# Electronic Supplementary Material (ESI) for Chemical Science.
# 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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#  from this site to visualise CIF-encoded structures and 
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data_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H48 N4 O2'
_chemical_formula_weight         857.02

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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   11.0962(17)
_cell_length_b                   21.800(3)
_cell_length_c                   19.774(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.379(3)
_cell_angle_gamma                90.00
_cell_volume                     4612.0(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1808
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9852
_exptl_absorpt_correction_T_max  0.9852
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            51289
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_sigmaI/netI    0.0944
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         32.09
_reflns_number_total             15183
_reflns_number_gt                8542
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0981P)²+1.2632P] 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         15183
_refine_ls_number_parameters     607
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0721
_refine_ls_wR_factor_ref         0.2139
_refine_ls_wR_factor_gt          0.1811
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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 -0.24579(19) -0.05077(9) 0.78621(10) 0.0184(4) Uani 1 1 d . . .
C2 C -0.23245(19) -0.09289(9) 0.68875(10) 0.0187(4) Uani 1 1 d . . .
C3 C -0.34057(19) -0.11478(9) 0.70235(10) 0.0184(4) Uani 1 1 d . . .
C4 C -0.0359(3) -0.13968(16) 0.53678(15) 0.0494(8) Uani 1 1 d . . .
H4A H 0.0094 -0.1504 0.5052 0.059 Uiso 1 1 calc R . .
C5 C -0.6465(3) -0.22519(12) 0.58951(14) 0.0384(6) Uani 1 1 d . . .
H5A H -0.7146 -0.2484 0.5652 0.046 Uiso 1 1 calc R . .
C6 C -0.0133(3) -0.08474(17) 0.57275(15) 0.0559(9) Uani 1 1 d . . .
H6A H 0.0471 -0.0581 0.5650 0.067 Uiso 1 1 calc R . .
C7 C -0.0806(3) -0.06899(13) 0.62052(13) 0.0408(7) Uani 1 1 d . . .
H7A H -0.0648 -0.0317 0.6441 0.049 Uiso 1 1 calc R . .
C8 C -0.2280(3) 0.15555(11) 0.89296(15) 0.0391(6) Uani 1 1 d . . .
H8A H -0.2142 0.1810 0.9320 0.047 Uiso 1 1 calc R . .
C9 C -0.2555(3) 0.18064(12) 0.82796(16) 0.0468(7) Uani 1 1 d . . .
H9A H -0.2584 0.2231 0.8230 0.056 Uiso 1 1 calc R . .
C10 C -0.1269(3) -0.17861(12) 0.54839(13) 0.0387(6) Uani 1 1 d . . .
H10A H -0.1431 -0.2155 0.5240 0.046 Uiso 1 1 calc R . .
C11 C -0.2800(3) 0.14309(11) 0.76774(14) 0.0390(6) Uani 1 1 d . . .
H11A H -0.3006 0.1610 0.7234 0.047 Uiso 1 1 calc R . .
C12 C -0.5911(3) -0.23670(12) 0.65963(14) 0.0399(6) Uani 1 1 d . . .
H12A H -0.6214 -0.2681 0.6825 0.048 Uiso 1 1 calc R . .
C13 C -0.5999(2) -0.17879(11) 0.55578(13) 0.0337(5) Uani 1 1 d . . .
H13A H -0.6362 -0.1711 0.5085 0.040 Uiso 1 1 calc R . .
C14 C -0.1142(2) -0.12507(11) 0.99403(12) 0.0311(5) Uani 1 1 d . . .
H14A H -0.0944 -0.1665 1.0000 0.037 Uiso 1 1 calc R . .
C15 C -0.1301(2) -0.02641(12) 1.04536(12) 0.0320(5) Uani 1 1 d . . .
H15A H -0.1222 -0.0020 1.0848 0.038 Uiso 1 1 calc R . .
C16 C -0.1035(2) -0.08721(12) 1.05359(13) 0.0342(5) Uani 1 1 d . . .
H16A H -0.0782 -0.1040 1.0984 0.041 Uiso 1 1 calc R . .
C17 C -0.4903(2) -0.20158(10) 0.69612(12) 0.0295(5) Uani 1 1 d . . .
H17A H -0.4536 -0.2097 0.7433 0.035 Uiso 1 1 calc R . .
C18 C -0.1941(2) -0.16340(10) 0.59587(11) 0.0265(5) Uani 1 1 d . . .
H18A H -0.2552 -0.1900 0.6028 0.032 Uiso 1 1 calc R . .
C19 C -0.4992(2) -0.14363(10) 0.59224(12) 0.0266(5) Uani 1 1 d . . .
H19A H -0.4686 -0.1125 0.5692 0.032 Uiso 1 1 calc R . .
C20 C -0.1532(2) -0.10135(10) 0.92807(12) 0.0257(5) Uani 1 1 d . . .
H20A H -0.1594 -0.1269 0.8897 0.031 Uiso 1 1 calc R . .
C21 C -0.1887(2) 0.06361(11) 0.96859(12) 0.0286(5) Uani 1 1 d . . .
H21A H -0.1806 0.0884 1.0078 0.034 Uiso 1 1 calc R . .
C22 C -0.2738(2) 0.08097(10) 0.77392(12) 0.0284(5) Uani 1 1 d . . .
H22A H -0.2919 0.0569 0.7337 0.034 Uiso 1 1 calc R . .
C23 C -0.2197(2) 0.09047(10) 0.90226(12) 0.0272(5) Uani 1 1 d . . .
C24 C -0.1697(2) 0.00060(11) 0.97770(11) 0.0253(5) Uani 1 1 d . . .
C25 C -0.2401(2) 0.05214(9) 0.84104(11) 0.0228(4) Uani 1 1 d . . .
C26 C -0.1710(2) -0.10816(10) 0.63359(11) 0.0221(4) Uani 1 1 d . . .
C27 C -0.4437(2) -0.15456(9) 0.66295(11) 0.0204(4) Uani 1 1 d . . .
C28 C -0.18486(19) -0.03794(10) 0.91670(11) 0.0219(4) Uani 1 1 d . . .
C29 C -0.22325(19) -0.01159(9) 0.84962(11) 0.0195(4) Uani 1 1 d . . .
C31 C 0.13376(19) 0.45199(8) 0.68713(11) 0.0185(4) Uani 1 1 d . . .
C32 C 0.23234(19) 0.37036(8) 0.66263(10) 0.0176(4) Uani 1 1 d . . .
C33 C 0.10791(18) 0.35716(8) 0.65504(10) 0.0173(4) Uani 1 1 d . . .
C34 C 0.5471(2) 0.29383(11) 0.69312(14) 0.0336(5) Uani 1 1 d . . .
H34A H 0.6233 0.2926 0.7271 0.040 Uiso 1 1 calc R . .
C35 C 0.1674(2) 0.60399(10) 0.87749(12) 0.0317(5) Uani 1 1 d . . .
H35A H 0.1682 0.6444 0.8928 0.038 Uiso 1 1 calc R . .
C36 C 0.0465(2) 0.59896(10) 0.53844(13) 0.0308(5) Uani 1 1 d . . .
H36A H 0.0334 0.5907 0.4909 0.037 Uiso 1 1 calc R . .
C37 C 0.5295(2) 0.25843(10) 0.63283(14) 0.0327(5) Uani 1 1 d . . .
H37A H 0.5931 0.2329 0.6269 0.039 Uiso 1 1 calc R . .
C38 C 0.1941(3) 0.55775(11) 0.92525(13) 0.0348(6) Uani 1 1 d . . .
H38A H 0.2134 0.5668 0.9729 0.042 Uiso 1 1 calc R . .
C39 C 0.1927(2) 0.49572(11) 0.90308(13) 0.0316(5) Uani 1 1 d . . .
H39A H 0.2091 0.4645 0.9363 0.038 Uiso 1 1 calc R . .
C40 C 0.0328(2) 0.18767(10) 0.64319(13) 0.0302(5) Uani 1 1 d . . .
H40A H 0.0738 0.1504 0.6545 0.036 Uiso 1 1 calc R . .
C41 C -0.0955(2) 0.18877(10) 0.61309(13) 0.0322(5) Uani 1 1 d . . .
H41A H -0.1410 0.1524 0.6056 0.039 Uiso 1 1 calc R . .
C42 C -0.1549(2) 0.24448(10) 0.59430(12) 0.0265(5) Uani 1 1 d . . .
H42A H -0.2405 0.2453 0.5735 0.032 Uiso 1 1 calc R . .
C43 C 0.0421(2) 0.66051(10) 0.56154(13) 0.0326(5) Uani 1 1 d . . .
H43A H 0.0263 0.6923 0.5290 0.039 Uiso 1 1 calc R . .
C44 C 0.0610(2) 0.67331(9) 0.63084(13) 0.0300(5) Uani 1 1 d . . .
H44A H 0.0569 0.7137 0.6451 0.036 Uiso 1 1 calc R . .
C45 C 0.4178(2) 0.26126(9) 0.58194(13) 0.0281(5) Uani 1 1 d . . .
H45A H 0.4065 0.2382 0.5412 0.034 Uiso 1 1 calc R . .
C46 C 0.0999(2) 0.24213(9) 0.65646(12) 0.0235(4) Uani 1 1 d . . .
H46A H 0.1854 0.2410 0.6777 0.028 Uiso 1 1 calc R . .
C47 C 0.1677(2) 0.48163(9) 0.83363(12) 0.0252(5) Uani 1 1 d . . .
