69.143(4)
_cell_angle_gamma                71.181(4)
_cell_volume                     2227.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7925
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      22.21

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             844
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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_reflns_number            45240
_diffrn_reflns_av_R_equivalents  0.1016
_diffrn_reflns_av_sigmaI/netI    0.1099
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         27.56
_reflns_number_total             10283
_reflns_number_gt                5245
_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)+(0.0647P)²+0.1049P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10197
_refine_ls_number_parameters     556
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1449
_refine_ls_R_factor_gt           0.0677
_refine_ls_wR_factor_ref         0.1831
_refine_ls_wR_factor_gt          0.1595
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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
C1 C 0.5872(2) 0.7810(2) -0.1609(2) 0.0767(7) Uani 1 1 d . . .
H1 H 0.5767 0.7335 -0.1867 0.092 Uiso 1 1 calc R . .
C2 C 0.6015(3) 0.8727(3) -0.2214(2) 0.0938(9) Uani 1 1 d . . .
H2 H 0.6001 0.8876 -0.2877 0.113 Uiso 1 1 calc R . .
C3 C 0.6176(3) 0.9423(3) -0.1853(3) 0.1070(11) Uani 1 1 d . . .
H3 H 0.6294 1.0044 -0.2272 0.128 Uiso 1 1 calc R . .
C4 C 0.6165(5) 0.9212(3) -0.0873(3) 0.1368(15) Uani 1 1 d . . .
H4 H 0.6253 0.9693 -0.0614 0.164 Uiso 1 1 calc R . .
C5 C 0.6021(4) 0.8282(3) -0.0272(3) 0.1271(14) Uani 1 1 d . . .
H5 H 0.6021 0.8137 0.0394 0.153 Uiso 1 1 calc R . .
C6 C 0.5879(2) 0.75714(19) -0.0630(2) 0.0676(7) Uani 1 1 d . . .
C7 C 0.5648(2) 0.6588(2) 0.0053(2) 0.0785(8) Uani 1 1 d . . .
H7A H 0.4893 0.6728 0.0561 0.094 Uiso 1 1 calc R . .
H7B H 0.5575 0.6179 -0.0334 0.094 Uiso 1 1 calc R . .
C8 C 0.6440(2) 0.59843(17) 0.15262(18) 0.0561(6) Uani 1 1 d . . .
C9 C 0.74646(18) 0.51583(16) 0.18522(16) 0.0506(5) Uani 1 1 d . . .
H9 H 0.7960 0.5492 0.1978 0.061 Uiso 1 1 calc R . .
C10 C 0.8164(2) 0.47574(17) 0.09096(17) 0.0545(6) Uani 1 1 d . . .
C11 C 0.9242(2) 0.40666(18) 0.06682(18) 0.0622(6) Uani 1 1 d . . .
H11 H 0.9651 0.3704 0.1143 0.075 Uiso 1 1 calc R . .
C12 C 0.9682(2) 0.3938(2) -0.0296(2) 0.0727(7) Uani 1 1 d . . .
C13 C 0.9121(3) 0.4460(2) -0.1026(2) 0.0853(9) Uani 1 1 d . . .
H13 H 0.9460 0.4344 -0.1673 0.102 Uiso 1 1 calc R . .
C14 C 0.8060(3) 0.5153(2) -0.0799(2) 0.0782(8) Uani 1 1 d . . .
H14 H 0.7664 0.5516 -0.1283 0.094 Uiso 1 1 calc R . .
C15 C 0.7595(2) 0.52972(18) 0.01733(18) 0.0599(6) Uani 1 1 d . . .
C16 C 0.88548(19) 0.45691(16) 0.36769(16) 0.0530(6) Uani 1 1 d . . .
H16 H 0.8170 0.5092 0.3753 0.064 Uiso 1 1 calc R . .
C17 C 0.9875(2) 0.46582(19) 0.37969(17) 0.0596(6) Uani 1 1 d . . .
H17 H 0.9860 0.5247 0.3953 0.072 Uiso 1 1 calc R . .
C18 C 1.0898(2) 0.3915(2) 0.36939(18) 0.0624(6) Uani 1 1 d . . .
C19 C 1.2014(2) 0.4032(3) 0.3826(2) 0.0981(10) Uani 1 1 d . . .
H19A H 1.2116 0.3628 0.4464 0.147 Uiso 1 1 calc R . .
H19B H 1.1932 0.4732 0.3799 0.147 Uiso 1 1 calc R . .
H19C H 1.2695 0.3810 0.3298 0.147 Uiso 1 1 calc R . .
C20 C 1.0896(2) 0.3043(2) 0.3472(2) 0.0704(7) Uani 1 1 d . . .
H20 H 1.1580 0.2519 0.3410 0.084 Uiso 1 1 calc R . .
C21 C 0.98933(19) 0.29348(18) 0.33396(18) 0.0616(6) Uani 1 1 d . . .
H21 H 0.9917 0.2345 0.3180 0.074 Uiso 1 1 calc R . .
C22 C 0.88583(17) 0.36953(15) 0.34419(15) 0.0461(5) Uani 1 1 d . . .
C23 C 0.77616(17) 0.35712(14) 0.33267(15) 0.0433(5) Uani 1 1 d . . .
C24 C 0.69231(17) 0.44915(15) 0.28473(15) 0.0436(5) Uani 1 1 d . . .
H24 H 0.6452 0.4917 0.3336 0.052 Uiso 1 1 calc R . .
C25 C 0.61637(17) 0.38237(15) 0.28333(15) 0.0452(5) Uani 1 1 d . . .
C26 C 0.71305(19) 0.30015(17) 0.23476(16) 0.0517(5) Uani 1 1 d . . .
C27 C 0.5234(2) 0.42881(17) 0.23226(17) 0.0528(5) Uani 1 1 d . . .
C28 C 0.57128(17) 0.33846(15) 0.39799(15) 0.0457(5) Uani 1 1 d . . .
H28 H 0.5142 0.3937 0.4291 0.055 Uiso 1 1 calc R . .
C29 C 0.50820(18) 0.25393(16) 0.42201(17) 0.0497(5) Uani 1 1 d . . .
C30 C 0.45567(18) 0.20657(16) 0.52747(17) 0.0509(5) Uani 1 1 d . . .
C31 C 0.4405(2) 0.2436(2) 0.60886(19) 0.0653(7) Uani 1 1 d . . .
H31 H 0.4629 0.3030 0.5990 0.078 Uiso 1 1 calc R . .
C32 C 0.3921(2) 0.1933(2) 0.7052(2) 0.0808(8) Uani 1 1 d . . .
H32 H 0.3822 0.2199 0.7591 0.097 Uiso 1 1 calc R . .
C33 C 0.3582(2) 0.1052(2) 0.7236(2) 0.0737(7) Uani 1 1 d . . .
C34 C 0.3051(3) 0.0506(3) 0.8295(2) 0.1080(11) Uani 1 1 d . . .
H34A H 0.2391 0.0282 0.8312 0.162 Uiso 1 1 calc R . .
H34B H 0.2782 0.0960 0.8741 0.162 Uiso 1 1 calc R . .
H34C H 0.3643 -0.0069 0.8503 0.162 Uiso 1 1 calc R . .
C35 C 0.3716(3) 0.0694(2) 0.6424(2) 0.0823(8) Uani 1 1 d . . .
H35 H 0.3480 0.0105 0.6526 0.099 Uiso 1 1 calc R . .
C36 C 0.4189(2) 0.11841(19) 0.5463(2) 0.0711(7) Uani 1 1 d . . .
H36 H 0.4267 0.0923 0.4927 0.085 Uiso 1 1 calc R . .
C37 C 0.66959(17) 0.36161(17) 0.51687(16) 0.0459(5) Uani 1 1 d . . .
C38 C 0.68705(16) 0.31083(14) 0.43187(15) 0.0434(5) Uani 1 1 d . . .
C39 C 0.73847(17) 0.20094(15) 0.47430(16) 0.0450(5) Uani 1 1 d . . .
C40 C 0.7690(2) 0.11519(16) 0.43787(18) 0.0585(6) Uani 1 1 d . . .
H40 H 0.7577 0.1178 0.3774 0.070 Uiso 1 1 calc R . .
C41 C 0.8172(2) 0.02523(17) 0.4945(2) 0.0715(7) Uani 1 1 d . . .
C42 C 0.8369(2) 0.0185(2) 0.5829(2) 0.0812(8) Uani 1 1 d . . .
H42 H 0.8711 -0.0440 0.6180 0.097 Uiso 1 1 calc R . .
C43 C 0.8062(2) 0.10440(19) 0.6202(2) 0.0703(7) Uani 1 1 d . . .
H43 H 0.8187 0.1015 0.6802 0.084 Uiso 1 1 calc R . .
C44 C 0.75597(19) 0.19481(16) 0.56447(17) 0.0524(5) Uani 1 1 d . . .
C45 C 0.7098(2) 0.3116(2) 0.68177(18) 0.0712(7) Uani 1 1 d . . .
H45A H 0.6566 0.2744 0.7363 0.085 Uiso 1 1 calc R . .
H45B H 0.6753 0.3833 0.6802 0.085 Uiso 1 1 calc R . .
C46 C 0.8274(2) 0.28305(18) 0.7037(2) 0.0658(7) Uani 1 1 d . . .
C47 C 0.8285(3) 0.2602(2) 0.8025(2) 0.1007(10) Uani 1 1 d . . .
H47 H 0.7575 0.2615 0.8539 0.121 Uiso 1 1 calc R . .
C48 C 0.9358(6) 0.2353(3) 0.8250(4) 0.1348(16) Uani 1 1 d . . .
H48 H 0.9364 0.2197 0.8916 0.162 Uiso 1 1 calc R . .
C49 C 1.0384(5) 0.2338(3) 0.7509(5) 0.1262(16) Uani 1 1 d . . .
H49 H 1.1094 0.2188 0.7666 0.151 Uiso 1 1 calc R . .
C50 C 1.0398(3) 0.2541(2) 0.6522(3) 0.1032(11) Uani 1 1 d . . .
H50 H 1.1113 0.2503 0.6013 0.124 Uiso 1 1 calc R . .
C51 C 0.9336(3) 0.2799(2) 0.6300(2) 0.0772(7) Uani 1 1 d . . .
H51 H 0.9338 0.2958 0.5632 0.093 Uiso 1 1 calc R . .
F1 F 1.07520(15) 0.32662(13) -0.05471(12) 0.0980(5) Uani 1 1 d . . .
F2 F 0.84833(17) -0.06068(11) 0.46017(15) 0.1089(6) Uani 1 1 d . . .
N1 N 0.65677(18) 0.60009(14) 0.05541(15) 0.0634(5) Uani 1 1 d . . .
N2 N 0.7196(2) 0.24698(18) 0.17878(17) 0.0741(6) Uani 1 1 d . . .
N3 N 0.45286(19) 0.46440(17) 0.19037(16) 0.0737(6) Uani 1 1 d . . .
N4 N 0.71669(15) 0.29161(14) 0.58754(13) 0.0523(5) Uani 1 1 d . . .
O1 O 0.56340(16) 0.65013(12) 0.20532(13) 0.0698(5) Uani 1 1 d . . .
O2 O 0.80939(12) 0.28717(10) 0.26763(10) 0.0497(4) Uani 1 1 d . . .
O3 O 0.50018(15) 0.22855(13) 0.35315(12) 0.0710(5) Uani 1 1 d . . .
O4 O 0.62380(13) 0.45075(11) 0.51795(11) 0.0583(4) Uani 1 1 d . . .
H2A H 0.653(3) 0.273(2) 0.160(2) 0.111(12) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.361(4) . ?
C1 C6 1.365(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.352(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.364(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.357(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.497(4) . ?
C7 N1 1.461(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O1 1.208(3) . ?
C8 N1 1.364(3) . ?
C8 C9 1.532(3) . ?
C9 C10 1.512(3) . ?
C9 C24 1.527(3) . ?
C9 H9 0.9800 . ?
C10 C11 1.382(3) . ?
C10 C15 1.387(3) . ?
C11 C12 1.364(3) . ?
C11 H11 0.9300 . ?
C12 F1 1.364(3) . ?
C12 C13 1.370(4) . ?
C13 C14 1.367(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.382(3) . ?
C14 H14 0.9300 . ?
C15 N1 1.397(3) . ?
C16 C17 1.385(3) . ?
C16 C22 1.390(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.360(3) . ?
C17 H17 0.9300 . ?
C18 C20 1.380(3) . ?
C18 C19 1.528(3) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.384(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.382(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.497(3) . ?
C23 O2 1.452(2) . ?
C23 C24 1.538(3) . ?
C23 C38 1.579(3) . ?
C24 C25 1.548(3) . ?
C24 H24 0.9800 . ?
C25 C27 1.462(3) . ?
C25 C26 1.522(3) . ?
C25 C28 1.555(3) . ?
C26 N2 1.243(3) . ?
C26 O2 1.378(2) . ?
C27 N3 1.139(3) . ?
C28 C29 1.530(3) . ?
C28 C38 1.574(3) . ?
C28 H28 0.9800 . ?
C29 O3 1.213(2) . ?
C29 C30 1.476(3) . ?
C30 C31 1.375(3) . ?
C30 C36 1.390(3) . ?
C31 C32 1.381(3) . ?
C31 H31 0.9300 . ?
C32 C33 1.371(4) . ?
C32 H32 0.9300 . ?
C33 C35 1.368(4) . ?
C33 C34 1.514(4) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.369(4) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 O4 1.217(2) . ?
C37 N4 1.349(3) . ?
C37 C38 1.541(3) . ?
C38 C39 1.512(3) . ?
C39 C40 1.372(3) . ?
C39 C44 1.381(3) . ?
C40 C41 1.375(3) . ?
C40 H40 0.9300 . ?
C41 F2 1.356(3) . ?
C41 C42 1.367(4) . ?
C42 C43 1.381(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.382(3) . ?
C43 H43 0.9300 . ?
C44 N4 1.412(3) . ?
C45 N4 1.457(3) . ?
C45 C46 1.504(3) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C51 1.368(4) . ?
C46 C47 1.381(4) . ?
C47 C48 1.391(5) . ?
C47 H47 0.9300 . ?
C48 C49 1.343(6) . ?
C48 H48 0.9300 . ?
C49 C50 1.375(6) . ?
C49 H49 0.9300 . ?
C50 C51 1.374(4) . ?
C50 H50 0.9300 . ?
C51 H51 0.9300 . ?
N2 H2A 0.90(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 121.3(3) . . ?
C2 C1 H1 119.4 . . ?
C6 C1 H1 119.4 . . ?
C3 C2 C1 120.2(3) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 C4 119.7(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 121.4(3) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C1 118.0(3) . . ?
C5 C6 C7 120.5(3) . . ?
C1 C6 C7 121.3(2) . . ?
N1 C7 C6 114.2(2) . . ?
N1 C7 H7A 108.7 . . ?
C6 C7 H7A 108.7 . . ?
N1 C7 H7B 108.7 . . ?
C6 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
O1 C8 N1 126.1(2) . . ?
O1 C8 C9 125.8(2) . . ?
N1 C8 C9 108.1(2) . . ?
C10 C9 C24 122.87(18) . . ?
C10 C9 C8 102.38(18) . . ?
C24 C9 C8 107.47(17) . . ?
C10 C9 H9 107.8 . . ?
C24 C9 H9 107.8 . . ?
C8 C9 H9 107.8 . . ?
C11 C10 C15 119.6(2) . . ?
C11 C10 C9 132.1(2) . . ?
C15 C10 C9 108.0(2) . . ?
C12 C11 C10 117.2(3) . . ?
C12 C11 H11 121.4 . . ?
C10 C11 H11 121.4 . . ?
C11 C12 F1 117.8(3) . . ?
C11 C12 C13 123.6(3) . . ?
F1 C12 C13 118.6(3) . . ?
C14 C13 C12 119.7(3) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 117.8(3) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
C14 C15 C10 122.1(2) . . ?
C14 C15 N1 127.5(2) . . ?
C10 C15 N1 110.4(2) . . ?
C17 C16 C22 119.8(2) . . ?
C17 C16 H16 120.1 . . ?
C22 C16 H16 120.1 . . ?
C18 C17 C16 122.4(2) . . ?
C18 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
C17 C18 C20 117.8(2) . . ?
C17 C18 C19 121.4(2) . . ?
C20 C18 C19 120.8(2) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 C21 121.2(2) . . ?
C18 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C22 C21 C20 120.6(2) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C16 118.22(19) . . ?
C21 C22 C23 120.89(18) . . ?
C16 C22 C23 120.88(18) . . ?
O2 C23 C22 109.61(15) . . ?
O2 C23 C24 102.57(15) . . ?
C22 C23 C24 119.99(16) . . ?
O2 C23 C38 104.36(14) . . ?
C22 C23 C38 116.27(16) . . ?
C24 C23 C38 102.18(15) . . ?
C9 C24 C23 118.26(16) . . ?
C9 C24 C25 117.76(16) . . ?
C23 C24 C25 92.39(14) . . ?
C9 C24 H24 109.1 . . ?
C23 C24 H24 109.1 . . ?
C25 C24 H24 109.1 . . ?
C27 C25 C26 112.16(17) . . ?
C27 C25 C24 118.88(16) . . ?
C26 C25 C24 100.72(15) . . ?
C27 C25 C28 114.93(17) . . ?
C26 C25 C28 108.85(16) . . ?
C24 C25 C28 99.71(15) . . ?
N2 C26 O2 119.8(2) . . ?
N2 C26 C25 134.9(2) . . ?
O2 C26 C25 105.30(16) . . ?
N3 C27 C25 178.3(2) . . ?
C29 C28 C25 112.98(17) . . ?
C29 C28 C38 117.58(16) . . ?
C25 C28 C38 102.08(15) . . ?
C29 C28 H28 107.9 . . ?
C25 C28 H28 107.9 . . ?
C38 C28 H28 107.9 . . ?
O3 C29 C30 121.09(19) . . ?
O3 C29 C28 118.80(19) . . ?
C30 C29 C28 120.09(19) . . ?
C31 C30 C36 117.5(2) . . ?
C31 C30 C29 124.5(2) . . ?
C36 C30 C29 118.1(2) . . ?
C30 C31 C32 120.5(2) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C33 C32 C31 121.9(3) . . ?
C33 C32 H32 119.0 . . ?
C31 C32 H32 119.0 . . ?
C35 C33 C32 117.5(2) . . ?
C35 C33 C34 121.0(3) . . ?
C32 C33 C34 121.5(3) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 C36 121.5(2) . . ?
C33 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
C35 C36 C30 121.2(2) . . ?
C35 C36 H36 119.4 . . ?
C30 C36 H36 119.4 . . ?
O4 C37 N4 126.16(19) . . ?
O4 C37 C38 125.21(19) . . ?
N4 C37 C38 108.59(17) . . ?
C39 C38 C37 101.76(16) . . ?
C39 C38 C28 118.79(16) . . ?
C37 C38 C28 112.70(15) . . ?
C39 C38 C23 112.44(16) . . ?
C37 C38 C23 109.60(15) . . ?
C28 C38 C23 101.68(15) . . ?
C40 C39 C44 120.18(19) . . ?
C40 C39 C38 131.48(19) . . ?
C44 C39 C38 108.32(17) . . ?
C39 C40 C41 117.2(2) . . ?
C39 C40 H40 121.4 . . ?
C41 C40 H40 121.4 . . ?
F2 C41 C42 118.4(2) . . ?
F2 C41 C40 118.4(2) . . ?
C42 C41 C40 123.2(2) . . ?
C41 C42 C43 120.0(2) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C42 C43 C44 117.2(2) . . ?
C42 C43 H43 121.4 . . ?
C44 C43 H43 121.4 . . ?
C39 C44 C43 122.3(2) . . ?
C39 C44 N4 110.30(18) . . ?
C43 C44 N4 127.4(2) . . ?
N4 C45 C46 114.4(2) . . ?
N4 C45 H45A 108.7 . . ?
C46 C45 H45A 108.7 . . ?
N4 C45 H45B 108.7 . . ?
C46 C45 H45B 108.7 . . ?
H45A C45 H45B 107.6 . . ?
C51 C46 C47 118.5(3) . . ?
C51 C46 C45 122.9(2) . . ?
C47 C46 C45 118.6(3) . . ?
C46 C47 C48 119.9(4) . . ?
C46 C47 H47 120.0 . . ?
C48 C47 H47 120.0 . . ?
C49 C48 C47 120.2(4) . . ?
C49 C48 H48 119.9 . . ?
C47 C48 H48 119.9 . . ?
C48 C49 C50 120.9(4) . . ?
C48 C49 H49 119.6 . . ?
C50 C49 H49 119.6 . . ?
C51 C50 C49 118.8(4) . . ?
C51 C50 H50 120.6 . . ?
C49 C50 H50 120.6 . . ?
C46 C51 C50 121.7(3) . . ?
C46 C51 H51 119.2 . . ?
C50 C51 H51 119.2 . . ?
C8 N1 C15 111.10(19) . . ?
C8 N1 C7 122.6(2) . . ?
C15 N1 C7 125.8(2) . . ?
C26 N2 H2A 106(2) . . ?
C37 N4 C44 110.68(17) . . ?
C37 N4 C45 123.59(19) . . ?
C44 N4 C45 125.06(19) . . ?
C26 O2 C23 107.90(15) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.042


