# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 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_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H30 N2 O3'
_chemical_formula_sum            'C30 H30 N2 O3'
_chemical_formula_weight         466.56

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   P21/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                   9.8277(4)
_cell_length_b                   9.8709(4)
_cell_length_c                   26.4181(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.566(2)
_cell_angle_gamma                90.00
_cell_volume                     2560.20(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    7911
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      23.2

_exptl_crystal_description       prisms
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
SADABS.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153(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  
;
 Nonius Kappa CCD with Bruker Apex II detector
;
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43491
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5876
_reflns_number_gt                3974
_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Apex II release 2010, Bruker AXS, Inc.'
_computing_cell_refinement       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_reduction        'Apex II release 2010, Bruker AXS, Inc.'

_computing_structure_solution    
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'





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

 The cyclopropenone ring was disordered.  The disorder was 
due to the inversion of configuration at C1.  The disorder involved the 
methyl carbon atom, C6, the adjacent carbonyl and methylene groups.  The 
disorder was modeled by assigning the variable x to the site occupancy 
factor for one set of atoms and (1-x) to the site occupancy for the 
alternate set of atoms.  A common isotropic displacement parameter was 
refined for all the atoms involved.  The geometry of the two groups was 
restrained to be equivalent throughout the refinement.  In this way, the 
site occupancy for the major component consisting of atoms, C1 C2, C5, C6 
and O1, refined to 63(2)%.  The atoms of both groups were refined 
anisotropically with their displacement parameters restrained to be 
approximately isotropic in the final refinement model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+1.9897P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5876
_refine_ls_number_parameters     368
_refine_ls_number_restraints     194
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0672
_refine_ls_wR_factor_ref         0.1462
_refine_ls_wR_factor_gt          0.1306
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.4544(15) 0.8632(10) 0.1238(5) 0.041(2) Uani 0.63 1 d PDU A 1
C1 C 0.3106(4) 0.6767(4) 0.09324(16) 0.0317(9) Uani 0.63 1 d PDU A 1
H1 H 0.3039 0.6965 0.0561 0.038 Uiso 0.63 1 calc PR A 1
C2 C 0.4395(6) 0.7435(9) 0.1157(3) 0.0319(15) Uani 0.63 1 d PDU A 1
C5 C 0.3371(12) 0.5252(6) 0.1004(5) 0.037(2) Uani 0.63 1 d PDU A 1
H5A H 0.2732 0.4863 0.1244 0.044 Uiso 0.63 1 calc PR A 1
H5B H 0.3251 0.4770 0.0676 0.044 Uiso 0.63 1 calc PR A 1
C6 C 0.1835(4) 0.7288(6) 0.1166(2) 0.0585(14) Uani 0.63 1 d PDU A 1
H6A H 0.1881 0.7096 0.1530 0.088 Uiso 0.63 1 calc PR A 1
H6B H 0.1036 0.6838 0.1008 0.088 Uiso 0.63 1 calc PR A 1
H6C H 0.1762 0.8268 0.1112 0.088 Uiso 0.63 1 calc PR A 1
O1A O 0.448(3) 0.8599(18) 0.1364(8) 0.043(4) Uani 0.37 1 d PDU A 2
C1A C 0.2922(8) 0.6712(8) 0.1198(3) 0.0424(16) Uani 0.37 1 d PDU A 2
H1A H 0.2467 0.6731 0.1529 0.051 Uiso 0.37 1 calc PR A 2
C2A C 0.4299(10) 0.7403(16) 0.1291(5) 0.033(2) Uani 0.37 1 d PDU A 2
C5A C 0.327(2) 0.5236(10) 0.1100(8) 0.033(3) Uani 0.37 1 d PDU A 2
H5A1 H 0.3025 0.4988 0.0744 0.039 Uiso 0.37 1 calc PR A 2
H5A2 H 0.2766 0.4633 0.1326 0.039 Uiso 0.37 1 calc PR A 2
C6A C 0.1995(9) 0.7435(9) 0.0830(4) 0.064(2) Uani 0.37 1 d PDU A 2
H6A1 H 0.2410 0.7472 0.0500 0.097 Uiso 0.37 1 calc PR A 2
H6A2 H 0.1840 0.8359 0.0951 0.097 Uiso 0.37 1 calc PR A 2
H6A3 H 0.1124 0.6953 0.0796 0.097 Uiso 0.37 1 calc PR A 2
C3 C 0.5378(2) 0.6349(2) 0.12842(8) 0.0287(5) Uani 1 1 d . . .
C4 C 0.4824(2) 0.5121(2) 0.12115(8) 0.0282(5) Uani 1 1 d . A .
C7 C 0.7319(2) 0.6124(2) 0.19047(8) 0.0260(5) Uani 1 1 d . . .
C8 C 0.8721(2) 0.6058(3) 0.20004(10) 0.0385(6) Uani 1 1 d . A .
H8 H 0.9336 0.6420 0.1768 0.046 Uiso 1 1 calc R . .
C9 C 0.9182(3) 0.5449(3) 0.24437(11) 0.0465(7) Uani 1 1 d . . .
H9 H 1.0133 0.5393 0.2524 0.056 Uiso 1 1 calc R A .
C10 C 0.8274(3) 0.4923(3) 0.27700(10) 0.0481(7) Uani 1 1 d . A .
H10 H 0.8579 0.4493 0.3076 0.058 Uiso 1 1 calc R . .
C11 C 0.6916(3) 0.5035(3) 0.26413(10) 0.0468(7) Uani 1 1 d . . .
H11 H 0.6285 0.4668 0.2866 0.056 Uiso 1 1 calc R A .
C12 C 0.7456(2) 0.7608(2) 0.11607(8) 0.0319(5) Uani 1 1 d . . .
C13 C 0.7314(3) 0.8749(3) 0.03427(10) 0.0516(7) Uani 1 1 d . . .
C14 C 0.6367(4) 0.8507(3) -0.01123(12) 0.0845(12) Uani 1 1 d . A .
H14A H 0.6569 0.7624 -0.0261 0.127 Uiso 1 1 calc R . .
H14B H 0.6494 0.9221 -0.0363 0.127 Uiso 1 1 calc R . .
H14C H 0.5423 0.8517 -0.0008 0.127 Uiso 1 1 calc R . .
C15 C 0.7099(4) 1.0139(3) 0.05707(12) 0.0664(9) Uani 1 1 d . A .
H15A H 0.6161 1.0213 0.0679 0.100 Uiso 1 1 calc R . .
H15B H 0.7262 1.0836 0.0316 0.100 Uiso 1 1 calc R . .
H15C H 0.7734 1.0265 0.0863 0.100 Uiso 1 1 calc R . .
C16 C 0.8784(4) 0.8516(4) 0.02198(14) 0.0813(11) Uani 1 1 d . A .
H16A H 0.9380 0.8796 0.0508 0.122 Uiso 1 1 calc R . .
H16B H 0.8999 0.9049 -0.0079 0.122 Uiso 1 1 calc R . .
H16C H 0.8927 0.7552 0.0151 0.122 Uiso 1 1 calc R . .
C17 C 0.5535(2) 0.3810(2) 0.12447(8) 0.0288(5) Uani 1 1 d . . .
C18 C 0.5002(2) 0.2678(2) 0.14367(8) 0.0330(5) Uani 1 1 d . A .
H18 H 0.5501 0.1871 0.1383 0.040 Uiso 1 1 calc R . .
C19 C 0.3753(2) 0.2513(2) 0.17183(9) 0.0323(5) Uani 1 1 d . . .
C20 C 0.3429(2) 0.3420(2) 0.20997(9) 0.0380(6) Uani 1 1 d . A .
H20 H 0.3981 0.4196 0.2164 0.046 Uiso 1 1 calc R . .
C21 C 0.2302(2) 0.3190(3) 0.23852(10) 0.0430(6) Uani 1 1 d . . .
H21 H 0.2090 0.3809 0.2646 0.052 Uiso 1 1 calc R A .
C22 C 0.1489(3) 0.2075(3) 0.22952(10) 0.0454(6) Uani 1 1 d . A .
H22 H 0.0715 0.1927 0.2491 0.055 Uiso 1 1 calc R . .
C23 C 0.1805(3) 0.1173(3) 0.19193(10) 0.0433(6) Uani 1 1 d . . .
H23 H 0.1242 0.0404 0.1855 0.052 Uiso 1 1 calc R A .
C24 C 0.2931(2) 0.1378(2) 0.16366(9) 0.0376(6) Uani 1 1 d . A .
H24 H 0.3149 0.0740 0.1384 0.045 Uiso 1 1 calc R . .
C25 C 0.6936(2) 0.3761(2) 0.10467(8) 0.0294(5) Uani 1 1 d . A .
C26 C 0.7216(2) 0.4352(2) 0.05860(9) 0.0369(6) Uani 1 1 d . . .
H26 H 0.6505 0.4780 0.0390 0.044 Uiso 1 1 calc R A .
C27 C 0.8517(3) 0.4326(3) 0.04101(11) 0.0493(7) Uani 1 1 d . A .
H27 H 0.8693 0.4722 0.0092 0.059 Uiso 1 1 calc R . .
C28 C 0.9558(3) 0.3729(3) 0.06945(11) 0.0530(7) Uani 1 1 d . . .
H28 H 1.0457 0.3726 0.0577 0.064 Uiso 1 1 calc R A .
C29 C 0.9291(3) 0.3135(3) 0.11500(11) 0.0528(7) Uani 1 1 d . A .
H29 H 1.0007 0.2712 0.1345 0.063 Uiso 1 1 calc R . .
C30 C 0.7987(2) 0.3150(3) 0.13258(10) 0.0399(6) Uani 1 1 d . . .
H30 H 0.7813 0.2737 0.1641 0.048 Uiso 1 1 calc R A .
N1 N 0.67389(16) 0.66817(18) 0.14446(7) 0.0261(4) Uani 1 1 d . A .
N2 N 0.64233(19) 0.5637(2) 0.22145(7) 0.0345(5) Uani 1 1 d . A .
O2 O 0.84579(17) 0.82000(18) 0.13101(7) 0.0454(4) Uani 1 1 d . A .
O3 O 0.68638(17) 0.76989(16) 0.06968(6) 0.0377(4) Uani 1 1 d . A .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.042(3) 0.025(2) 0.056(6) -0.009(2) -0.005(3) 0.0107(18)
C1 0.0266(18) 0.0342(19) 0.034(2) -0.0024(19) -0.0076(17) 0.0081(15)
C2 0.031(2) 0.030(2) 0.035(3) -0.006(2) -0.001(2) 0.0093(18)
C5 0.028(3) 0.033(3) 0.048(4) 0.001(2) -0.008(3) 0.002(2)
C6 0.029(2) 0.062(3) 0.084(4) -0.019(3) 0.000(3) 0.010(2)
O1A 0.046(5) 0.033(4) 0.049(8) -0.014(4) -0.006(5) 0.015(3)
C1A 0.038(3) 0.041(3) 0.048(3) -0.003(3) -0.008(3) 0.008(3)
C2A 0.029(3) 0.029(3) 0.039(5) -0.004(4) -0.006(3) 0.008(3)
C5A 0.029(4) 0.032(4) 0.036(5) 0.002(3) -0.008(3) 0.004(3)
C6A 0.061(5) 0.048(4) 0.080(6) 0.000(5) -0.036(5) 0.010(4)
C3 0.0263(11) 0.0270(12) 0.0324(12) -0.0045(10) -0.0050(9) 0.0065(9)
C4 0.0299(11) 0.0264(12) 0.0276(11) -0.0014(9) -0.0054(9) 0.0058(9)
C7 0.0283(11) 0.0228(11) 0.0264(11) -0.0061(9) -0.0024(9) 0.0056(9)
C8 0.0280(12) 0.0427(14) 0.0444(14) -0.0006(12) -0.0035(10) 0.0056(11)
C9 0.0379(14) 0.0426(15) 0.0568(17) -0.0078(13) -0.0213(13) 0.0121(12)
C10 0.0632(18) 0.0407(15) 0.0386(15) 0.0028(12) -0.0200(13) 0.0082(13)
C11 0.0572(17) 0.0503(17) 0.0326(14) 0.0063(12) -0.0027(12) 0.0027(13)
C12 0.0342(12) 0.0305(12) 0.0311(12) -0.0068(10) 0.0015(10) 0.0053(10)
C13 0.084(2) 0.0363(15) 0.0353(14) 0.0029(12) 0.0081(14) 0.0020(14)
C14 0.158(4) 0.055(2) 0.0380(17) 0.0089(15) -0.023(2) -0.011(2)
C15 0.112(3) 0.0322(15) 0.0551(19) 0.0014(14) -0.0003(18) 0.0026(16)
C16 0.105(3) 0.071(2) 0.071(2) 0.0107(19) 0.048(2) 0.001(2)
C17 0.0333(12) 0.0249(11) 0.0279(11) -0.0032(9) -0.0023(9) 0.0056(9)
C18 0.0375(13) 0.0276(12) 0.0339(12) -0.0037(10) 0.0024(10) 0.0083(10)
C19 0.0362(12) 0.0265(12) 0.0342(12) 0.0038(10) -0.0006(10) 0.0060(10)
C20 0.0378(13) 0.0346(14) 0.0418(14) -0.0046(11) 0.0032(11) -0.0008(11)
C21 0.0415(14) 0.0445(15) 0.0436(15) -0.0068(12) 0.0081(12) 0.0020(12)
C22 0.0401(14) 0.0489(17) 0.0478(16) 0.0087(13) 0.0078(12) 0.0021(12)
C23 0.0452(15) 0.0300(13) 0.0544(16) 0.0102(12) -0.0002(12) -0.0017(11)
C24 0.0494(15) 0.0262(12) 0.0371(13) 0.0023(10) -0.0009(11) 0.0077(11)
C25 0.0344(12) 0.0229(11) 0.0310(12) -0.0061(9) 0.0013(9) 0.0035(9)
C26 0.0382(13) 0.0364(14) 0.0363(13) -0.0023(11) 0.0041(11) 0.0074(11)
C27 0.0513(16) 0.0535(17) 0.0446(16) -0.0016(13) 0.0186(13) 0.0021(13)
C28 0.0372(14) 0.0610(19) 0.0619(19) -0.0147(16) 0.0139(13) 0.0058(13)
C29 0.0422(15) 0.0579(18) 0.0574(18) -0.0084(15) -0.0056(13) 0.0200(13)
C30 0.0438(14) 0.0365(14) 0.0391(14) -0.0016(11) 0.0001(11) 0.0118(11)
N1 0.0236(9) 0.0263(10) 0.0281(9) -0.0039(8) -0.0025(7) 0.0033(7)
N2 0.0326(10) 0.0406(12) 0.0303(10) 0.0019(9) 0.0001(8) 0.0032(9)
O2 0.0394(10) 0.0502(11) 0.0464(11) 0.0006(9) 0.0005(8) -0.0116(9)
O3 0.0534(10) 0.0312(9) 0.0281(9) -0.0020(7) -0.0019(7) 0.0018(8)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.208(5) . ?
C1 C6 1.509(5) . ?
C1 C2 1.525(5) . ?
C1 C5 1.528(5) . ?
C1 H1 1.0000 . ?
C2 C3 1.472(9) . ?
C5 C4 1.513(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
O1A C2A 1.208(7) . ?
C1A C6A 1.485(7) . ?
C1A C5A 1.520(7) . ?
C1A C2A 1.525(7) . ?
C1A H1A 1.0000 . ?
C2A C3 1.487(15) . ?
C5A C4 1.551(19) . ?
C5A H5A1 0.9900 . ?
C5A H5A2 0.9900 . ?
C6A H6A1 0.9800 . ?
C6A H6A2 0.9800 . ?
C6A H6A3 0.9800 . ?
C3 C4 1.339(3) . ?
C3 N1 1.423(3) . ?
C4 C17 1.471(3) . ?
C7 N2 1.319(3) . ?
C7 C8 1.391(3) . ?
C7 N1 1.430(3) . ?
C8 C9 1.375(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.370(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.367(4) . ?
C10 H10 0.9500 . ?
C11 N2 1.345(3) . ?
C11 H11 0.9500 . ?
C12 O2 1.197(3) . ?
C12 O3 1.336(3) . ?
C12 N1 1.393(3) . ?
C13 O3 1.477(3) . ?
C13 C14 1.506(4) . ?
C13 C16 1.513(4) . ?
C13 C15 1.517(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.343(3) . ?
C17 C25 1.496(3) . ?
C18 C19 1.472(3) . ?
C18 H18 0.9500 . ?
C19 C24 1.393(3) . ?
C19 C20 1.395(3) . ?
C20 C21 1.386(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.374(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.380(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.380(3) . ?
C25 C26 1.389(3) . ?
C26 C27 1.379(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.375(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.374(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.383(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?