H47A H 0.1683 0.4408 0.8200 0.030 Uiso 1 1 calc R . .
C48 C 0.4512(2) 0.33110(10) 0.70288(12) 0.0261(5) Uani 1 1 d . . .
H48A H 0.4634 0.3547 0.7433 0.031 Uiso 1 1 calc R . .
C49 C 0.1108(2) 0.63791(9) 0.75360(12) 0.0255(5) Uani 1 1 d . . .
H49A H 0.1086 0.6783 0.7683 0.031 Uiso 1 1 calc R . .
C50 C 0.33696(19) 0.33316(8) 0.65209(11) 0.0195(4) Uani 1 1 d . . .
C51 C 0.3216(2) 0.29856(9) 0.59125(11) 0.0221(4) Uani 1 1 d . . .
H51A H 0.2464 0.3004 0.5565 0.027 Uiso 1 1 calc R . .
C52 C 0.11770(19) 0.51602(8) 0.70932(11) 0.0195(4) Uani 1 1 d . . .
C53 C 0.0697(2) 0.55207(10) 0.58560(12) 0.0252(4) Uani 1 1 d . . .
H53A H 0.0718 0.5120 0.5697 0.030 Uiso 1 1 calc R . .
C54 C 0.1381(2) 0.59130(9) 0.80381(12) 0.0230(4) Uani 1 1 d . . .
C55 C 0.0869(2) 0.62565(9) 0.68206(12) 0.0230(4) Uani 1 1 d . . .
C56 C 0.14041(19) 0.52857(9) 0.78134(11) 0.0204(4) Uani 1 1 d . . .
C57 C 0.0907(2) 0.56324(9) 0.65892(11) 0.0212(4) Uani 1 1 d . . .
C58 C -0.0882(2) 0.29904(9) 0.60619(11) 0.0221(4) Uani 1 1 d . . .
H58A H -0.1292 0.3361 0.5929 0.027 Uiso 1 1 calc R . .
C59 C 0.04049(19) 0.29859(9) 0.63816(11) 0.0186(4) Uani 1 1 d . . .
N1 N -0.17475(16) -0.05243(8) 0.74184(9) 0.0199(3) Uani 1 1 d . . .
N2 N -0.34580(16) -0.08808(7) 0.76468(9) 0.0185(3) Uani 1 1 d . . .
H2A H -0.4028 -0.0941 0.7861 0.022 Uiso 1 1 calc R . .
N3 N 0.04666(16) 0.40870(7) 0.67054(9) 0.0190(3) Uani 1 1 d . . .
N4 N 0.24635(16) 0.43087(7) 0.68338(9) 0.0191(3) Uani 1 1 d . . .
H4B H 0.3147 0.4516 0.6924 0.023 Uiso 1 1 calc R . .
O1 O 0.45141(14) 0.50396(6) 0.71577(8) 0.0223(3) Uani 1 1 d . . .
O2 O -0.1113(3) 0.60231(12) 0.90486(14) 0.0730(7) Uani 1 1 d . . .
C60 C 0.4487(2) 0.56065(10) 0.75062(14) 0.0293(5) Uani 1 1 d . . .
C61 C -0.1376(5) 0.53911(18) 0.9173(2) 0.0810(13) Uani 1 1 d . . .
H1 H 0.528(4) 0.4859(19) 0.733(2) 0.097 Uiso 1 1 d . . .
H2 H 0.373(4) 0.5848(19) 0.725(2) 0.097 Uiso 1 1 d . . .
H3 H 0.446(4) 0.5584(18) 0.801(2) 0.097 Uiso 1 1 d . . .
H4 H 0.515(4) 0.5852(19) 0.747(2) 0.097 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 N1 1.326(3) . ?
C1 N2 1.350(3) . ?
C1 C29 1.483(3) . ?
C2 C3 1.382(3) . ?
C2 N1 1.391(3) . ?
C2 C26 1.470(3) . ?
C3 N2 1.378(2) . ?
C3 C27 1.482(3) . ?
C4 C6 1.382(4) . ?
C4 C10 1.384(4) . ?
C5 C12 1.383(4) . ?
C5 C13 1.385(4) . ?
C6 C7 1.393(3) . ?
C7 C26 1.393(3) . ?
C8 C9 1.355(4) . ?
C8 C23 1.430(3) . ?
C9 C11 1.411(4) . ?
C10 C18 1.385(3) . ?
C11 C22 1.360(3) . ?
C12 C17 1.389(3) . ?
C13 C19 1.388(3) . ?
C14 C20 1.362(3) . ?
C14 C16 1.417(3) . ?
C15 C16 1.358(4) . ?
C15 C24 1.421(3) . ?
C17 C27 1.388(3) . ?
C18 C26 1.404(3) . ?
C19 C27 1.391(3) . ?
C20 C28 1.429(3) . ?
C21 C23 1.394(3) . ?
C21 C24 1.394(3) . ?
C22 C25 1.426(3) . ?
C23 C25 1.438(3) . ?
C24 C28 1.443(3) . ?
C25 C29 1.406(3) . ?
C28 C29 1.404(3) . ?
C31 N3 1.328(3) . ?
C31 N4 1.352(3) . ?
C31 C52 1.488(3) . ?
C32 N4 1.378(2) . ?
C32 C33 1.379(3) . ?
C32 C50 1.476(3) . ?
C33 N3 1.389(2) . ?
C33 C59 1.473(3) . ?
C34 C37 1.390(4) . ?
C34 C48 1.393(3) . ?
C35 C38 1.359(3) . ?
C35 C54 1.433(3) . ?
C36 C53 1.361(3) . ?
C36 C43 1.422(3) . ?
C37 C45 1.375(4) . ?
C38 C39 1.421(3) . ?
C39 C47 1.362(3) . ?
C40 C46 1.389(3) . ?
C40 C41 1.389(4) . ?
C41 C42 1.385(3) . ?
C42 C58 1.388(3) . ?
C43 C44 1.359(3) . ?
C44 C55 1.426(3) . ?
C45 C51 1.393(3) . ?
C46 C59 1.398(3) . ?
C47 C56 1.429(3) . ?
C48 C50 1.394(3) . ?
C49 C55 1.394(3) . ?
C49 C54 1.396(3) . ?
C50 C51 1.391(3) . ?
C52 C56 1.406(3) . ?
C52 C57 1.409(3) . ?
C53 C57 1.427(3) . ?
C54 C56 1.440(3) . ?
C55 C57 1.440(3) . ?
C58 C59 1.400(3) . ?
O1 C60 1.419(3) . ?
O2 C61 1.443(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
N1 C1 N2 110.97(17) . . ?
N1 C1 C29 125.34(18) . . ?
N2 C1 C29 123.64(17) . . ?
C3 C2 N1 108.78(17) . . ?
C3 C2 C26 131.59(18) . . ?
N1 C2 C26 119.50(18) . . ?
N2 C3 C2 105.83(17) . . ?
N2 C3 C27 120.49(18) . . ?
C2 C3 C27 133.56(18) . . ?
C6 C4 C10 119.1(2) . . ?
C12 C5 C13 119.5(2) . . ?
C4 C6 C7 120.4(3) . . ?
C26 C7 C6 121.1(2) . . ?
C9 C8 C23 120.9(2) . . ?
C8 C9 C11 120.7(2) . . ?
C4 C10 C18 120.9(2) . . ?
C22 C11 C9 120.5(2) . . ?
C5 C12 C17 120.2(2) . . ?
C5 C13 C19 120.3(2) . . ?
C20 C14 C16 120.7(2) . . ?
C16 C15 C24 121.4(2) . . ?
C15 C16 C14 120.1(2) . . ?
C27 C17 C12 120.7(2) . . ?
C10 C18 C26 120.7(2) . . ?
C13 C19 C27 120.5(2) . . ?
C14 C20 C28 121.3(2) . . ?
C23 C21 C24 121.78(19) . . ?
C11 C22 C25 121.1(2) . . ?
C21 C23 C8 121.9(2) . . ?
C21 C23 C25 119.5(2) . . ?
C8 C23 C25 118.5(2) . . ?
C21 C24 C15 121.9(2) . . ?
C21 C24 C28 119.1(2) . . ?
C15 C24 C28 119.0(2) . . ?
C29 C25 C22 122.79(18) . . ?
C29 C25 C23 119.1(2) . . ?
C22 C25 C23 118.10(19) . . ?
C7 C26 C18 117.8(2) . . ?
C7 C26 C2 119.86(19) . . ?
C18 C26 C2 122.20(19) . . ?
C17 C27 C19 118.7(2) . . ?
C17 C27 C3 121.07(19) . . ?
C19 C27 C3 120.17(19) . . ?
C29 C28 C20 123.00(19) . . ?
C29 C28 C24 119.4(2) . . ?
C20 C28 C24 117.5(2) . . ?
C28 C29 C25 121.04(18) . . ?
C28 C29 C1 120.27(18) . . ?
C25 C29 C1 118.69(18) . . ?
N3 C31 N4 111.52(16) . . ?
N3 C31 C52 127.10(18) . . ?
N4 C31 C52 121.36(17) . . ?
N4 C32 C33 105.24(16) . . ?
N4 C32 C50 122.50(17) . . ?
C33 C32 C50 132.26(17) . . ?
C32 C33 N3 109.97(16) . . ?
C32 C33 C59 129.74(17) . . ?
N3 C33 C59 120.17(17) . . ?
C37 C34 C48 120.3(2) . . ?
C38 C35 C54 120.8(2) . . ?
