# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               Org.Biomol.Chem.
_journal_coden_cambridge         0177
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_email       ycheng2@bnu.edu.cn
_publ_contact_author_name        'Ying Cheng'
loop_
_publ_author_name
'Xiao-Rong Wang'
'Cai-Xia Yan'
'Ying Cheng'

data_091014a5
_database_code_depnum_ccdc_archive 'CCDC 844397'
#TrackingRef '4c-CCDC.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H21 N5 O2'
_chemical_formula_weight         411.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   8.9350(18)
_cell_length_b                   20.224(4)
_cell_length_c                   11.920(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.98(3)
_cell_angle_gamma                90.00
_cell_volume                     2036.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    5399
_cell_measurement_theta_min      2.0684
_cell_measurement_theta_max      27.8625

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9773
_exptl_absorpt_correction_T_max  0.9825
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
;
????
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Rigaku Saturn CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16701
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         27.85
_reflns_number_total             4841
_reflns_number_gt                3845
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.0737P)^2^+0.0411P] 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     SHELXL
_refine_ls_extinction_coef       0.037(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4841
_refine_ls_number_parameters     284
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1367
_refine_ls_wR_factor_gt          0.1250
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_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
N1 N -0.00336(12) 0.84897(5) 0.19296(10) 0.0225(3) Uani 1 1 d . . .
N2 N 0.09901(13) 0.98662(6) 0.39499(10) 0.0273(3) Uani 1 1 d . . .
N3 N 0.19928(13) 0.94243(6) 0.44774(10) 0.0265(3) Uani 1 1 d . . .
N4 N 0.35477(14) 0.83979(6) 0.25770(11) 0.0288(3) Uani 1 1 d . . .
N5 N -0.19648(13) 0.99385(6) 0.09474(11) 0.0305(3) Uani 1 1 d . . .
O1 O 0.03825(11) 0.73624(5) 0.23026(9) 0.0306(2) Uani 1 1 d . . .
O2 O -0.35678(12) 0.82179(5) -0.28539(8) 0.0336(3) Uani 1 1 d . . .
C1 C 0.05102(14) 0.90538(7) 0.25855(11) 0.0219(3) Uani 1 1 d . . .
C2 C 0.19073(15) 0.88791(7) 0.36369(11) 0.0229(3) Uani 1 1 d . . .
C3 C 0.14371(16) 0.81728(7) 0.39230(12) 0.0243(3) Uani 1 1 d . . .
C4 C 0.05981(15) 0.79259(7) 0.26468(12) 0.0238(3) Uani 1 1 d . . .
C5 C 0.00358(15) 0.96705(7) 0.27702(12) 0.0235(3) Uani 1 1 d . . .
C6 C 0.27544(17) 0.77132(7) 0.46281(13) 0.0318(3) Uani 1 1 d . . .
H6A H 0.3288 0.7905 0.5411 0.048 Uiso 1 1 calc R . .
H6B H 0.3520 0.7655 0.4205 0.048 Uiso 1 1 calc R . .
H6C H 0.2305 0.7283 0.4722 0.048 Uiso 1 1 calc R . .
C7 C 0.01576(17) 0.82215(8) 0.45303(12) 0.0305(3) Uani 1 1 d . . .
H7A H -0.0383 0.7795 0.4472 0.046 Uiso 1 1 calc R . .
H7B H -0.0613 0.8563 0.4138 0.046 Uiso 1 1 calc R . .
H7C H 0.0655 0.8338 0.5368 0.046 Uiso 1 1 calc R . .
C8 C -0.09626(14) 0.84427(7) 0.07021(12) 0.0224(3) Uani 1 1 d . . .
C9 C -0.22970(15) 0.80415(7) 0.03484(12) 0.0232(3) Uani 1 1 d . . .
H9 H -0.2625 0.7811 0.0922 0.028 Uiso 1 1 calc R . .
C10 C -0.31467(15) 0.79806(7) -0.08506(12) 0.0257(3) Uani 1 1 d . . .