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 262 66 ' '
2 0.333 0.639 0.007 8 0 ' '
3 0.667 0.361 -0.007 8 0 ' '
_platon_squeeze_details          
; 
;
_database_code_depnum_ccdc_archive 'CCDC 1009895'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1e

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C49 H32 Cl4 N4 O4'
_chemical_formula_sum            'C49 H32 Cl4 N4 O4'
_chemical_formula_weight         882.59

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   12.598(3)
_cell_length_b                   14.608(3)
_cell_length_c                   14.773(3)
_cell_angle_alpha                107.152(6)
_cell_angle_beta                 102.115(6)
_cell_angle_gamma                110.323(6)
_cell_volume                     2283.3(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5462
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      19.63

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             908
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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_reflns_number            48278
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_sigmaI/netI    0.1173
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         27.48
_reflns_number_total             10477
_reflns_number_gt                4319
_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)+(0.0750P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10409
_refine_ls_number_parameters     554
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1748
_refine_ls_R_factor_gt           0.0574
_refine_ls_wR_factor_ref         0.1536
_refine_ls_wR_factor_gt          0.1275
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_restrained_S_all      0.904
_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
C1 C 0.9452(3) 0.0144(3) 0.2131(3) 0.0785(10) Uani 1 1 d . . .
H1 H 0.9387 0.0656 0.1898 0.094 Uiso 1 1 calc R . .
C2 C 1.0559(4) 0.0150(3) 0.2453(3) 0.0974(12) Uani 1 1 d . . .
H2 H 1.1244 0.0673 0.2456 0.117 Uiso 1 1 calc R . .
C3 C 1.0647(5) -0.0609(5) 0.2766(4) 0.1220(17) Uani 1 1 d . . .
H3 H 1.1394 -0.0610 0.2983 0.146 Uiso 1 1 calc R . .
C4 C 0.9644(6) -0.1378(4) 0.2768(4) 0.1234(16) Uani 1 1 d . . .
H4 H 0.9712 -0.1898 0.2984 0.148 Uiso 1 1 calc R . .
C5 C 0.8552(4) -0.1378(3) 0.2455(3) 0.0968(12) Uani 1 1 d . . .
H5 H 0.7872 -0.1908 0.2449 0.116 Uiso 1 1 calc R . .
C6 C 0.8439(3) -0.0605(2) 0.2147(2) 0.0627(8) Uani 1 1 d . . .
C7 C 0.7225(3) -0.0623(2) 0.1823(3) 0.0691(9) Uani 1 1 d . . .
H7A H 0.6832 -0.1042 0.1100 0.083 Uiso 1 1 calc R . .
H7B H 0.6737 -0.0974 0.2157 0.083 Uiso 1 1 calc R . .
C8 C 0.6814(2) 0.0745(2) 0.1335(2) 0.0446(7) Uani 1 1 d . . .
C9 C 0.7084(2) 0.19181(19) 0.18654(18) 0.0407(6) Uani 1 1 d . . .
C10 C 0.7703(2) 0.2165(2) 0.29539(19) 0.0430(6) Uani 1 1 d . . .
C11 C 0.8170(2) 0.3076(2) 0.3821(2) 0.0535(7) Uani 1 1 d . . .
H11 H 0.8135 0.3693 0.3792 0.064 Uiso 1 1 calc R . .
C12 C 0.8690(3) 0.3062(3) 0.4730(2) 0.0622(8) Uani 1 1 d . . .
C13 C 0.8718(3) 0.2153(3) 0.4795(2) 0.0735(10) Uani 1 1 d . . .
H13 H 0.9051 0.2157 0.5421 0.088 Uiso 1 1 calc R . .
C14 C 0.8253(3) 0.1228(3) 0.3928(3) 0.0681(9) Uani 1 1 d . . .
H14 H 0.8271 0.0607 0.3961 0.082 Uiso 1 1 calc R . .
C15 C 0.7768(2) 0.1259(2) 0.3025(2) 0.0485(7) Uani 1 1 d . . .
C16 C 0.5920(2) 0.20981(19) 0.15922(18) 0.0416(6) Uani 1 1 d . . .
H16 H 0.5287 0.1444 0.1033 0.050 Uiso 1 1 calc R . .
C17 C 0.5422(2) 0.2363(2) 0.2433(2) 0.0505(7) Uani 1 1 d . . .
C18 C 0.4887(2) 0.1544(2) 0.2821(2) 0.0461(7) Uani 1 1 d . . .
C19 C 0.4607(3) 0.0487(2) 0.2360(2) 0.0632(8) Uani 1 1 d . . .
H19 H 0.4730 0.0242 0.1752 0.076 Uiso 1 1 calc R . .
C20 C 0.4150(3) -0.0218(2) 0.2778(3) 0.0739(9) Uani 1 1 d . . .
H20 H 0.3955 -0.0935 0.2449 0.089 Uiso 1 1 calc R . .
C21 C 0.3982(3) 0.0132(3) 0.3666(3) 0.0639(9) Uani 1 1 d . . .
C22 C 0.4219(4) 0.1173(3) 0.4140(3) 0.0900(11) Uani 1 1 d . . .
H22 H 0.4084 0.1409 0.4743 0.108 Uiso 1 1 calc R . .
C23 C 0.4666(3) 0.1871(3) 0.3698(2) 0.0799(10) Uani 1 1 d . . .
H23 H 0.4819 0.2581 0.4009 0.096 Uiso 1 1 calc R . .
C24 C 0.7366(2) 0.3971(2) 0.19677(19) 0.0463(7) Uani 1 1 d . . .
C25 C 0.6307(2) 0.2976(2) 0.11705(18) 0.0446(7) Uani 1 1 d . . .
C26 C 0.5304(3) 0.3169(2) 0.0695(2) 0.0503(7) Uani 1 1 d . . .
C27 C 0.5576(3) 0.4988(2) -0.2768(2) 0.0694(9) Uani 1 1 d . . .
H27 H 0.5284 0.5412 -0.2395 0.083 Uiso 1 1 calc R . .
C28 C 0.5801(4) 0.5123(3) -0.3605(3) 0.0866(11) Uani 1 1 d . . .
H28 H 0.5642 0.5624 -0.3803 0.104 Uiso 1 1 calc R . .
C29 C 0.6258(3) 0.4523(3) -0.4145(3) 0.0872(11) Uani 1 1 d . . .
H29 H 0.6433 0.4626 -0.4698 0.105 Uiso 1 1 calc R . .
C30 C 0.6453(3) 0.3773(4) -0.3865(3) 0.0952(12) Uani 1 1 d . . .
H30 H 0.6755 0.3356 -0.4234 0.114 Uiso 1 1 calc R . .
C31 C 0.6213(3) 0.3627(3) -0.3052(3) 0.0830(11) Uani 1 1 d . . .
H31 H 0.6344 0.3106 -0.2874 0.100 Uiso 1 1 calc R . .
C32 C 0.5775(2) 0.4242(2) -0.2483(2) 0.0537(7) Uani 1 1 d . . .
C33 C 0.5500(3) 0.4070(2) -0.1586(2) 0.0616(8) Uani 1 1 d . . .
H33A H 0.5420 0.4681 -0.1180 0.074 Uiso 1 1 calc R . .
H33B H 0.4732 0.3450 -0.1826 0.074 Uiso 1 1 calc R . .
C34 C 0.6308(3) 0.2959(3) -0.0971(2) 0.0502(7) Uani 1 1 d . . .
C35 C 0.7411(2) 0.31179(19) -0.01574(18) 0.0446(7) Uani 1 1 d . . .
H35 H 0.7844 0.2772 -0.0496 0.053 Uiso 1 1 calc R . .
C36 C 0.8164(2) 0.4306(2) 0.02597(18) 0.0448(7) Uani 1 1 d . . .
C37 C 0.9303(2) 0.4963(2) 0.09529(19) 0.0493(7) Uani 1 1 d . . .
H37 H 0.9754 0.4695 0.1284 0.059 Uiso 1 1 calc R . .
C38 C 0.9762(2) 0.6037(2) 0.1145(2) 0.0569(8) Uani 1 1 d . . .
C39 C 0.9134(3) 0.6447(2) 0.0654(2) 0.0693(9) Uani 1 1 d . . .
H39 H 0.9478 0.7172 0.0798 0.083 Uiso 1 1 calc R . .
C40 C 0.7989(3) 0.5793(2) -0.0056(2) 0.0660(9) Uani 1 1 d . . .
H40 H 0.7548 0.6066 -0.0389 0.079 Uiso 1 1 calc R . .
C41 C 0.7530(2) 0.4733(2) -0.0251(2) 0.0503(7) Uani 1 1 d . . .
C42 C 0.6960(2) 0.2543(2) 0.05026(18) 0.0414(6) Uani 1 1 d . . .
H42 H 0.6436 0.1789 0.0070 0.050 Uiso 1 1 calc R . .
C43 C 0.7896(2) 0.26204(19) 0.14114(18) 0.0420(6) Uani 1 1 d . . .
C44 C 0.8954(2) 0.2424(2) 0.12770(19) 0.0423(6) Uani 1 1 d . . .
C45 C 0.8827(3) 0.1629(2) 0.0411(2) 0.0492(7) Uani 1 1 d . . .
H45 H 0.8075 0.1224 -0.0101 0.059 Uiso 1 1 calc R . .
C46 C 0.9783(3) 0.1424(2) 0.0290(2) 0.0586(8) Uani 1 1 d . . .
H46 H 0.9681 0.0886 -0.0295 0.070 Uiso 1 1 calc R . .
C47 C 1.0884(3) 0.2020(3) 0.1039(3) 0.0620(8) Uani 1 1 d . . .
C48 C 1.1044(3) 0.2808(3) 0.1895(3) 0.0693(9) Uani 1 1 d . . .
H48 H 1.1805 0.3213 0.2395 0.083 Uiso 1 1 calc R . .
C49 C 1.0080(2) 0.3015(2) 0.2030(2) 0.0559(8) Uani 1 1 d . . .
H49 H 1.0190 0.3548 0.2623 0.067 Uiso 1 1 calc R . .
Cl1 Cl 0.93721(9) 0.42218(8) 0.58261(6) 0.0924(3) Uani 1 1 d . . .
Cl2 Cl 0.34323(8) -0.07446(7) 0.42205(7) 0.0946(3) Uani 1 1 d . . .
Cl3 Cl 1.11978(7) 0.68890(6) 0.20521(6) 0.0756(3) Uani 1 1 d . . .
Cl4 Cl 1.21014(8) 0.17718(9) 0.08928(9) 0.1090(4) Uani 1 1 d . . .
N1 N 0.72708(19) 0.04379(17) 0.20503(18) 0.0521(6) Uani 1 1 d . . .
N2 N 0.7431(3) 0.4866(3) 0.2406(2) 0.0689(8) Uani 1 1 d . . .
N3 N 0.4530(3) 0.3321(2) 0.0329(2) 0.0729(8) Uani 1 1 d . . .
N4 N 0.6420(2) 0.39148(18) -0.09511(16) 0.0514(6) Uani 1 1 d . . .
O1 O 0.62948(16) 0.01943(14) 0.04387(14) 0.0562(5) Uani 1 1 d . . .
O2 O 0.5471(2) 0.32476(17) 0.27878(16) 0.0752(6) Uani 1 1 d . . .
O3 O 0.83202(15) 0.37160(12) 0.21214(12) 0.0446(4) Uani 1 1 d . . .
O4 O 0.54480(18) 0.20968(16) -0.15190(14) 0.0644(6) Uani 1 1 d . . .
H2A H 0.805(3) 0.532(3) 0.280(3) 0.087(14) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.372(5) . ?
C1 C6 1.374(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.350(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.369(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.356(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.376(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.492(4) . ?
C7 N1 1.464(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O1 1.213(3) . ?
C8 N1 1.362(3) . ?
C8 C9 1.535(4) . ?
C9 C10 1.503(3) . ?
C9 C16 1.569(3) . ?
C9 C43 1.586(3) . ?
C10 C11 1.375(3) . ?
C10 C15 1.387(3) . ?
C11 C12 1.375(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.372(4) . ?
C12 Cl1 1.737(3) . ?
C13 C14 1.386(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.367(4) . ?
C14 H14 0.9300 . ?
C15 N1 1.409(3) . ?
C16 C17 1.516(4) . ?
C16 C25 1.561(3) . ?
C16 H16 0.9800 . ?
C17 O2 1.217(3) . ?
C17 C18 1.490(4) . ?
C18 C23 1.365(4) . ?
C18 C19 1.368(4) . ?
C19 C20 1.372(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.351(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.364(4) . ?
C21 Cl2 1.741(3) . ?
C22 C23 1.390(4) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 N2 1.241(4) . ?
C24 O3 1.372(3) . ?
C24 C25 1.505(4) . ?
C25 C26 1.469(4) . ?
C25 C42 1.546(3) . ?
C26 N3 1.136(3) . ?
C27 C32 1.358(4) . ?
C27 C28 1.379(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.365(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.357(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.356(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.382(4) . ?
C31 H31 0.9300 . ?
C32 C33 1.505(4) . ?
C33 N4 1.458(3) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 O4 1.224(3) . ?
C34 N4 1.345(3) . ?
C34 C35 1.530(4) . ?
C35 C36 1.507(3) . ?
C35 C42 1.537(3) . ?
C35 H35 0.9800 . ?
C36 C37 1.370(3) . ?
C36 C41 1.402(3) . ?
C37 C38 1.384(4) . ?
C37 H37 0.9300 . ?
C38 C39 1.361(4) . ?
C38 Cl3 1.747(3) . ?
C39 C40 1.382(4) . ?
C39 H39 0.9300 . ?
C40 C41 1.365(4) . ?
C40 H40 0.9300 . ?
C41 N4 1.399(3) . ?
C42 C43 1.535(3) . ?
C42 H42 0.9800 . ?
C43 O3 1.459(3) . ?
C43 C44 1.497(4) . ?
C44 C49 1.384(3) . ?
C44 C45 1.386(3) . ?
C45 C46 1.371(4) . ?
C45 H45 0.9300 . ?
C46 C47 1.362(4) . ?
C46 H46 0.9300 . ?
C47 C48 1.355(4) . ?
C47 Cl4 1.736(3) . ?
C48 C49 1.388(4) . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
N2 H2A 0.78(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 121.0(3) . . ?
C2 C1 H1 119.5 . . ?
C6 C1 H1 119.5 . . ?
C3 C2 C1 119.4(4) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 120.6(4) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 119.9(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.8(4) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 118.3(3) . . ?
C1 C6 C7 122.5(3) . . ?
C5 C6 C7 119.2(3) . . ?
N1 C7 C6 113.5(2) . . ?
N1 C7 H7A 108.9 . . ?
C6 C7 H7A 108.9 . . ?
N1 C7 H7B 108.9 . . ?
C6 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
O1 C8 N1 126.2(2) . . ?
O1 C8 C9 126.2(2) . . ?
N1 C8 C9 107.7(2) . . ?
C10 C9 C8 102.5(2) . . ?
C10 C9 C16 118.0(2) . . ?
C8 C9 C16 111.68(19) . . ?
C10 C9 C43 113.9(2) . . ?
C8 C9 C43 109.9(2) . . ?
C16 C9 C43 101.03(18) . . ?
C11 C10 C15 118.9(2) . . ?
C11 C10 C9 132.2(2) . . ?
C15 C10 C9 108.9(2) . . ?
C12 C11 C10 119.0(3) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C13 C12 C11 121.5(3) . . ?
C13 C12 Cl1 118.4(2) . . ?
C11 C12 Cl1 120.1(3) . . ?
C12 C13 C14 120.2(3) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 117.8(3) . . ?
C15 C14 H14 121.1 . . ?
C13 C14 H14 121.1 . . ?
C14 C15 C10 122.5(3) . . ?
C14 C15 N1 128.3(3) . . ?
C10 C15 N1 109.2(2) . . ?
C17 C16 C25 114.4(2) . . ?
C17 C16 C9 116.3(2) . . ?
C25 C16 C9 102.62(19) . . ?
C17 C16 H16 107.7 . . ?
C25 C16 H16 107.7 . . ?
C9 C16 H16 107.7 . . ?
O2 C17 C18 120.7(3) . . ?
O2 C17 C16 119.4(2) . . ?
C18 C17 C16 119.9(2) . . ?
C23 C18 C19 117.8(3) . . ?
C23 C18 C17 117.8(3) . . ?
C19 C18 C17 124.4(3) . . ?
C18 C19 C20 121.3(3) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.4 . . ?
C21 C20 C19 119.9(3) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 120.9(3) . . ?
C20 C21 Cl2 120.6(3) . . ?
C22 C21 Cl2 118.5(3) . . ?
C21 C22 C23 118.3(3) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 H22 120.8 . . ?
C18 C23 C22 121.8(3) . . ?
C18 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
N2 C24 O3 124.4(3) . . ?
N2 C24 C25 129.7(3) . . ?
O3 C24 C25 106.0(2) . . ?
C26 C25 C24 113.6(2) . . ?
C26 C25 C42 118.2(2) . . ?
C24 C25 C42 99.6(2) . . ?
C26 C25 C16 113.8(2) . . ?
C24 C25 C16 110.3(2) . . ?
C42 C25 C16 99.73(19) . . ?
N3 C26 C25 179.8(4) . . ?
C32 C27 C28 120.7(3) . . ?
C32 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C29 C28 C27 120.2(3) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C30 C29 C28 119.3(3) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
C31 C30 C29 120.6(4) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C32 121.0(3) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 H31 119.5 . . ?
C27 C32 C31 118.2(3) . . ?
C27 C32 C33 121.0(3) . . ?
C31 C32 C33 120.7(3) . . ?
N4 C33 C32 113.6(2) . . ?
N4 C33 H33A 108.9 . . ?
C32 C33 H33A 108.9 . . ?
N4 C33 H33B 108.9 . . ?
C32 C33 H33B 108.9 . . ?
H33A C33 H33B 107.7 . . ?
O4 C34 N4 126.2(3) . . ?
O4 C34 C35 124.7(3) . . ?
N4 C34 C35 109.0(2) . . ?
C36 C35 C34 101.8(2) . . ?
C36 C35 C42 122.5(2) . . ?
C34 C35 C42 108.0(2) . . ?
C36 C35 H35 107.9 . . ?
C34 C35 H35 107.9 . . ?
C42 C35 H35 107.9 . . ?
C37 C36 C41 119.3(2) . . ?
C37 C36 C35 132.2(2) . . ?
C41 C36 C35 108.3(2) . . ?
C36 C37 C38 117.9(2) . . ?
C36 C37 H37 121.0 . . ?
C38 C37 H37 121.0 . . ?
C39 C38 C37 122.3(3) . . ?
C39 C38 Cl3 119.3(2) . . ?
C37 C38 Cl3 118.4(2) . . ?
C38 C39 C40 120.5(3) . . ?
C38 C39 H39 119.7 . . ?
C40 C39 H39 119.7 . . ?
C41 C40 C39 117.6(3) . . ?
C41 C40 H40 121.2 . . ?
C39 C40 H40 121.2 . . ?
C40 C41 N4 128.2(3) . . ?
C40 C41 C36 122.3(3) . . ?
N4 C41 C36 109.5(2) . . ?
C43 C42 C35 118.6(2) . . ?
C43 C42 C25 92.34(18) . . ?
C35 C42 C25 118.4(2) . . ?
C43 C42 H42 108.8 . . ?
C35 C42 H42 108.8 . . ?
C25 C42 H42 108.8 . . ?
O3 C43 C44 109.6(2) . . ?
O3 C43 C42 101.98(18) . . ?
C44 C43 C42 119.5(2) . . ?
O3 C43 C9 104.40(19) . . ?
C44 C43 C9 116.6(2) . . ?
C42 C43 C9 102.92(19) . . ?
C49 C44 C45 118.2(2) . . ?
C49 C44 C43 120.7(2) . . ?
C45 C44 C43 121.1(2) . . ?
C46 C45 C44 121.6(3) . . ?
C46 C45 H45 119.2 . . ?
C44 C45 H45 119.2 . . ?
C47 C46 C45 119.1(3) . . ?
C47 C46 H46 120.4 . . ?
C45 C46 H46 120.4 . . ?
C48 C47 C46 121.0(3) . . ?
C48 C47 Cl4 119.5(3) . . ?
C46 C47 Cl4 119.5(3) . . ?
C47 C48 C49 120.4(3) . . ?
C47 C48 H48 119.8 . . ?
C49 C48 H48 119.8 . . ?
C44 C49 C48 119.7(3) . . ?
C44 C49 H49 120.2 . . ?
C48 C49 H49 120.2 . . ?
C8 N1 C15 111.6(2) . . ?
C8 N1 C7 123.5(2) . . ?
C15 N1 C7 124.9(2) . . ?
C24 N2 H2A 119(3) . . ?
C34 N4 C41 111.3(2) . . ?
C34 N4 C33 124.0(2) . . ?
C41 N4 C33 124.7(2) . . ?
C24 O3 C43 107.36(19) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.047