C53 C36 C43 120.3(2) . . ?
C45 C37 C34 119.8(2) . . ?
C35 C38 C39 120.6(2) . . ?
C47 C39 C38 120.6(2) . . ?
C46 C40 C41 120.2(2) . . ?
C42 C41 C40 119.4(2) . . ?
C41 C42 C58 120.8(2) . . ?
C44 C43 C36 120.5(2) . . ?
C43 C44 C55 121.0(2) . . ?
C37 C45 C51 120.2(2) . . ?
C40 C46 C59 120.7(2) . . ?
C39 C47 C56 121.0(2) . . ?
C34 C48 C50 120.1(2) . . ?
C55 C49 C54 121.94(19) . . ?
C51 C50 C48 119.02(19) . . ?
C51 C50 C32 119.96(19) . . ?
C48 C50 C32 121.02(18) . . ?
C50 C51 C45 120.6(2) . . ?
C56 C52 C57 121.46(18) . . ?
C56 C52 C31 118.55(18) . . ?
C57 C52 C31 119.77(18) . . ?
C36 C53 C57 121.2(2) . . ?
C49 C54 C35 122.03(19) . . ?
C49 C54 C56 119.3(2) . . ?
C35 C54 C56 118.63(19) . . ?
C49 C55 C44 121.96(19) . . ?
C49 C55 C57 119.33(19) . . ?
C44 C55 C57 118.7(2) . . ?
C52 C56 C47 122.71(18) . . ?
C52 C56 C54 118.96(18) . . ?
C47 C56 C54 118.32(19) . . ?
C52 C57 C53 122.75(18) . . ?
C52 C57 C55 118.97(19) . . ?
C53 C57 C55 118.26(18) . . ?
C42 C58 C59 120.3(2) . . ?
C46 C59 C58 118.53(18) . . ?
C46 C59 C33 121.89(19) . . ?
C58 C59 C33 119.49(18) . . ?
C1 N1 C2 106.33(17) . . ?
C1 N2 C3 108.08(16) . . ?
C31 N3 C33 105.23(16) . . ?
C31 N4 C32 108.03(16) . . ?

_diffrn_measured_fraction_theta_max 0.940
_diffrn_reflns_theta_full        32.09
_diffrn_measured_fraction_theta_full 0.940
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.066
_database_code_depnum_ccdc_archive 'CCDC 993932'
#######################################################################
#
#                 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_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26.40 H22.40 N1.60 O1.60'
_chemical_formula_weight         387.66

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           Orthorhombic
_symmetry_space_group_name_H-M   'P bca'

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

_cell_length_a                   12.859(5)
_cell_length_b                   15.737(6)
_cell_length_c                   25.688(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5198(3)
_cell_formula_units_Z            10
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2048
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9847
_exptl_absorpt_correction_T_max  0.9847
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52231
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         27.45
_reflns_number_total             5952
_reflns_number_gt                3898
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0722P)²+1.8565P] 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         5952
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0768
_refine_ls_wR_factor_ref         0.2019
_refine_ls_wR_factor_gt          0.1763
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_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 0.7496(3) -0.1810(2) 0.23217(14) 0.0831(10) Uani 1 1 d . . .
H1A H 0.7705 -0.1794 0.2668 0.100 Uiso 1 1 calc R . .
C2 C 0.8169(3) -0.2110(2) 0.19497(17) 0.0855(10) Uani 1 1 d . . .
H2A H 0.8829 -0.2297 0.2044 0.103 Uiso 1 1 calc R . .
C3 C 0.0599(3) -0.3325(2) 0.10091(14) 0.0796(9) Uani 1 1 d . . .
H3A H 0.0083 -0.3715 0.1095 0.096 Uiso 1 1 calc R . .
C4 C 0.1359(3) -0.3096(2) 0.13829(13) 0.0805(9) Uani 1 1 d . . .
H4A H 0.1333 -0.3333 0.1714 0.097 Uiso 1 1 calc R . .
C5 C 0.0625(2) -0.29774(19) 0.05267(13) 0.0688(8) Uani 1 1 d . . .
H5A H 0.0128 -0.3137 0.0282 0.083 Uiso 1 1 calc R . .
C6 C 0.3590(2) -0.0087(2) -0.04734(12) 0.0688(8) Uani 1 1 d . . .
H6A H 0.4058 0.0343 -0.0556 0.083 Uiso 1 1 calc R . .
C7 C 0.2839(2) -0.0340(2) -0.08430(11) 0.0692(8) Uani 1 1 d . . .
H7A H 0.2819 -0.0078 -0.1167 0.083 Uiso 1 1 calc R . .
C8 C 0.2125(2) -0.25340(19) 0.12638(11) 0.0653(7) Uani 1 1 d . . .
H8A H 0.2625 -0.2403 0.1513 0.078 Uiso 1 1 calc R . .
C9 C 0.2152(2) -0.09585(19) -0.07280(10) 0.0623(7) Uani 1 1 d . . .
H9A H 0.1665 -0.1119 -0.0977 0.075 Uiso 1 1 calc R . .
C10 C 0.4675(3) 0.12680(19) 0.28809(11) 0.0726(9) Uani 1 1 d . . .
H10A H 0.4715 0.1687 0.3135 0.087 Uiso 1 1 calc R . .
C11 C 0.6885(2) -0.18504(18) 0.12989(12) 0.0631(7) Uani 1 1 d . . .
H11A H 0.6691 -0.1867 0.0950 0.076 Uiso 1 1 calc R . .
C12 C 0.6499(2) -0.15296(18) 0.21857(11) 0.0665(8) Uani 1 1 d . . .
H12A H 0.6048 -0.1335 0.2442 0.080 Uiso 1 1 calc R . .
C13 C 0.3636(2) -0.04657(18) 0.00019(11) 0.0595(7) Uani 1 1 d . . .
H13A H 0.4137 -0.0291 0.0240 0.071 Uiso 1 1 calc R . .
C14 C 0.1425(2) -0.19866(17) -0.01025(10) 0.0554(6) Uani 1 1 d . . .
H14A H 0.0935 -0.2149 -0.0350 0.067 Uiso 1 1 calc R . .
C15 C 0.3739(3) 0.08808(19) 0.27732(11) 0.0677(8) Uani 1 1 d . . .
H15A H 0.3144 0.1043 0.2954 0.081 Uiso 1 1 calc R . .
C16 C 0.3676(2) 0.02462(17) 0.23936(10) 0.0582(7) Uani 1 1 d . . .
H16A H 0.3041 -0.0014 0.2327 0.070 Uiso 1 1 calc R . .
C17 C 0.5554(3) 0.10302(18) 0.26092(11) 0.0673(8) Uani 1 1 d . . .
H17A H 0.6188 0.1289 0.2682 0.081 Uiso 1 1 calc R . .
C18 C 0.14022(19) -0.23691(16) 0.03868(10) 0.0527(6) Uani 1 1 d . . .
C19 C 0.21522(19) -0.13724(16) -0.02338(9) 0.0492(6) Uani 1 1 d . . .
C20 C 0.5496(2) 0.04025(17) 0.22254(10) 0.0569(6) Uani 1 1 d . . .
H20A H 0.6091 0.0251 0.2042 0.068 Uiso 1 1 calc R . .
C21 C 0.61824(19) -0.15413(14) 0.16680(10) 0.0489(6) Uani 1 1 d . . .
C22 C 0.44825(19) -0.06456(15) 0.16985(9) 0.0465(5) Uani 1 1 d . . .
C23 C 0.29278(18) -0.11273(16) 0.01413(9) 0.0480(6) Uani 1 1 d . . .
C24 C 0.21757(19) -0.21405(16) 0.07633(9) 0.0506(6) Uani 1 1 d . . .
C25 C 0.37522(19) -0.13022(16) 0.10243(9) 0.0484(6) Uani 1 1 d . . .
C26 C 0.29351(19) -0.15276(16) 0.06341(9) 0.0496(6) Uani 1 1 d . . .
C27 C 0.51388(18) -0.12612(15) 0.14975(9) 0.0468(5) Uani 1 1 d . . .
C28 C 0.45550(19) 0.00000(15) 0.21147(9) 0.0476(6) Uani 1 1 d . . .
C29 C 0.7865(2) -0.2133(2) 0.14428(15) 0.0788(9) Uani 1 1 d . . .
H29A H 0.8317 -0.2340 0.1191 0.095 Uiso 1 1 calc R . .
C30 C -0.0016(3) 0.0739(3) -0.13301(15) 0.0994(12) Uani 1 1 d . . .
H30A H -0.0235 0.1045 -0.1634 0.149 Uiso 1 1 calc R . .
H30B H 0.0628 0.0453 -0.1401 0.149 Uiso 1 1 calc R . .
H30C H 0.0080 0.1129 -0.1047 0.149 Uiso 1 1 calc R . .
C31 C -0.0821(3) 0.0104(2) -0.11876(14) 0.0793(9) Uani 1 1 d . . .
C32 C -0.1289(4) -0.1006(4) -0.0602(2) 0.140(2) Uani 1 1 d . . .
H32A H -0.1994 -0.0855 -0.0699 0.168 Uiso 1 1 calc R . .
H32B H -0.1115 -0.1539 -0.0770 0.168 Uiso 1 1 calc R . .
C33 C -0.1219(3) -0.1099(3) -0.00452(18) 0.1151(14) Uani 1 1 d . . .
H33A H -0.1695 -0.1532 0.0068 0.173 Uiso 1 1 calc R . .