H10 H -0.4057 0.7705 -0.1098 0.031 Uiso 1 1 calc R . .
C11 C -0.26707(15) 0.83206(7) -0.16903(12) 0.0255(3) Uani 1 1 d . . .
C12 C -0.13457(16) 0.87277(7) -0.13270(13) 0.0303(3) Uani 1 1 d . . .
H12 H -0.1027 0.8967 -0.1897 0.036 Uiso 1 1 calc R . .
C13 C -0.04913(16) 0.87832(7) -0.01297(12) 0.0284(3) Uani 1 1 d . . .
H13 H 0.0422 0.9057 0.0119 0.034 Uiso 1 1 calc R . .
C14 C -0.3130(2) 0.85849(8) -0.37263(13) 0.0411(4) Uani 1 1 d . . .
H14A H -0.3190 0.9059 -0.3579 0.062 Uiso 1 1 calc R . .
H14B H -0.3855 0.8477 -0.4518 0.062 Uiso 1 1 calc R . .
H14C H -0.2046 0.8470 -0.3679 0.062 Uiso 1 1 calc R . .
C15 C 0.34095(15) 0.88958(7) 0.32726(11) 0.0234(3) Uani 1 1 d . . .
C16 C 0.45076(16) 0.94053(7) 0.36170(12) 0.0292(3) Uani 1 1 d . . .
H16 H 0.4366 0.9754 0.4107 0.035 Uiso 1 1 calc R . .
C17 C 0.58113(17) 0.93952(8) 0.32325(13) 0.0344(4) Uani 1 1 d . . .
H17 H 0.6590 0.9733 0.3466 0.041 Uiso 1 1 calc R . .
C18 C 0.59652(16) 0.88859(8) 0.25031(13) 0.0321(3) Uani 1 1 d . . .
H18 H 0.6840 0.8870 0.2217 0.038 Uiso 1 1 calc R . .
C19 C 0.48116(17) 0.84002(7) 0.22015(13) 0.0308(3) Uani 1 1 d . . .
H19 H 0.4919 0.8050 0.1702 0.037 Uiso 1 1 calc R . .
C20 C -0.12404(15) 1.01059(6) 0.20911(12) 0.0252(3) Uani 1 1 d . . .
C21 C -0.16861(17) 1.06539(7) 0.26172(14) 0.0328(3) Uani 1 1 d . . .
H21 H -0.1142 1.0761 0.3423 0.039 Uiso 1 1 calc R . .
C22 C -0.29361(19) 1.10397(8) 0.19431(15) 0.0396(4) Uani 1 1 d . . .
H22 H -0.3267 1.1415 0.2280 0.047 Uiso 1 1 calc R . .
C23 C -0.36931(19) 1.08705(8) 0.07756(15) 0.0386(4) Uani 1 1 d . . .
H23 H -0.4560 1.1124 0.0295 0.046 Uiso 1 1 calc R . .
C24 C -0.31607(17) 1.03227(8) 0.03199(14) 0.0354(4) Uani 1 1 d . . .