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 112.5(4) . . ?
C6 C1 C5 115.0(6) . . ?
C2 C1 C5 104.0(4) . . ?
C6 C1 H1 108.4 . . ?
C2 C1 H1 108.4 . . ?
C5 C1 H1 108.4 . . ?
O1 C2 C3 126.8(8) . . ?
O1 C2 C1 125.7(7) . . ?
C3 C2 C1 107.4(5) . . ?
C4 C5 C1 106.3(6) . . ?
C4 C5 H5A 110.5 . . ?
C1 C5 H5A 110.5 . . ?
C4 C5 H5B 110.5 . . ?
C1 C5 H5B 110.5 . . ?
H5A C5 H5B 108.7 . . ?
C6A C1A C5A 118.9(9) . . ?
C6A C1A C2A 113.9(7) . . ?
C5A C1A C2A 104.7(8) . . ?
C6A C1A H1A 106.2 . . ?
C5A C1A H1A 106.2 . . ?
C2A C1A H1A 106.2 . . ?
O1A C2A C3 126.0(14) . . ?
O1A C2A C1A 125.7(12) . . ?
C3 C2A C1A 108.3(9) . . ?
C1A C5A C4 105.2(10) . . ?
C1A C5A H5A1 110.7 . . ?
C4 C5A H5A1 110.7 . . ?
C1A C5A H5A2 110.7 . . ?
C4 C5A H5A2 110.7 . . ?
H5A1 C5A H5A2 108.8 . . ?
C1A C6A H6A1 109.5 . . ?
C1A C6A H6A2 109.5 . . ?
H6A1 C6A H6A2 109.5 . . ?
C1A C6A H6A3 109.5 . . ?
H6A1 C6A H6A3 109.5 . . ?
H6A2 C6A H6A3 109.5 . . ?
C4 C3 N1 128.49(19) . . ?
C4 C3 C2 111.6(3) . . ?
N1 C3 C2 119.9(3) . . ?
C4 C3 C2A 110.4(4) . . ?
N1 C3 C2A 119.8(4) . . ?
C3 C4 C17 126.78(19) . . ?
C3 C4 C5 110.2(3) . . ?
C17 C4 C5 122.3(3) . . ?
C3 C4 C5A 110.7(4) . . ?
C17 C4 C5A 122.5(4) . . ?
N2 C7 C8 123.6(2) . . ?
N2 C7 N1 114.57(18) . . ?
C8 C7 N1 121.8(2) . . ?
C9 C8 C7 117.5(2) . . ?
C9 C8 H8 121.3 . . ?
C7 C8 H8 121.3 . . ?
C10 C9 C8 120.1(2) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 117.9(2) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
N2 C11 C10 123.7(3) . . ?
N2 C11 H11 118.1 . . ?
C10 C11 H11 118.1 . . ?
O2 C12 O3 126.0(2) . . ?
O2 C12 N1 124.8(2) . . ?
O3 C12 N1 109.15(19) . . ?
O3 C13 C14 101.7(2) . . ?
O3 C13 C16 110.2(2) . . ?
C14 C13 C16 111.5(3) . . ?
O3 C13 C15 109.4(2) . . ?
C14 C13 C15 111.6(3) . . ?
C16 C13 C15 111.9(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C4 124.2(2) . . ?
C18 C17 C25 119.06(19) . . ?
C4 C17 C25 116.73(19) . . ?
C17 C18 C19 129.1(2) . . ?
C17 C18 H18 115.4 . . ?
C19 C18 H18 115.4 . . ?
C24 C19 C20 118.6(2) . . ?
C24 C19 C18 120.1(2) . . ?
C20 C19 C18 121.1(2) . . ?
C21 C20 C19 120.1(2) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C20 120.6(2) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 119.6(2) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 120.5(2) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C19 120.6(2) . . ?
C23 C24 H24 119.7 . . ?
C19 C24 H24 119.7 . . ?
C30 C25 C26 118.6(2) . . ?
C30 C25 C17 120.4(2) . . ?
C26 C25 C17 121.0(2) . . ?
C27 C26 C25 120.7(2) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C28 C27 C26 120.1(3) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C29 C28 C27 119.7(2) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 120.4(2) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C25 C30 C29 120.5(2) . . ?
C25 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C12 N1 C3 118.83(18) . . ?
C12 N1 C7 121.21(17) . . ?
C3 N1 C7 119.87(18) . . ?
C7 N2 C11 117.1(2) . . ?
C12 O3 C13 119.87(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 O1 -44.8(10) . . . . ?
C5 C1 C2 O1 -169.8(10) . . . . ?
C6 C1 C2 C3 131.8(5) . . . . ?
C5 C1 C2 C3 6.8(7) . . . . ?
C6 C1 C5 C4 -129.0(6) . . . . ?
C2 C1 C5 C4 -5.6(8) . . . . ?
C6A C1A C2A O1A 45.3(19) . . . . ?
C5A C1A C2A O1A 176.8(17) . . . . ?
C6A C1A C2A C3 -135.4(8) . . . . ?
C5A C1A C2A C3 -3.9(13) . . . . ?
C6A C1A C5A C4 135.7(10) . . . . ?
C2A C1A C5A C4 7.2(14) . . . . ?
O1 C2 C3 C4 170.9(9) . . . . ?
C1 C2 C3 C4 -5.7(5) . . . . ?
O1 C2 C3 N1 -11.1(10) . . . . ?
C1 C2 C3 N1 172.4(3) . . . . ?
O1 C2 C3 C2A 83(2) . . . . ?
C1 C2 C3 C2A -94(2) . . . . ?
O1A C2A C3 C4 177.8(15) . . . . ?
C1A C2A C3 C4 -1.5(10) . . . . ?
O1A C2A C3 N1 9.7(18) . . . . ?
C1A C2A C3 N1 -169.5(5) . . . . ?
O1A C2A C3 C2 -85(3) . . . . ?
C1A C2A C3 C2 96(2) . . . . ?
N1 C3 C4 C17 -5.1(4) . . . . ?
C2 C3 C4 C17 172.8(4) . . . . ?
C2A C3 C4 C17 -171.8(6) . . . . ?
N1 C3 C4 C5 -175.9(5) . . . . ?
C2 C3 C4 C5 2.0(6) . . . . ?
C2A C3 C4 C5 17.4(8) . . . . ?
N1 C3 C4 C5A 173.0(8) . . . . ?
C2 C3 C4 C5A -9.1(9) . . . . ?
C2A C3 C4 C5A 6.3(10) . . . . ?
C1 C5 C4 C3 2.5(8) . . . . ?
C1 C5 C4 C17 -168.8(4) . . . . ?
C1 C5 C4 C5A 97(3) . . . . ?
C1A C5A C4 C3 -8.7(13) . . . . ?
C1A C5A C4 C17 169.5(6) . . . . ?
C1A C5A C4 C5 -98(3) . . . . ?
N2 C7 C8 C9 0.0(4) . . . . ?
N1 C7 C8 C9 -177.2(2) . . . . ?
C7 C8 C9 C10 0.7(4) . . . . ?
C8 C9 C10 C11 -0.5(4) . . . . ?
C9 C10 C11 N2 -0.3(4) . . . . ?
C3 C4 C17 C18 142.5(3) . . . . ?
C5 C4 C17 C18 -47.7(6) . . . . ?
C5A C4 C17 C18 -35.4(10) . . . . ?
C3 C4 C17 C25 -37.9(3) . . . . ?
C5 C4 C17 C25 132.0(6) . . . . ?
C5A C4 C17 C25 144.2(9) . . . . ?
C4 C17 C18 C19 -10.3(4) . . . . ?
C25 C17 C18 C19 170.0(2) . . . . ?
C17 C18 C19 C24 141.8(2) . . . . ?
C17 C18 C19 C20 -43.6(4) . . . . ?
C24 C19 C20 C21 -0.6(3) . . . . ?
C18 C19 C20 C21 -175.2(2) . . . . ?
C19 C20 C21 C22 -0.3(4) . . . . ?
C20 C21 C22 C23 0.5(4) . . . . ?
C21 C22 C23 C24 0.4(4) . . . . ?
C22 C23 C24 C19 -1.3(4) . . . . ?
C20 C19 C24 C23 1.4(3) . . . . ?
C18 C19 C24 C23 176.1(2) . . . . ?
C18 C17 C25 C30 -46.8(3) . . . . ?
C4 C17 C25 C30 133.5(2) . . . . ?
C18 C17 C25 C26 134.7(2) . . . . ?
C4 C17 C25 C26 -45.0(3) . . . . ?
C30 C25 C26 C27 0.2(4) . . . . ?
C17 C25 C26 C27 178.7(2) . . . . ?
C25 C26 C27 C28 -1.0(4) . . . . ?
C26 C27 C28 C29 1.3(4) . . . . ?
C27 C28 C29 C30 -0.8(4) . . . . ?
C26 C25 C30 C29 0.2(4) . . . . ?
C17 C25 C30 C29 -178.3(2) . . . . ?
C28 C29 C30 C25 0.0(4) . . . . ?
O2 C12 N1 C3 162.0(2) . . . . ?
O3 C12 N1 C3 -19.4(3) . . . . ?
O2 C12 N1 C7 -14.6(3) . . . . ?
O3 C12 N1 C7 164.03(17) . . . . ?
C4 C3 N1 C12 128.7(3) . . . . ?
C2 C3 N1 C12 -49.0(4) . . . . ?
C2A C3 N1 C12 -65.7(6) . . . . ?
C4 C3 N1 C7 -54.7(3) . . . . ?
C2 C3 N1 C7 127.6(4) . . . . ?
C2A C3 N1 C7 111.0(6) . . . . ?
N2 C7 N1 C12 158.75(19) . . . . ?
C8 C7 N1 C12 -23.9(3) . . . . ?
N2 C7 N1 C3 -17.8(3) . . . . ?
C8 C7 N1 C3 159.6(2) . . . . ?
C8 C7 N2 C11 -0.8(3) . . . . ?
N1 C7 N2 C11 176.6(2) . . . . ?
C10 C11 N2 C7 0.9(4) . . . . ?
O2 C12 O3 C13 -9.7(3) . . . . ?
N1 C12 O3 C13 171.72(19) . . . . ?
C14 C13 O3 C12 -178.4(2) . . . . ?
C16 C13 O3 C12 63.2(3) . . . . ?
C15 C13 O3 C12 -60.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.042
_database_code_depnum_ccdc_archive 'CCDC 966192'
#######################################################################
#
#                 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_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H27 N O3'
_chemical_formula_sum            'C25 H27 N O3'
_chemical_formula_weight         389.48