H33B H -0.1393 -0.0570 0.0119 0.173 Uiso 1 1 calc R . .
H33C H -0.0523 -0.1259 0.0048 0.173 Uiso 1 1 calc R . .
N1 N 0.36026(16) -0.06942(13) 0.13910(7) 0.0510(5) Uani 1 1 d . . .
H1B H 0.3052 -0.0390 0.1426 0.061 Uiso 1 1 calc R . .
N2 N 0.46716(16) -0.16612(13) 0.10748(8) 0.0513(5) Uani 1 1 d . . .
O1 O -0.16160(18) -0.00040(19) -0.14248(10) 0.1051(9) Uani 1 1 d . . .
O2 O -0.0572(2) -0.0345(2) -0.07715(11) 0.1110(9) 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 C12 1.401(4) . ?
C2 C29 1.360(5) . ?
C3 C5 1.355(4) . ?
C3 C4 1.417(5) . ?
C4 C8 1.358(4) . ?
C5 C18 1.430(4) . ?
C6 C13 1.360(4) . ?
C6 C7 1.411(4) . ?
C7 C9 1.348(4) . ?
C8 C24 1.429(4) . ?
C9 C19 1.427(4) . ?
C10 C15 1.378(4) . ?
C10 C17 1.380(4) . ?
C11 C29 1.387(4) . ?
C11 C21 1.397(4) . ?
C12 C21 1.391(4) . ?
C13 C23 1.429(4) . ?
C14 C19 1.387(4) . ?
C14 C18 1.394(4) . ?
C15 C16 1.398(4) . ?
C16 C28 1.393(3) . ?
C17 C20 1.398(4) . ?
C18 C24 1.433(3) . ?
C19 C23 1.439(3) . ?
C20 C28 1.395(3) . ?
C21 C27 1.479(3) . ?
C22 N1 1.382(3) . ?
C22 C27 1.385(3) . ?
C22 C28 1.478(3) . ?
C23 C26 1.414(3) . ?
C24 C26 1.412(3) . ?
C25 N2 1.317(3) . ?
C25 N1 1.356(3) . ?
C25 C26 1.495(3) . ?
C27 N2 1.391(3) . ?
C30 C31 1.484(5) . ?
C31 O1 1.203(4) . ?
C31 O2 1.321(4) . ?
C32 C33 1.440(5) . ?
C32 O2 1.457(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 C12 120.8(3) . . ?
C29 C2 C1 119.7(3) . . ?
C5 C3 C4 120.0(3) . . ?
C8 C4 C3 120.9(3) . . ?
C3 C5 C18 121.1(3) . . ?
C13 C6 C7 120.7(3) . . ?
C9 C7 C6 120.3(3) . . ?
C4 C8 C24 121.2(3) . . ?
C7 C9 C19 121.6(3) . . ?
C15 C10 C17 119.6(3) . . ?
C29 C11 C21 121.2(3) . . ?
C21 C12 C1 120.2(3) . . ?
C6 C13 C23 121.1(3) . . ?
C19 C14 C18 122.3(2) . . ?
C10 C15 C16 120.4(3) . . ?
C28 C16 C15 120.7(3) . . ?
C10 C17 C20 120.3(3) . . ?
C14 C18 C5 122.0(2) . . ?
C14 C18 C24 119.1(2) . . ?
C5 C18 C24 118.9(2) . . ?
C14 C19 C9 122.3(2) . . ?
C14 C19 C23 119.4(2) . . ?
C9 C19 C23 118.3(2) . . ?
C28 C20 C17 120.8(3) . . ?
C12 C21 C11 117.7(3) . . ?
C12 C21 C27 123.0(2) . . ?
C11 C21 C27 119.3(2) . . ?
N1 C22 C27 104.3(2) . . ?
N1 C22 C28 120.2(2) . . ?
C27 C22 C28 135.4(2) . . ?
C26 C23 C13 123.0(2) . . ?
C26 C23 C19 119.0(2) . . ?
C13 C23 C19 118.0(2) . . ?
C26 C24 C8 122.6(2) . . ?
C26 C24 C18 119.5(2) . . ?
C8 C24 C18 117.8(2) . . ?
N2 C25 N1 111.2(2) . . ?
N2 C25 C26 126.5(2) . . ?
N1 C25 C26 122.2(2) . . ?
C24 C26 C23 120.7(2) . . ?
C24 C26 C25 119.4(2) . . ?
C23 C26 C25 119.9(2) . . ?
C22 C27 N2 110.1(2) . . ?
C22 C27 C21 130.6(2) . . ?
N2 C27 C21 119.2(2) . . ?
C16 C28 C20 118.2(2) . . ?
C16 C28 C22 120.8(2) . . ?
C20 C28 C22 121.0(2) . . ?
C2 C29 C11 120.5(3) . . ?
O1 C31 O2 122.7(4) . . ?
O1 C31 C30 124.3(4) . . ?
O2 C31 C30 113.0(3) . . ?
C33 C32 O2 109.3(4) . . ?
C25 N1 C22 108.7(2) . . ?
C25 N2 C27 105.7(2) . . ?
C31 O2 C32 118.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.044
_database_code_depnum_ccdc_archive 'CCDC 993933'
#######################################################################
#
#                 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_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C87 H62 N6 O'
_chemical_formula_weight         1207.43

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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   19.548(9)
_cell_length_b                   18.292(8)
_cell_length_c                   21.819(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.996(5)
_cell_angle_gamma                90.00
_cell_volume                     7377(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2536
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9872
_exptl_absorpt_correction_T_max  0.9872
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            77220
_diffrn_reflns_av_R_equivalents  0.1763
_diffrn_reflns_av_sigmaI/netI    0.1314
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         27.52
_reflns_number_total             16918
_reflns_number_gt                6801
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)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         16918
_refine_ls_number_parameters     847
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.3205
_refine_ls_R_factor_gt           0.1879
_refine_ls_wR_factor_ref         0.4361
_refine_ls_wR_factor_gt          0.3855
_refine_ls_goodness_of_fit_ref   1.625
_refine_ls_restrained_S_all      1.625
_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 0.3940(4) -0.2580(3) 1.0190(3) 0.0508(17) Uani 1 1 d . . .
C2 C 0.3175(3) -0.1803(4) 0.9515(3) 0.0469(16) Uani 1 1 d . . .
C3 C 0.3046(3) -0.1823(3) 1.0103(3) 0.0468(15) Uani 1 1 d . . .
C4 C 0.4482(4) -0.3171(4) 1.0412(3) 0.0599(19) Uani 1 1 d . . .
C5 C 0.5220(4) -0.3018(5) 1.0561(3) 0.062(2) Uani 1 1 d . . .
C6 C 0.5485(4) -0.2318(5) 1.0513(3) 0.073(2) Uani 1 1 d . . .
H6A H 0.5158 -0.1937 1.0367 0.088 Uiso 1 1 calc R . .
C7 C 0.6202(5) -0.2176(6) 1.0670(4) 0.089(3) Uani 1 1 d . . .
H7A H 0.6363 -0.1704 1.0640 0.107 Uiso 1 1 calc R . .
C8 C 0.6716(6) -0.2772(8) 1.0886(5) 0.106(4) Uani 1 1 d . . .
H8A H 0.7208 -0.2679 1.0990 0.127 Uiso 1 1 calc R . .
C9 C 0.6487(6) -0.3453(8) 1.0938(5) 0.113(4) Uani 1 1 d . . .
H9A H 0.6826 -0.3826 1.1072 0.136 Uiso 1 1 calc R . .
C10 C 0.5735(5) -0.3620(6) 1.0791(4) 0.078(3) Uani 1 1 d . . .
C11 C 0.5468(7) -0.4322(6) 1.0839(4) 0.097(3) Uani 1 1 d . . .
H11A H 0.5798 -0.4704 1.0966 0.117 Uiso 1 1 calc R . .
C12 C 0.4739(6) -0.4480(5) 1.0706(4) 0.085(3) Uani 1 1 d . . .
C13 C 0.4488(8) -0.5221(6) 1.0754(5) 0.113(4) Uani 1 1 d . . .
H13A H 0.4816 -0.5606 1.0875 0.136 Uiso 1 1 calc R . .
C14 C 0.3797(9) -0.5338(6) 1.0624(6) 0.131(5) Uani 1 1 d . . .
H14A H 0.3642 -0.5802 1.0692 0.157 Uiso 1 1 calc R . .
C15 C 0.3267(7) -0.4771(6) 1.0379(5) 0.116(4) Uani 1 1 d . . .
H15A H 0.2777 -0.4883 1.0256 0.139 Uiso 1 1 calc R . .
C16 C 0.3483(5) -0.4070(5) 1.0324(4) 0.084(3) Uani 1 1 d . . .
H16A H 0.3138 -0.3703 1.0181 0.101 Uiso 1 1 calc R . .
C17 C 0.4239(5) -0.3895(4) 1.0487(3) 0.064(2) Uani 1 1 d . . .
C18 C 0.2832(4) -0.1413(4) 0.8911(3) 0.0558(18) Uani 1 1 d . . .
C19 C 0.2691(4) -0.1743(5) 0.8310(4) 0.079(2) Uani 1 1 d . . .
H19A H 0.2816 -0.2231 0.8290 0.095 Uiso 1 1 calc R . .
C20 C 0.2374(6) -0.1368(7) 0.7749(4) 0.101(3) Uani 1 1 d . . .
H20A H 0.2296 -0.1602 0.7354 0.121 Uiso 1 1 calc R . .