H24 H -0.3678 1.0213 -0.0489 0.042 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
N1 0.0246(6) 0.0194(6) 0.0229(6) -0.0016(4) 0.0071(4) -0.0017(4)
N2 0.0283(6) 0.0262(6) 0.0291(6) -0.0040(5) 0.0118(5) -0.0031(5)
N3 0.0287(6) 0.0253(6) 0.0270(6) -0.0036(5) 0.0113(5) -0.0035(5)
N4 0.0275(6) 0.0274(7) 0.0329(7) -0.0036(5) 0.0116(5) -0.0028(5)
N5 0.0301(7) 0.0275(7) 0.0327(7) -0.0004(5) 0.0087(5) 0.0027(5)
O1 0.0379(6) 0.0197(5) 0.0329(6) -0.0014(4) 0.0096(4) -0.0017(4)
O2 0.0360(6) 0.0360(6) 0.0235(5) 0.0007(4) 0.0021(4) -0.0047(4)
C1 0.0217(6) 0.0234(7) 0.0216(6) -0.0009(5) 0.0085(5) -0.0032(5)
C2 0.0239(7) 0.0233(7) 0.0216(6) -0.0022(5) 0.0076(5) -0.0021(5)
C3 0.0275(7) 0.0220(7) 0.0238(6) 0.0008(5) 0.0087(5) -0.0020(5)
C4 0.0228(7) 0.0225(7) 0.0271(7) 0.0000(5) 0.0096(5) -0.0022(5)
C5 0.0252(7) 0.0219(7) 0.0253(7) -0.0018(5) 0.0107(5) -0.0027(5)
C6 0.0328(8) 0.0279(8) 0.0325(8) 0.0047(6) 0.0078(6) 0.0001(6)
C7 0.0334(8) 0.0322(8) 0.0292(7) -0.0001(6) 0.0149(6) -0.0046(6)
C8 0.0206(6) 0.0224(7) 0.0247(7) -0.0029(5) 0.0078(5) 0.0013(5)
C9 0.0240(7) 0.0213(7) 0.0272(7) -0.0009(5) 0.0122(5) 0.0005(5)
C10 0.0212(7) 0.0251(7) 0.0301(7) -0.0030(5) 0.0073(5) -0.0033(5)
C11 0.0257(7) 0.0244(7) 0.0242(7) -0.0019(5) 0.0051(5) 0.0021(5)
C12 0.0331(8) 0.0311(8) 0.0276(7) 0.0020(6) 0.0111(6) -0.0065(6)
C13 0.0277(7) 0.0288(7) 0.0288(7) -0.0025(6) 0.0093(6) -0.0087(5)
C14 0.0547(10) 0.0352(9) 0.0267(8) 0.0050(7) 0.0043(7) -0.0005(7)
C15 0.0241(7) 0.0231(7) 0.0217(6) 0.0013(5) 0.0057(5) -0.0002(5)
C16 0.0299(7) 0.0286(8) 0.0288(7) -0.0042(6) 0.0092(6) -0.0047(6)
C17 0.0286(8) 0.0364(9) 0.0379(8) -0.0012(7) 0.0106(6) -0.0109(6)
C18 0.0251(7) 0.0371(9) 0.0357(8) 0.0042(7) 0.0121(6) -0.0007(6)
C19 0.0280(8) 0.0321(8) 0.0349(8) -0.0021(6) 0.0139(6) 0.0018(6)
C20 0.0256(7) 0.0206(7) 0.0325(7) 0.0021(5) 0.0139(6) -0.0013(5)
C21 0.0383(8) 0.0257(8) 0.0362(8) -0.0012(6) 0.0146(6) 0.0033(6)
C22 0.0463(9) 0.0268(8) 0.0492(10) 0.0011(7) 0.0206(8) 0.0099(6)
C23 0.0353(8) 0.0330(9) 0.0467(10) 0.0090(7) 0.0123(7) 0.0088(6)
C24 0.0323(8) 0.0344(9) 0.0371(8) 0.0033(7) 0.0079(6) 0.0043(6)

_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 C1 1.3791(16) . ?
N1 C4 1.4267(17) . ?
N1 C8 1.4315(17) . ?
N2 N3 1.2769(16) . ?
N2 C5 1.4426(18) . ?
N3 C2 1.4749(17) . ?
N4 C15 1.3355(17) . ?
N4 C19 1.3433(18) . ?
N5 C24 1.3361(18) . ?
N5 C20 1.3484(19) . ?
O1 C4 1.2054(16) . ?
O2 C11 1.3734(17) . ?
O2 C14 1.4316(19) . ?
C1 C5 1.3582(18) . ?
C1 C2 1.4954(19) . ?
C2 C15 1.5396(18) . ?
C2 C3 1.5578(18) . ?
C3 C6 1.5206(19) . ?