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 319 71 ' '
_platon_squeeze_details          
; 
;
_database_code_depnum_ccdc_archive 'CCDC 1009896'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1g

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H42 Cl2 N4 O6'
_chemical_formula_sum            'C45 H42 Cl2 N4 O6'
_chemical_formula_weight         805.73

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   14.488(3)
_cell_length_b                   17.229(3)
_cell_length_c                   17.887(4)
_cell_angle_alpha                88.517(5)
_cell_angle_beta                 70.954(5)
_cell_angle_gamma                81.751(5)
_cell_volume                     4175.7(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7861
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      21.01

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1688
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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            78482
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_sigmaI/netI    0.0994
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         25.68
_reflns_number_total             15846
_reflns_number_gt                6717
_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)+(0.1227P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15827
_refine_ls_number_parameters     1117
_refine_ls_number_restraints     1557
_refine_ls_R_factor_all          0.1797
_refine_ls_R_factor_gt           0.0693
_refine_ls_wR_factor_ref         0.2235
_refine_ls_wR_factor_gt          0.1853
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_restrained_S_all      0.916
_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
C1 C 0.2901(4) 0.8077(4) 1.0066(3) 0.152(2) Uani 1 1 d . . .
H1A H 0.2777 0.8387 1.0536 0.227 Uiso 1 1 calc R . .
H1B H 0.3027 0.7532 1.0178 0.227 Uiso 1 1 calc R . .
H1C H 0.2335 0.8167 0.9891 0.227 Uiso 1 1 calc R . .
C2 C 0.3780(4) 0.8304(3) 0.9430(3) 0.1149(17) Uani 1 1 d . . .
H2A H 0.4293 0.8355 0.9657 0.138 Uiso 1 1 calc R . .
H2B H 0.3596 0.8813 0.9234 0.138 Uiso 1 1 calc R . .
C3 C 0.4195(3) 0.7720(3) 0.8739(2) 0.0934(13) Uani 1 1 d . . .
H3A H 0.3678 0.7644 0.8525 0.112 Uiso 1 1 calc R . .
H3B H 0.4426 0.7218 0.8923 0.112 Uiso 1 1 calc R . .
C4 C 0.5047(3) 0.8010(2) 0.8091(2) 0.0841(12) Uani 1 1 d . . .
H4A H 0.4793 0.8470 0.7855 0.101 Uiso 1 1 calc R . .
H4B H 0.5512 0.8165 0.8326 0.101 Uiso 1 1 calc R . .
C5 C 0.5358(3) 0.7375(2) 0.6785(2) 0.0596(9) Uani 1 1 d . . .
C6 C 0.6014(2) 0.66546(18) 0.63075(17) 0.0534(8) Uani 1 1 d . . .
C7 C 0.6524(3) 0.6300(2) 0.68839(19) 0.0579(9) Uani 1 1 d . . .
C8 C 0.7145(3) 0.5610(2) 0.6839(2) 0.0758(11) Uani 1 1 d . . .
H8A H 0.7362 0.5285 0.6390 0.091 Uiso 1 1 calc R . .
C9 C 0.7439(3) 0.5419(3) 0.7500(3) 0.0930(13) Uani 1 1 d . . .
C10 C 0.7138(4) 0.5889(3) 0.8148(3) 0.0997(15) Uani 1 1 d . . .
H10A H 0.7351 0.5741 0.8575 0.120 Uiso 1 1 calc R . .
C11 C 0.6527(3) 0.6577(3) 0.8193(2) 0.0883(13) Uani 1 1 d . . .
H11A H 0.6321 0.6901 0.8641 0.106 Uiso 1 1 calc R . .
C12 C 0.6224(3) 0.6776(2) 0.7546(2) 0.0648(10) Uani 1 1 d . . .
C13 C 0.5425(2) 0.60872(19) 0.60236(17) 0.0546(9) Uani 1 1 d . . .
H13A H 0.5610 0.5554 0.6181 0.066 Uiso 1 1 calc R . .
C14 C 0.4305(3) 0.62827(19) 0.6343(2) 0.0605(9) Uani 1 1 d . . .
C15 C 0.3801(3) 0.61421(19) 0.7180(2) 0.0581(9) Uani 1 1 d . . .
C16 C 0.4259(3) 0.57302(19) 0.7669(2) 0.0620(9) Uani 1 1 d . . .
H16A H 0.4922 0.5522 0.7461 0.074 Uiso 1 1 calc R . .
C17 C 0.3764(3) 0.5621(2) 0.8449(2) 0.0690(10) Uani 1 1 d . . .
H17A H 0.4084 0.5335 0.8763 0.083 Uiso 1 1 calc R . .
C18 C 0.2786(3) 0.5940(2) 0.8766(2) 0.0814(12) Uani 1 1 d . . .
C19 C 0.1354(4) 0.6144(3) 0.9927(3) 0.173(3) Uani 1 1 d . . .
H19A H 0.1153 0.6017 1.0478 0.259 Uiso 1 1 calc R . .
H19B H 0.0940 0.5940 0.9680 0.259 Uiso 1 1 calc R . .
H19C H 0.1297 0.6704 0.9876 0.259 Uiso 1 1 calc R . .
C20 C 0.2308(3) 0.6351(2) 0.8298(3) 0.0852(12) Uani 1 1 d . . .
H20A H 0.1648 0.6566 0.8512 0.102 Uiso 1 1 calc R . .
C21 C 0.2816(3) 0.6442(2) 0.7508(2) 0.0750(11) Uani 1 1 d . . .
H21A H 0.2487 0.6712 0.7190 0.090 Uiso 1 1 calc R . .
C22 C 0.6901(3) 0.5688(3) 0.49485(19) 0.0648(10) Uani 1 1 d . . .
C23 C 0.5868(3) 0.61253(19) 0.51045(17) 0.0554(9) Uani 1 1 d . . .
C24 C 0.5350(3) 0.5826(2) 0.4626(2) 0.0653(10) Uani 1 1 d . . .
C25 C 0.6058(2) 0.69891(18) 0.49796(17) 0.0541(9) Uani 1 1 d . . .
H25A H 0.5447 0.7336 0.5252 0.065 Uiso 1 1 calc R . .
C26 C 0.6718(2) 0.69104(19) 0.54908(18) 0.0561(9) Uani 1 1 d . . .
C27 C 0.7309(3) 0.7567(2) 0.54867(18) 0.0614(9) Uani 1 1 d . . .
C28 C 0.8305(3) 0.7431(2) 0.5365(2) 0.0798(11) Uani 1 1 d . . .
H28A H 0.8629 0.6918 0.5296 0.096 Uiso 1 1 calc R . .
C29 C 0.8834(4) 0.8041(3) 0.5343(3) 0.1018(15) Uani 1 1 d . . .
H29A H 0.9509 0.7937 0.5258 0.122 Uiso 1 1 calc R . .
C30 C 0.8371(5) 0.8797(3) 0.5447(3) 0.0986(16) Uani 1 1 d . . .
C31 C 0.8562(5) 1.0126(4) 0.5597(3) 0.151(2) Uani 1 1 d . . .
H31A H 0.9053 1.0437 0.5617 0.226 Uiso 1 1 calc R . .
H31B H 0.8050 1.0155 0.6102 0.226 Uiso 1 1 calc R . .
H31C H 0.8284 1.0323 0.5198 0.226 Uiso 1 1 calc R . .
C32 C 0.7382(4) 0.8959(2) 0.5555(2) 0.0843(13) Uani 1 1 d . . .
H32A H 0.7068 0.9475 0.5616 0.101 Uiso 1 1 calc R . .
C33 C 0.6848(3) 0.8340(2) 0.5573(2) 0.0749(11) Uani 1 1 d . . .
H33A H 0.6177 0.8447 0.5643 0.090 Uiso 1 1 calc R . .
C34 C 0.5625(3) 0.7636(3) 0.3847(2) 0.0785(12) Uani 1 1 d . A .
C35 C 0.6480(2) 0.72616(19) 0.41237(18) 0.0572(9) Uani 1 1 d . . .
H35A H 0.6894 0.7664 0.4122 0.069 Uiso 1 1 calc R . .
C36 C 0.7038(3) 0.6687(2) 0.3452(2) 0.0679(10) Uani 1 1 d . . .
C37 C 0.7919(3) 0.6209(2) 0.3283(2) 0.0818(12) Uani 1 1 d . . .
H37A H 0.8290 0.6187 0.3622 0.098 Uiso 1 1 calc R . .
C38 C 0.8250(4) 0.5753(2) 0.2587(3) 0.0940(14) Uani 1 1 d . . .
C39 C 0.7720(5) 0.5777(3) 0.2076(3) 0.1075(17) Uani 1 1 d . . .
H39A H 0.7951 0.5465 0.1618 0.129 Uiso 1 1 calc R . .
C40 C 0.6843(4) 0.6270(3) 0.2249(3) 0.1002(15) Uani 1 1 d . . .
H40A H 0.6472 0.6290 0.1909 0.120 Uiso 1 1 calc R . .
C41 C 0.6514(4) 0.6728(3) 0.2915(2) 0.0761(12) Uani 1 1 d . A .
C42 C 0.5062(13) 0.7443(9) 0.2661(12) 0.110(4) Uani 0.562(10) 1 d PDU A 1
H42A H 0.5476 0.7438 0.2111 0.131 Uiso 0.562(10) 1 calc PR A 1
H42B H 0.4674 0.7959 0.2789 0.131 Uiso 0.562(10) 1 calc PR A 1
C43 C 0.4378(11) 0.6837(9) 0.2768(9) 0.126(4) Uani 0.562(10) 1 d PDU A 1
H43A H 0.4733 0.6317 0.2780 0.152 Uiso 0.562(10) 1 calc PR A 1
H43B H 0.4120 0.6850 0.2330 0.152 Uiso 0.562(10) 1 calc PR A 1
C44 C 0.3437(11) 0.7039(11) 0.3632(8) 0.125(4) Uani 0.562(10) 1 d PU A 1
H44A H 0.3029 0.6623 0.3732 0.150 Uiso 0.562(10) 1 calc PR A 1
H44B H 0.3708 0.7048 0.4061 0.150 Uiso 0.562(10) 1 calc PR A 1
C45 C 0.2859(10) 0.7742(10) 0.3629(9) 0.203(5) Uani 0.562(10) 1 d PU A 1
H45A H 0.2700 0.7780 0.3148 0.304 Uiso 0.562(10) 1 calc PR A 1
H45B H 0.3210 0.8164 0.3665 0.304 Uiso 0.562(10) 1 calc PR A 1
H45C H 0.2262 0.7773 0.4073 0.304 Uiso 0.562(10) 1 calc PR A 1
C46 C 1.1466(4) 0.7036(4) -0.4341(4) 0.156(2) Uani 1 1 d U . .
H46A H 1.1751 0.6688 -0.4794 0.234 Uiso 1 1 calc R . .
H46B H 1.1951 0.7078 -0.4090 0.234 Uiso 1 1 calc R . .
H46C H 1.1251 0.7545 -0.4506 0.234 Uiso 1 1 calc R . .
C47 C 1.0590(5) 0.6715(3) -0.3760(4) 0.149(2) Uani 1 1 d U . .
H47A H 1.0139 0.6609 -0.4031 0.178 Uiso 1 1 calc R . .
H47B H 1.0817 0.6226 -0.3553 0.178 Uiso 1 1 calc R . .
C48 C 1.0083(4) 0.7270(3) -0.3118(3) 0.1162(16) Uani 1 1 d U . .
H48A H 0.9898 0.7764 -0.3339 0.139 Uiso 1 1 calc R . .
H48B H 1.0542 0.7360 -0.2848 0.139 Uiso 1 1 calc R . .
C49 C 0.9137(3) 0.7029(2) -0.2489(2) 0.0835(11) Uani 1 1 d U . .
H49A H 0.8654 0.6964 -0.2743 0.100 Uiso 1 1 calc R . .
H49B H 0.9305 0.6532 -0.2265 0.100 Uiso 1 1 calc R . .
C50 C 0.9018(3) 0.7631(2) -0.1214(2) 0.0572(8) Uani 1 1 d U . .
C51 C 0.8484(2) 0.83652(18) -0.07224(17) 0.0518(8) Uani 1 1 d U . .
C52 C 0.7878(2) 0.8752(2) -0.12061(19) 0.0569(8) Uani 1 1 d U . .
C53 C 0.7228(3) 0.9439(2) -0.1086(2) 0.0669(9) Uani 1 1 d U . .
H53A H 0.7107 0.9760 -0.0645 0.080 Uiso 1 1 calc R . .
C54 C 0.6759(3) 0.9640(2) -0.1643(2) 0.0761(10) Uani 1 1 d U . .
C55 C 0.6939(3) 0.9186(3) -0.2293(3) 0.0840(11) Uani 1 1 d U . .
H55A H 0.6614 0.9338 -0.2656 0.101 Uiso 1 1 calc R . .
C56 C 0.7600(3) 0.8497(2) -0.2431(2) 0.0763(10) Uani 1 1 d U . .
H56A H 0.7735 0.8190 -0.2885 0.092 Uiso 1 1 calc R . .
C57 C 0.8052(3) 0.8281(2) -0.1869(2) 0.0595(9) Uani 1 1 d U . .
C58 C 0.9224(2) 0.88755(18) -0.05488(18) 0.0552(8) Uani 1 1 d U . .
H58A H 0.9086 0.9413 -0.0717 0.066 Uiso 1 1 calc R . .
C59 C 1.0317(3) 0.85845(19) -0.0928(2) 0.0588(8) Uani 1 1 d U . .
C60 C 1.0801(3) 0.87263(19) -0.1778(2) 0.0599(9) Uani 1 1 d U . .
C61 C 1.1786(3) 0.8440(2) -0.2110(2) 0.0724(10) Uani 1 1 d U . .
H61A H 1.2116 0.8162 -0.1798 0.087 Uiso 1 1 calc R . .
C62 C 1.2290(3) 0.8552(2) -0.2883(3) 0.0853(11) Uani 1 1 d U . .
H62A H 1.2959 0.8362 -0.3093 0.102 Uiso 1 1 calc R . .
C63 C 1.1803(3) 0.8949(2) -0.3350(2) 0.0776(11) Uani 1 1 d U . .
C64 C 1.3253(4) 0.8733(3) -0.4507(3) 0.1205(17) Uani 1 1 d U . .
H64A H 1.3493 0.8916 -0.5037 0.181 Uiso 1 1 calc R . .
H64B H 1.3281 0.8173 -0.4520 0.181 Uiso 1 1 calc R . .
H64C H 1.3657 0.8870 -0.4212 0.181 Uiso 1 1 calc R . .
C65 C 1.0819(3) 0.9247(2) -0.3032(2) 0.0760(10) Uani 1 1 d U . .
H65A H 1.0493 0.9523 -0.3349 0.091 Uiso 1 1 calc R . .
C66 C 1.0316(3) 0.91390(19) -0.2249(2) 0.0648(9) Uani 1 1 d U . .
H66A H 0.9651 0.9342 -0.2035 0.078 Uiso 1 1 calc R . .
C67 C 0.7903(3) 0.9373(2) 0.06239(19) 0.0598(9) Uani 1 1 d U . .
C68 C 0.8621(2) 0.80422(17) 0.05675(17) 0.0498(8) Uani 1 1 d U . .
H68A H 0.9175 0.7654 0.0270 0.060 Uiso 1 1 calc R . .
C69 C 0.8897(2) 0.88733(18) 0.03710(18) 0.0546(8) Uani 1 1 d U . .
C70 C 0.9588(3) 0.91494(19) 0.0714(2) 0.0646(9) Uani 1 1 d U . .
C71 C 0.7856(2) 0.81661(17) 0.01403(17) 0.0495(8) Uani 1 1 d U . .
C72 C 0.7178(2) 0.75625(18) 0.02125(17) 0.0475(8) Uani 1 1 d U . .
C73 C 0.7544(2) 0.67634(19) 0.01471(17) 0.0536(8) Uani 1 1 d U . .
H73A H 0.8214 0.6605 0.0057 0.064 Uiso 1 1 calc R . .
C74 C 0.6934(3) 0.62072(19) 0.02137(17) 0.0557(8) Uani 1 1 d U . .
H74A H 0.7194 0.5678 0.0168 0.067 Uiso 1 1 calc R . .
C75 C 0.5942(3) 0.6425(2) 0.03474(18) 0.0564(9) Uani 1 1 d U . .
C76 C 0.4377(3) 0.5999(3) 0.0555(3) 0.1060(15) Uani 1 1 d U . .
H76A H 0.4100 0.5520 0.0594 0.159 Uiso 1 1 calc R . .
H76B H 0.4253 0.6302 0.0131 0.159 Uiso 1 1 calc R . .