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   P21/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                   7.5842(5)
_cell_length_b                   14.8337(12)
_cell_length_c                   19.3190(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.285(3)
_cell_angle_gamma                90.00
_cell_volume                     2169.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    6094
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.4

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
SADABS.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153(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  'Nonius Kappa CCD with Bruker APEX II detector'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39407
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3796
_reflns_number_gt                2509
_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Apex II release 2010, Bruker AXS, Inc.'
_computing_cell_refinement       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_reduction        'Apex II release 2010, Bruker AXS, Inc.'

_computing_structure_solution    
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'







_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
	The methyl groups of the t-butyl group were disrodered.  The disorder 
was modeled by assigning the variable x to the site occupancy factors for 
one component of the disorder.  The variable (1-x) was assigned to the site 
occupancy factors for the alternate component.  A common isotropic 
displacement parameter was refined while refining x.  The geometry of the 
two components was restrained to be equivalent throughout the refinement 
process.  In this way, the major component of the disorder consisting of 
atoms, C9, C10 and C11, had a refined site occupancy of 53(1)%.  The non-H 
atoms involved in the disorder were refined anisotropically with their 
displacement parameters restrained to be approximately isotropic in the 
final refinement model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+1.0332P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0049(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3796
_refine_ls_number_parameters     303
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1253
_refine_ls_wR_factor_gt          0.1027
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001