C3 C7 1.5424(19) . ?
C3 C4 1.5439(19) . ?
C5 C20 1.4595(19) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C13 1.3806(19) . ?
C8 C9 1.3895(18) . ?
C9 C10 1.3887(19) . ?
C9 H9 0.9500 . ?
C10 C11 1.3901(19) . ?
C10 H10 0.9500 . ?
C11 C12 1.3905(19) . ?
C12 C13 1.387(2) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.3895(18) . ?
C16 C17 1.384(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.383(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(2) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.3938(19) . ?
C21 C22 1.385(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.378(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.384(2) . ?
C23 H23 0.9500 . ?
C24 H24 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
C1 N1 C4 108.88(11) . . ?
C1 N1 C8 127.92(11) . . ?
C4 N1 C8 122.99(11) . . ?
N3 N2 C5 112.69(11) . . ?
N2 N3 C2 108.40(11) . . ?
C15 N4 C19 117.49(12) . . ?
C24 N5 C20 116.98(13) . . ?
C11 O2 C14 116.60(11) . . ?
C5 C1 N1 141.32(12) . . ?
C5 C1 C2 107.49(11) . . ?
N1 C1 C2 108.90(11) . . ?
N3 C2 C1 103.74(11) . . ?
N3 C2 C15 108.53(10) . . ?
C1 C2 C15 108.98(10) . . ?
N3 C2 C3 119.66(10) . . ?
C1 C2 C3 100.89(10) . . ?
C15 C2 C3 113.82(11) . . ?
C6 C3 C7 109.77(11) . . ?
C6 C3 C4 112.80(12) . . ?
C7 C3 C4 106.65(11) . . ?
C6 C3 C2 117.78(11) . . ?
C7 C3 C2 109.75(11) . . ?
C4 C3 C2 99.21(10) . . ?
O1 C4 N1 124.29(13) . . ?
O1 C4 C3 127.87(13) . . ?
N1 C4 C3 107.62(11) . . ?
C1 C5 N2 107.05(11) . . ?
C1 C5 C20 133.85(13) . . ?
N2 C5 C20 118.86(12) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C13 C8 C9 120.36(13) . . ?
C13 C8 N1 119.35(11) . . ?
C9 C8 N1 120.26(12) . . ?
C10 C9 C8 119.48(12) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 120.28(12) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
O2 C11 C10 115.95(12) . . ?
O2 C11 C12 124.21(13) . . ?
C10 C11 C12 119.83(13) . . ?
C13 C12 C11 119.76(13) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C8 C13 C12 120.28(12) . . ?
C8 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
O2 C14 H14A 109.5 . . ?
O2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 C16 122.94(12) . . ?
N4 C15 C2 115.06(11) . . ?
C16 C15 C2 121.97(12) . . ?
C17 C16 C15 118.73(13) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C18 C17 C16 119.06(13) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C17 C18 C19 118.29(13) . . ?
C17 C18 H18 120.9 . . ?
C19 C18 H18 120.9 . . ?
N4 C19 C18 123.48(14) . . ?
N4 C19 H19 118.3 . . ?
C18 C19 H19 118.3 . . ?
N5 C20 C21 122.75(13) . . ?
N5 C20 C5 116.17(12) . . ?
C21 C20 C5 121.07(13) . . ?
C22 C21 C20 118.78(15) . . ?
C22 C21 H21 120.6 . . ?
C20 C21 H21 120.6 . . ?
C23 C22 C21 118.97(15) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 118.46(15) . . ?
C22 C23 H23 120.8 . . ?
C24 C23 H23 120.8 . . ?
N5 C24 C23 124.05(15) . . ?
N5 C24 H24 118.0 . . ?
C23 C24 H24 118.0 . . ?

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
C5 N2 N3 C2 4.69(14) . . . . ?
C4 N1 C1 C5 -142.26(17) . . . . ?
C8 N1 C1 C5 42.9(2) . . . . ?