H76C H 0.4079 0.6295 0.1043 0.159 Uiso 1 1 calc R . .
C77 C 0.5565(3) 0.7207(2) 0.04117(19) 0.0612(9) Uani 1 1 d U . .
H77A H 0.4895 0.7361 0.0504 0.073 Uiso 1 1 calc R . .
C78 C 0.6184(3) 0.77699(19) 0.03387(18) 0.0570(8) Uani 1 1 d U . .
H78A H 0.5922 0.8298 0.0376 0.068 Uiso 1 1 calc R . .
C79 C 0.9155(3) 0.7446(2) 0.1670(2) 0.0650(9) Uani 1 1 d U B .
C80 C 0.8269(2) 0.78115(18) 0.14440(17) 0.0523(8) Uani 1 1 d U . .
H80A H 0.7849 0.7403 0.1487 0.063 Uiso 1 1 calc R . .
C81 C 0.7736(3) 0.83961(19) 0.21032(19) 0.0580(8) Uani 1 1 d U . .
C82 C 0.6848(3) 0.8884(2) 0.2287(2) 0.0728(10) Uani 1 1 d U . .
H82A H 0.6472 0.8911 0.1952 0.087 Uiso 1 1 calc R . .
C83 C 0.6525(3) 0.9331(2) 0.2977(2) 0.0813(11) Uani 1 1 d U . .
C84 C 0.7052(4) 0.9283(2) 0.3499(2) 0.0853(12) Uani 1 1 d U . .
H84A H 0.6815 0.9585 0.3963 0.102 Uiso 1 1 calc R . .
C85 C 0.7935(3) 0.8780(2) 0.3327(2) 0.0789(11) Uani 1 1 d U . .
H85A H 0.8296 0.8740 0.3674 0.095 Uiso 1 1 calc R . .
C86 C 0.8263(3) 0.8347(2) 0.2641(2) 0.0627(9) Uani 1 1 d U B .
C87 C 0.9824(7) 0.7466(7) 0.2753(6) 0.087(3) Uani 0.637(8) 1 d PDU B 1
H87A H 1.0006 0.6907 0.2641 0.104 Uiso 0.637(8) 1 calc PR B 1
H87B H 0.9524 0.7541 0.3321 0.104 Uiso 0.637(8) 1 calc PR B 1
C88 C 1.0730(7) 0.7853(4) 0.2483(6) 0.110(3) Uani 0.637(8) 1 d PDU B 1
H88A H 1.1222 0.7563 0.2684 0.132 Uiso 0.637(8) 1 calc PR B 1
H88B H 1.0990 0.7816 0.1910 0.132 Uiso 0.637(8) 1 calc PR B 1
C89 C 1.0596(6) 0.8690(4) 0.2729(5) 0.113(3) Uani 0.637(8) 1 d PDU B 1
H89A H 1.0387 0.8723 0.3302 0.135 Uiso 0.637(8) 1 calc PR B 1
H89B H 1.0068 0.8974 0.2565 0.135 Uiso 0.637(8) 1 calc PR B 1
C90 C 1.1501(7) 0.9091(6) 0.2399(7) 0.131(3) Uani 0.637(8) 1 d PDU B 1
H90A H 1.1312 0.9649 0.2449 0.197 Uiso 0.637(8) 1 calc PR B 1
H90B H 1.1818 0.8945 0.1850 0.197 Uiso 0.637(8) 1 calc PR B 1
H90C H 1.1950 0.8933 0.2686 0.197 Uiso 0.637(8) 1 calc PR B 1
C42' C 0.5030(17) 0.7690(12) 0.2751(15) 0.108(4) Uani 0.438(10) 1 d PDU A 2
H42C H 0.4708 0.8182 0.3028 0.130 Uiso 0.438(10) 1 calc PR A 2
H42D H 0.5432 0.7814 0.2224 0.130 Uiso 0.438(10) 1 calc PR A 2
C43' C 0.4274(16) 0.7259(13) 0.2676(12) 0.137(4) Uani 0.438(10) 1 d PU A 2
H43C H 0.3894 0.7587 0.2400 0.164 Uiso 0.438(10) 1 calc PR A 2
H43D H 0.4603 0.6801 0.2339 0.164 Uiso 0.438(10) 1 calc PR A 2
C44' C 0.3688(19) 0.7034(16) 0.3282(13) 0.143(4) Uani 0.438(10) 1 d PU A 2
H44C H 0.3325 0.7521 0.3550 0.171 Uiso 0.438(10) 1 calc PR A 2
H44D H 0.4110 0.6830 0.3587 0.171 Uiso 0.438(10) 1 calc PR A 2
C45' C 0.2856(11) 0.6449(10) 0.3500(9) 0.180(6) Uani 0.438(10) 1 d PU A 2
H45D H 0.2737 0.6281 0.4035 0.270 Uiso 0.438(10) 1 calc PR A 2
H45E H 0.3083 0.6000 0.3147 0.270 Uiso 0.438(10) 1 calc PR A 2
H45F H 0.2255 0.6721 0.3447 0.270 Uiso 0.438(10) 1 calc PR A 2
C87' C 0.9668(16) 0.7614(14) 0.2910(13) 0.109(5) Uani 0.363(8) 1 d PDU B 2
H87C H 1.0053 0.7098 0.2772 0.131 Uiso 0.363(8) 1 calc PR B 2
H87D H 0.9205 0.7585 0.3439 0.131 Uiso 0.363(8) 1 calc PR B 2
C88' C 1.0353(11) 0.8173(13) 0.2942(9) 0.128(4) Uani 0.363(8) 1 d PDU B 2
H88C H 1.0579 0.8047 0.3391 0.154 Uiso 0.363(8) 1 calc PR B 2
H88D H 0.9990 0.8699 0.3031 0.154 Uiso 0.363(8) 1 calc PR B 2
C89' C 1.1233(11) 0.8164(12) 0.2213(9) 0.134(4) Uani 0.363(8) 1 d PDU B 2
H89C H 1.1028 0.8401 0.1784 0.161 Uiso 0.363(8) 1 calc PR B 2
H89D H 1.1528 0.7627 0.2058 0.161 Uiso 0.363(8) 1 calc PR B 2
C90' C 1.1983(16) 0.8608(14) 0.2358(16) 0.187(7) Uani 0.363(8) 1 d PDU B 2
H90D H 1.2633 0.8331 0.2109 0.281 Uiso 0.363(8) 1 calc PR B 2
H90E H 1.1861 0.8655 0.2916 0.281 Uiso 0.363(8) 1 calc PR B 2
H90F H 1.1933 0.9121 0.2140 0.281 Uiso 0.363(8) 1 calc PR B 2
Cl1 Cl 0.81898(13) 0.45422(11) 0.74912(10) 0.1736(8) Uani 1 1 d . . .
Cl2 Cl 0.93701(13) 0.51542(8) 0.23773(9) 0.1523(6) Uani 1 1 d . . .
Cl3 Cl 0.59081(10) 1.04862(8) -0.14939(9) 0.1284(5) Uani 1 1 d . . .
Cl4 Cl 0.54251(11) 0.99645(8) 0.31928(8) 0.1299(5) Uani 1 1 d . . .
H2 H 0.683(4) 0.481(3) 0.460(3) 0.156 Uiso 1 1 d . . .
H6 H 0.809(4) 1.023(3) 0.090(3) 0.156 Uiso 1 1 d . . .
N1 N 0.5562(2) 0.74147(18) 0.74741(16) 0.0671(8) Uani 1 1 d . . .
N2 N 0.7313(3) 0.5005(2) 0.4724(2) 0.0856(10) Uani 1 1 d . . .
N3 N 0.5015(3) 0.55912(19) 0.42050(18) 0.0889(11) Uani 1 1 d . . .
N4 N 0.5684(3) 0.7299(2) 0.3160(2) 0.0827(10) Uani 1 1 d D . .
N5 N 0.8714(2) 0.76214(16) -0.18620(16) 0.0597(7) Uani 1 1 d . . .
N6 N 0.7588(3) 1.00576(19) 0.0871(2) 0.0855(11) Uani 1 1 d . . .
N7 N 1.0074(3) 0.93912(19) 0.1008(2) 0.0888(11) Uani 1 1 d . . .
N8 N 0.9100(2) 0.77778(18) 0.23681(18) 0.0685(8) Uani 1 1 d D . .
O1 O 0.47636(19) 0.78283(15) 0.65866(13) 0.0728(7) Uani 1 1 d . . .
O2 O 0.2358(2) 0.58031(17) 0.95523(16) 0.1183(12) Uani 1 1 d . . .
O3 O 0.38626(19) 0.65313(16) 0.58921(15) 0.0858(8) Uani 1 1 d . . .
O4 O 0.8997(3) 0.9341(2) 0.5412(2) 0.1361(13) Uani 1 1 d . . .
O5 O 0.74127(17) 0.62049(14) 0.51725(12) 0.0642(6) Uani 1 1 d . . .
O6 O 0.4988(2) 0.8166(2) 0.41985(17) 0.1025(9) Uani 1 1 d . . .
O7 O 0.96163(18) 0.71299(14) -0.10627(13) 0.0677(6) Uani 1 1 d . . .
O8 O 1.2240(2) 0.90939(17) -0.41308(16) 0.1068(10) Uani 1 1 d . . .
O9 O 1.07737(18) 0.82596(16) -0.05170(15) 0.0855(8) Uani 1 1 d . . .
O10 O 0.72676(15) 0.89074(12) 0.04845(12) 0.0565(6) Uani 1 1 d . . .
O11 O 0.5412(2) 0.58226(14) 0.04031(15) 0.0803(7) Uani 1 1 d . . .
O12 O 0.9811(2) 0.69446(17) 0.13037(16) 0.0901(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.499(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.518(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.527(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.459(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O1 1.212(4) . ?
C5 N1 1.363(4) . ?
C5 C6 1.536(5) . ?
C6 C7 1.522(4) . ?
C6 C13 1.577(4) . ?
C6 C26 1.579(4) . ?
C7 C12 1.370(5) . ?
C7 C8 1.372(5) . ?
C8 C9 1.400(5) . ?
C8 H8A 0.9300 . ?
C9 C10 1.344(6) . ?
C9 Cl1 1.727(5) . ?
C10 C11 1.361(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.384(5) . ?
C11 H11A 0.9300 . ?
C12 N1 1.385(4) . ?
C13 C14 1.523(5) . ?
C13 C23 1.561(4) . ?
C13 H13A 0.9800 . ?
C14 O3 1.218(4) . ?
C14 C15 1.467(4) . ?
C15 C21 1.381(5) . ?
C15 C16 1.386(4) . ?
C16 C17 1.366(4) . ?
C16 H16A 0.9300 . ?
C17 C18 1.378(5) . ?
C17 H17A 0.9300 . ?
C18 O2 1.369(4) . ?
C18 C20 1.374(5) . ?
C19 O2 1.431(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.382(5) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 N2 1.252(5) . ?
C22 O5 1.381(4) . ?
C22 C23 1.517(5) . ?
C23 C24 1.453(5) . ?
C23 C25 1.550(4) . ?
C24 N3 1.131(4) . ?
C25 C26 1.515(4) . ?
C25 C35 1.540(4) . ?
C25 H25A 0.9800 . ?
C26 O5 1.458(4) . ?
C26 C27 1.512(4) . ?
C27 C28 1.373(5) . ?
C27 C33 1.391(5) . ?
C28 C29 1.380(5) . ?
C28 H28A 0.9300 . ?
C29 C30 1.365(6) . ?
C29 H29A 0.9300 . ?
C30 C32 1.370(6) . ?
C30 O4 1.382(5) . ?
C31 O4 1.407(6) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.398(5) . ?
C32 H32A 0.9300 . ?
C33 H33A 0.9300 . ?
C34 O6 1.220(5) . ?
C34 N4 1.345(5) . ?
C34 C35 1.533(5) . ?
C35 C36 1.508(5) . ?
C35 H35A 0.9800 . ?
C36 C37 1.364(5) . ?
C36 C41 1.399(5) . ?
C37 C38 1.397(6) . ?
C37 H37A 0.9300 . ?
C38 C39 1.369(6) . ?
C38 Cl2 1.726(5) . ?
C39 C40 1.370(6) . ?
C39 H39A 0.9300 . ?
C40 C41 1.357(6) . ?
C40 H40A 0.9300 . ?
C41 N4 1.394(5) . ?
C42 N4 1.456(7) . ?
C42 C43 1.507(8) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.70(2) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.37(2) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 C47 1.519(7) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 C48 1.442(7) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 C49 1.564(6) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 N5 1.451(4) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C50 O7 1.223(4) . ?
C50 N5 1.370(4) . ?
C50 C51 1.517(5) . ?
C51 C52 1.505(4) . ?
C51 C71 1.573(4) . ?
C51 C58 1.588(4) . ?
C52 C53 1.376(4) . ?
C52 C57 1.387(4) . ?
C53 C54 1.389(5) . ?
C53 H53A 0.9300 . ?
C54 C55 1.351(5) . ?
C54 Cl3 1.734(4) . ?
C55 C56 1.386(5) . ?
C55 H55A 0.9300 . ?
C56 C57 1.385(5) . ?
C56 H56A 0.9300 . ?
C57 N5 1.381(4) . ?
C58 C59 1.518(5) . ?
C58 C69 1.557(4) . ?
C58 H58A 0.9800 . ?
C59 O9 1.218(4) . ?
C59 C60 1.482(5) . ?
C60 C61 1.375(5) . ?
C60 C66 1.386(4) . ?
C61 C62 1.361(5) . ?
C61 H61A 0.9300 . ?
C62 C63 1.371(5) . ?
C62 H62A 0.9300 . ?
C63 O8 1.366(4) . ?
C63 C65 1.377(5) . ?
C64 O8 1.453(5) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 C66 1.374(5) . ?
C65 H65A 0.9300 . ?
C66 H66A 0.9300 . ?
C67 N6 1.240(4) . ?
C67 O10 1.386(4) . ?
C67 C69 1.503(5) . ?
C68 C71 1.528(4) . ?
C68 C80 1.543(4) . ?
C68 C69 1.543(4) . ?
C68 H68A 0.9800 . ?
C69 C70 1.469(5) . ?
C70 N7 1.133(4) . ?
C71 O10 1.457(3) . ?
C71 C72 1.506(4) . ?
C72 C78 1.377(4) . ?
C72 C73 1.396(4) . ?
C73 C74 1.372(4) . ?
C73 H73A 0.9300 . ?
C74 C75 1.375(4) . ?
C74 H74A 0.9300 . ?
C75 O11 1.361(4) . ?
C75 C77 1.372(4) . ?
C76 O11 1.422(4) . ?
C76 H76A 0.9600 . ?
C76 H76B 0.9600 . ?
C76 H76C 0.9600 . ?
C77 C78 1.388(4) . ?
C77 H77A 0.9300 . ?
C78 H78A 0.9300 . ?
C79 O12 1.211(4) . ?
C79 N8 1.361(4) . ?
C79 C80 1.516(5) . ?
C80 C81 1.498(5) . ?
C80 H80A 0.9800 . ?
C81 C82 1.378(5) . ?
C81 C86 1.404(4) . ?
C82 C83 1.380(5) . ?
C82 H82A 0.9300 . ?
C83 C84 1.380(5) . ?
C83 Cl4 1.732(4) . ?
C84 C85 1.385(5) . ?
C84 H84A 0.9300 . ?
C85 C86 1.363(5) . ?
C85 H85A 0.9300 . ?
C86 N8 1.403(4) . ?
C87 N8 1.467(6) . ?
C87 C88 1.490(7) . ?
C87 H87A 0.9700 . ?
C87 H87B 0.9700 . ?
C88 C89 1.485(7) . ?
C88 H88A 0.9700 . ?
C88 H88B 0.9700 . ?
C89 C90 1.510(7) . ?
C89 H89A 0.9700 . ?
C89 H89B 0.9700 . ?
C90 H90A 0.9600 . ?
C90 H90B 0.9600 . ?
C90 H90C 0.9600 . ?
C42' C43' 1.45(2) . ?
C42' N4 1.460(7) . ?
C42' H42C 0.9700 . ?
C42' H42D 0.9700 . ?
C43' C44' 1.23(3) . ?
C43' H43C 0.9700 . ?
C43' H43D 0.9700 . ?
C44' C45' 1.63(3) . ?
C44' H44C 0.9700 . ?
C44' H44D 0.9700 . ?
C45' H45D 0.9600 . ?
C45' H45E 0.9600 . ?
C45' H45F 0.9600 . ?
C87' N8 1.462(8) . ?
C87' C88' 1.492(8) . ?
C87' H87C 0.9700 . ?
C87' H87D 0.9700 . ?
C88' C89' 1.495(8) . ?
C88' H88C 0.9700 . ?
C88' H88D 0.9700 . ?
C89' C90' 1.504(8) . ?
C89' H89C 0.9700 . ?
C89' H89D 0.9700 . ?
C90' H90D 0.9600 . ?
C90' H90E 0.9600 . ?
C90' H90F 0.9600 . ?
N2 H2 0.91(5) . ?
N6 H6 0.83(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 C3 113.5(5) . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
C3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C2 C3 C4 110.8(4) . . ?
C2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
N1 C4 C3 112.4(3) . . ?