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 0.3882(3) 0.32898(15) 0.64545(11) 0.0329(6) Uani 1 1 d . . .
H1 H 0.2592 0.3207 0.6334 0.039 Uiso 1 1 calc R . .
C2 C 0.4673(3) 0.38421(15) 0.58918(11) 0.0253(5) Uani 1 1 d . . .
C3 C 0.5839(3) 0.32608(14) 0.55051(10) 0.0227(5) Uani 1 1 d . . .
C4 C 0.5978(3) 0.24438(14) 0.58062(11) 0.0262(5) Uani 1 1 d . . .
C5 C 0.4804(3) 0.23739(15) 0.64121(12) 0.0357(6) Uani 1 1 d . . .
H5A H 0.5516 0.2247 0.6847 0.043 Uiso 1 1 calc R . .
H5B H 0.3925 0.1886 0.6333 0.043 Uiso 1 1 calc R . .
C6 C 0.4104(4) 0.37470(17) 0.71490(12) 0.0454(7) Uani 1 1 d . . .
H6A H 0.5364 0.3812 0.7281 0.068 Uiso 1 1 calc R . .
H6B H 0.3540 0.3383 0.7497 0.068 Uiso 1 1 calc R . .
H6C H 0.3550 0.4344 0.7121 0.068 Uiso 1 1 calc R . .
C7 C 0.8298(3) 0.34295(14) 0.47500(11) 0.0245(5) Uani 1 1 d . . .
C8 C 1.0363(3) 0.38386(17) 0.38785(12) 0.0345(6) Uani 1 1 d . . .
C9 C 1.190(2) 0.3982(8) 0.4442(7) 0.041(3) Uani 0.53 1 d PDU A 1
H9A H 1.2069 0.3429 0.4715 0.062 Uiso 0.53 1 calc PR A 1
H9B H 1.1596 0.4479 0.4748 0.062 Uiso 0.53 1 calc PR A 1
H9C H 1.2986 0.4127 0.4217 0.062 Uiso 0.53 1 calc PR A 1
C10 C 1.0422(15) 0.3030(6) 0.3501(5) 0.046(2) Uani 0.53 1 d PDU A 1
H10A H 1.1523 0.3003 0.3260 0.070 Uiso 0.53 1 calc PR A 1
H10B H 0.9414 0.3005 0.3160 0.070 Uiso 0.53 1 calc PR A 1
H10C H 1.0369 0.2517 0.3818 0.070 Uiso 0.53 1 calc PR A 1
C11 C 1.0361(11) 0.4714(5) 0.3417(4) 0.055(2) Uani 0.53 1 d PDU A 1
H11A H 1.1414 0.4717 0.3145 0.083 Uiso 0.53 1 calc PR A 1
H11B H 1.0369 0.5248 0.3716 0.083 Uiso 0.53 1 calc PR A 1
H11C H 0.9300 0.4721 0.3103 0.083 Uiso 0.53 1 calc PR A 1
C9A C 1.170(3) 0.4219(10) 0.4326(8) 0.069(5) Uani 0.47 1 d PDU A 2
H9A1 H 1.1826 0.3867 0.4755 0.103 Uiso 0.47 1 calc PR A 2
H9A2 H 1.1392 0.4842 0.4435 0.103 Uiso 0.47 1 calc PR A 2
H9A3 H 1.2826 0.4213 0.4098 0.103 Uiso 0.47 1 calc PR A 2
C10A C 1.076(2) 0.2781(7) 0.3722(7) 0.064(4) Uani 0.47 1 d PDU A 2
H10D H 0.9731 0.2511 0.3472 0.096 Uiso 0.47 1 calc PR A 2
H10E H 1.1000 0.2460 0.4161 0.096 Uiso 0.47 1 calc PR A 2
H10F H 1.1789 0.2734 0.3440 0.096 Uiso 0.47 1 calc PR A 2
C11A C 1.0002(12) 0.4273(6) 0.3185(4) 0.059(3) Uani 0.47 1 d PDU A 2
H11D H 1.1101 0.4312 0.2944 0.089 Uiso 0.47 1 calc PR A 2
H11E H 0.9529 0.4880 0.3249 0.089 Uiso 0.47 1 calc PR A 2
H11F H 0.9139 0.3912 0.2909 0.089 Uiso 0.47 1 calc PR A 2
C12 C 0.6995(3) 0.16423(14) 0.56008(11) 0.0285(5) Uani 1 1 d . . .
C13 C 0.8224(3) 0.12579(15) 0.60288(11) 0.0319(6) Uani 1 1 d . . .
H13 H 0.8670 0.0694 0.5884 0.038 Uiso 1 1 calc R . .
C14 C 0.8966(3) 0.16042(15) 0.66969(11) 0.0307(5) Uani 1 1 d . . .
C15 C 0.9192(3) 0.25214(16) 0.68305(13) 0.0381(6) Uani 1 1 d . . .
H15 H 0.8879 0.2947 0.6477 0.046 Uiso 1 1 calc R . .
C16 C 0.9863(3) 0.28204(18) 0.74695(13) 0.0413(6) Uani 1 1 d . . .
H16 H 0.9989 0.3449 0.7552 0.050 Uiso 1 1 calc R . .
C17 C 1.0354(3) 0.22149(18) 0.79899(12) 0.0387(6) Uani 1 1 d . . .
H17 H 1.0795 0.2424 0.8431 0.046 Uiso 1 1 calc R . .
C18 C 1.0196(3) 0.13049(17) 0.78608(12) 0.0373(6) Uani 1 1 d . . .
H18 H 1.0557 0.0883 0.8211 0.045 Uiso 1 1 calc R . .
C19 C 0.9512(3) 0.10024(16) 0.72234(12) 0.0341(6) Uani 1 1 d . . .
H19 H 0.9412 0.0372 0.7142 0.041 Uiso 1 1 calc R . .
C20 C 0.6461(3) 0.12253(14) 0.49216(11) 0.0319(6) Uani 1 1 d . . .
C21 C 0.4725(3) 0.12734(16) 0.46556(12) 0.0389(6) Uani 1 1 d . . .
H21 H 0.3890 0.1616 0.4893 0.047 Uiso 1 1 calc R . .
C22 C 0.4196(4) 0.08294(17) 0.40488(13) 0.0494(7) Uani 1 1 d . . .
H22 H 0.2999 0.0863 0.3876 0.059 Uiso 1 1 calc R . .
C23 C 0.5393(5) 0.03390(18) 0.36935(13) 0.0548(8) Uani 1 1 d . . .
H23 H 0.5021 0.0023 0.3283 0.066 Uiso 1 1 calc R . .
C24 C 0.7124(5) 0.03095(19) 0.39366(14) 0.0569(8) Uani 1 1 d . . .
H24 H 0.7961 -0.0015 0.3687 0.068 Uiso 1 1 calc R . .
C25 C 0.7663(4) 0.07508(17) 0.45453(13) 0.0460(7) Uani 1 1 d . . .
H25 H 0.8869 0.0728 0.4707 0.055 Uiso 1 1 calc R . .
N2 N 0.6627(2) 0.36273(13) 0.49354(9) 0.0237(4) Uani 1 1 d . . .
O1 O 0.44155(19) 0.46424(10) 0.57823(7) 0.0298(4) Uani 1 1 d . . .
O2 O 0.9285(2) 0.29149(12) 0.50521(10) 0.0514(5) Uani 1 1 d . . .
O3 O 0.86369(19) 0.39045(11) 0.41890(8) 0.0354(4) Uani 1 1 d . A .
H2N H 0.616(3) 0.4103(16) 0.4762(12) 0.034(7) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0386(14) 0.0320(13) 0.0286(13) 0.0036(11) 0.0079(11) 0.0020(11)
C2 0.0269(13) 0.0282(13) 0.0206(12) 0.0011(10) -0.0013(9) -0.0003(10)
C3 0.0246(12) 0.0252(12) 0.0181(11) 0.0017(9) -0.0009(9) -0.0006(9)
C4 0.0305(13) 0.0247(12) 0.0231(12) 0.0000(10) -0.0003(10) -0.0016(10)
C5 0.0455(15) 0.0293(13) 0.0333(13) 0.0070(11) 0.0122(11) 0.0014(11)
C6 0.0682(19) 0.0379(15) 0.0313(14) 0.0035(12) 0.0132(13) 0.0023(13)
C7 0.0267(13) 0.0246(12) 0.0217(12) 0.0003(10) -0.0014(10) -0.0002(10)
C8 0.0203(13) 0.0549(16) 0.0285(13) 0.0030(12) 0.0038(10) 0.0032(11)
C9 0.025(4) 0.052(4) 0.047(6) 0.002(4) -0.003(4) -0.010(3)
C10 0.027(4) 0.068(6) 0.045(5) -0.023(4) 0.006(3) -0.005(4)
C11 0.037(4) 0.079(5) 0.050(5) 0.033(4) 0.014(3) 0.005(4)
C9A 0.061(10) 0.111(11) 0.035(5) -0.009(7) 0.008(5) -0.042(9)
C10A 0.057(8) 0.070(6) 0.067(8) -0.010(5) 0.025(6) 0.018(5)
C11A 0.041(5) 0.099(7) 0.039(5) 0.022(4) 0.017(3) 0.004(5)
C12 0.0378(14) 0.0220(12) 0.0259(12) 0.0038(10) 0.0042(10) 0.0006(10)
C13 0.0434(15) 0.0239(12) 0.0287(13) 0.0037(10) 0.0035(11) 0.0061(11)
C14 0.0321(13) 0.0330(13) 0.0272(13) 0.0043(11) 0.0024(10) 0.0050(11)
C15 0.0460(15) 0.0327(14) 0.0347(14) 0.0070(11) -0.0046(11) -0.0010(12)
C16 0.0451(16) 0.0394(15) 0.0384(15) -0.0035(12) -0.0062(12) -0.0029(12)
C17 0.0332(15) 0.0538(17) 0.0286(14) -0.0026(12) -0.0038(11) 0.0006(12)
C18 0.0363(15) 0.0492(16) 0.0265(13) 0.0093(12) 0.0022(11) 0.0110(12)
C19 0.0368(14) 0.0338(13) 0.0323(14) 0.0048(11) 0.0056(11) 0.0079(11)
C20 0.0509(17) 0.0215(12) 0.0236(12) 0.0044(10) 0.0050(11) 0.0035(11)
C21 0.0533(18) 0.0295(14) 0.0335(14) -0.0006(11) 0.0003(12) -0.0017(12)
C22 0.070(2) 0.0381(15) 0.0389(16) 0.0003(13) -0.0095(14) -0.0108(14)
C23 0.105(3) 0.0337(15) 0.0251(14) -0.0014(12) -0.0036(16) -0.0013(16)
C24 0.095(3) 0.0459(17) 0.0313(15) -0.0053(13) 0.0116(16) 0.0159(17)
C25 0.0644(18) 0.0433(15) 0.0307(15) 0.0013(12) 0.0056(13) 0.0146(13)
N2 0.0252(11) 0.0257(10) 0.0204(10) 0.0064(8) 0.0025(8) 0.0057(9)
O1 0.0370(9) 0.0257(9) 0.0268(9) 0.0043(7) 0.0033(7) 0.0057(7)
O2 0.0337(10) 0.0592(12) 0.0623(12) 0.0341(10) 0.0117(9) 0.0169(9)
O3 0.0280(9) 0.0523(11) 0.0266(9) 0.0147(8) 0.0087(7) 0.0100(8)

_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 1.504(3) . ?
C1 C2 1.512(3) . ?
C1 C5 1.532(3) . ?
C1 H1 1.0000 . ?
C2 O1 1.220(2) . ?
C2 C3 1.470(3) . ?
C3 C4 1.346(3) . ?
C3 N2 1.392(3) . ?
C4 C12 1.484(3) . ?
C4 C5 1.515(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 O2 1.197(2) . ?
C7 O3 1.330(2) . ?
C7 N2 1.369(3) . ?
C8 C10 1.407(9) . ?
C8 C9A 1.414(14) . ?
C8 O3 1.474(3) . ?
C8 C11A 1.498(8) . ?
C8 C9 1.561(11) . ?
C8 C11 1.575(7) . ?
C8 C10A 1.630(11) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10A H10D 0.9800 . ?
C10A H10E 0.9800 . ?
C10A H10F 0.9800 . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12 C13 1.337(3) . ?
C12 C20 1.486(3) . ?
C13 C14 1.471(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.393(3) . ?
C14 C19 1.398(3) . ?
C15 C16 1.381(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.383(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.377(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.383(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.387(3) . ?
C20 C25 1.390(3) . ?
C21 C22 1.384(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.377(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.370(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.387(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
N2 H2N 0.85(2) . ?