C21 C 0.2167(5) -0.0649(7) 0.7758(5) 0.101(3) Uani 1 1 d . . .
H21A H 0.1956 -0.0398 0.7371 0.121 Uiso 1 1 calc R . .
C22 C 0.2270(5) -0.0316(5) 0.8321(5) 0.095(3) Uani 1 1 d . . .
H22A H 0.2110 0.0161 0.8329 0.113 Uiso 1 1 calc R . .
C23 C 0.2620(5) -0.0682(5) 0.8908(4) 0.080(2) Uani 1 1 d . . .
H23A H 0.2713 -0.0434 0.9299 0.096 Uiso 1 1 calc R . .
C24 C 0.2495(4) -0.1457(4) 1.0317(4) 0.0568(18) Uani 1 1 d . . .
C25 C 0.1807(4) -0.1356(5) 0.9911(5) 0.081(2) Uani 1 1 d . . .
H25A H 0.1673 -0.1492 0.9477 0.097 Uiso 1 1 calc R . .
C26 C 0.1291(5) -0.1031(6) 1.0174(7) 0.111(4) Uani 1 1 d . . .
H26A H 0.0817 -0.0962 0.9906 0.133 Uiso 1 1 calc R . .
C27 C 0.1480(8) -0.0826(7) 1.0795(7) 0.125(4) Uani 1 1 d . . .
H27A H 0.1136 -0.0616 1.0952 0.150 Uiso 1 1 calc R . .
C28 C 0.2163(7) -0.0920(6) 1.1195(6) 0.120(4) Uani 1 1 d . . .
H28A H 0.2291 -0.0774 1.1626 0.144 Uiso 1 1 calc R . .
C29 C 0.2675(5) -0.1238(5) 1.0959(4) 0.080(2) Uani 1 1 d . . .
H29A H 0.3145 -0.1304 1.1237 0.097 Uiso 1 1 calc R . .
C31 C 0.4690(7) 0.0406(6) 0.8859(6) 0.129(4) Uani 1 1 d . . .
H31A H 0.4502 0.0871 0.8873 0.155 Uiso 1 1 calc R . .
C32 C 0.4368(7) -0.4782(6) 0.6591(7) 0.141(5) Uani 1 1 d . . .
H32A H 0.4275 -0.5282 0.6579 0.169 Uiso 1 1 calc R . .
C33 C 0.5414(6) 0.0285(5) 0.9150(6) 0.117(4) Uani 1 1 d . . .
H33A H 0.5716 0.0669 0.9349 0.140 Uiso 1 1 calc R . .
C34 C 0.4504(6) -0.3720(7) 0.6033(5) 0.106(3) Uani 1 1 d . . .
H34A H 0.4528 -0.3494 0.5659 0.128 Uiso 1 1 calc R . .
C35 C 0.7747(5) -0.2091(6) 0.9799(5) 0.095(3) Uani 1 1 d . . .
H35A H 0.8234 -0.2175 1.0024 0.114 Uiso 1 1 calc R . .
C36 C 0.4228(5) -0.0160(5) 0.8541(5) 0.105(3) Uani 1 1 d . . .
H36A H 0.3745 -0.0057 0.8320 0.126 Uiso 1 1 calc R . .
C37 C 0.4452(6) -0.4374(5) 0.7178(5) 0.101(3) Uani 1 1 d . . .
H37A H 0.4455 -0.4610 0.7557 0.122 Uiso 1 1 calc R . .
C38 C 0.2249(5) -0.3773(5) 0.7452(5) 0.086(3) Uani 1 1 d . . .
H38A H 0.1873 -0.3752 0.7059 0.103 Uiso 1 1 calc R . .
C39 C 0.5701(4) -0.0416(4) 0.9150(4) 0.074(2) Uani 1 1 d . . .
C40 C 0.4426(6) -0.4435(7) 0.6050(6) 0.116(4) Uani 1 1 d . . .
H40A H 0.4409 -0.4712 0.5688 0.140 Uiso 1 1 calc R . .
C41 C 0.7473(5) -0.1417(6) 0.9761(4) 0.090(3) Uani 1 1 d . . .
H41A H 0.7782 -0.1033 0.9948 0.108 Uiso 1 1 calc R . .
C42 C 0.4473(4) -0.0860(4) 0.8548(4) 0.075(2) Uani 1 1 d . . .
H42A H 0.4154 -0.1233 0.8352 0.090 Uiso 1 1 calc R . .
C43 C 0.2140(5) -0.4079(5) 0.7988(5) 0.086(3) Uani 1 1 d . . .
H43A H 0.1683 -0.4252 0.7959 0.104 Uiso 1 1 calc R . .
C44 C 0.6438(5) -0.0569(5) 0.9426(4) 0.083(3) Uani 1 1 d . . .
H44A H 0.6751 -0.0185 0.9606 0.100 Uiso 1 1 calc R . .
C45 C 0.2682(5) -0.4132(5) 0.8554(5) 0.081(3) Uani 1 1 d . . .
H45A H 0.2604 -0.4361 0.8906 0.097 Uiso 1 1 calc R . .
C46 C 0.7288(5) -0.2672(5) 0.9493(4) 0.083(3) Uani 1 1 d . . .
H46A H 0.7480 -0.3139 0.9503 0.100 Uiso 1 1 calc R . .
C47 C 0.4549(4) -0.3312(5) 0.6575(4) 0.075(2) Uani 1 1 d . . .
H47A H 0.4598 -0.2807 0.6555 0.090 Uiso 1 1 calc R . .
C48 C 0.2926(4) -0.3497(4) 0.7503(4) 0.068(2) Uani 1 1 d . . .
H48A H 0.3004 -0.3303 0.7137 0.081 Uiso 1 1 calc R . .
C49 C 0.6725(4) -0.1262(5) 0.9444(4) 0.065(2) Uani 1 1 d . . .
C50 C 0.6571(4) -0.2561(4) 0.9184(3) 0.0603(19) Uani 1 1 d . . .
H50A H 0.6278 -0.2955 0.8993 0.072 Uiso 1 1 calc R . .
C51 C 0.4526(4) -0.3624(4) 0.7162(4) 0.0600(19) Uani 1 1 d . . .
C52 C 0.5218(4) -0.1016(4) 0.8854(3) 0.0553(17) Uani 1 1 d . . .
C53 C 0.4183(3) -0.3140(3) 0.8149(3) 0.0464(15) Uani 1 1 d . . .
C54 C 0.3365(4) -0.3842(4) 0.8613(4) 0.0601(19) Uani 1 1 d . . .
H54A H 0.3738 -0.3877 0.9007 0.072 Uiso 1 1 calc R . .
C55 C 0.6259(4) -0.1847(4) 0.9148(3) 0.0543(17) Uani 1 1 d . . .
C56 C 0.4585(3) -0.3167(3) 0.7735(3) 0.0475(16) Uani 1 1 d . . .
C57 C 0.5034(3) -0.2330(4) 0.8501(3) 0.0457(15) Uani 1 1 d . . .
C58 C 0.5516(3) -0.1722(4) 0.8851(3) 0.0469(16) Uani 1 1 d . . .
C59 C 0.3489(3) -0.3503(3) 0.8089(3) 0.0447(15) Uani 1 1 d . . .
C61 C 0.7660(9) -0.4590(9) 0.8429(7) 0.131(5) Uani 1 1 d . . .
H61A H 0.8039 -0.4850 0.8714 0.157 Uiso 1 1 calc R . .
C62 C 0.9231(11) -0.1617(13) 0.8935(9) 0.205(11) Uani 1 1 d . . .
H62A H 0.9641 -0.1375 0.9195 0.246 Uiso 1 1 calc R . .
C63 C 0.8669(9) -0.1197(10) 0.8457(7) 0.179(7) Uani 1 1 d . . .
H63A H 0.8732 -0.0706 0.8380 0.215 Uiso 1 1 calc R . .
C64 C 0.6470(7) -0.4545(6) 0.7656(6) 0.114(4) Uani 1 1 d . . .
H64A H 0.6048 -0.4788 0.7420 0.137 Uiso 1 1 calc R . .
C65 C 0.3582(6) -0.0995(6) 0.6146(7) 0.110(4) Uani 1 1 d . . .
H65A H 0.3110 -0.0821 0.6025 0.132 Uiso 1 1 calc R . .
C66 C 0.7055(10) -0.4937(7) 0.8123(7) 0.142(6) Uani 1 1 d . . .
H66A H 0.7003 -0.5429 0.8206 0.171 Uiso 1 1 calc R . .
C67 C 0.7751(6) -0.3857(7) 0.8343(5) 0.091(3) Uani 1 1 d . . .
C68 C 0.4011(6) -0.0963(6) 0.6752(6) 0.099(3) Uani 1 1 d . . .
H68A H 0.3821 -0.0793 0.7065 0.119 Uiso 1 1 calc R . .
C69 C 0.9174(7) -0.2362(12) 0.9016(7) 0.175(7) Uani 1 1 d . . .
H69A H 0.9548 -0.2614 0.9316 0.210 Uiso 1 1 calc R . .
C70 C 0.8053(6) -0.1558(7) 0.8133(4) 0.107(4) Uani 1 1 d . . .
H70A H 0.7672 -0.1291 0.7857 0.128 Uiso 1 1 calc R . .
C71 C 0.8369(7) -0.3518(9) 0.8676(5) 0.118(5) Uani 1 1 d . . .
H71A H 0.8731 -0.3797 0.8963 0.142 Uiso 1 1 calc R . .