N1 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
O1 C5 N1 125.9(3) . . ?
O1 C5 C6 126.2(3) . . ?
N1 C5 C6 107.9(3) . . ?
C7 C6 C5 101.3(3) . . ?
C7 C6 C13 114.9(3) . . ?
C5 C6 C13 113.7(3) . . ?
C7 C6 C26 115.6(3) . . ?
C5 C6 C26 110.5(2) . . ?
C13 C6 C26 101.3(2) . . ?
C12 C7 C8 120.7(3) . . ?
C12 C7 C6 108.7(3) . . ?
C8 C7 C6 130.5(3) . . ?
C7 C8 C9 116.8(4) . . ?
C7 C8 H8A 121.6 . . ?
C9 C8 H8A 121.6 . . ?
C10 C9 C8 122.0(4) . . ?
C10 C9 Cl1 119.1(4) . . ?
C8 C9 Cl1 118.9(4) . . ?
C9 C10 C11 121.3(4) . . ?
C9 C10 H10A 119.3 . . ?
C11 C10 H10A 119.3 . . ?
C10 C11 C12 117.6(4) . . ?
C10 C11 H11A 121.2 . . ?
C12 C11 H11A 121.2 . . ?
C7 C12 C11 121.5(4) . . ?
C7 C12 N1 110.4(3) . . ?
C11 C12 N1 127.9(4) . . ?
C14 C13 C23 113.9(3) . . ?
C14 C13 C6 115.7(3) . . ?
C23 C13 C6 102.2(2) . . ?
C14 C13 H13A 108.2 . . ?
C23 C13 H13A 108.2 . . ?
C6 C13 H13A 108.2 . . ?
O3 C14 C15 122.7(3) . . ?
O3 C14 C13 119.0(3) . . ?
C15 C14 C13 118.3(3) . . ?
C21 C15 C16 117.6(3) . . ?
C21 C15 C14 118.6(3) . . ?
C16 C15 C14 123.9(3) . . ?
C17 C16 C15 121.9(3) . . ?
C17 C16 H16A 119.1 . . ?
C15 C16 H16A 119.1 . . ?
C16 C17 C18 119.4(3) . . ?
C16 C17 H17A 120.3 . . ?
C18 C17 H17A 120.3 . . ?
O2 C18 C20 124.8(4) . . ?
O2 C18 C17 114.9(4) . . ?
C20 C18 C17 120.3(4) . . ?
O2 C19 H19A 109.5 . . ?
O2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 C21 119.5(4) . . ?
C18 C20 H20A 120.3 . . ?
C21 C20 H20A 120.3 . . ?
C15 C21 C20 121.4(4) . . ?
C15 C21 H21A 119.3 . . ?
C20 C21 H21A 119.3 . . ?
N2 C22 O5 119.7(4) . . ?
N2 C22 C23 134.9(3) . . ?
O5 C22 C23 105.3(3) . . ?
C24 C23 C22 112.8(3) . . ?
C24 C23 C25 116.8(3) . . ?
C22 C23 C25 102.2(3) . . ?
C24 C23 C13 118.5(3) . . ?
C22 C23 C13 101.8(3) . . ?
C25 C23 C13 102.5(2) . . ?
N3 C24 C23 174.6(4) . . ?
C26 C25 C35 118.3(3) . . ?
C26 C25 C23 92.6(2) . . ?
C35 C25 C23 117.8(3) . . ?
C26 C25 H25A 109.0 . . ?
C35 C25 H25A 109.0 . . ?
C23 C25 H25A 109.0 . . ?
O5 C26 C27 107.8(3) . . ?
O5 C26 C25 103.5(2) . . ?
C27 C26 C25 118.0(3) . . ?
O5 C26 C6 104.6(2) . . ?
C27 C26 C6 118.8(3) . . ?
C25 C26 C6 102.4(2) . . ?
C28 C27 C33 118.1(3) . . ?
C28 C27 C26 122.2(4) . . ?
C33 C27 C26 119.6(3) . . ?
C27 C28 C29 121.2(4) . . ?
C27 C28 H28A 119.4 . . ?
C29 C28 H28A 119.4 . . ?
C30 C29 C28 120.3(4) . . ?
C30 C29 H29A 119.9 . . ?
C28 C29 H29A 119.9 . . ?
C29 C30 C32 120.4(4) . . ?
C29 C30 O4 113.4(5) . . ?
C32 C30 O4 126.2(5) . . ?
O4 C31 H31A 109.5 . . ?
O4 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O4 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 C33 119.3(4) . . ?
C30 C32 H32A 120.4 . . ?
C33 C32 H32A 120.4 . . ?
C27 C33 C32 120.7(4) . . ?
C27 C33 H33A 119.6 . . ?
C32 C33 H33A 119.6 . . ?
O6 C34 N4 125.2(4) . . ?
O6 C34 C35 124.8(4) . . ?
N4 C34 C35 110.1(4) . . ?
C36 C35 C34 101.2(3) . . ?
C36 C35 C25 121.6(3) . . ?
C34 C35 C25 108.9(3) . . ?
C36 C35 H35A 108.1 . . ?
C34 C35 H35A 108.1 . . ?
C25 C35 H35A 108.1 . . ?
C37 C36 C41 119.5(4) . . ?
C37 C36 C35 132.4(4) . . ?
C41 C36 C35 108.0(4) . . ?
C36 C37 C38 118.3(4) . . ?
C36 C37 H37A 120.9 . . ?
C38 C37 H37A 120.9 . . ?
C39 C38 C37 122.0(5) . . ?
C39 C38 Cl2 120.3(4) . . ?
C37 C38 Cl2 117.8(5) . . ?
C38 C39 C40 119.0(5) . . ?
C38 C39 H39A 120.5 . . ?
C40 C39 H39A 120.5 . . ?
C41 C40 C39 120.1(5) . . ?
C41 C40 H40A 120.0 . . ?
C39 C40 H40A 120.0 . . ?
C40 C41 N4 128.2(5) . . ?
C40 C41 C36 121.1(5) . . ?
N4 C41 C36 110.6(3) . . ?
N4 C42 C43 112.0(10) . . ?
N4 C42 H42A 109.2 . . ?
C43 C42 H42A 109.2 . . ?
N4 C42 H42B 109.2 . . ?
C43 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
C42 C43 C44 108.5(13) . . ?
C42 C43 H43A 110.0 . . ?
C44 C43 H43A 110.0 . . ?
C42 C43 H43B 110.0 . . ?
C44 C43 H43B 110.0 . . ?
H43A C43 H43B 108.4 . . ?
C45 C44 C43 112.8(11) . . ?
C45 C44 H44A 109.0 . . ?
C43 C44 H44A 109.0 . . ?
C45 C44 H44B 109.0 . . ?
C43 C44 H44B 109.0 . . ?
H44A C44 H44B 107.8 . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C47 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 C46 110.5(5) . . ?
C48 C47 H47A 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C48 C47 H47B 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 108.1 . . ?
C47 C48 C49 116.1(4) . . ?
C47 C48 H48A 108.3 . . ?
C49 C48 H48A 108.3 . . ?
C47 C48 H48B 108.3 . . ?
C49 C48 H48B 108.3 . . ?
H48A C48 H48B 107.4 . . ?
N5 C49 C48 110.8(3) . . ?
N5 C49 H49A 109.5 . . ?
C48 C49 H49A 109.5 . . ?
N5 C49 H49B 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 108.1 . . ?
O7 C50 N5 125.3(3) . . ?
O7 C50 C51 126.5(3) . . ?
N5 C50 C51 108.2(3) . . ?
C52 C51 C50 102.2(3) . . ?
C52 C51 C71 113.9(3) . . ?
C50 C51 C71 111.9(2) . . ?
C52 C51 C58 115.8(2) . . ?
C50 C51 C58 112.2(3) . . ?
C71 C51 C58 101.2(2) . . ?
C53 C52 C57 120.1(3) . . ?
C53 C52 C51 131.6(3) . . ?
C57 C52 C51 108.3(3) . . ?
C52 C53 C54 118.2(3) . . ?
C52 C53 H53A 120.9 . . ?
C54 C53 H53A 120.9 . . ?
C55 C54 C53 121.6(4) . . ?
C55 C54 Cl3 119.1(3) . . ?
C53 C54 Cl3 119.4(3) . . ?
C54 C55 C56 121.2(4) . . ?
C54 C55 H55A 119.4 . . ?
C56 C55 H55A 119.4 . . ?
C57 C56 C55 117.6(4) . . ?
C57 C56 H56A 121.2 . . ?
C55 C56 H56A 121.2 . . ?
N5 C57 C56 128.6(3) . . ?
N5 C57 C52 110.2(3) . . ?
C56 C57 C52 121.2(4) . . ?
C59 C58 C69 112.3(3) . . ?
C59 C58 C51 116.4(3) . . ?
C69 C58 C51 101.8(2) . . ?
C59 C58 H58A 108.7 . . ?
C69 C58 H58A 108.7 . . ?
C51 C58 H58A 108.7 . . ?
O9 C59 C60 122.0(3) . . ?
O9 C59 C58 118.7(3) . . ?
C60 C59 C58 119.3(3) . . ?
C61 C60 C66 118.7(3) . . ?
C61 C60 C59 118.0(3) . . ?
C66 C60 C59 123.4(3) . . ?
C62 C61 C60 121.8(4) . . ?
C62 C61 H61A 119.1 . . ?
C60 C61 H61A 119.1 . . ?
C61 C62 C63 119.3(4) . . ?
C61 C62 H62A 120.3 . . ?
C63 C62 H62A 120.3 . . ?
O8 C63 C62 124.0(4) . . ?
O8 C63 C65 115.9(4) . . ?
C62 C63 C65 120.2(4) . . ?
O8 C64 H64A 109.5 . . ?
O8 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
O8 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C66 C65 C63 120.2(4) . . ?
C66 C65 H65A 119.9 . . ?
C63 C65 H65A 119.9 . . ?
C65 C66 C60 119.8(3) . . ?
C65 C66 H66A 120.1 . . ?
C60 C66 H66A 120.1 . . ?
N6 C67 O10 119.7(3) . . ?
N6 C67 C69 135.1(3) . . ?
O10 C67 C69 105.1(3) . . ?
C71 C68 C80 117.6(3) . . ?
C71 C68 C69 92.1(2) . . ?
C80 C68 C69 118.3(2) . . ?
C71 C68 H68A 109.2 . . ?
C80 C68 H68A 109.2 . . ?
C69 C68 H68A 109.2 . . ?
C70 C69 C67 112.7(3) . . ?
C70 C69 C68 118.5(3) . . ?
C67 C69 C68 102.0(3) . . ?
C70 C69 C58 114.9(3) . . ?
C67 C69 C58 103.8(3) . . ?
C68 C69 C58 103.0(2) . . ?
N7 C70 C69 175.9(4) . . ?
O10 C71 C72 108.9(2) . . ?
O10 C71 C68 102.6(2) . . ?
C72 C71 C68 119.2(2) . . ?
O10 C71 C51 105.1(2) . . ?
C72 C71 C51 116.6(2) . . ?
C68 C71 C51 102.8(2) . . ?
C78 C72 C73 117.4(3) . . ?
C78 C72 C71 122.0(3) . . ?
C73 C72 C71 120.6(3) . . ?
C74 C73 C72 121.2(3) . . ?
C74 C73 H73A 119.4 . . ?
C72 C73 H73A 119.4 . . ?
C73 C74 C75 120.6(3) . . ?
C73 C74 H74A 119.7 . . ?
C75 C74 H74A 119.7 . . ?
O11 C75 C77 125.4(3) . . ?
O11 C75 C74 115.3(3) . . ?
C77 C75 C74 119.3(3) . . ?
O11 C76 H76A 109.5 . . ?
O11 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
O11 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C75 C77 C78 120.1(3) . . ?
C75 C77 H77A 120.0 . . ?
C78 C77 H77A 120.0 . . ?
C72 C78 C77 121.4(3) . . ?
C72 C78 H78A 119.3 . . ?
C77 C78 H78A 119.3 . . ?
O12 C79 N8 124.4(4) . . ?
O12 C79 C80 127.1(3) . . ?
N8 C79 C80 108.5(3) . . ?
C81 C80 C79 103.0(3) . . ?
C81 C80 C68 122.7(3) . . ?
C79 C80 C68 109.0(3) . . ?
C81 C80 H80A 107.1 . . ?
C79 C80 H80A 107.1 . . ?
C68 C80 H80A 107.1 . . ?
C82 C81 C86 118.8(3) . . ?
C82 C81 C80 132.9(3) . . ?
C86 C81 C80 108.1(3) . . ?
C81 C82 C83 119.0(4) . . ?
C81 C82 H82A 120.5 . . ?
C83 C82 H82A 120.5 . . ?
C82 C83 C84 121.7(4) . . ?
C82 C83 Cl4 118.9(4) . . ?
C84 C83 Cl4 119.4(3) . . ?
C83 C84 C85 119.6(4) . . ?
C83 C84 H84A 120.2 . . ?
C85 C84 H84A 120.2 . . ?
C86 C85 C84 118.8(4) . . ?
C86 C85 H85A 120.6 . . ?
C84 C85 H85A 120.6 . . ?
C85 C86 N8 128.5(4) . . ?
C85 C86 C81 122.0(4) . . ?
N8 C86 C81 109.4(3) . . ?
N8 C87 C88 112.4(6) . . ?
N8 C87 H87A 109.1 . . ?
C88 C87 H87A 109.1 . . ?
N8 C87 H87B 109.1 . . ?
C88 C87 H87B 109.1 . . ?
H87A C87 H87B 107.8 . . ?
C89 C88 C87 115.5(10) . . ?
C89 C88 H88A 108.4 . . ?
C87 C88 H88A 108.4 . . ?
C89 C88 H88B 108.4 . . ?
C87 C88 H88B 108.4 . . ?
H88A C88 H88B 107.5 . . ?
C88 C89 C90 114.9(9) . . ?
C88 C89 H89A 108.5 . . ?
C90 C89 H89A 108.5 . . ?
C88 C89 H89B 108.5 . . ?
C90 C89 H89B 108.5 . . ?
H89A C89 H89B 107.5 . . ?
C43' C42' N4 116.5(15) . . ?
C43' C42' H42C 108.2 . . ?
N4 C42' H42C 108.2 . . ?
C43' C42' H42D 108.2 . . ?
N4 C42' H42D 108.2 . . ?
H42C C42' H42D 107.3 . . ?
C44' C43' C42' 119(2) . . ?
C44' C43' H43C 107.7 . . ?
C42' C43' H43C 107.7 . . ?
C44' C43' H43D 107.7 . . ?
C42' C43' H43D 107.7 . . ?
H43C C43' H43D 107.1 . . ?
C43' C44' C45' 137(2) . . ?
C43' C44' H44C 103.0 . . ?
C45' C44' H44C 103.0 . . ?
C43' C44' H44D 103.0 . . ?
C45' C44' H44D 103.0 . . ?
H44C C44' H44D 105.1 . . ?
C44' C45' H45D 109.5 . . ?
C44' C45' H45E 109.5 . . ?
H45D C45' H45E 109.5 . . ?
C44' C45' H45F 109.5 . . ?
H45D C45' H45F 109.5 . . ?
H45E C45' H45F 109.5 . . ?
N8 C87' C88' 118.1(14) . . ?
N8 C87' H87C 107.8 . . ?
C88' C87' H87C 107.8 . . ?
N8 C87' H87D 107.8 . . ?
C88' C87' H87D 107.8 . . ?
H87C C87' H87D 107.1 . . ?
C87' C88' C89' 114(2) . . ?
C87' C88' H88C 108.7 . . ?
C89' C88' H88C 108.7 . . ?
C87' C88' H88D 108.7 . . ?
C89' C88' H88D 108.7 . . ?
H88C C88' H88D 107.6 . . ?
C88' C89' C90' 110.7(18) . . ?
C88' C89' H89C 109.5 . . ?
C90' C89' H89C 109.5 . . ?
C88' C89' H89D 109.5 . . ?
C90' C89' H89D 109.5 . . ?
H89C C89' H89D 108.1 . . ?
C89' C90' H90D 109.5 . . ?
C89' C90' H90E 109.5 . . ?
H90D C90' H90E 109.5 . . ?
C89' C90' H90F 109.5 . . ?
H90D C90' H90F 109.5 . . ?
H90E C90' H90F 109.5 . . ?
C5 N1 C12 111.5(3) . . ?
C5 N1 C4 123.1(3) . . ?
C12 N1 C4 124.9(3) . . ?
C22 N2 H2 101(4) . . ?
C34 N4 C41 110.1(4) . . ?
C34 N4 C42 131.4(9) . . ?
C41 N4 C42 118.5(9) . . ?
C34 N4 C42' 116.1(11) . . ?
C41 N4 C42' 132.4(12) . . ?
C42 N4 C42' 17.7(14) . . ?
C50 N5 C57 111.0(3) . . ?
C50 N5 C49 122.6(3) . . ?
C57 N5 C49 126.0(3) . . ?
C67 N6 H6 103(4) . . ?
C79 N8 C86 111.1(3) . . ?
C79 N8 C87' 133.5(11) . . ?
C86 N8 C87' 115.1(11) . . ?
C79 N8 C87 118.9(6) . . ?
C86 N8 C87 129.7(6) . . ?
C87' N8 C87 14.7(15) . . ?
C18 O2 C19 117.9(4) . . ?
C30 O4 C31 117.0(5) . . ?
C22 O5 C26 107.3(3) . . ?
C63 O8 C64 117.6(3) . . ?
C67 O10 C71 107.3(2) . . ?
C75 O11 C76 118.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.046