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 111.61(19) . . ?
C6 C1 C5 114.8(2) . . ?
C2 C1 C5 103.94(17) . . ?
C6 C1 H1 108.8 . . ?
C2 C1 H1 108.8 . . ?
C5 C1 H1 108.8 . . ?
O1 C2 C3 125.29(19) . . ?
O1 C2 C1 125.87(19) . . ?
C3 C2 C1 108.82(18) . . ?
C4 C3 N2 131.83(19) . . ?
C4 C3 C2 110.06(18) . . ?
N2 C3 C2 118.07(18) . . ?
C3 C4 C12 129.42(19) . . ?
C3 C4 C5 111.15(18) . . ?
C12 C4 C5 119.32(18) . . ?
C4 C5 C1 105.72(17) . . ?
C4 C5 H5A 110.6 . . ?
C1 C5 H5A 110.6 . . ?
C4 C5 H5B 110.6 . . ?
C1 C5 H5B 110.6 . . ?
H5A C5 H5B 108.7 . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O2 C7 O3 126.2(2) . . ?
O2 C7 N2 124.8(2) . . ?
O3 C7 N2 108.94(18) . . ?
C10 C8 O3 108.9(5) . . ?
C9A C8 O3 110.4(10) . . ?
C9A C8 C11A 117.6(8) . . ?
O3 C8 C11A 102.4(4) . . ?
C10 C8 C9 115.7(6) . . ?
O3 C8 C9 110.5(7) . . ?
C10 C8 C11 114.1(5) . . ?
O3 C8 C11 101.8(3) . . ?
C9 C8 C11 105.0(6) . . ?
C9A C8 C10A 111.3(8) . . ?
O3 C8 C10A 108.5(6) . . ?
C11A C8 C10A 106.0(6) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
C8 C9A H9A1 109.5 . . ?
C8 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C8 C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C8 C10A H10D 109.5 . . ?
C8 C10A H10E 109.5 . . ?
H10D C10A H10E 109.5 . . ?
C8 C10A H10F 109.5 . . ?
H10D C10A H10F 109.5 . . ?
H10E C10A H10F 109.5 . . ?
C8 C11A H11D 109.5 . . ?
C8 C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
C8 C11A H11F 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C13 C12 C4 122.1(2) . . ?
C13 C12 C20 120.9(2) . . ?
C4 C12 C20 116.75(19) . . ?
C12 C13 C14 127.7(2) . . ?
C12 C13 H13 116.1 . . ?
C14 C13 H13 116.1 . . ?
C15 C14 C19 117.4(2) . . ?
C15 C14 C13 122.7(2) . . ?
C19 C14 C13 119.9(2) . . ?
C16 C15 C14 120.9(2) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 120.7(2) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 119.2(2) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 120.3(2) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C14 121.4(2) . . ?
C18 C19 H19 119.3 . . ?
C14 C19 H19 119.3 . . ?
C21 C20 C25 118.0(2) . . ?
C21 C20 C12 120.7(2) . . ?
C25 C20 C12 121.3(2) . . ?
C22 C21 C20 120.8(2) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C23 C22 C21 120.4(3) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C24 C23 C22 119.5(3) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 120.4(3) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C20 120.8(3) . . ?
C24 C25 H25 119.6 . . ?
C20 C25 H25 119.6 . . ?
C7 N2 C3 124.65(19) . . ?
C7 N2 H2N 116.4(16) . . ?
C3 N2 H2N 116.7(16) . . ?
C7 O3 C8 120.91(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 O1 -49.3(3) . . . . ?
C5 C1 C2 O1 -173.6(2) . . . . ?
C6 C1 C2 C3 129.5(2) . . . . ?
C5 C1 C2 C3 5.2(2) . . . . ?
O1 C2 C3 C4 173.1(2) . . . . ?
C1 C2 C3 C4 -5.7(3) . . . . ?
O1 C2 C3 N2 -4.8(3) . . . . ?
C1 C2 C3 N2 176.39(18) . . . . ?
N2 C3 C4 C12 -2.7(4) . . . . ?
C2 C3 C4 C12 179.7(2) . . . . ?
N2 C3 C4 C5 -178.8(2) . . . . ?
C2 C3 C4 C5 3.6(3) . . . . ?
C3 C4 C5 C1 -0.2(3) . . . . ?
C12 C4 C5 C1 -176.8(2) . . . . ?
C6 C1 C5 C4 -125.2(2) . . . . ?
C2 C1 C5 C4 -3.1(2) . . . . ?
C3 C4 C12 C13 122.2(3) . . . . ?
C5 C4 C12 C13 -62.0(3) . . . . ?
C3 C4 C12 C20 -63.9(3) . . . . ?
C5 C4 C12 C20 111.9(2) . . . . ?
C4 C12 C13 C14 -9.9(4) . . . . ?
C20 C12 C13 C14 176.5(2) . . . . ?
C12 C13 C14 C15 -33.0(4) . . . . ?
C12 C13 C14 C19 148.4(2) . . . . ?
C19 C14 C15 C16 -2.6(3) . . . . ?
C13 C14 C15 C16 178.8(2) . . . . ?
C14 C15 C16 C17 1.0(4) . . . . ?
C15 C16 C17 C18 1.1(4) . . . . ?
C16 C17 C18 C19 -1.6(4) . . . . ?
C17 C18 C19 C14 -0.1(4) . . . . ?
C15 C14 C19 C18 2.1(3) . . . . ?
C13 C14 C19 C18 -179.2(2) . . . . ?
C13 C12 C20 C21 144.6(2) . . . . ?
C4 C12 C20 C21 -29.4(3) . . . . ?
C13 C12 C20 C25 -33.2(3) . . . . ?
C4 C12 C20 C25 152.8(2) . . . . ?
C25 C20 C21 C22 2.7(3) . . . . ?
C12 C20 C21 C22 -175.2(2) . . . . ?
C20 C21 C22 C23 -0.8(4) . . . . ?
C21 C22 C23 C24 -1.4(4) . . . . ?
C22 C23 C24 C25 1.6(4) . . . . ?
C23 C24 C25 C20 0.4(4) . . . . ?
C21 C20 C25 C24 -2.5(4) . . . . ?
C12 C20 C25 C24 175.3(2) . . . . ?
O2 C7 N2 C3 0.4(4) . . . . ?
O3 C7 N2 C3 -179.17(18) . . . . ?
C4 C3 N2 C7 -33.7(4) . . . . ?
C2 C3 N2 C7 143.7(2) . . . . ?
O2 C7 O3 C8 -0.6(3) . . . . ?
N2 C7 O3 C8 178.95(18) . . . . ?
C10 C8 O3 C7 77.1(4) . . . . ?
C9A C8 O3 C7 -68.1(7) . . . . ?
C11A C8 O3 C7 165.9(4) . . . . ?
C9 C8 O3 C7 -51.0(5) . . . . ?
C11 C8 O3 C7 -162.1(3) . . . . ?
C10A C8 O3 C7 54.2(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
N2 H2N O1 0.85(2) 2.17(3) 3.002(2) 166(2) 3_666



_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.041
_database_code_depnum_ccdc_archive 'CCDC 966193'
#######################################################################
#
#                 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_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H72 N8 O4'
_chemical_formula_weight         1401.62

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           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   16.425
_cell_length_b                   14.739
_cell_length_c                   16.609
_cell_angle_alpha                90.00
_cell_angle_beta                 90.30
_cell_angle_gamma                90.00
_cell_volume                     4020.8
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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            9136
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2157
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.49
_reflns_number_total             9137
_reflns_number_gt                4167
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+2.5245P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(5)
_refine_ls_number_reflns         9137
_refine_ls_number_parameters     508
_refine_ls_number_restraints     338
_refine_ls_R_factor_all          0.2171
_refine_ls_R_factor_gt           0.1100
_refine_ls_wR_factor_ref         0.3097
_refine_ls_wR_factor_gt          0.2471
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.010