C72 C 0.8511(5) -0.2764(9) 0.8620(4) 0.108(4) Uani 1 1 d . . .
C73 C 0.6175(5) -0.0920(7) 0.4473(5) 0.107(4) Uani 1 1 d . . .
H73A H 0.6154 -0.0762 0.4062 0.128 Uiso 1 1 calc R . .
C74 C 0.3867(5) -0.1308(5) 0.5680(5) 0.097(3) Uani 1 1 d . . .
H74A H 0.3568 -0.1359 0.5252 0.117 Uiso 1 1 calc R . .
C75 C 0.6518(5) -0.1550(6) 0.4722(4) 0.100(3) Uani 1 1 d . . .
H75A H 0.6729 -0.1829 0.4475 0.120 Uiso 1 1 calc R . .
C76 C 0.5853(5) -0.0514(6) 0.4850(5) 0.104(4) Uani 1 1 d . . .
H76A H 0.5618 -0.0078 0.4690 0.124 Uiso 1 1 calc R . .
C77 C 0.4745(5) -0.1174(4) 0.6948(4) 0.077(2) Uani 1 1 d . . .
H77A H 0.5038 -0.1118 0.7377 0.093 Uiso 1 1 calc R . .
C78 C 0.7957(5) -0.2315(6) 0.8189(4) 0.083(3) Uani 1 1 d . . .
C79 C 0.6547(5) -0.3801(5) 0.7565(4) 0.082(3) Uani 1 1 d . . .
H79A H 0.6170 -0.3542 0.7276 0.099 Uiso 1 1 calc R . .
C80 C 0.4572(4) -0.1535(4) 0.5849(4) 0.073(2) Uani 1 1 d . . .
H80A H 0.4751 -0.1734 0.5539 0.087 Uiso 1 1 calc R . .
C81 C 0.6562(4) -0.1788(5) 0.5331(4) 0.073(2) Uani 1 1 d . . .
H81A H 0.6809 -0.2218 0.5489 0.087 Uiso 1 1 calc R . .
C82 C 0.6742(4) -0.2263(4) 0.7298(3) 0.0526(17) Uani 1 1 d . . .
C83 C 0.5881(4) -0.0755(4) 0.5464(4) 0.070(2) Uani 1 1 d . . .
H83A H 0.5656 -0.0486 0.5706 0.084 Uiso 1 1 calc R . .
C84 C 0.7205(4) -0.3432(5) 0.7915(4) 0.066(2) Uani 1 1 d . . .
C85 C 0.7307(4) -0.2674(5) 0.7829(3) 0.0613(19) Uani 1 1 d . . .
C86 C 0.6246(4) -0.1401(4) 0.5717(3) 0.0562(18) Uani 1 1 d . . .
C87 C 0.6279(4) -0.1697(4) 0.6364(3) 0.0542(17) Uani 1 1 d . . .
C88 C 0.5022(4) -0.1464(4) 0.6492(4) 0.0603(19) Uani 1 1 d . . .
C89 C 0.5785(4) -0.1719(4) 0.6700(3) 0.0545(17) Uani 1 1 d . . .
N1 N 0.3752(3) -0.2290(3) 0.9576(2) 0.0509(14) Uani 1 1 d . . .
N2 N 0.3522(3) -0.2317(3) 1.0510(3) 0.0551(15) Uani 1 1 d . . .
H2A H 0.3541 -0.2431 1.0898 0.066 Uiso 1 1 calc R . .
N3 N 0.4480(3) -0.2620(3) 0.8622(3) 0.0492(13) Uani 1 1 d . . .
H3A H 0.4328 -0.2508 0.8938 0.059 Uiso 1 1 calc R . .
N4 N 0.5121(3) -0.2645(3) 0.7950(2) 0.0461(13) Uani 1 1 d . . .
N5 N 0.6092(3) -0.2081(3) 0.7279(3) 0.0531(14) Uani 1 1 d . . .
H5A H 0.5894 -0.2169 0.7570 0.064 Uiso 1 1 calc R . .
N6 N 0.6895(3) -0.2044(3) 0.6761(2) 0.0524(14) Uani 1 1 d . . .
O1W O 0.8263(3) -0.2049(3) 0.6616(3) 0.0823(17) 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 N2 1.326(8) . ?
C1 N1 1.376(8) . ?
C1 C4 1.480(9) . ?
C2 C3 1.385(8) . ?
C2 N1 1.409(8) . ?
C2 C18 1.455(9) . ?
C3 N2 1.390(8) . ?
C3 C24 1.467(9) . ?
C4 C5 1.400(10) . ?
C4 C17 1.435(10) . ?
C5 C6 1.398(11) . ?
C5 C10 1.466(11) . ?
C6 C7 1.354(11) . ?
C7 C8 1.452(14) . ?
C8 C9 1.340(15) . ?
C9 C10 1.433(14) . ?
C10 C11 1.403(13) . ?
C11 C12 1.388(13) . ?
C12 C17 1.423(11) . ?
C12 C13 1.458(14) . ?
C13 C14 1.304(15) . ?
C14 C15 1.439(16) . ?
C15 C16 1.367(12) . ?
C16 C17 1.439(11) . ?
C18 C19 1.388(10) . ?
C18 C23 1.398(10) . ?
C19 C20 1.363(11) . ?
C20 C21 1.379(13) . ?
C21 C22 1.327(13) . ?
C22 C23 1.409(11) . ?
C24 C25 1.362(10) . ?
C24 C29 1.390(10) . ?
C25 C26 1.441(13) . ?
C26 C27 1.336(14) . ?
C27 C28 1.347(15) . ?
C28 C29 1.393(12) . ?
C31 C33 1.367(14) . ?
C31 C36 1.401(13) . ?
C32 C40 1.377(15) . ?
C32 C37 1.445(13) . ?
C33 C39 1.400(11) . ?
C34 C40 1.318(14) . ?
C34 C47 1.378(11) . ?
C35 C41 1.336(12) . ?
C35 C46 1.411(12) . ?
C36 C42 1.365(11) . ?
C37 C51 1.381(11) . ?
C38 C43 1.375(12) . ?
C38 C48 1.387(10) . ?
C39 C44 1.397(11) . ?
C39 C52 1.454(10) . ?
C41 C49 1.428(11) . ?
C42 C52 1.419(10) . ?
C43 C45 1.343(12) . ?
C44 C49 1.381(11) . ?
C45 C54 1.404(10) . ?
C46 C50 1.359(10) . ?
C47 C51 1.416(10) . ?
C48 C59 1.390(9) . ?
C49 C55 1.418(10) . ?
C50 C55 1.433(9) . ?
C51 C56 1.477(9) . ?
C52 C58 1.417(9) . ?
C53 C56 1.378(8) . ?
C53 N3 1.385(8) . ?
C53 C59 1.478(8) . ?
C54 C59 1.389(9) . ?
C55 C58 1.403(9) . ?
C56 N4 1.382(8) . ?
C57 N3 1.307(7) . ?
C57 N4 1.392(7) . ?
C57 C58 1.497(9) . ?
C61 C66 1.316(18) . ?
C61 C67 1.373(16) . ?
C62 C69 1.38(2) . ?
C62 C63 1.46(2) . ?
C63 C70 1.352(15) . ?
C64 C79 1.391(12) . ?
C64 C66 1.450(17) . ?
C65 C68 1.316(14) . ?
C65 C74 1.429(14) . ?
C67 C71 1.341(15) . ?
C67 C84 1.403(11) . ?
C68 C77 1.412(12) . ?
C69 C72 1.496(18) . ?
C70 C78 1.408(13) . ?
C71 C72 1.420(16) . ?
C72 C78 1.437(14) . ?
C73 C75 1.355(13) . ?
C73 C76 1.403(14) . ?
C74 C80 1.370(11) . ?
C75 C81 1.374(11) . ?
C76 C83 1.394(12) . ?
C77 C88 1.384(10) . ?
C78 C85 1.419(11) . ?
C79 C84 1.432(12) . ?
C80 C88 1.399(10) . ?
C81 C86 1.388(10) . ?
C82 N5 1.301(8) . ?
C82 N6 1.361(8) . ?
C82 C85 1.515(10) . ?
C83 C86 1.397(10) . ?
C84 C85 1.423(10) . ?
C86 C87 1.494(9) . ?
C87 N6 1.386(8) . ?
C87 C89 1.391(9) . ?
C88 C89 1.486(9) . ?
C89 N5 1.379(8) . ?

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
N2 C1 N1 111.0(6) . . ?
N2 C1 C4 126.3(6) . . ?
N1 C1 C4 122.4(5) . . ?
C3 C2 N1 106.0(5) . . ?
C3 C2 C18 133.0(6) . . ?
N1 C2 C18 121.0(5) . . ?
C2 C3 N2 108.9(5) . . ?
C2 C3 C24 130.9(6) . . ?
N2 C3 C24 120.0(6) . . ?
C5 C4 C17 120.8(7) . . ?
C5 C4 C1 120.3(7) . . ?
C17 C4 C1 118.9(7) . . ?
C6 C5 C4 123.0(7) . . ?
C6 C5 C10 118.9(8) . . ?
C4 C5 C10 118.1(8) . . ?
C7 C6 C5 122.3(9) . . ?
C6 C7 C8 119.2(10) . . ?
C9 C8 C7 120.7(10) . . ?
C8 C9 C10 121.7(11) . . ?
C11 C10 C9 124.0(10) . . ?