C4 N1 C1 C2 17.12(14) . . . . ?
C8 N1 C1 C2 -157.69(11) . . . . ?
N2 N3 C2 C1 -7.53(13) . . . . ?
N2 N3 C2 C15 108.26(12) . . . . ?
N2 N3 C2 C3 -118.82(12) . . . . ?
C5 C1 C2 N3 7.75(13) . . . . ?
N1 C1 C2 N3 -158.91(10) . . . . ?
C5 C1 C2 C15 -107.72(12) . . . . ?
N1 C1 C2 C15 85.62(12) . . . . ?
C5 C1 C2 C3 132.21(11) . . . . ?
N1 C1 C2 C3 -34.45(13) . . . . ?
N3 C2 C3 C6 -89.33(15) . . . . ?
C1 C2 C3 C6 157.85(12) . . . . ?
C15 C2 C3 C6 41.31(16) . . . . ?
N3 C2 C3 C7 37.22(16) . . . . ?
C1 C2 C3 C7 -75.60(12) . . . . ?
C15 C2 C3 C7 167.85(11) . . . . ?
N3 C2 C3 C4 148.73(11) . . . . ?
C1 C2 C3 C4 35.91(12) . . . . ?
C15 C2 C3 C4 -80.64(12) . . . . ?
C1 N1 C4 O1 -177.01(12) . . . . ?
C8 N1 C4 O1 -1.9(2) . . . . ?
C1 N1 C4 C3 8.13(13) . . . . ?
C8 N1 C4 C3 -176.74(10) . . . . ?
C6 C3 C4 O1 31.83(19) . . . . ?
C7 C3 C4 O1 -88.75(16) . . . . ?
C2 C3 C4 O1 157.31(14) . . . . ?
C6 C3 C4 N1 -153.55(11) . . . . ?
C7 C3 C4 N1 85.87(12) . . . . ?
C2 C3 C4 N1 -28.07(12) . . . . ?
N1 C1 C5 N2 154.26(16) . . . . ?
C2 C1 C5 N2 -5.29(13) . . . . ?
N1 C1 C5 C20 -19.9(3) . . . . ?
C2 C1 C5 C20 -179.41(14) . . . . ?
N3 N2 C5 C1 0.46(14) . . . . ?
N3 N2 C5 C20 175.61(11) . . . . ?
C1 N1 C8 C13 50.19(18) . . . . ?
C4 N1 C8 C13 -123.96(14) . . . . ?
C1 N1 C8 C9 -131.86(14) . . . . ?
C4 N1 C8 C9 53.99(17) . . . . ?
C13 C8 C9 C10 0.6(2) . . . . ?
N1 C8 C9 C10 -177.35(11) . . . . ?
C8 C9 C10 C11 -0.3(2) . . . . ?
C14 O2 C11 C10 177.59(13) . . . . ?
C14 O2 C11 C12 -3.2(2) . . . . ?
C9 C10 C11 O2 178.72(12) . . . . ?
C9 C10 C11 C12 -0.5(2) . . . . ?
O2 C11 C12 C13 -178.10(13) . . . . ?
C10 C11 C12 C13 1.1(2) . . . . ?
C9 C8 C13 C12 0.0(2) . . . . ?
N1 C8 C13 C12 177.92(12) . . . . ?
C11 C12 C13 C8 -0.8(2) . . . . ?
C19 N4 C15 C16 -0.2(2) . . . . ?
C19 N4 C15 C2 177.89(12) . . . . ?
N3 C2 C15 N4 175.29(11) . . . . ?
C1 C2 C15 N4 -72.37(14) . . . . ?
C3 C2 C15 N4 39.36(16) . . . . ?
N3 C2 C15 C16 -6.64(17) . . . . ?
C1 C2 C15 C16 105.71(15) . . . . ?
C3 C2 C15 C16 -142.56(13) . . . . ?
N4 C15 C16 C17 -0.6(2) . . . . ?