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.7224(5) -0.1381(4) 0.6957(5) 0.073(2) Uani 1 1 d U . .
N1 N 0.7920(5) 0.0103(5) 0.7812(5) 0.0485(19) Uani 1 1 d U . .
N2 N 0.7430(5) 0.1457(5) 0.8342(4) 0.0480(18) Uani 1 1 d U . .
C1 C 0.7150(6) -0.0597(7) 0.6682(6) 0.060(3) Uani 1 1 d U . .
C2 C 0.7537(5) 0.0205(5) 0.7061(6) 0.045(2) Uani 1 1 d U . .
C3 C 0.7411(5) 0.0923(6) 0.6588(6) 0.047(2) Uani 1 1 d U . .
C4 C 0.6914(7) 0.0678(7) 0.5842(6) 0.061(3) Uani 1 1 d U . .
H4A H 0.7241 0.0758 0.5348 0.074 Uiso 1 1 calc R . .
H4B H 0.6421 0.1063 0.5801 0.074 Uiso 1 1 calc R . .
C5 C 0.6678(7) -0.0332(6) 0.5957(7) 0.065(3) Uani 1 1 d U . .
H5 H 0.6869 -0.0692 0.5484 0.078 Uiso 1 1 calc R . .
C6 C 0.5779(7) -0.0460(7) 0.6057(7) 0.068(3) Uani 1 1 d U . .
H6A H 0.5596 -0.0129 0.6534 0.102 Uiso 1 1 calc R . .
H6B H 0.5659 -0.1107 0.6121 0.102 Uiso 1 1 calc R . .
H6C H 0.5494 -0.0227 0.5580 0.102 Uiso 1 1 calc R . .
C7 C 0.7941(5) 0.0733(5) 0.8426(6) 0.042(2) Uani 1 1 d U . .
C8 C 0.7441(6) 0.2076(6) 0.8949(6) 0.050(2) Uani 1 1 d U . .
H8 H 0.7107 0.2599 0.8897 0.060 Uiso 1 1 calc R . .
C9 C 0.7900(6) 0.1990(7) 0.9621(7) 0.061(3) Uani 1 1 d U . .
H9 H 0.7877 0.2438 1.0031 0.074 Uiso 1 1 calc R . .
C10 C 0.8421(6) 0.1216(7) 0.9710(7) 0.064(3) Uani 1 1 d U . .
H10 H 0.8764 0.1145 1.0168 0.077 Uiso 1 1 calc R . .
C11 C 0.8401(7) 0.0580(6) 0.9106(7) 0.056(3) Uani 1 1 d U . .
H11 H 0.8705 0.0035 0.9158 0.067 Uiso 1 1 calc R . .
C12 C 0.7772(6) 0.1868(6) 0.6671(6) 0.050(2) Uani 1 1 d U . .
C13 C 0.7338(5) 0.2616(6) 0.6559(6) 0.042(2) Uani 1 1 d U . .
H13 H 0.7643 0.3156 0.6479 0.050 Uiso 1 1 calc R . .
C14 C 0.6463(5) 0.2721(5) 0.6543(5) 0.041(2) Uani 1 1 d U . .
C15 C 0.5926(6) 0.2161(6) 0.6965(6) 0.049(2) Uani 1 1 d U . .
H15 H 0.6145 0.1684 0.7284 0.059 Uiso 1 1 calc R . .
C16 C 0.5099(6) 0.2271(7) 0.6938(6) 0.049(2) Uani 1 1 d U . .
H16 H 0.4757 0.1860 0.7218 0.059 Uiso 1 1 calc R . .
C17 C 0.4755(6) 0.2981(7) 0.6503(6) 0.061(3) Uani 1 1 d U . .
H17 H 0.4181 0.3062 0.6481 0.073 Uiso 1 1 calc R . .
C18 C 0.5286(7) 0.3583(7) 0.6091(7) 0.064(3) Uani 1 1 d U . .
H18 H 0.5068 0.4084 0.5801 0.076 Uiso 1 1 calc R . .
C19 C 0.6088(6) 0.3447(6) 0.6110(6) 0.051(2) Uani 1 1 d U . .
H19 H 0.6427 0.3854 0.5821 0.062 Uiso 1 1 calc R . .
C20 C 0.8656(6) 0.1898(5) 0.6832(5) 0.043(2) Uani 1 1 d U . .
C21 C 0.9198(6) 0.1233(6) 0.6563(7) 0.057(2) Uani 1 1 d U . .
H21 H 0.8988 0.0744 0.6252 0.068 Uiso 1 1 calc R . .
C22 C 1.0023(6) 0.1253(8) 0.6727(7) 0.067(3) Uani 1 1 d U . .
H22 H 1.0369 0.0773 0.6559 0.080 Uiso 1 1 calc R . .
C23 C 1.0323(8) 0.1971(8) 0.7133(8) 0.077(3) Uani 1 1 d U . .
H23 H 1.0890 0.2005 0.7246 0.092 Uiso 1 1 calc R . .
C24 C 0.9814(6) 0.2658(7) 0.7385(7) 0.056(2) Uani 1 1 d U . .
H24 H 1.0042 0.3177 0.7638 0.068 Uiso 1 1 calc R . .
C25 C 0.9012(6) 0.2610(6) 0.7282(6) 0.054(2) Uani 1 1 d U . .
H25 H 0.8674 0.3061 0.7514 0.064 Uiso 1 1 calc R . .
O2 O 0.8740(4) 0.8521(4) 0.8469(5) 0.066(2) Uani 1 1 d U . .
N3 N 0.7985(5) 0.7031(4) 0.7698(5) 0.0482(19) Uani 1 1 d U . .
N4 N 0.7396(6) 0.6522(6) 0.6444(6) 0.068(3) Uani 1 1 d U . .
C26 C 0.8800(5) 0.7763(6) 0.8743(6) 0.051(2) Uani 1 1 d U . .
C27 C 0.9232(8) 0.7500(6) 0.9498(8) 0.072(3) Uani 1 1 d U . .
H27 H 0.8914 0.7777 0.9947 0.086 Uiso 1 1 calc R . .
C28 C 0.9118(7) 0.6485(6) 0.9576(7) 0.060(3) Uani 1 1 d U . .
H28A H 0.9650 0.6170 0.9563 0.072 Uiso 1 1 calc R . .
H28B H 0.8844 0.6335 1.0089 0.072 Uiso 1 1 calc R . .
C29 C 0.8605(6) 0.6209(6) 0.8880(6) 0.049(2) Uani 1 1 d U . .
C30 C 0.8444(6) 0.6940(5) 0.8377(6) 0.045(2) Uani 1 1 d U . .
C31 C 1.0030(9) 0.7855(9) 0.9569(10) 0.105(5) Uani 1 1 d U . .
H31A H 1.0392 0.7532 0.9200 0.157 Uiso 1 1 calc R . .
H31B H 1.0225 0.7778 1.0123 0.157 Uiso 1 1 calc R . .
H31C H 1.0025 0.8502 0.9432 0.157 Uiso 1 1 calc R . .
C32 C 0.7966(6) 0.6371(6) 0.7063(6) 0.047(2) Uani 1 1 d U . .
C33 C 0.7362(6) 0.5856(6) 0.5848(6) 0.050(2) Uani 1 1 d U . .
H33 H 0.6980 0.5908 0.5419 0.060 Uiso 1 1 calc R . .
C34 C 0.7884(6) 0.5121(6) 0.5882(6) 0.054(2) Uani 1 1 d U . .
H34 H 0.7874 0.4659 0.5483 0.064 Uiso 1 1 calc R . .
C35 C 0.8425(6) 0.5092(6) 0.6528(6) 0.051(2) Uani 1 1 d U . .
H35 H 0.8797 0.4600 0.6551 0.061 Uiso 1 1 calc R . .
C36 C 0.8458(4) 0.5699(4) 0.7111(4) 0.0272(15) Uani 1 1 d U . .
H36 H 0.8831 0.5641 0.7547 0.033 Uiso 1 1 calc R . .
C37 C 0.8200(6) 0.5302(6) 0.8790(6) 0.049(2) Uani 1 1 d U . .
C38 C 0.8644(6) 0.4521(7) 0.8915(6) 0.056(3) Uani 1 1 d U . .
H38 H 0.8330 0.3988 0.9000 0.067 Uiso 1 1 calc R . .
C39 C 0.9505(5) 0.4394(6) 0.8938(5) 0.046(2) Uani 1 1 d U . .
C40 C 1.0063(5) 0.4922(6) 0.8481(6) 0.051(2) Uani 1 1 d U . .
H40 H 0.9866 0.5421 0.8175 0.062 Uiso 1 1 calc R . .
C41 C 1.0861(6) 0.4729(7) 0.8474(7) 0.057(2) Uani 1 1 d U . .
H41 H 1.1222 0.5100 0.8173 0.068 Uiso 1 1 calc R . .
C42 C 1.1164(6) 0.3998(7) 0.8897(6) 0.058(3) Uani 1 1 d U . .
H42 H 1.1730 0.3866 0.8877 0.069 Uiso 1 1 calc R . .
C43 C 1.0671(7) 0.3471(7) 0.9338(6) 0.056(3) Uani 1 1 d U . .
H43 H 1.0890 0.2968 0.9624 0.067 Uiso 1 1 calc R . .
C44 C 0.9829(6) 0.3660(6) 0.9381(6) 0.054(2) Uani 1 1 d U . .
H44 H 0.9484 0.3296 0.9706 0.065 Uiso 1 1 calc R . .
C45 C 0.7302(5) 0.5262(5) 0.8681(5) 0.040(2) Uani 1 1 d U . .
C46 C 0.6791(7) 0.5912(7) 0.8994(6) 0.057(2) Uani 1 1 d U . .
H46 H 0.7019 0.6421 0.9265 0.068 Uiso 1 1 calc R . .
C47 C 0.5966(6) 0.5841(7) 0.8924(7) 0.058(3) Uani 1 1 d U . .
H47 H 0.5629 0.6278 0.9180 0.069 Uiso 1 1 calc R . .
C48 C 0.5597(7) 0.5125(7) 0.8475(7) 0.061(3) Uani 1 1 d U . .
H48 H 0.5023 0.5090 0.8408 0.073 Uiso 1 1 calc R . .
C49 C 0.6113(7) 0.4476(6) 0.8137(7) 0.061(3) Uani 1 1 d U . .
H49 H 0.5889 0.3982 0.7842 0.073 Uiso 1 1 calc R . .