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.500 132 30 ' '
2 0.000 0.500 0.000 53 11 ' '
3 0.500 0.000 0.500 21 3 ' '
_platon_squeeze_details          
; 
;
_database_code_depnum_ccdc_archive 'CCDC 1009897'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1i

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C53 H45 N3 O6'
_chemical_formula_sum            'C53 H45 N3 O6'
_chemical_formula_weight         819.92

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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   11.1491(15)
_cell_length_b                   14.4233(19)
_cell_length_c                   16.278(2)
_cell_angle_alpha                92.642(4)
_cell_angle_beta                 90.979(4)
_cell_angle_gamma                111.404(4)
_cell_volume                     2432.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9946
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      27.58

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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            40728
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_sigmaI/netI    0.0855
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8587
_reflns_number_gt                4833
_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)+(0.1100P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8567
_refine_ls_number_parameters     585
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0673
_refine_ls_wR_factor_ref         0.2008
_refine_ls_wR_factor_gt          0.1787
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3854(4) 0.6763(3) 0.3141(2) 0.0795(11) Uani 1 1 d . . .
H1 H 0.3824 0.6231 0.2786 0.095 Uiso 1 1 calc R . .
C2 C 0.3312(5) 0.7428(4) 0.2896(3) 0.1083(15) Uani 1 1 d . . .
H2 H 0.2924 0.7351 0.2373 0.130 Uiso 1 1 calc R . .
C3 C 0.3348(6) 0.8213(4) 0.3434(4) 0.1251(18) Uani 1 1 d . . .
H3A H 0.2996 0.8671 0.3268 0.150 Uiso 1 1 calc R . .
C4 C 0.3885(6) 0.8315(4) 0.4188(4) 0.1221(18) Uani 1 1 d . . .
H4 H 0.3880 0.8834 0.4548 0.147 Uiso 1 1 calc R . .
C5 C 0.4448(4) 0.7660(3) 0.4441(3) 0.0936(13) Uani 1 1 d . . .
H5 H 0.4829 0.7744 0.4966 0.112 Uiso 1 1 calc R . .
C6 C 0.4444(3) 0.6884(2) 0.3914(2) 0.0653(9) Uani 1 1 d . . .
C7 C 0.5063(4) 0.6177(3) 0.42079(19) 0.0683(10) Uani 1 1 d . . .
H7A H 0.5781 0.6543 0.4585 0.082 Uiso 1 1 calc R . .
H7B H 0.4439 0.5665 0.4510 0.082 Uiso 1 1 calc R . .
C8 C 0.5165(3) 0.4695(2) 0.34041(16) 0.0415(7) Uani 1 1 d . . .
C9 C 0.5909(2) 0.44913(19) 0.26806(15) 0.0354(6) Uani 1 1 d . . .
C10 C 0.6814(2) 0.55360(19) 0.25018(16) 0.0400(7) Uani 1 1 d . . .
C11 C 0.7801(3) 0.5879(2) 0.19617(17) 0.0503(8) Uani 1 1 d . . .
H11 H 0.7988 0.5435 0.1601 0.060 Uiso 1 1 calc R . .
C12 C 0.8507(3) 0.6887(3) 0.1964(2) 0.0663(9) Uani 1 1 d . . .
H12 H 0.9181 0.7125 0.1608 0.080 Uiso 1 1 calc R . .
C13 C 0.8221(4) 0.7545(3) 0.2491(2) 0.0795(11) Uani 1 1 d . . .
H13 H 0.8701 0.8223 0.2479 0.095 Uiso 1 1 calc R . .
C14 C 0.7231(3) 0.7219(2) 0.3040(2) 0.0695(10) Uani 1 1 d . . .
H14 H 0.7042 0.7666 0.3396 0.083 Uiso 1 1 calc R . .
C15 C 0.6543(3) 0.6212(2) 0.30355(17) 0.0476(7) Uani 1 1 d . . .
C16 C 0.6524(2) 0.37031(19) 0.28774(16) 0.0396(7) Uani 1 1 d . . .
H16 H 0.6133 0.3385 0.3376 0.047 Uiso 1 1 calc R . .
C17 C 0.7977(3) 0.4106(2) 0.30308(18) 0.0472(7) Uani 1 1 d . . .
C18 C 0.8522(3) 0.4851(2) 0.37233(18) 0.0492(8) Uani 1 1 d . . .
C19 C 0.7821(3) 0.4949(3) 0.43892(19) 0.0669(9) Uani 1 1 d . . .
H19 H 0.6966 0.4524 0.4417 0.080 Uiso 1 1 calc R . .
C20 C 0.8365(4) 0.5663(3) 0.5011(2) 0.0785(11) Uani 1 1 d . . .
H20 H 0.7874 0.5710 0.5456 0.094 Uiso 1 1 calc R . .
C21 C 0.9630(5) 0.6316(3) 0.4989(3) 0.0825(12) Uani 1 1 d . . .
C22 C 1.0205(5) 0.7104(3) 0.5679(3) 0.1255(19) Uani 1 1 d . . .
H22A H 0.9572 0.7046 0.6086 0.188 Uiso 1 1 calc R . .
H22B H 1.0470 0.7754 0.5462 0.188 Uiso 1 1 calc R . .
H22C H 1.0939 0.7012 0.5927 0.188 Uiso 1 1 calc R . .
C23 C 1.0329(4) 0.6205(3) 0.4327(3) 0.0889(12) Uani 1 1 d . . .
H23 H 1.1185 0.6630 0.4301 0.107 Uiso 1 1 calc R . .
C24 C 0.9802(3) 0.5487(3) 0.3703(2) 0.0711(10) Uani 1 1 d . . .
H24 H 1.0302 0.5427 0.3267 0.085 Uiso 1 1 calc R . .
C25 C 0.0544(3) -0.0888(2) 0.0747(2) 0.0663(9) Uani 1 1 d . . .
H25 H 0.0642 -0.0301 0.1051 0.080 Uiso 1 1 calc R . .
C26 C -0.0604(3) -0.1408(3) 0.0321(2) 0.0757(11) Uani 1 1 d . . .
H26 H -0.1268 -0.1163 0.0329 0.091 Uiso 1 1 calc R . .
C27 C -0.0768(3) -0.2276(3) -0.0108(2) 0.0754(10) Uani 1 1 d . . .
H27 H -0.1541 -0.2625 -0.0397 0.090 Uiso 1 1 calc R . .
C28 C 0.0214(4) -0.2638(3) -0.0116(2) 0.0767(10) Uani 1 1 d . . .
H28 H 0.0098 -0.3240 -0.0399 0.092 Uiso 1 1 calc R . .
C29 C 0.1359(3) -0.2115(2) 0.0293(2) 0.0629(9) Uani 1 1 d . . .
H29 H 0.2022 -0.2361 0.0278 0.075 Uiso 1 1 calc R . .
C30 C 0.1546(3) -0.1229(2) 0.07265(18) 0.0510(8) Uani 1 1 d . . .
C31 C 0.2822(3) -0.0686(2) 0.1186(2) 0.0675(9) Uani 1 1 d . . .
H31A H 0.2741 -0.0854 0.1758 0.081 Uiso 1 1 calc R . .
H31B H 0.3473 -0.0909 0.0954 0.081 Uiso 1 1 calc R . .
C32 C 0.3261(3) 0.1030(2) 0.1790(2) 0.0539(8) Uani 1 1 d . . .
C33 C 0.3628(3) 0.20685(19) 0.14870(16) 0.0420(7) Uani 1 1 d . . .
H33 H 0.2840 0.2220 0.1490 0.050 Uiso 1 1 calc R . .
C34 C 0.3895(2) 0.1922(2) 0.05846(17) 0.0427(7) Uani 1 1 d . . .
C35 C 0.4185(3) 0.2537(2) -0.00581(18) 0.0534(8) Uani 1 1 d . . .
H35 H 0.4334 0.3211 0.0036 0.064 Uiso 1 1 calc R . .
C36 C 0.4260(3) 0.2165(3) -0.0844(2) 0.0659(9) Uani 1 1 d . . .
H36 H 0.4480 0.2590 -0.1275 0.079 Uiso 1 1 calc R . .
C37 C 0.4005(3) 0.1153(3) -0.0987(2) 0.0721(10) Uani 1 1 d . . .
H37 H 0.4056 0.0907 -0.1518 0.086 Uiso 1 1 calc R . .
C38 C 0.3679(3) 0.0508(3) -0.0363(2) 0.0656(9) Uani 1 1 d . . .
H38 H 0.3507 -0.0170 -0.0459 0.079 Uiso 1 1 calc R . .
C39 C 0.3615(3) 0.0911(2) 0.04218(19) 0.0482(7) Uani 1 1 d . . .
C40 C 0.4588(2) 0.28363(19) 0.21053(16) 0.0391(7) Uani 1 1 d . . .
H40 H 0.4244 0.2732 0.2658 0.047 Uiso 1 1 calc R . .
C41 C 0.4962(2) 0.39409(18) 0.19279(15) 0.0357(6) Uani 1 1 d . . .
C42 C 0.3911(2) 0.43180(19) 0.17257(15) 0.0370(6) Uani 1 1 d . . .
C43 C 0.2761(3) 0.3994(2) 0.21408(17) 0.0437(7) Uani 1 1 d . . .
H43 H 0.2647 0.3541 0.2548 0.052 Uiso 1 1 calc R . .
C44 C 0.1786(3) 0.4339(2) 0.19540(18) 0.0476(7) Uani 1 1 d . . .
H44 H 0.1024 0.4109 0.2236 0.057 Uiso 1 1 calc R . .
C45 C 0.1925(3) 0.5018(2) 0.13575(18) 0.0493(7) Uani 1 1 d . . .
C46 C 0.0857(3) 0.5400(3) 0.1158(2) 0.0719(10) Uani 1 1 d . . .
H46A H 0.0036 0.4884 0.1233 0.108 Uiso 1 1 calc R . .
H46B H 0.0911 0.5585 0.0597 0.108 Uiso 1 1 calc R . .
H46C H 0.0950 0.5970 0.1517 0.108 Uiso 1 1 calc R . .
C47 C 0.3071(3) 0.5340(2) 0.09422(17) 0.0516(8) Uani 1 1 d . . .
H47 H 0.3181 0.5793 0.0535 0.062 Uiso 1 1 calc R . .
C48 C 0.4058(3) 0.4997(2) 0.11228(17) 0.0459(7) Uani 1 1 d . . .
H48 H 0.4819 0.5225 0.0839 0.055 Uiso 1 1 calc R . .
C49 C 0.6501(3) 0.3436(2) 0.13633(17) 0.0431(7) Uani 1 1 d . . .
C50 C 0.6020(2) 0.29065(19) 0.21443(16) 0.0410(7) Uani 1 1 d . . .
C51 C 0.6232(3) 0.1947(2) 0.2221(2) 0.0530(8) Uani 1 1 d U A .
N1 N 0.5526(2) 0.57000(17) 0.35466(14) 0.0487(6) Uani 1 1 d . . .
N2 N 0.3242(2) 0.03925(17) 0.11456(16) 0.0541(7) Uani 1 1 d . . .
N3 N 0.7353(3) 0.3445(2) 0.08667(15) 0.0578(7) Uani 1 1 d . . .
H3B H 0.772(4) 0.303(3) 0.102(2) 0.087 Uiso 1 1 d . . .
O1 O 0.43796(19) 0.40629(15) 0.38040(11) 0.0522(5) Uani 1 1 d . . .
O2 O 0.8649(2) 0.38024(17) 0.25958(13) 0.0653(6) Uani 1 1 d . . .
O3 O 0.3003(3) 0.07814(17) 0.24988(15) 0.0845(8) Uani 1 1 d . . .
O4 O 0.58050(16) 0.40411(13) 0.12402(10) 0.0406(5) Uani 1 1 d . . .
C52 C 0.6700(12) 0.0864(8) 0.3109(7) 0.120(2) Uani 0.571(8) 1 d PDU A 1
H52A H 0.5990 0.0280 0.2888 0.144 Uiso 0.571(8) 1 calc PR A 1
H52B H 0.6765 0.0795 0.3696 0.144 Uiso 0.571(8) 1 calc PR A 1
C53 C 0.7942(11) 0.0825(8) 0.2736(7) 0.138(2) Uani 0.571(8) 1 d PDU A 1
H53A H 0.7868 0.0815 0.2146 0.206 Uiso 0.571(8) 1 calc PR A 1
H53B H 0.8069 0.0234 0.2894 0.206 Uiso 0.571(8) 1 calc PR A 1
H53C H 0.8664 0.1402 0.2933 0.206 Uiso 0.571(8) 1 calc PR A 1
C52' C 0.5861(15) 0.0607(9) 0.3148(10) 0.124(3) Uani 0.429(8) 1 d PDU A 2
H52C H 0.5314 0.0438 0.3617 0.149 Uiso 0.429(8) 1 calc PR A 2
H52D H 0.5417 0.0196 0.2666 0.149 Uiso 0.429(8) 1 calc PR A 2
C53' C 0.7115(15) 0.0544(10) 0.3310(10) 0.136(2) Uani 0.429(8) 1 d PDU A 2
H53D H 0.7353 0.0233 0.2839 0.204 Uiso 0.429(8) 1 calc PR A 2
H53E H 0.7073 0.0154 0.3779 0.204 Uiso 0.429(8) 1 calc PR A 2
H53F H 0.7747 0.1202 0.3420 0.204 Uiso 0.429(8) 1 calc PR A 2
O5 O 0.6248(2) 0.13996(17) 0.16508(15) 0.0780(7) Uani 1 1 d . . .
O6 O 0.6336(3) 0.17434(18) 0.29946(15) 0.0991(9) Uani 1 1 d DU . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.376(5) . ?
C1 C6 1.383(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.388(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.334(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.386(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.376(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.515(5) . ?
C7 N1 1.452(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O1 1.230(3) . ?
C8 N1 1.363(3) . ?
C8 C9 1.530(4) . ?
C9 C10 1.521(4) . ?
C9 C16 1.569(3) . ?
C9 C41 1.581(3) . ?
C10 C11 1.381(4) . ?
C10 C15 1.393(4) . ?
C11 C12 1.377(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.375(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.390(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.373(4) . ?
C14 H14 0.9300 . ?
C15 N1 1.414(4) . ?
C16 C17 1.520(4) . ?
C16 C50 1.562(4) . ?
C16 H16 0.9800 . ?
C17 O2 1.218(3) . ?
C17 C18 1.477(4) . ?
C18 C19 1.379(4) . ?
C18 C24 1.388(4) . ?
C19 C20 1.371(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.382(6) . ?
C20 H20 0.9300 . ?
C21 C23 1.378(5) . ?
C21 C22 1.514(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.374(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C30 1.375(4) . ?
C25 C26 1.380(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.356(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.373(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.365(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.375(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.515(4) . ?
C31 N2 1.456(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 O3 1.232(3) . ?
C32 N2 1.357(4) . ?
C32 C33 1.510(4) . ?
C33 C34 1.524(4) . ?
C33 C40 1.543(4) . ?
C33 H33 0.9800 . ?
C34 C35 1.369(4) . ?
C34 C39 1.388(4) . ?
C35 C36 1.380(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.389(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.373(5) . ?
C37 H37 0.9300 . ?
C38 C39 1.392(4) . ?
C38 H38 0.9300 . ?
C39 N2 1.411(4) . ?
C40 C41 1.535(4) . ?
C40 C50 1.562(4) . ?
C40 H40 0.9800 . ?
C41 O4 1.452(3) . ?
C41 C42 1.499(3) . ?
C42 C48 1.388(4) . ?
C42 C43 1.393(4) . ?
C43 C44 1.385(4) . ?
C43 H43 0.9300 . ?
C44 C45 1.381(4) . ?
C44 H44 0.9300 . ?
C45 C47 1.389(4) . ?
C45 C46 1.519(4) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 C48 1.394(4) . ?
C47 H47 0.9300 . ?
C48 H48 0.9300 . ?
C49 N3 1.254(3) . ?
C49 O4 1.382(3) . ?
C49 C50 1.517(4) . ?
C50 C51 1.496(4) . ?
C51 O5 1.196(3) . ?
C51 O6 1.319(4) . ?
N3 H3B 0.88(4) . ?
C52 O6 1.485(8) . ?
C52 C53 1.540(12) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C52' C53' 1.455(14) . ?
C52' O6 1.561(11) . ?
C52' H52C 0.9700 . ?
C52' H52D 0.9700 . ?
C53' H53D 0.9600 . ?
C53' H53E 0.9600 . ?
C53' H53F 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
C2 C1 C6 120.3(4) . . ?
C2 C1 H1 119.9 . . ?
C6 C1 H1 119.9 . . ?
C1 C2 C3 119.4(4) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 120.4(4) . . ?
C4 C3 H3A 119.8 . . ?
C2 C3 H3A 119.8 . . ?
C3 C4 C5 120.9(4) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 119.8(4) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 119.1(3) . . ?
C5 C6 C7 118.8(3) . . ?
C1 C6 C7 122.1(3) . . ?
N1 C7 C6 113.7(3) . . ?
N1 C7 H7A 108.8 . . ?
C6 C7 H7A 108.8 . . ?
N1 C7 H7B 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
O1 C8 N1 125.0(3) . . ?
O1 C8 C9 126.2(2) . . ?
N1 C8 C9 108.8(2) . . ?
C10 C9 C8 102.2(2) . . ?
C10 C9 C16 117.8(2) . . ?
C8 C9 C16 111.9(2) . . ?
C10 C9 C41 113.0(2) . . ?
C8 C9 C41 110.9(2) . . ?
C16 C9 C41 101.30(18) . . ?
C11 C10 C15 119.7(3) . . ?
C11 C10 C9 132.3(2) . . ?
C15 C10 C9 108.0(2) . . ?
C12 C11 C10 119.1(3) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 121.6(3) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C15 C14 C13 117.4(3) . . ?
C15 C14 H14 121.3 . . ?
C13 C14 H14 121.3 . . ?
C14 C15 C10 121.8(3) . . ?
C14 C15 N1 128.0(3) . . ?
C10 C15 N1 110.2(2) . . ?
C17 C16 C50 114.9(2) . . ?
C17 C16 C9 116.1(2) . . ?
C50 C16 C9 103.30(19) . . ?
C17 C16 H16 107.4 . . ?
C50 C16 H16 107.4 . . ?
C9 C16 H16 107.4 . . ?
O2 C17 C18 122.2(3) . . ?
O2 C17 C16 119.9(3) . . ?
C18 C17 C16 117.9(3) . . ?
C19 C18 C24 118.2(3) . . ?
C19 C18 C17 123.2(3) . . ?
C24 C18 C17 118.5(3) . . ?
C20 C19 C18 121.1(4) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C21 121.3(4) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C23 C21 C20 117.4(3) . . ?
C23 C21 C22 122.4(4) . . ?
C20 C21 C22 120.3(5) . . ?
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 . . ?
C24 C23 C21 122.0(4) . . ?
C24 C23 H23 119.0 . . ?
C21 C23 H23 119.0 . . ?
C23 C24 C18 120.0(4) . . ?
C23 C24 H24 120.0 . . ?
C18 C24 H24 120.0 . . ?
C30 C25 C26 120.5(3) . . ?
C30 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C27 C26 C25 120.2(3) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 119.7(3) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C29 C28 C27 120.1(3) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C28 C29 C30 120.9(3) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
C29 C30 C25 118.4(3) . . ?
C29 C30 C31 119.1(3) . . ?
C25 C30 C31 122.5(3) . . ?
N2 C31 C30 112.4(2) . . ?
N2 C31 H31A 109.1 . . ?
C30 C31 H31A 109.1 . . ?
N2 C31 H31B 109.1 . . ?
C30 C31 H31B 109.1 . . ?
H31A C31 H31B 107.9 . . ?
O3 C32 N2 124.4(3) . . ?
O3 C32 C33 126.7(3) . . ?
N2 C32 C33 108.9(3) . . ?
C32 C33 C34 102.7(2) . . ?
C32 C33 C40 110.3(2) . . ?
C34 C33 C40 124.3(2) . . ?
C32 C33 H33 106.1 . . ?
C34 C33 H33 106.1 . . ?
C40 C33 H33 106.1 . . ?
C35 C34 C39 118.6(3) . . ?
C35 C34 C33 133.6(3) . . ?
C39 C34 C33 107.4(2) . . ?
C34 C35 C36 120.6(3) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C37 119.7(3) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C38 C37 C36 121.5(3) . . ?
C38 C37 H37 119.3 . . ?
C36 C37 H37 119.3 . . ?
C37 C38 C39 117.2(3) . . ?
C37 C38 H38 121.4 . . ?
C39 C38 H38 121.4 . . ?
C34 C39 C38 122.4(3) . . ?
C34 C39 N2 110.2(3) . . ?
C38 C39 N2 127.3(3) . . ?
C41 C40 C33 116.8(2) . . ?
C41 C40 C50 93.14(19) . . ?
C33 C40 C50 118.9(2) . . ?
C41 C40 H40 109.0 . . ?
C33 C40 H40 109.0 . . ?
C50 C40 H40 109.0 . . ?
O4 C41 C42 110.61(19) . . ?
O4 C41 C40 102.26(18) . . ?
C42 C41 C40 118.6(2) . . ?
O4 C41 C9 104.10(18) . . ?
C42 C41 C9 116.8(2) . . ?
C40 C41 C9 102.69(19) . . ?
C48 C42 C43 118.4(2) . . ?
C48 C42 C41 121.0(2) . . ?
C43 C42 C41 120.6(2) . . ?
C44 C43 C42 120.8(3) . . ?
C44 C43 H43 119.6 . . ?
C42 C43 H43 119.6 . . ?
C45 C44 C43 121.3(3) . . ?
C45 C44 H44 119.4 . . ?
C43 C44 H44 119.4 . . ?
C44 C45 C47 118.0(2) . . ?
C44 C45 C46 121.1(3) . . ?
C47 C45 C46 120.9(3) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 C48 121.3(3) . . ?
C45 C47 H47 119.3 . . ?
C48 C47 H47 119.3 . . ?
C42 C48 C47 120.2(2) . . ?
C42 C48 H48 119.9 . . ?
C47 C48 H48 119.9 . . ?
N3 C49 O4 118.9(3) . . ?
N3 C49 C50 134.7(3) . . ?
O4 C49 C50 106.4(2) . . ?
C51 C50 C49 115.2(2) . . ?
C51 C50 C40 116.5(2) . . ?
C49 C50 C40 100.4(2) . . ?
C51 C50 C16 116.9(2) . . ?
C49 C50 C16 107.0(2) . . ?
C40 C50 C16 98.43(19) . . ?
O5 C51 O6 123.2(3) . . ?
O5 C51 C50 124.3(3) . . ?
O6 C51 C50 112.4(3) . . ?
C8 N1 C15 110.5(2) . . ?
C8 N1 C7 124.7(3) . . ?
C15 N1 C7 124.3(3) . . ?
C32 N2 C39 110.7(2) . . ?
C32 N2 C31 124.6(3) . . ?
C39 N2 C31 124.6(3) . . ?
C49 N3 H3B 109(2) . . ?
C49 O4 C41 107.48(18) . . ?
O6 C52 C53 119.7(8) . . ?
O6 C52 H52A 107.4 . . ?
C53 C52 H52A 107.4 . . ?
O6 C52 H52B 107.4 . . ?
C53 C52 H52B 107.4 . . ?
H52A C52 H52B 106.9 . . ?
C53' C52' O6 97.9(10) . . ?
C53' C52' H52C 112.2 . . ?
O6 C52' H52C 112.2 . . ?
C53' C52' H52D 112.2 . . ?
O6 C52' H52D 112.2 . . ?
H52C C52' H52D 109.8 . . ?
C52' C53' H53D 109.5 . . ?
C52' C53' H53E 109.5 . . ?
H53D C53' H53E 109.5 . . ?
C52' C53' H53F 109.5 . . ?
H53D C53' H53F 109.5 . . ?
H53E C53' H53F 109.5 . . ?
C51 O6 C52 114.7(5) . . ?
C51 O6 C52' 114.6(6) . . ?
C52 O6 C52' 33.3(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3B O5 0.88(4) 2.60(4) 3.098(4) 117(3) .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.054

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 403 81 ' '
_platon_squeeze_details          
; 
;
_database_code_depnum_ccdc_archive 'CCDC 1009898'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H19 N3 O3'
_chemical_formula_sum            'C22 H19 N3 O3'
_chemical_formula_weight         373.40

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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.5200(11)
_cell_length_b                   11.3170(12)
_cell_length_c                   20.585(2)
_cell_angle_alpha                95.648(3)
_cell_angle_beta                 102.202(3)
_cell_angle_gamma                112.343(3)
_cell_volume                     1965.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7682
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      24.62