C11 C10 C5 118.8(8) . . ?
C9 C10 C5 117.2(10) . . ?
C12 C11 C10 123.8(9) . . ?
C11 C12 C17 117.4(9) . . ?
C11 C12 C13 121.7(10) . . ?
C17 C12 C13 120.8(10) . . ?
C14 C13 C12 119.0(12) . . ?
C13 C14 C15 122.2(12) . . ?
C16 C15 C14 120.2(12) . . ?
C15 C16 C17 120.5(10) . . ?
C12 C17 C4 121.0(8) . . ?
C12 C17 C16 117.0(8) . . ?
C4 C17 C16 121.9(7) . . ?
C19 C18 C23 116.3(7) . . ?
C19 C18 C2 122.2(7) . . ?
C23 C18 C2 121.5(7) . . ?
C20 C19 C18 121.5(9) . . ?
C19 C20 C21 121.1(9) . . ?
C22 C21 C20 119.5(9) . . ?
C21 C22 C23 120.5(9) . . ?
C18 C23 C22 120.9(8) . . ?
C25 C24 C29 119.2(7) . . ?
C25 C24 C3 121.9(7) . . ?
C29 C24 C3 118.9(7) . . ?
C24 C25 C26 117.9(9) . . ?
C27 C26 C25 121.5(10) . . ?
C26 C27 C28 120.6(10) . . ?
C27 C28 C29 119.6(11) . . ?
C24 C29 C28 121.2(9) . . ?
C33 C31 C36 120.8(10) . . ?
C40 C32 C37 120.2(9) . . ?
C31 C33 C39 120.2(9) . . ?
C40 C34 C47 119.3(10) . . ?
C41 C35 C46 119.0(8) . . ?
C42 C36 C31 121.4(9) . . ?
C51 C37 C32 118.3(9) . . ?
C43 C38 C48 119.3(9) . . ?
C44 C39 C33 122.7(8) . . ?
C44 C39 C52 118.0(7) . . ?
C33 C39 C52 119.2(8) . . ?
C34 C40 C32 121.7(10) . . ?
C35 C41 C49 122.7(8) . . ?
C36 C42 C52 119.8(8) . . ?
C45 C43 C38 121.2(8) . . ?
C49 C44 C39 123.2(7) . . ?
C43 C45 C54 120.0(8) . . ?
C50 C46 C35 121.1(8) . . ?
C34 C47 C51 123.1(9) . . ?
C38 C48 C59 121.3(8) . . ?
C44 C49 C55 119.0(7) . . ?
C44 C49 C41 122.6(8) . . ?
C55 C49 C41 118.4(8) . . ?
C46 C50 C55 121.0(7) . . ?
C37 C51 C47 117.2(7) . . ?
C37 C51 C56 121.4(7) . . ?
C47 C51 C56 121.4(7) . . ?
C58 C52 C42 122.8(6) . . ?
C58 C52 C39 118.7(7) . . ?
C42 C52 C39 118.4(7) . . ?
C56 C53 N3 108.8(5) . . ?
C56 C53 C59 129.0(6) . . ?
N3 C53 C59 121.6(5) . . ?
C59 C54 C45 120.5(7) . . ?
C58 C55 C49 120.1(7) . . ?
C58 C55 C50 122.2(6) . . ?
C49 C55 C50 117.7(6) . . ?
C53 C56 N4 106.4(5) . . ?
C53 C56 C51 132.1(6) . . ?
N4 C56 C51 121.4(5) . . ?
N3 C57 N4 110.4(5) . . ?
N3 C57 C58 128.6(6) . . ?
N4 C57 C58 121.0(5) . . ?
C55 C58 C52 120.8(6) . . ?
C55 C58 C57 119.9(6) . . ?
C52 C58 C57 119.2(6) . . ?
C54 C59 C48 117.6(6) . . ?
C54 C59 C53 121.9(6) . . ?
C48 C59 C53 120.4(6) . . ?
C66 C61 C67 122.5(14) . . ?
C69 C62 C63 122.3(16) . . ?
C70 C63 C62 116.8(16) . . ?
C79 C64 C66 119.1(12) . . ?
C68 C65 C74 117.8(10) . . ?
C61 C66 C64 119.4(13) . . ?
C71 C67 C61 120.8(12) . . ?
C71 C67 C84 117.5(11) . . ?
C61 C67 C84 121.8(12) . . ?
C65 C68 C77 122.9(10) . . ?
C62 C69 C72 120.1(15) . . ?
C63 C70 C78 123.8(13) . . ?
C67 C71 C72 124.6(10) . . ?
C71 C72 C78 119.0(10) . . ?
C71 C72 C69 125.8(13) . . ?
C78 C72 C69 115.0(14) . . ?
C75 C73 C76 118.2(8) . . ?
C80 C74 C65 121.3(9) . . ?
C73 C75 C81 121.6(9) . . ?
C83 C76 C73 120.8(8) . . ?
C88 C77 C68 119.0(9) . . ?
C70 C78 C85 121.9(9) . . ?
C70 C78 C72 121.7(10) . . ?
C85 C78 C72 116.5(10) . . ?
C64 C79 C84 120.4(10) . . ?
C74 C80 C88 119.4(8) . . ?
C75 C81 C86 121.7(8) . . ?
N5 C82 N6 112.6(6) . . ?
N5 C82 C85 127.8(6) . . ?
N6 C82 C85 119.7(6) . . ?
C76 C83 C86 120.1(8) . . ?
C67 C84 C85 121.2(9) . . ?
C67 C84 C79 116.8(9) . . ?
C85 C84 C79 121.9(7) . . ?
C78 C85 C84 121.1(8) . . ?
C78 C85 C82 119.5(7) . . ?
C84 C85 C82 119.1(7) . . ?
C81 C86 C83 117.6(7) . . ?
C81 C86 C87 119.8(7) . . ?
C83 C86 C87 122.6(6) . . ?
N6 C87 C89 105.5(6) . . ?
N6 C87 C86 121.2(6) . . ?
C89 C87 C86 133.2(7) . . ?
C77 C88 C80 119.5(7) . . ?
C77 C88 C89 119.3(7) . . ?
C80 C88 C89 121.2(7) . . ?
N5 C89 C87 109.1(6) . . ?
N5 C89 C88 121.7(6) . . ?
C87 C89 C88 129.1(7) . . ?
C1 N1 C2 106.8(5) . . ?
C1 N2 C3 107.3(5) . . ?
C57 N3 C53 107.6(5) . . ?
C56 N4 C57 106.7(5) . . ?
C82 N5 C89 106.3(5) . . ?
C82 N6 C87 106.5(5) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.925
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.169
_database_code_depnum_ccdc_archive 'CCDC 993934'
#######################################################################
#
#                 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_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H28 N2 O2'
_chemical_formula_weight         484.57

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           Orthorhombic
_symmetry_space_group_name_H-M   'P bca'

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

_cell_length_a                   12.852(5)
_cell_length_b                   15.692(5)
_cell_length_c                   25.641(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5171(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2048
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9847
_exptl_absorpt_correction_T_max  0.9847
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52261
_diffrn_reflns_av_R_equivalents  0.1095
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         27.49
_reflns_number_total             5941
_reflns_number_gt                4437
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0681P)²+1.6496P] 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         5941
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0763
_refine_ls_wR_factor_ref         0.1886
_refine_ls_wR_factor_gt          0.1726
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_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
N1 N 0.13990(14) 0.06931(12) 0.63919(7) 0.0489(4) Uani 1 1 d . . .
H1B H 0.1949 0.0387 0.6428 0.059 Uiso 1 1 calc R . .
N2 N 0.03303(14) 0.16628(12) 0.60745(7) 0.0495(4) Uani 1 1 d . . .
C1 C -0.2494(3) 0.18080(19) 0.73209(13) 0.0798(9) Uani 1 1 d . . .
H1A H -0.2704 0.1789 0.7668 0.096 Uiso 1 1 calc R . .
C2 C -0.3167(2) 0.21100(18) 0.69491(15) 0.0818(9) Uani 1 1 d . . .
H2A H -0.3828 0.2296 0.7044 0.098 Uiso 1 1 calc R . .
C3 C -0.2863(2) 0.21358(18) 0.64385(13) 0.0752(8) Uani 1 1 d . . .
H3A H -0.3315 0.2345 0.6186 0.090 Uiso 1 1 calc R . .
C4 C 0.4400(2) 0.33247(19) 0.60116(12) 0.0778(8) Uani 1 1 d . . .
H4A H 0.4915 0.3717 0.6098 0.093 Uiso 1 1 calc R . .
C5 C 0.4379(2) 0.29752(17) 0.55283(11) 0.0675(7) Uani 1 1 d . . .
H5A H 0.4880 0.3132 0.5285 0.081 Uiso 1 1 calc R . .
C6 C -0.1496(2) 0.15282(16) 0.71860(10) 0.0642(7) Uani 1 1 d . . .
H6A H -0.1044 0.1334 0.7443 0.077 Uiso 1 1 calc R . .
C7 C -0.04943(19) -0.04053(15) 0.72265(9) 0.0544(5) Uani 1 1 d . . .
H7A H -0.1090 -0.0255 0.7042 0.065 Uiso 1 1 calc R . .
C8 C -0.18839(19) 0.18504(16) 0.62982(10) 0.0603(6) Uani 1 1 d . . .
H8A H -0.1690 0.1865 0.5949 0.072 Uiso 1 1 calc R . .