C50 C 0.6927(6) 0.4549(5) 0.8228(6) 0.045(2) Uani 1 1 d U . .
H50 H 0.7265 0.4108 0.7980 0.055 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.100(5) 0.024(3) 0.095(5) -0.003(3) -0.032(5) 0.003(3)
N1 0.055(4) 0.042(4) 0.049(4) -0.005(3) -0.005(4) 0.002(3)
N2 0.065(4) 0.033(4) 0.045(4) 0.002(3) -0.005(4) 0.006(3)
C1 0.073(6) 0.048(5) 0.060(6) -0.010(4) -0.009(5) 0.001(4)
C2 0.054(5) 0.033(4) 0.047(5) -0.007(4) -0.007(4) -0.006(4)
C3 0.054(5) 0.035(4) 0.053(5) -0.003(4) -0.010(4) -0.005(4)
C4 0.087(6) 0.048(5) 0.050(5) -0.005(4) -0.011(5) 0.006(4)
C5 0.088(6) 0.042(5) 0.064(6) -0.003(4) -0.034(5) -0.005(4)
C6 0.085(7) 0.052(6) 0.067(7) -0.004(5) -0.026(6) -0.004(5)
C7 0.041(4) 0.032(4) 0.052(5) -0.006(4) 0.000(4) -0.010(3)
C8 0.054(5) 0.038(4) 0.058(5) -0.010(4) 0.007(4) -0.002(4)
C9 0.069(6) 0.058(5) 0.057(5) -0.023(4) 0.009(5) 0.003(5)
C10 0.061(5) 0.071(6) 0.059(5) -0.012(5) 0.002(5) 0.001(5)
C11 0.068(5) 0.036(5) 0.064(6) -0.011(4) -0.006(5) 0.001(4)
C12 0.061(5) 0.038(4) 0.051(5) -0.002(4) 0.021(4) -0.014(4)
C13 0.045(4) 0.029(4) 0.053(5) -0.003(4) 0.009(4) -0.005(3)
C14 0.045(4) 0.030(4) 0.049(5) -0.001(4) -0.004(4) -0.004(3)
C15 0.052(5) 0.042(4) 0.053(5) 0.013(4) 0.003(4) 0.002(4)
C16 0.051(5) 0.050(5) 0.046(5) 0.012(4) 0.008(4) -0.001(4)
C17 0.053(5) 0.069(6) 0.059(5) 0.005(5) -0.004(4) -0.005(5)
C18 0.072(6) 0.047(5) 0.072(6) 0.003(4) -0.009(5) 0.002(4)
C19 0.056(5) 0.045(5) 0.054(5) 0.010(4) 0.004(4) -0.008(4)
C20 0.051(5) 0.036(4) 0.041(5) 0.003(3) 0.001(4) 0.002(4)
C21 0.056(5) 0.047(5) 0.067(6) -0.008(4) 0.006(4) -0.008(4)
C22 0.063(6) 0.063(6) 0.075(6) -0.006(5) 0.008(5) 0.007(5)
C23 0.069(6) 0.089(7) 0.072(6) 0.001(5) -0.005(5) 0.008(5)
C24 0.054(5) 0.053(5) 0.063(5) -0.003(4) 0.004(4) -0.008(4)
C25 0.062(5) 0.045(5) 0.055(5) 0.004(4) 0.005(4) -0.001(4)
O2 0.084(5) 0.036(4) 0.079(5) 0.010(3) -0.024(4) 0.007(3)
N3 0.070(4) 0.028(3) 0.047(4) -0.003(3) -0.010(4) -0.004(3)
N4 0.074(5) 0.066(5) 0.063(5) -0.001(4) -0.005(4) -0.005(4)
C26 0.050(5) 0.040(5) 0.062(5) 0.002(4) -0.010(4) -0.005(4)
C27 0.101(7) 0.045(5) 0.069(6) 0.000(5) -0.033(5) -0.012(5)
C28 0.073(5) 0.047(5) 0.059(5) 0.010(4) -0.015(5) -0.012(4)
C29 0.061(5) 0.040(4) 0.046(5) 0.000(4) 0.006(4) -0.004(4)
C30 0.051(5) 0.035(4) 0.049(5) 0.002(4) -0.006(4) 0.001(4)
C31 0.102(9) 0.095(9) 0.117(10) 0.044(8) -0.037(8) -0.034(7)
C32 0.051(5) 0.043(4) 0.048(5) 0.015(4) 0.004(4) -0.007(4)
C33 0.054(5) 0.050(5) 0.047(5) -0.002(4) -0.008(4) -0.001(4)
C34 0.068(5) 0.044(5) 0.048(5) -0.003(4) 0.007(5) -0.010(4)
C35 0.058(5) 0.039(4) 0.056(5) 0.008(4) 0.004(4) 0.001(4)
C36 0.032(4) 0.021(3) 0.028(4) 0.002(3) 0.000(3) -0.002(3)
C37 0.063(5) 0.042(5) 0.042(5) 0.002(4) 0.001(4) 0.000(4)
C38 0.073(6) 0.050(5) 0.045(5) 0.005(4) -0.005(4) -0.005(4)
C39 0.050(5) 0.045(4) 0.043(5) -0.006(4) -0.008(4) 0.010(4)
C40 0.056(5) 0.047(4) 0.051(5) 0.003(4) -0.002(4) -0.010(4)
C41 0.057(5) 0.056(5) 0.058(5) -0.002(4) -0.009(4) 0.000(4)
C42 0.046(5) 0.061(5) 0.066(6) -0.010(5) -0.002(4) 0.006(4)
C43 0.062(5) 0.050(5) 0.057(5) 0.013(4) -0.011(5) -0.006(4)
C44 0.067(6) 0.043(5) 0.052(5) 0.001(4) -0.009(5) -0.010(4)
C45 0.037(4) 0.038(4) 0.045(5) 0.002(3) 0.013(4) 0.000(3)
C46 0.072(6) 0.050(5) 0.049(5) -0.004(4) 0.000(4) 0.009(4)
C47 0.058(5) 0.056(5) 0.059(5) -0.004(4) -0.001(4) 0.008(4)
C48 0.063(5) 0.058(5) 0.063(6) 0.008(5) 0.000(5) -0.008(5)
C49 0.074(6) 0.046(5) 0.062(6) 0.000(4) 0.002(5) -0.001(4)
C50 0.052(5) 0.035(4) 0.050(5) 0.004(4) 0.002(4) 0.010(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.249(11) . ?
N1 C7 1.379(11) . ?
N1 C2 1.403(12) . ?
N2 C8 1.359(11) . ?
N2 C7 1.364(11) . ?
C1 C5 1.480(15) . ?
C1 C2 1.481(12) . ?
C2 C3 1.335(12) . ?
C3 C12 1.520(12) . ?
C3 C4 1.523(14) . ?
C4 C5 1.550(14) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.498(16) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C11 1.374(15) . ?
C8 C9 1.349(15) . ?
C8 H8 0.9500 . ?
C9 C10 1.434(14) . ?
C9 H9 0.9500 . ?
C10 C11 1.373(14) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.325(13) . ?
C12 C20 1.475(14) . ?
C13 C14 1.445(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.399(12) . ?
C14 C19 1.427(12) . ?
C15 C16 1.369(13) . ?
C15 H15 0.9500 . ?
C16 C17 1.389(14) . ?
C16 H16 0.9500 . ?
C17 C18 1.422(15) . ?
C17 H17 0.9500 . ?
C18 C19 1.333(15) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.399(13) . ?
C20 C25 1.413(13) . ?
C21 C22 1.382(15) . ?
C21 H21 0.9500 . ?
C22 C23 1.347(16) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(15) . ?
C23 H23 0.9500 . ?
C24 C25 1.329(14) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
O2 C26 1.212(10) . ?
N3 C30 1.360(12) . ?
N3 C32 1.436(12) . ?
N4 C33 1.394(13) . ?
N4 C32 1.404(14) . ?
C26 C30 1.475(12) . ?
C26 C27 1.488(15) . ?
C27 C31 1.416(16) . ?
C27 C28 1.513(13) . ?
C27 H27 1.0000 . ?
C28 C29 1.483(15) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.389(13) . ?
C29 C37 1.500(13) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C36 1.280(11) . ?
C33 C34 1.383(13) . ?
C33 H33 0.9500 . ?
C34 C35 1.390(14) . ?
C34 H34 0.9500 . ?
C35 C36 1.319(12) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.379(13) . ?
C37 C45 1.486(13) . ?
C38 C39 1.426(14) . ?
C38 H38 0.9500 . ?
C39 C44 1.411(12) . ?
C39 C40 1.425(13) . ?
C40 C41 1.342(13) . ?
C40 H40 0.9500 . ?
C41 C42 1.377(14) . ?
C41 H41 0.9500 . ?
C42 C43 1.343(14) . ?
C42 H42 0.9500 . ?
C43 C44 1.413(15) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C46 1.378(12) . ?
C45 C50 1.430(12) . ?
C46 C47 1.364(15) . ?
C46 H46 0.9500 . ?
C47 C48 1.426(15) . ?
C47 H47 0.9500 . ?
C48 C49 1.396(15) . ?
C48 H48 0.9500 . ?
C49 C50 1.350(13) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?