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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_reflns_number            31862
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.03
_diffrn_reflns_theta_max         27.63
_reflns_number_total             9155
_reflns_number_gt                4582
_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)+(0.0933P)²+1.0564P] 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         9070
_refine_ls_number_parameters     507
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1682
_refine_ls_R_factor_gt           0.0806
_refine_ls_wR_factor_ref         0.2298
_refine_ls_wR_factor_gt          0.1887
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
C1 C 0.5754(4) 0.0749(4) 0.41240(19) 0.0704(9) Uani 1 1 d . . .
H1 H 0.5083 -0.0117 0.3933 0.084 Uiso 1 1 calc R . .
C2 C 0.6765(5) 0.1055(5) 0.4760(2) 0.0923(12) Uani 1 1 d . . .
H2 H 0.6775 0.0399 0.4998 0.111 Uiso 1 1 calc R . .
C3 C 0.7747(6) 0.2312(7) 0.5039(3) 0.1124(16) Uani 1 1 d . . .
H3 H 0.8426 0.2516 0.5471 0.135 Uiso 1 1 calc R . .
C4 C 0.7753(5) 0.3288(5) 0.4694(3) 0.1142(17) Uani 1 1 d . . .
H4 H 0.8442 0.4148 0.4889 0.137 Uiso 1 1 calc R . .
C5 C 0.6727(4) 0.2991(4) 0.4050(2) 0.0839(11) Uani 1 1 d . . .
H5 H 0.6721 0.3652 0.3815 0.101 Uiso 1 1 calc R . .
C6 C 0.5721(3) 0.1716(3) 0.37625(17) 0.0579(8) Uani 1 1 d . . .
C7 C 0.4599(4) 0.1383(3) 0.30702(16) 0.0576(8) Uani 1 1 d . . .
H7A H 0.5194 0.1724 0.2751 0.069 Uiso 1 1 calc R . .
H7B H 0.4075 0.0443 0.2926 0.069 Uiso 1 1 calc R . .
C8 C 0.3463(4) 0.2983(3) 0.27947(15) 0.0511(7) Uani 1 1 d . . .
C9 C 0.1997(3) 0.3185(3) 0.28509(15) 0.0479(7) Uani 1 1 d . . .
H9 H 0.1289 0.2945 0.2392 0.057 Uiso 1 1 calc R . .
C10 C 0.1258(3) 0.2163(3) 0.32353(14) 0.0479(7) Uani 1 1 d . . .
C11 C -0.0084(4) 0.1845(3) 0.34520(18) 0.0647(9) Uani 1 1 d . . .
H11 H -0.0677 0.2336 0.3393 0.078 Uiso 1 1 calc R . .
C12 C -0.0535(4) 0.0779(4) 0.37594(19) 0.0731(10) Uani 1 1 d . . .
H12 H -0.1436 0.0557 0.3913 0.088 Uiso 1 1 calc R . .
C13 C 0.0330(4) 0.0045(3) 0.38411(17) 0.0650(9) Uani 1 1 d . . .
H13 H 0.0004 -0.0667 0.4049 0.078 Uiso 1 1 calc R . .
C14 C 0.1670(4) 0.0344(3) 0.36210(15) 0.0532(7) Uani 1 1 d . . .
H14 H 0.2251 -0.0158 0.3673 0.064 Uiso 1 1 calc R . .
C15 C 0.2115(3) 0.1412(2) 0.33211(14) 0.0441(7) Uani 1 1 d . . .
C16 C 0.2355(4) 0.4608(3) 0.31340(15) 0.0495(7) Uani 1 1 d . . .
H16 H 0.1396 0.4632 0.3226 0.059 Uiso 1 1 calc R . .
C17 C 0.3640(5) 0.5121(3) 0.37933(16) 0.0663(10) Uani 1 1 d . . .
C18 C 0.5618(6) 0.6977(5) 0.4587(2) 0.1059(15) Uani 1 1 d . . .
H18A H 0.5537 0.7742 0.4803 0.127 Uiso 1 1 calc R . .
H18B H 0.5511 0.6373 0.4896 0.127 Uiso 1 1 calc R . .
C19 C 0.7089(7) 0.7339(7) 0.4455(3) 0.173(3) Uani 1 1 d . . .
H19A H 0.7240 0.6571 0.4314 0.259 Uiso 1 1 calc R . .
H19B H 0.7903 0.7860 0.4858 0.259 Uiso 1 1 calc R . .
H19C H 0.7135 0.7833 0.4101 0.259 Uiso 1 1 calc R . .
C20 C 0.2828(3) 0.5509(3) 0.26216(14) 0.0477(7) Uani 1 1 d . . .
H20 H 0.3911 0.5666 0.2616 0.057 Uiso 1 1 calc R . .
C21 C 0.2767(4) 0.6778(3) 0.28019(16) 0.0556(8) Uani 1 1 d . . .
C22 C 0.1797(4) 0.4907(3) 0.19314(19) 0.0611(8) Uani 1 1 d . . .
C23 C 0.4469(4) 0.9650(3) 0.0936(2) 0.0690(9) Uani 1 1 d . . .
H23 H 0.5077 1.0542 0.1074 0.083 Uiso 1 1 calc R . .
C24 C 0.3337(5) 0.9180(4) 0.0324(2) 0.0838(11) Uani 1 1 d . . .
H24 H 0.3188 0.9754 0.0052 0.101 Uiso 1 1 calc R . .
C25 C 0.2428(5) 0.7871(4) 0.0114(2) 0.0864(12) Uani 1 1 d . . .
H25 H 0.1668 0.7551 -0.0301 0.104 Uiso 1 1 calc R . .
C26 C 0.2652(5) 0.7033(4) 0.0524(2) 0.0910(13) Uani 1 1 d . . .
H26 H 0.2023 0.6144 0.0390 0.109 Uiso 1 1 calc R . .
C27 C 0.3791(4) 0.7498(3) 0.1128(2) 0.0747(10) Uani 1 1 d . . .
H27 H 0.3949 0.6920 0.1395 0.090 Uiso 1 1 calc R . .
C28 C 0.4715(3) 0.8821(3) 0.13465(16) 0.0524(7) Uani 1 1 d . . .
C29 C 0.5948(4) 0.9321(3) 0.20176(16) 0.0562(8) Uani 1 1 d . . .
H29A H 0.6396 1.0266 0.2112 0.067 Uiso 1 1 calc R . .
H29B H 0.5451 0.9027 0.2372 0.067 Uiso 1 1 calc R . .
C30 C 0.7294(3) 0.7864(3) 0.23139(14) 0.0453(7) Uani 1 1 d . . .
C31 C 0.8781(3) 0.7717(2) 0.22319(13) 0.0416(6) Uani 1 1 d . . .
H31 H 0.9502 0.7900 0.2683 0.050 Uiso 1 1 calc R . .
C32 C 0.9480(3) 0.8803(2) 0.18695(13) 0.0417(6) Uani 1 1 d . . .
C33 C 1.0820(3) 0.9206(3) 0.16518(16) 0.0541(8) Uani 1 1 d . . .
H33 H 1.1481 0.8772 0.1713 0.065 Uiso 1 1 calc R . .
C34 C 1.1172(4) 1.0275(3) 0.13378(17) 0.0628(9) Uani 1 1 d . . .
H34 H 1.2082 1.0562 0.1190 0.075 Uiso 1 1 calc R . .
C35 C 1.0200(4) 1.0914(3) 0.12422(17) 0.0605(8) Uani 1 1 d . . .
H35 H 1.0461 1.1625 0.1029 0.073 Uiso 1 1 calc R . .
C36 C 0.8842(4) 1.0525(3) 0.14553(15) 0.0527(7) Uani 1 1 d . . .
H36 H 0.8181 1.0958 0.1391 0.063 Uiso 1 1 calc R . .
C37 C 0.8506(3) 0.9463(2) 0.17692(13) 0.0427(6) Uani 1 1 d . . .
C38 C 0.8438(3) 0.6339(2) 0.18645(14) 0.0434(6) Uani 1 1 d . . .
H38 H 0.9439 0.6310 0.1837 0.052 Uiso 1 1 calc R . .
C39 C 0.7398(4) 0.6055(3) 0.11554(15) 0.0526(7) Uani 1 1 d . . .
C40 C 0.7396(5) 0.6317(4) 0.00189(17) 0.0901(12) Uani 1 1 d . . .
H40A H 0.6415 0.5539 -0.0113 0.108 Uiso 1 1 calc R . .
H40B H 0.8033 0.6237 -0.0279 0.108 Uiso 1 1 calc R . .
C41 C 0.7053(7) 0.7465(5) -0.0058(2) 0.1168(17) Uani 1 1 d . . .
H41A H 0.6295 0.7471 0.0182 0.175 Uiso 1 1 calc R . .
H41B H 0.6635 0.7431 -0.0530 0.175 Uiso 1 1 calc R . .
H41C H 0.8007 0.8242 0.0122 0.175 Uiso 1 1 calc R . .
C42 C 0.7632(3) 0.5276(3) 0.22465(15) 0.0495(7) Uani 1 1 d . . .
H42 H 0.6596 0.5264 0.2245 0.059 Uiso 1 1 calc R . .
C43 C 0.8545(4) 0.5537(3) 0.2946(2) 0.0692(9) Uani 1 1 d . . .
C44 C 0.7403(5) 0.3981(3) 0.1933(2) 0.0775(11) Uani 1 1 d . . .
N1 N 0.3412(3) 0.1905(2) 0.30505(12) 0.0479(6) Uani 1 1 d . . .
N2 N 0.0987(4) 0.4440(3) 0.14012(18) 0.0928(11) Uani 1 1 d . . .
N3 N 0.2655(4) 0.7739(3) 0.29137(16) 0.0786(9) Uani 1 1 d . . .
N4 N 0.7216(3) 0.8889(2) 0.20367(11) 0.0460(6) Uani 1 1 d . . .
N5 N 0.9291(5) 0.5723(4) 0.3481(2) 0.1165(14) Uani 1 1 d . . .
N6 N 0.7250(6) 0.2972(3) 0.1707(3) 0.1344(17) Uani 1 1 d . . .
O1 O 0.4495(3) 0.3655(2) 0.25566(13) 0.0710(7) Uani 1 1 d . . .
O2 O 0.3993(6) 0.4457(3) 0.41340(17) 0.170(2) Uani 1 1 d . . .
O3 O 0.4347(3) 0.6361(3) 0.39562(13) 0.1017(10) Uani 1 1 d . . .
O4 O 0.6337(3) 0.7191(2) 0.25870(11) 0.0610(6) Uani 1 1 d . . .
O5 O 0.5996(3) 0.5586(3) 0.10252(12) 0.0865(8) Uani 1 1 d . . .
O6 O 0.8234(3) 0.6415(2) 0.07191(11) 0.0732(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.372(5) . ?
C1 C6 1.389(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.352(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.375(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.503(4) . ?
C7 N1 1.455(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O1 1.222(3) . ?
C8 N1 1.364(4) . ?
C8 C9 1.523(4) . ?
C9 C10 1.502(4) . ?
C9 C16 1.538(4) . ?
C9 H9 0.9800 . ?
C10 C11 1.372(4) . ?
C10 C15 1.384(4) . ?
C11 C12 1.382(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.373(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.376(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.375(4) . ?
C14 H14 0.9300 . ?
C15 N1 1.405(3) . ?
C16 C17 1.509(4) . ?
C16 C20 1.555(4) . ?
C16 H16 0.9800 . ?
C17 O2 1.170(4) . ?
C17 O3 1.275(4) . ?
C18 C19 1.398(7) . ?
C18 O3 1.467(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C22 1.469(5) . ?
C20 C21 1.474(4) . ?
C20 H20 0.9800 . ?
C21 N3 1.139(4) . ?
C22 N2 1.134(4) . ?
C23 C28 1.374(4) . ?
C23 C24 1.375(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.367(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.376(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.365(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.385(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.504(4) . ?
C29 N4 1.459(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 O4 1.224(3) . ?
C30 N4 1.362(3) . ?
C30 C31 1.528(4) . ?
C31 C32 1.509(4) . ?
C31 C38 1.546(4) . ?
C31 H31 0.9800 . ?
C32 C33 1.370(4) . ?
C32 C37 1.392(4) . ?
C33 C34 1.390(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.371(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.379(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.383(4) . ?
C36 H36 0.9300 . ?
C37 N4 1.408(3) . ?
C38 C39 1.506(4) . ?
C38 C42 1.547(4) . ?
C38 H38 0.9800 . ?
C39 O5 1.190(4) . ?
C39 O6 1.317(4) . ?
C40 O6 1.463(4) . ?
C40 C41 1.470(6) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C43 1.452(5) . ?
C42 C44 1.457(4) . ?
C42 H42 0.9800 . ?
C43 N5 1.128(4) . ?
C44 N6 1.132(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 120.8(4) . . ?
C2 C1 H1 119.6 . . ?
C6 C1 H1 119.6 . . ?
C3 C2 C1 119.8(5) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 120.8(5) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C5 119.9(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.7(4) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 118.9(3) . . ?
C5 C6 C7 120.2(3) . . ?
C1 C6 C7 120.8(3) . . ?
N1 C7 C6 112.9(2) . . ?
N1 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
N1 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
O1 C8 N1 125.8(3) . . ?
O1 C8 C9 126.4(3) . . ?
N1 C8 C9 107.8(2) . . ?
C10 C9 C8 102.7(2) . . ?
C10 C9 C16 118.2(2) . . ?
C8 C9 C16 113.0(2) . . ?
C10 C9 H9 107.5 . . ?
C8 C9 H9 107.5 . . ?
C16 C9 H9 107.5 . . ?
C11 C10 C15 119.8(3) . . ?
C11 C10 C9 131.6(3) . . ?
C15 C10 C9 108.4(2) . . ?
C10 C11 C12 118.6(3) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
C13 C12 C11 120.8(3) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 121.3(3) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C13 117.3(3) . . ?
C15 C14 H14 121.3 . . ?
C13 C14 H14 121.3 . . ?
C14 C15 C10 122.1(3) . . ?
C14 C15 N1 128.2(3) . . ?
C10 C15 N1 109.7(2) . . ?
C17 C16 C9 110.8(2) . . ?
C17 C16 C20 109.8(2) . . ?
C9 C16 C20 112.2(2) . . ?
C17 C16 H16 108.0 . . ?
C9 C16 H16 108.0 . . ?
C20 C16 H16 108.0 . . ?
O2 C17 O3 121.3(3) . . ?
O2 C17 C16 123.9(3) . . ?
O3 C17 C16 114.8(3) . . ?
C19 C18 O3 110.5(4) . . ?
C19 C18 H18A 109.6 . . ?
O3 C18 H18A 109.6 . . ?
C19 C18 H18B 109.6 . . ?
O3 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C20 C21 107.2(2) . . ?
C22 C20 C16 111.8(2) . . ?
C21 C20 C16 112.8(2) . . ?
C22 C20 H20 108.3 . . ?
C21 C20 H20 108.3 . . ?
C16 C20 H20 108.3 . . ?
N3 C21 C20 176.5(3) . . ?
N2 C22 C20 179.3(4) . . ?
C28 C23 C24 120.9(3) . . ?
C28 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C25 C24 C23 120.3(4) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C26 119.3(4) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C27 C26 C25 120.4(4) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C28 120.8(3) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C23 C28 C27 118.2(3) . . ?
C23 C28 C29 121.6(3) . . ?
C27 C28 C29 120.2(3) . . ?
N4 C29 C28 112.9(2) . . ?
N4 C29 H29A 109.0 . . ?
C28 C29 H29A 109.0 . . ?
N4 C29 H29B 109.0 . . ?
C28 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
O4 C30 N4 125.4(3) . . ?
O4 C30 C31 126.4(3) . . ?
N4 C30 C31 108.3(2) . . ?
C32 C31 C30 102.5(2) . . ?
C32 C31 C38 115.1(2) . . ?
C30 C31 C38 112.9(2) . . ?
C32 C31 H31 108.7 . . ?
C30 C31 H31 108.7 . . ?
C38 C31 H31 108.7 . . ?
C33 C32 C37 119.6(3) . . ?
C33 C32 C31 132.0(2) . . ?
C37 C32 C31 108.3(2) . . ?
C32 C33 C34 118.6(3) . . ?
C32 C33 H33 120.7 . . ?
C34 C33 H33 120.7 . . ?
C35 C34 C33 121.1(3) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C34 C35 C36 121.4(3) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 H35 119.3 . . ?
C35 C36 C37 117.1(3) . . ?
C35 C36 H36 121.5 . . ?
C37 C36 H36 121.5 . . ?
C36 C37 C32 122.2(3) . . ?
C36 C37 N4 128.0(2) . . ?
C32 C37 N4 109.7(2) . . ?
C39 C38 C31 109.9(2) . . ?
C39 C38 C42 109.3(2) . . ?
C31 C38 C42 111.9(2) . . ?
C39 C38 H38 108.6 . . ?
C31 C38 H38 108.6 . . ?
C42 C38 H38 108.6 . . ?
O5 C39 O6 125.7(3) . . ?
O5 C39 C38 122.6(3) . . ?
O6 C39 C38 111.6(3) . . ?
O6 C40 C41 111.3(3) . . ?
O6 C40 H40A 109.4 . . ?
C41 C40 H40A 109.4 . . ?
O6 C40 H40B 109.4 . . ?
C41 C40 H40B 109.4 . . ?
H40A C40 H40B 108.0 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C44 107.4(3) . . ?
C43 C42 C38 111.7(2) . . ?
C44 C42 C38 112.5(3) . . ?
C43 C42 H42 108.4 . . ?
C44 C42 H42 108.4 . . ?
C38 C42 H42 108.4 . . ?
N5 C43 C42 177.4(4) . . ?
N6 C44 C42 178.0(5) . . ?
C8 N1 C15 111.1(2) . . ?
C8 N1 C7 124.0(2) . . ?
C15 N1 C7 124.9(2) . . ?
C30 N4 C37 111.1(2) . . ?
C30 N4 C29 124.0(2) . . ?
C37 N4 C29 124.9(2) . . ?
C17 O3 C18 119.9(3) . . ?
C39 O6 C40 118.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.63
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.060
_database_code_depnum_ccdc_archive 'CCDC 1009899'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H21 N3 O3'
_chemical_formula_sum            'C26 H21 N3 O3'
_chemical_formula_weight         423.46

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'
_symmetry_space_group_name_Hall  '-P 1'


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

_cell_length_a                   9.7982(14)
_cell_length_b                   10.5620(14)
_cell_length_c                   11.3755(15)
_cell_angle_alpha                84.953(4)
_cell_angle_beta                 81.586(4)
_cell_angle_gamma                79.358(4)
_cell_volume                     1142.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7466
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      27.28