C9 C 0.1262(2) -0.08788(17) 0.77731(9) 0.0652(7) Uani 1 1 d . . .
H9A H 0.1857 -0.1041 0.7954 0.078 Uiso 1 1 calc R . .
C10 C -0.0550(2) -0.10323(16) 0.76093(10) 0.0652(7) Uani 1 1 d . . .
H10A H -0.1183 -0.1294 0.7681 0.078 Uiso 1 1 calc R . .
C11 C 0.0326(3) -0.12678(16) 0.78826(10) 0.0695(7) Uani 1 1 d . . .
H11A H 0.0286 -0.1686 0.8139 0.083 Uiso 1 1 calc R . .
C12 C 0.14092(19) 0.00864(18) 0.45271(10) 0.0655(7) Uani 1 1 d . . .
H12A H 0.0941 -0.0345 0.4445 0.079 Uiso 1 1 calc R . .
C13 C 0.2157(2) 0.03390(18) 0.41560(10) 0.0664(7) Uani 1 1 d . . .
H13A H 0.2174 0.0078 0.3830 0.080 Uiso 1 1 calc R . .
C14 C 0.2874(2) 0.25338(16) 0.62640(9) 0.0613(6) Uani 1 1 d . . .
H14A H 0.2371 0.2405 0.6513 0.074 Uiso 1 1 calc R . .
C15 C 0.3642(2) 0.30940(18) 0.63842(11) 0.0754(8) Uani 1 1 d . . .
H15A H 0.3669 0.3329 0.6717 0.090 Uiso 1 1 calc R . .
C16 C 0.13241(19) -0.02477(15) 0.73955(9) 0.0556(6) Uani 1 1 d . . .
H16A H 0.1959 0.0013 0.7328 0.067 Uiso 1 1 calc R . .
C17 C 0.2850(2) 0.09576(17) 0.42713(9) 0.0595(6) Uani 1 1 d . . .
H17A H 0.3340 0.1117 0.4023 0.071 Uiso 1 1 calc R . .
C18 C -0.11799(17) 0.15407(13) 0.66666(8) 0.0471(5) Uani 1 1 d . . .
C19 C 0.13649(17) 0.04651(16) 0.50010(10) 0.0569(6) Uani 1 1 d . . .
H19A H 0.0863 0.0290 0.5239 0.068 Uiso 1 1 calc R . .
C20 C 0.12510(16) 0.13006(14) 0.60255(8) 0.0464(5) Uani 1 1 d . . .
C21 C 0.20651(16) 0.15280(14) 0.56334(8) 0.0463(5) Uani 1 1 d . . .
C22 C 0.20738(16) 0.11277(14) 0.51428(8) 0.0455(5) Uani 1 1 d . . .
C23 C 0.05183(16) 0.06464(13) 0.66986(8) 0.0444(5) Uani 1 1 d . . .
C24 C 0.35794(17) 0.19864(15) 0.48980(9) 0.0526(5) Uani 1 1 d . . .
H24A H 0.4073 0.2147 0.4651 0.063 Uiso 1 1 calc R . .
C25 C -0.01380(16) 0.12593(13) 0.64970(8) 0.0442(5) Uani 1 1 d . . .
C26 C 0.35980(17) 0.23685(14) 0.53865(9) 0.0504(5) Uani 1 1 d . . .
C27 C 0.28466(16) 0.13724(14) 0.47667(8) 0.0469(5) Uani 1 1 d . . .
C28 C 0.04429(17) -0.00011(13) 0.71170(8) 0.0454(5) Uani 1 1 d . . .
C29 C 0.28245(17) 0.21386(14) 0.57636(8) 0.0477(5) Uani 1 1 d . . .
C30 C 0.4182(2) 0.0108(2) 0.61897(12) 0.0758(8) Uani 1 1 d . . .
O2 O 0.33845(16) -0.00045(17) 0.64261(9) 0.1004(8) Uani 1 1 d . . .
O1 O 0.44295(18) -0.03453(18) 0.57734(10) 0.1065(8) Uani 1 1 d . . .
C31 C 0.4990(3) 0.0739(2) 0.63301(14) 0.0933(10) Uani 1 1 d . . .
H31A H 0.4775 0.1046 0.6635 0.140 Uiso 1 1 calc R . .
H31B H 0.5085 0.1130 0.6046 0.140 Uiso 1 1 calc R . .
H31C H 0.5633 0.0449 0.6400 0.140 Uiso 1 1 calc R . .
C33 C 0.3780(3) -0.1098(3) 0.50448(16) 0.1118(12) Uani 1 1 d . . .
H33A H 0.3301 -0.1528 0.4930 0.168 Uiso 1 1 calc R . .
H33B H 0.4475 -0.1260 0.4951 0.168 Uiso 1 1 calc R . .
H33C H 0.3609 -0.0565 0.4882 0.168 Uiso 1 1 calc R . .
C32 C 0.3709(4) -0.1009(3) 0.56031(18) 0.1343(17) Uani 1 1 d . . .
H32A H 0.3884 -0.1545 0.5770 0.161 Uiso 1 1 calc R . .
H32B H 0.3004 -0.0858 0.5701 0.161 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
N1 C20 1.352(3) . ?
N1 C23 1.380(3) . ?
N2 C20 1.319(3) . ?
N2 C25 1.392(3) . ?
C1 C2 1.372(5) . ?
C1 C6 1.399(4) . ?
C2 C3 1.367(4) . ?
C3 C8 1.384(4) . ?
C4 C5 1.356(4) . ?
C4 C15 1.412(4) . ?
C5 C26 1.430(3) . ?
C6 C18 1.393(3) . ?
C7 C28 1.390(3) . ?
C7 C10 1.392(3) . ?
C8 C18 1.395(3) . ?
C9 C11 1.378(4) . ?
C9 C16 1.387(3) . ?
C10 C11 1.376(4) . ?
C12 C19 1.354(3) . ?
C12 C13 1.410(4) . ?
C13 C17 1.350(4) . ?
C14 C15 1.357(4) . ?
C14 C29 1.427(3) . ?
C16 C28 1.394(3) . ?
C17 C27 1.427(3) . ?
C18 C25 1.475(3) . ?
C19 C22 1.429(3) . ?
C20 C21 1.494(3) . ?
C21 C22 1.406(3) . ?
C21 C29 1.408(3) . ?
C22 C27 1.437(3) . ?
C23 C25 1.380(3) . ?
C23 C28 1.481(3) . ?
C24 C27 1.389(3) . ?
C24 C26 1.389(3) . ?
C26 C29 1.433(3) . ?
C30 O2 1.204(3) . ?
C30 O1 1.321(4) . ?
C30 C31 1.479(5) . ?
O1 C32 1.460(4) . ?
C33 C32 1.441(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
C20 N1 C23 108.54(17) . . ?
C20 N2 C25 105.44(17) . . ?
C2 C1 C6 121.0(3) . . ?
C3 C2 C1 119.7(3) . . ?
C2 C3 C8 120.0(3) . . ?
C5 C4 C15 120.1(3) . . ?
C4 C5 C26 121.1(2) . . ?
C18 C6 C1 120.0(3) . . ?
C28 C7 C10 120.6(2) . . ?
C3 C8 C18 121.8(3) . . ?
C11 C9 C16 120.6(2) . . ?
C11 C10 C7 120.5(2) . . ?
C10 C11 C9 119.4(2) . . ?
C19 C12 C13 120.7(2) . . ?
C17 C13 C12 120.3(2) . . ?
C15 C14 C29 121.2(2) . . ?
C14 C15 C4 120.9(3) . . ?
C9 C16 C28 120.6(2) . . ?
C13 C17 C27 121.4(2) . . ?
C6 C18 C8 117.6(2) . . ?
C6 C18 C25 122.8(2) . . ?
C8 C18 C25 119.6(2) . . ?
C12 C19 C22 121.4(2) . . ?
N2 C20 N1 111.34(18) . . ?
N2 C20 C21 126.12(19) . . ?
N1 C20 C21 122.52(19) . . ?
C22 C21 C29 120.71(19) . . ?
C22 C21 C20 120.05(19) . . ?
C29 C21 C20 119.24(19) . . ?
C21 C22 C19 123.2(2) . . ?
C21 C22 C27 119.1(2) . . ?
C19 C22 C27 117.7(2) . . ?
C25 C23 N1 104.53(17) . . ?
C25 C23 C28 135.21(19) . . ?
N1 C23 C28 120.19(18) . . ?
C27 C24 C26 122.0(2) . . ?
C23 C25 N2 110.14(18) . . ?
C23 C25 C18 130.77(19) . . ?
N2 C25 C18 119.06(18) . . ?
C24 C26 C5 121.9(2) . . ?
C24 C26 C29 119.2(2) . . ?
C5 C26 C29 118.9(2) . . ?
C24 C27 C17 122.0(2) . . ?
C24 C27 C22 119.4(2) . . ?
C17 C27 C22 118.5(2) . . ?
C7 C28 C16 118.3(2) . . ?
C7 C28 C23 121.07(19) . . ?
C16 C28 C23 120.57(19) . . ?
C21 C29 C14 122.7(2) . . ?
C21 C29 C26 119.5(2) . . ?
C14 C29 C26 117.8(2) . . ?
O2 C30 O1 122.2(3) . . ?
O2 C30 C31 125.0(3) . . ?
O1 C30 C31 112.8(3) . . ?
C30 O1 C32 118.2(3) . . ?
C33 C32 O1 109.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.044
_database_code_depnum_ccdc_archive 'CCDC 993935'