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
C7 N1 C2 126.5(7) . . ?
C8 N2 C7 116.4(8) . . ?
O1 C1 C5 126.2(9) . . ?
O1 C1 C2 122.8(9) . . ?
C5 C1 C2 111.0(8) . . ?
C3 C2 N1 132.6(8) . . ?
C3 C2 C1 108.5(8) . . ?
N1 C2 C1 118.9(8) . . ?
C2 C3 C12 127.9(8) . . ?
C2 C3 C4 111.8(7) . . ?
C12 C3 C4 119.9(8) . . ?
C3 C4 C5 105.1(8) . . ?
C3 C4 H4A 110.7 . . ?
C5 C4 H4A 110.7 . . ?
C3 C4 H4B 110.7 . . ?
C5 C4 H4B 110.7 . . ?
H4A C4 H4B 108.8 . . ?
C1 C5 C6 112.9(10) . . ?
C1 C5 C4 102.9(8) . . ?
C6 C5 C4 112.4(9) . . ?
C1 C5 H5 109.5 . . ?
C6 C5 H5 109.5 . . ?
C4 C5 H5 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C11 123.1(9) . . ?
N2 C7 N1 116.0(8) . . ?
C11 C7 N1 120.6(8) . . ?
C9 C8 N2 123.7(9) . . ?
C9 C8 H8 118.1 . . ?
N2 C8 H8 118.2 . . ?
C8 C9 C10 119.4(9) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 117.1(10) . . ?
C11 C10 H10 121.5 . . ?
C9 C10 H10 121.5 . . ?
C7 C11 C10 120.0(9) . . ?
C7 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C12 C20 121.9(8) . . ?
C13 C12 C3 122.7(9) . . ?
C20 C12 C3 115.3(8) . . ?
C12 C13 C14 128.8(8) . . ?
C12 C13 H13 115.6 . . ?
C14 C13 H13 115.6 . . ?
C15 C14 C19 115.0(8) . . ?
C15 C14 C13 123.8(8) . . ?
C19 C14 C13 121.1(8) . . ?
C16 C15 C14 122.8(8) . . ?
C16 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
C15 C16 C17 120.5(9) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C18 118.1(9) . . ?
C16 C17 H17 120.9 . . ?
C18 C17 H17 120.9 . . ?
C19 C18 C17 120.2(10) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C14 123.3(9) . . ?
C18 C19 H19 118.4 . . ?
C14 C19 H19 118.4 . . ?
C21 C20 C25 115.3(9) . . ?
C21 C20 C12 123.2(8) . . ?
C25 C20 C12 121.5(8) . . ?
C22 C21 C20 123.1(10) . . ?
C22 C21 H21 118.4 . . ?
C20 C21 H21 118.4 . . ?
C23 C22 C21 118.1(10) . . ?
C23 C22 H22 120.9 . . ?
C21 C22 H22 120.9 . . ?
C22 C23 C24 120.5(11) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C25 C24 C23 121.6(10) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C24 C25 C20 121.0(10) . . ?
C24 C25 H25 119.5 . . ?
C20 C25 H25 119.5 . . ?
C30 N3 C32 123.6(7) . . ?
C33 N4 C32 115.6(9) . . ?
O2 C26 C30 124.9(9) . . ?
O2 C26 C27 126.5(8) . . ?
C30 C26 C27 108.6(8) . . ?
C31 C27 C26 114.2(11) . . ?
C31 C27 C28 118.3(11) . . ?
C26 C27 C28 105.7(8) . . ?
C31 C27 H27 105.9 . . ?
C26 C27 H27 105.9 . . ?
C28 C27 H27 105.9 . . ?
C29 C28 C27 105.9(8) . . ?
C29 C28 H28A 110.6 . . ?
C27 C28 H28A 110.6 . . ?
C29 C28 H28B 110.6 . . ?
C27 C28 H28B 110.5 . . ?
H28A C28 H28B 108.7 . . ?
C30 C29 C28 111.2(8) . . ?
C30 C29 C37 123.2(9) . . ?
C28 C29 C37 124.9(9) . . ?
N3 C30 C29 132.7(8) . . ?
N3 C30 C26 118.5(7) . . ?
C29 C30 C26 108.4(8) . . ?
C27 C31 H31A 109.5 . . ?
C27 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C27 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C36 C32 N4 125.9(9) . . ?
C36 C32 N3 117.8(8) . . ?
N4 C32 N3 116.3(8) . . ?
C34 C33 N4 120.0(9) . . ?
C34 C33 H33 120.0 . . ?
N4 C33 H33 120.0 . . ?
C33 C34 C35 116.6(9) . . ?
C33 C34 H34 121.7 . . ?
C35 C34 H34 121.7 . . ?
C36 C35 C34 124.8(9) . . ?
C36 C35 H35 117.6 . . ?
C34 C35 H35 117.6 . . ?
C32 C36 C35 117.0(8) . . ?
C32 C36 H36 121.5 . . ?
C35 C36 H36 121.5 . . ?
C38 C37 C45 120.6(8) . . ?
C38 C37 C29 119.7(9) . . ?
C45 C37 C29 119.2(8) . . ?
C37 C38 C39 129.5(9) . . ?
C37 C38 H38 115.2 . . ?
C39 C38 H38 115.2 . . ?
C44 C39 C40 117.0(8) . . ?
C44 C39 C38 119.1(9) . . ?
C40 C39 C38 123.7(8) . . ?
C41 C40 C39 121.4(9) . . ?
C41 C40 H40 119.3 . . ?
C39 C40 H40 119.3 . . ?
C40 C41 C42 120.8(10) . . ?
C40 C41 H41 119.6 . . ?
C42 C41 H41 119.6 . . ?
C43 C42 C41 120.9(9) . . ?
C43 C42 H42 119.6 . . ?
C41 C42 H42 119.5 . . ?
C42 C43 C44 120.5(9) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C43 C44 C39 119.4(9) . . ?
C43 C44 H44 120.3 . . ?
C39 C44 H44 120.3 . . ?
C46 C45 C50 116.6(8) . . ?
C46 C45 C37 122.2(9) . . ?
C50 C45 C37 121.2(7) . . ?
C47 C46 C45 121.5(10) . . ?
C47 C46 H46 119.3 . . ?
C45 C46 H46 119.3 . . ?
C46 C47 C48 121.3(10) . . ?
C46 C47 H47 119.3 . . ?
C48 C47 H47 119.3 . . ?
C49 C48 C47 117.4(10) . . ?
C49 C48 H48 121.3 . . ?
C47 C48 H48 121.3 . . ?
C50 C49 C48 120.2(10) . . ?
C50 C49 H49 119.9 . . ?
C48 C49 H49 119.9 . . ?
C49 C50 C45 122.8(8) . . ?
C49 C50 H50 118.6 . . ?
C45 C50 H50 118.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N1 C2 C3 32.6(16) . . . . ?
C7 N1 C2 C1 -144.5(9) . . . . ?
O1 C1 C2 C3 174.1(10) . . . . ?
C5 C1 C2 C3 -6.0(12) . . . . ?
O1 C1 C2 N1 -8.1(16) . . . . ?
C5 C1 C2 N1 171.8(9) . . . . ?
N1 C2 C3 C12 10.4(17) . . . . ?
C1 C2 C3 C12 -172.2(9) . . . . ?
N1 C2 C3 C4 -176.7(10) . . . . ?
C1 C2 C3 C4 0.6(12) . . . . ?
C2 C3 C4 C5 4.6(12) . . . . ?
C12 C3 C4 C5 178.0(9) . . . . ?
O1 C1 C5 C6 66.9(15) . . . . ?
C2 C1 C5 C6 -113.0(10) . . . . ?
O1 C1 C5 C4 -171.7(11) . . . . ?
C2 C1 C5 C4 8.4(12) . . . . ?
C3 C4 C5 C1 -7.6(12) . . . . ?
C3 C4 C5 C6 114.1(10) . . . . ?
C8 N2 C7 C11 5.1(13) . . . . ?
C8 N2 C7 N1 179.3(8) . . . . ?
C2 N1 C7 N2 11.5(13) . . . . ?
C2 N1 C7 C11 -174.1(9) . . . . ?
C7 N2 C8 C9 -2.4(14) . . . . ?
N2 C8 C9 C10 1.1(16) . . . . ?
C8 C9 C10 C11 -2.1(16) . . . . ?
N2 C7 C11 C10 -6.4(16) . . . . ?
N1 C7 C11 C10 179.6(9) . . . . ?
C9 C10 C11 C7 4.7(16) . . . . ?
C2 C3 C12 C13 -137.9(11) . . . . ?
C4 C3 C12 C13 49.8(14) . . . . ?
C2 C3 C12 C20 46.0(13) . . . . ?
C4 C3 C12 C20 -126.3(10) . . . . ?
C20 C12 C13 C14 -167.5(9) . . . . ?
C3 C12 C13 C14 16.6(17) . . . . ?
C12 C13 C14 C15 28.5(16) . . . . ?
C12 C13 C14 C19 -154.2(10) . . . . ?
C19 C14 C15 C16 2.9(13) . . . . ?
C13 C14 C15 C16 -179.7(9) . . . . ?
C14 C15 C16 C17 -2.4(15) . . . . ?
C15 C16 C17 C18 0.0(15) . . . . ?
C16 C17 C18 C19 1.7(16) . . . . ?
C17 C18 C19 C14 -1.2(16) . . . . ?
C15 C14 C19 C18 -1.1(14) . . . . ?
C13 C14 C19 C18 -178.6(10) . . . . ?
C13 C12 C20 C21 -146.3(10) . . . . ?
C3 C12 C20 C21 29.8(13) . . . . ?
C13 C12 C20 C25 34.1(14) . . . . ?
C3 C12 C20 C25 -149.7(9) . . . . ?
C25 C20 C21 C22 0.8(14) . . . . ?
C12 C20 C21 C22 -178.8(10) . . . . ?
C20 C21 C22 C23 -3.4(17) . . . . ?
C21 C22 C23 C24 0.9(18) . . . . ?
C22 C23 C24 C25 4.2(18) . . . . ?
C23 C24 C25 C20 -6.9(16) . . . . ?
C21 C20 C25 C24 4.3(13) . . . . ?
C12 C20 C25 C24 -176.1(10) . . . . ?
O2 C26 C27 C31 -49.0(18) . . . . ?
C30 C26 C27 C31 131.4(11) . . . . ?
O2 C26 C27 C28 179.2(11) . . . . ?
C30 C26 C27 C28 -0.4(13) . . . . ?
C31 C27 C28 C29 -131.2(13) . . . . ?
C26 C27 C28 C29 -1.7(13) . . . . ?
C27 C28 C29 C30 3.4(13) . . . . ?
C27 C28 C29 C37 -167.6(10) . . . . ?
C32 N3 C30 C29 -41.9(16) . . . . ?
C32 N3 C30 C26 145.4(9) . . . . ?
C28 C29 C30 N3 -176.9(11) . . . . ?
C37 C29 C30 N3 -5.8(17) . . . . ?
C28 C29 C30 C26 -3.7(12) . . . . ?
C37 C29 C30 C26 167.5(9) . . . . ?
O2 C26 C30 N3 -2.8(15) . . . . ?
C27 C26 C30 N3 176.8(10) . . . . ?
O2 C26 C30 C29 -177.1(10) . . . . ?
C27 C26 C30 C29 2.5(12) . . . . ?
C33 N4 C32 C36 1.8(14) . . . . ?
C33 N4 C32 N3 -177.5(8) . . . . ?
C30 N3 C32 C36 -5.9(13) . . . . ?
C30 N3 C32 N4 173.5(9) . . . . ?
C32 N4 C33 C34 -1.6(13) . . . . ?
N4 C33 C34 C35 0.1(13) . . . . ?
C33 C34 C35 C36 1.6(14) . . . . ?
N4 C32 C36 C35 -0.3(13) . . . . ?
N3 C32 C36 C35 179.0(8) . . . . ?
C34 C35 C36 C32 -1.5(13) . . . . ?
C30 C29 C37 C38 141.4(10) . . . . ?
C28 C29 C37 C38 -48.7(15) . . . . ?
C30 C29 C37 C45 -47.3(14) . . . . ?
C28 C29 C37 C45 122.6(11) . . . . ?
C45 C37 C38 C39 171.7(10) . . . . ?
C29 C37 C38 C39 -17.1(16) . . . . ?
C37 C38 C39 C44 154.5(10) . . . . ?
C37 C38 C39 C40 -31.1(16) . . . . ?
C44 C39 C40 C41 0.0(13) . . . . ?
C38 C39 C40 C41 -174.6(10) . . . . ?
C39 C40 C41 C42 1.4(15) . . . . ?
C40 C41 C42 C43 -1.2(16) . . . . ?
C41 C42 C43 C44 -0.4(16) . . . . ?
C42 C43 C44 C39 1.7(15) . . . . ?
C40 C39 C44 C43 -1.5(13) . . . . ?
C38 C39 C44 C43 173.4(9) . . . . ?
C38 C37 C45 C46 142.2(10) . . . . ?
C29 C37 C45 C46 -29.0(14) . . . . ?
C38 C37 C45 C50 -39.1(14) . . . . ?
C29 C37 C45 C50 149.7(8) . . . . ?
C50 C45 C46 C47 4.6(14) . . . . ?
C37 C45 C46 C47 -176.6(10) . . . . ?
C45 C46 C47 C48 -4.5(17) . . . . ?
C46 C47 C48 C49 2.6(16) . . . . ?
C47 C48 C49 C50 -1.2(15) . . . . ?
C48 C49 C50 C45 1.6(15) . . . . ?
C46 C45 C50 C49 -3.2(13) . . . . ?
C37 C45 C50 C49 177.9(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.076

_database_code_depnum_ccdc_archive 'CCDC 966194'