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             444
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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            17361
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         27.58
_reflns_number_total             5285
_reflns_number_gt                3616
_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)+(0.0601P)²+0.1809P] 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         5185
_refine_ls_number_parameters     290
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1307
_refine_ls_wR_factor_gt          0.1205
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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
C1 C 0.2737(2) 0.25212(18) 1.22949(15) 0.0555(5) Uani 1 1 d . . .
H1 H 0.2653 0.3308 1.2631 0.067 Uiso 1 1 calc R . .
C2 C 0.2170(2) 0.1529(2) 1.29414(17) 0.0688(6) Uani 1 1 d . . .
H2 H 0.1721 0.1647 1.3712 0.083 Uiso 1 1 calc R . .
C3 C 0.2267(3) 0.0382(2) 1.2456(2) 0.0756(6) Uani 1 1 d . . .
H3A H 0.1874 -0.0280 1.2890 0.091 Uiso 1 1 calc R . .
C4 C 0.2943(3) 0.0202(2) 1.1326(2) 0.0763(6) Uani 1 1 d . . .
H4 H 0.3009 -0.0585 1.0994 0.092 Uiso 1 1 calc R . .
C5 C 0.3525(2) 0.11788(17) 1.06790(17) 0.0570(5) Uani 1 1 d . . .
H5 H 0.3989 0.1045 0.9915 0.068 Uiso 1 1 calc R . .
C6 C 0.34280(16) 0.23582(15) 1.11536(14) 0.0421(4) Uani 1 1 d . . .
C7 C 0.40209(17) 0.34367(16) 1.04177(15) 0.0467(4) Uani 1 1 d . . .
H7A H 0.4349 0.3962 1.0938 0.056 Uiso 1 1 calc R . .
H7B H 0.4819 0.3072 0.9866 0.056 Uiso 1 1 calc R . .
C8 C 0.26961(16) 0.39249(15) 0.86950(13) 0.0402(4) Uani 1 1 d . . .
C9 C 0.15229(15) 0.49461(14) 0.82804(12) 0.0365(3) Uani 1 1 d . . .
H9 H 0.0685 0.4545 0.8370 0.044 Uiso 1 1 calc R . .
C10 C 0.12837(15) 0.59090(14) 0.92263(12) 0.0363(3) Uani 1 1 d . . .
C11 C 0.03751(17) 0.70641(16) 0.93625(14) 0.0455(4) Uani 1 1 d . . .
H11 H -0.0219 0.7386 0.8798 0.055 Uiso 1 1 calc R . .
C12 C 0.0364(2) 0.77385(17) 1.03585(16) 0.0551(5) Uani 1 1 d . . .
H12 H -0.0235 0.8525 1.0459 0.066 Uiso 1 1 calc R . .
C13 C 0.1235(2) 0.72487(18) 1.11991(16) 0.0559(5) Uani 1 1 d . . .
H13 H 0.1208 0.7713 1.1862 0.067 Uiso 1 1 calc R . .
C14 C 0.21473(19) 0.60871(17) 1.10855(15) 0.0494(4) Uani 1 1 d . . .
H14 H 0.2727 0.5759 1.1660 0.059 Uiso 1 1 calc R . .
C15 C 0.21617(16) 0.54349(15) 1.00849(13) 0.0380(3) Uani 1 1 d . . .
C16 C 0.17582(15) 0.54744(14) 0.69774(12) 0.0347(3) Uani 1 1 d . . .
H16 H 0.0892 0.6036 0.6794 0.042 Uiso 1 1 calc R . .
C17 C 0.21437(16) 0.44129(15) 0.60787(13) 0.0388(3) Uani 1 1 d . . .
H17 H 0.2800 0.3709 0.6418 0.047 Uiso 1 1 calc R . .
C18 C 0.09916(18) 0.38555(15) 0.57831(14) 0.0436(4) Uani 1 1 d . . .
C19 C 0.29633(16) 0.50424(16) 0.50049(14) 0.0420(4) Uani 1 1 d . . .
C20 C 0.29841(15) 0.62444(14) 0.66424(12) 0.0356(3) Uani 1 1 d . . .
C21 C 0.25802(16) 0.76793(15) 0.68418(13) 0.0376(3) Uani 1 1 d . . .
C22 C 0.3090(2) 0.82145(18) 0.77144(15) 0.0532(4) Uani 1 1 d . . .
H22 H 0.3694 0.7697 0.8191 0.064 Uiso 1 1 calc R . .
C23 C 0.2703(3) 0.9522(2) 0.78816(19) 0.0718(6) Uani 1 1 d . . .
H23 H 0.3046 0.9877 0.8474 0.086 Uiso 1 1 calc R . .
C24 C 0.1825(2) 1.02933(19) 0.71877(19) 0.0695(6) Uani 1 1 d . . .
H24 H 0.1572 1.1171 0.7304 0.083 Uiso 1 1 calc R . .
C25 C 0.1317(2) 0.97736(18) 0.63204(18) 0.0606(5) Uani 1 1 d . . .
H25 H 0.0716 1.0300 0.5847 0.073 Uiso 1 1 calc R . .
C26 C 0.16858(18) 0.84800(17) 0.61402(15) 0.0490(4) Uani 1 1 d . . .
H26 H 0.1335 0.8137 0.5545 0.059 Uiso 1 1 calc R . .
N1 N 0.29879(14) 0.42542(12) 0.97478(11) 0.0409(3) Uani 1 1 d . . .
N2 N 0.01189(18) 0.33836(16) 0.55695(15) 0.0648(4) Uani 1 1 d . . .
N3 N 0.33595(13) 0.60534(13) 0.53788(11) 0.0409(3) Uani 1 1 d . . .
H3C H 0.3809 0.6563 0.4906 0.049 Uiso 1 1 calc R . .
O1 O 0.32565(13) 0.29304(11) 0.82211(10) 0.0535(3) Uani 1 1 d . . .
O2 O 0.32390(12) 0.46411(13) 0.40034(10) 0.0572(3) Uani 1 1 d . . .
O3 O 0.40748(11) 0.56406(11) 0.72911(9) 0.0443(3) Uani 1 1 d . . .
H3B H 0.4831 0.5647 0.6875 0.066 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
C1 C2 1.381(3) . ?
C1 C6 1.383(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.357(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.370(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.375(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.383(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.507(2) . ?
C7 N1 1.462(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O1 1.2229(18) . ?
C8 N1 1.3591(19) . ?
C8 C9 1.523(2) . ?
C9 C10 1.509(2) . ?
C9 C16 1.537(2) . ?
C9 H9 0.9800 . ?
C10 C11 1.377(2) . ?
C10 C15 1.395(2) . ?
C11 C12 1.388(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.378(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.382(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.378(2) . ?
C14 H14 0.9300 . ?
C15 N1 1.406(2) . ?
C16 C17 1.542(2) . ?
C16 C20 1.556(2) . ?
C16 H16 0.9800 . ?
C17 C18 1.458(2) . ?
C17 C19 1.532(2) . ?
C17 H17 0.9800 . ?
C18 N2 1.131(2) . ?
C19 O2 1.2260(18) . ?
C19 N3 1.324(2) . ?
C20 O3 1.4105(17) . ?
C20 N3 1.4529(18) . ?
C20 C21 1.522(2) . ?
C21 C22 1.379(2) . ?
C21 C26 1.390(2) . ?
C22 C23 1.385(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.361(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.364(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.373(2) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
N3 H3C 0.8600 . ?
O3 H3B 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 120.76(17) . . ?
C2 C1 H1 119.6 . . ?
C6 C1 H1 119.6 . . ?
C3 C2 C1 120.26(19) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 C4 119.91(19) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 C5 120.29(19) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 120.70(18) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 118.07(16) . . ?
C5 C6 C7 120.12(15) . . ?
C1 C6 C7 121.77(15) . . ?
N1 C7 C6 112.20(13) . . ?
N1 C7 H7A 109.2 . . ?
C6 C7 H7A 109.2 . . ?
N1 C7 H7B 109.2 . . ?
C6 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
O1 C8 N1 123.93(14) . . ?
O1 C8 C9 127.45(14) . . ?
N1 C8 C9 108.52(13) . . ?
C10 C9 C8 102.35(11) . . ?
C10 C9 C16 117.04(12) . . ?
C8 C9 C16 116.19(12) . . ?
C10 C9 H9 106.9 . . ?
C8 C9 H9 106.9 . . ?
C16 C9 H9 106.9 . . ?
C11 C10 C15 119.95(14) . . ?
C11 C10 C9 131.60(14) . . ?
C15 C10 C9 108.42(13) . . ?
C10 C11 C12 118.71(16) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C13 C12 C11 120.36(17) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 121.92(16) . . ?
C12 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C15 C14 C13 117.16(16) . . ?
C15 C14 H14 121.4 . . ?
C13 C14 H14 121.4 . . ?
C14 C15 C10 121.89(15) . . ?
C14 C15 N1 128.75(15) . . ?
C10 C15 N1 109.37(12) . . ?
C9 C16 C17 113.56(12) . . ?
C9 C16 C20 116.19(11) . . ?
C17 C16 C20 101.95(11) . . ?
C9 C16 H16 108.3 . . ?
C17 C16 H16 108.2 . . ?
C20 C16 H16 108.3 . . ?
C18 C17 C19 113.97(12) . . ?
C18 C17 C16 116.60(13) . . ?
C19 C17 C16 103.71(12) . . ?
C18 C17 H17 107.4 . . ?
C19 C17 H17 107.4 . . ?
C16 C17 H17 107.4 . . ?
N2 C18 C17 177.65(18) . . ?
O2 C19 N3 127.15(16) . . ?
O2 C19 C17 125.62(15) . . ?
N3 C19 C17 107.18(13) . . ?
O3 C20 N3 111.16(12) . . ?
O3 C20 C21 111.82(11) . . ?
N3 C20 C21 110.09(12) . . ?
O3 C20 C16 107.15(11) . . ?
N3 C20 C16 101.92(11) . . ?
C21 C20 C16 114.29(12) . . ?
C22 C21 C26 118.57(15) . . ?
C22 C21 C20 121.12(14) . . ?
C26 C21 C20 120.31(13) . . ?
C21 C22 C23 120.04(17) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.68(17) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 119.72(18) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C24 C25 C26 120.58(18) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C21 120.41(16) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
C8 N1 C15 111.25(12) . . ?
C8 N1 C7 122.33(13) . . ?
C15 N1 C7 126.41(13) . . ?
C19 N3 C20 115.47(13) . . ?
C19 N3 H3C 122.3 . . ?
C20 N3 H3C 122.3 . . ?
C20 O3 H3B 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3B O2 0.82 1.99 2.7997(16) 170.0 2_666

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.038


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 1.000 0.500 132 36 ' '
_platon_squeeze_details          
; 
;
_database_code_depnum_ccdc_archive 'CCDC 1009900'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H22 Cl N3 O3'
_chemical_formula_sum            'C27 H22 Cl N3 O3'
_chemical_formula_weight         471.93

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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


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

_cell_length_a                   9.893(5)
_cell_length_b                   10.872(6)
_cell_length_c                   13.772(7)
_cell_angle_alpha                84.911(16)
_cell_angle_beta                 70.201(15)
_cell_angle_gamma                80.210(16)
_cell_volume                     1372.6(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2870
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      21.28

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             492
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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_reflns_number            20479
_diffrn_reflns_av_R_equivalents  0.1223
_diffrn_reflns_av_sigmaI/netI    0.2150
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         27.63
_reflns_number_total             6384
_reflns_number_gt                2240
_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)+(0.0861P)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_number_reflns         6297
_refine_ls_number_parameters     309
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2177
_refine_ls_R_factor_gt           0.0791
_refine_ls_wR_factor_ref         0.2168
_refine_ls_wR_factor_gt          0.1841
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_restrained_S_all      0.921
_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
C1 C 0.1384(4) 0.6992(4) 1.2113(3) 0.0658(11) Uani 1 1 d . . .
H1 H 0.1372 0.7417 1.1498 0.079 Uiso 1 1 calc R . .
C2 C 0.0463(6) 0.7486(5) 1.3040(5) 0.1024(17) Uani 1 1 d . . .
H2 H -0.0142 0.8241 1.3040 0.123 Uiso 1 1 calc R . .
C3 C 0.0438(7) 0.6884(8) 1.3942(5) 0.128(3) Uani 1 1 d . . .
H3 H -0.0207 0.7205 1.4561 0.153 Uiso 1 1 calc R . .
C4 C 0.1375(8) 0.5785(8) 1.3941(4) 0.117(2) Uani 1 1 d . . .
H4 H 0.1390 0.5391 1.4566 0.141 Uiso 1 1 calc R . .
C5 C 0.2321(5) 0.5247(4) 1.2997(3) 0.0728(12) Uani 1 1 d . . .
H5 H 0.2923 0.4490 1.2994 0.087 Uiso 1 1 calc R . .
C6 C 0.2313(4) 0.5894(3) 1.2076(3) 0.0469(9) Uani 1 1 d . . .
C7 C 0.3307(4) 0.5386(3) 1.1073(2) 0.0483(9) Uani 1 1 d . . .
H7A H 0.3764 0.6059 1.0648 0.058 Uiso 1 1 calc R . .
H7B H 0.4068 0.4773 1.1202 0.058 Uiso 1 1 calc R . .
C8 C 0.2155(4) 0.3672(3) 1.0770(3) 0.0444(9) Uani 1 1 d . . .
C9 C 0.1499(3) 0.3336(3) 1.0014(2) 0.0375(8) Uani 1 1 d . . .
H9 H 0.0451 0.3389 1.0372 0.045 Uiso 1 1 calc R . .
C10 C 0.1718(3) 0.4405(3) 0.9219(2) 0.0367(8) Uani 1 1 d . . .
C11 C 0.1412(3) 0.4644(3) 0.8329(2) 0.0422(8) Uani 1 1 d . . .
H11 H 0.0975 0.4078 0.8113 0.051 Uiso 1 1 calc R . .
C12 C 0.1742(4) 0.5731(3) 0.7728(2) 0.0506(9) Uani 1 1 d . . .
C13 C 0.1431(5) 0.5981(4) 0.6732(3) 0.0733(12) Uani 1 1 d . . .
H13A H 0.1721 0.5230 0.6348 0.110 Uiso 1 1 calc R . .
H13B H 0.1963 0.6621 0.6335 0.110 Uiso 1 1 calc R . .
H13C H 0.0409 0.6252 0.6873 0.110 Uiso 1 1 calc R . .
C14 C 0.2363(4) 0.6573(3) 0.8095(3) 0.0552(10) Uani 1 1 d . . .
H14 H 0.2565 0.7310 0.7714 0.066 Uiso 1 1 calc R . .
C15 C 0.2690(4) 0.6353(3) 0.9006(3) 0.0477(9) Uani 1 1 d . . .
H15 H 0.3118 0.6918 0.9231 0.057 Uiso 1 1 calc R . .
C16 C 0.2355(3) 0.5260(3) 0.9564(2) 0.0391(8) Uani 1 1 d . . .
C17 C 0.2043(3) 0.2013(3) 0.9571(2) 0.0409(8) Uani 1 1 d . . .
H17 H 0.1444 0.1873 0.9163 0.049 Uiso 1 1 calc R . .
C18 C 0.3654(3) 0.1753(3) 0.8886(2) 0.0407(8) Uani 1 1 d . . .
C19 C 0.3931(4) 0.2065(3) 0.7755(3) 0.0453(9) Uani 1 1 d . . .
C20 C 0.4696(4) 0.3006(3) 0.7253(3) 0.0653(11) Uani 1 1 d . . .
H20 H 0.5061 0.3468 0.7617 0.078 Uiso 1 1 calc R . .
C21 C 0.4932(4) 0.3278(4) 0.6220(3) 0.0764(13) Uani 1 1 d . . .
H21 H 0.5457 0.3917 0.5892 0.092 Uiso 1 1 calc R . .
C22 C 0.4407(5) 0.2626(5) 0.5681(3) 0.0777(13) Uani 1 1 d . . .
C23 C 0.3639(4) 0.1669(4) 0.6153(3) 0.0787(13) Uani 1 1 d . . .
H23 H 0.3275 0.1212 0.5783 0.094 Uiso 1 1 calc R . .
C24 C 0.3422(4) 0.1405(4) 0.7184(3) 0.0639(11) Uani 1 1 d . . .
H24 H 0.2912 0.0755 0.7506 0.077 Uiso 1 1 calc R . .
C25 C 0.3096(4) -0.0077(3) 0.9906(3) 0.0495(9) Uani 1 1 d . . .
C26 C 0.1936(4) 0.0962(3) 1.0417(3) 0.0445(9) Uani 1 1 d . . .
H26 H 0.2218 0.1263 1.0961 0.053 Uiso 1 1 calc R . .
C27 C 0.0493(5) 0.0588(3) 1.0910(3) 0.0535(10) Uani 1 1 d . . .
Cl1 Cl 0.46841(18) 0.29778(17) 0.43647(10) 0.1394(7) Uani 1 1 d . . .
N1 N 0.2595(3) 0.4801(2) 1.04980(19) 0.0410(7) Uani 1 1 d . . .
N2 N -0.0618(4) 0.0294(3) 1.1295(3) 0.0833(11) Uani 1 1 d . . .
N3 N 0.4006(3) 0.0429(2) 0.9058(2) 0.0506(8) Uani 1 1 d . . .
H3A H 0.4750 -0.0012 0.8645 0.061 Uiso 1 1 calc R . .
O1 O 0.2289(3) 0.3063(2) 1.15566(18) 0.0613(7) Uani 1 1 d . . .
O2 O 0.4480(2) 0.2407(2) 0.92823(19) 0.0550(7) Uani 1 1 d . . .
H2A H 0.3961 0.3024 0.9581 0.083 Uiso 1 1 calc R . .
O3 O 0.3221(3) -0.1164(2) 1.0207(2) 0.0657(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.371(5) . ?
C1 C2 1.385(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.346(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.426(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.396(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.486(4) . ?
C7 N1 1.465(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O1 1.253(4) . ?
C8 N1 1.351(4) . ?
C8 C9 1.500(4) . ?
C9 C10 1.515(4) . ?
C9 C17 1.549(4) . ?
C9 H9 0.9800 . ?
C10 C11 1.353(4) . ?
C10 C16 1.402(4) . ?
C11 C12 1.401(5) . ?
C11 H11 0.9300 . ?
C12 C14 1.398(5) . ?
C12 C13 1.497(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.390(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.382(4) . ?
C15 H15 0.9300 . ?
C16 N1 1.420(4) . ?
C17 C18 1.544(4) . ?
C17 C26 1.548(4) . ?
C17 H17 0.9800 . ?
C18 O2 1.428(4) . ?
C18 N3 1.441(4) . ?
C18 C19 1.505(5) . ?
C19 C24 1.370(5) . ?
C19 C20 1.372(5) . ?
C20 C21 1.375(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.343(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.378(6) . ?
C22 Cl1 1.756(4) . ?
C23 C24 1.373(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O3 1.218(4) . ?
C25 N3 1.349(4) . ?
C25 C26 1.498(5) . ?
C26 C27 1.468(5) . ?
C26 H26 0.9800 . ?
C27 N2 1.134(4) . ?
N3 H3A 0.8600 . ?
O2 H2A 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 121.8(4) . . ?
C6 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 120.6(6) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 119.5(5) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C5 121.0(5) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 117.8(5) . . ?
C6 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
C1 C6 C5 119.2(3) . . ?
C1 C6 C7 121.0(3) . . ?
C5 C6 C7 119.8(4) . . ?
N1 C7 C6 114.2(3) . . ?
N1 C7 H7A 108.7 . . ?
C6 C7 H7A 108.7 . . ?
N1 C7 H7B 108.7 . . ?
C6 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
O1 C8 N1 122.1(3) . . ?
O1 C8 C9 128.4(3) . . ?
N1 C8 C9 109.5(3) . . ?
C8 C9 C10 103.3(2) . . ?
C8 C9 C17 116.4(3) . . ?
C10 C9 C17 115.3(2) . . ?
C8 C9 H9 107.1 . . ?
C10 C9 H9 107.1 . . ?
C17 C9 H9 107.1 . . ?
C11 C10 C16 120.1(3) . . ?
C11 C10 C9 133.0(3) . . ?
C16 C10 C9 106.9(3) . . ?
C10 C11 C12 121.1(3) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C14 C12 C11 117.6(3) . . ?
C14 C12 C13 121.4(3) . . ?
C11 C12 C13 121.0(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C12 122.6(3) . . ?
C15 C14 H14 118.7 . . ?
C12 C14 H14 118.7 . . ?
C16 C15 C14 117.4(3) . . ?
C16 C15 H15 121.3 . . ?
C14 C15 H15 121.3 . . ?
C15 C16 C10 121.2(3) . . ?
C15 C16 N1 128.8(3) . . ?
C10 C16 N1 109.9(3) . . ?
C18 C17 C26 102.6(3) . . ?
C18 C17 C9 116.3(2) . . ?
C26 C17 C9 113.2(3) . . ?
C18 C17 H17 108.1 . . ?
C26 C17 H17 108.1 . . ?
C9 C17 H17 108.1 . . ?
O2 C18 N3 109.7(2) . . ?
O2 C18 C19 110.9(3) . . ?
N3 C18 C19 110.6(3) . . ?
O2 C18 C17 108.5(2) . . ?
N3 C18 C17 102.0(2) . . ?
C19 C18 C17 114.7(3) . . ?
C24 C19 C20 117.3(3) . . ?
C24 C19 C18 120.6(3) . . ?
C20 C19 C18 122.1(3) . . ?
C19 C20 C21 121.2(4) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C22 C21 C20 120.3(4) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 120.5(4) . . ?
C21 C22 Cl1 120.7(4) . . ?
C23 C22 Cl1 118.9(4) . . ?
C24 C23 C22 118.4(4) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C19 C24 C23 122.4(4) . . ?
C19 C24 H24 118.8 . . ?
C23 C24 H24 118.8 . . ?
O3 C25 N3 126.3(4) . . ?
O3 C25 C26 127.0(4) . . ?
N3 C25 C26 106.7(3) . . ?
C27 C26 C25 114.1(3) . . ?
C27 C26 C17 115.9(3) . . ?
C25 C26 C17 104.5(3) . . ?
C27 C26 H26 107.3 . . ?
C25 C26 H26 107.3 . . ?
C17 C26 H26 107.3 . . ?
N2 C27 C26 179.6(4) . . ?
C8 N1 C16 110.2(3) . . ?
C8 N1 C7 122.9(3) . . ?
C16 N1 C7 126.7(3) . . ?
C25 N3 C18 115.8(3) . . ?
C25 N3 H3A 122.1 . . ?
C18 N3 H3A 122.1 . . ?
C18 O2 H2A 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A N1 0.82 2.35 3.173(4) 175.9 .

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.63
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.061


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 285 67 ' '
_platon_squeeze_details          
; 
;
#===========================================================

_database_code_depnum_ccdc_archive 'CCDC 1009901'