C2 C15 C16 C17 -178.49(12) . . . . ?
C15 C16 C17 C18 1.1(2) . . . . ?
C16 C17 C18 C19 -0.9(2) . . . . ?
C15 N4 C19 C18 0.4(2) . . . . ?
C17 C18 C19 N4 0.2(2) . . . . ?
C24 N5 C20 C21 -0.4(2) . . . . ?
C24 N5 C20 C5 178.46(12) . . . . ?
C1 C5 C20 N5 -14.2(2) . . . . ?
N2 C5 C20 N5 172.18(11) . . . . ?
C1 C5 C20 C21 164.62(14) . . . . ?
N2 C5 C20 C21 -8.95(19) . . . . ?
N5 C20 C21 C22 0.7(2) . . . . ?
C5 C20 C21 C22 -178.06(13) . . . . ?
C20 C21 C22 C23 -0.2(2) . . . . ?
C21 C22 C23 C24 -0.6(2) . . . . ?
C20 N5 C24 C23 -0.5(2) . . . . ?
C22 C23 C24 N5 1.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.85
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.053

# Attachment '5c-CCDC.cif'

data_r91125c
_database_code_depnum_ccdc_archive 'CCDC 844398'
#TrackingRef '5c-CCDC.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H21 N5 O2'
_chemical_formula_weight         411.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.926(2)
_cell_length_b                   10.434(2)
_cell_length_c                   10.832(2)
_cell_angle_alpha                105.94(3)
_cell_angle_beta                 101.26(3)
_cell_angle_gamma                102.67(3)
_cell_volume                     1012.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    3276
_cell_measurement_theta_min      2.186
_cell_measurement_theta_max      27.866

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             432
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9806
_exptl_absorpt_correction_T_max  0.9859
_exptl_absorpt_process_details   crystalclear

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  'rigaku saturn CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8354
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         27.85
_reflns_number_total             4712
_reflns_number_gt                3274
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'crystalclear(Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       crystalclear
_computing_data_reduction        crystalclear
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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^)+(0.0617P)^2^+0.0000P] 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     SHELXL
_refine_ls_extinction_coef       0.173(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4712
_refine_ls_number_parameters     284
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.1036
_refine_ls_wR_factor_gt          0.0975
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
N1 N 0.30018(10) 1.05527(9) 0.25690(10) 0.0180(2) Uani 1 1 d . . .
N2 N 0.38733(10) 1.31266(10) -0.02179(10) 0.0209(2) Uani 1 1 d . . .
N3 N 0.06989(9) 0.70288(9) -0.11813(10) 0.0193(2) Uani 1 1 d . . .
N4 N 0.07769(10) 0.91666(10) -0.08552(10) 0.0206(2) Uani 1 1 d . . .
N5 N 0.01076(10) 0.79005(10) -0.16863(10) 0.0232(2) Uani 1 1 d . . .
O1 O 0.43430(9) 1.22613(9) 0.45582(8) 0.0259(2) Uani 1 1 d . . .
O2 O 0.03927(9) 0.68449(9) 0.48428(9) 0.0296(2) Uani 1 1 d . . .
C1 C 0.39274(11) 1.18425(11) 0.33440(12) 0.0180(2) Uani 1 1 d . . .
C2 C 0.42834(11) 1.26544(11) 0.24155(11) 0.0169(2) Uani 1 1 d . . .
C3 C 0.34977(11) 1.15916(11) 0.10458(11) 0.0167(2) Uani 1 1 d . . .
C4 C 0.27507(11) 1.04196(11) 0.11911(11) 0.0159(2) Uani 1 1 d . . .
C5 C 0.36995(12) 1.39222(11) 0.27702(12) 0.0221(3) Uani 1 1 d . . .
H5A H 0.3956 1.4508 0.2234 0.033 Uiso 1 1 calc R . .
H5B H 0.4119 1.4463 0.3720 0.033 Uiso 1 1 calc R . .
H5C H 0.2653 1.3601 0.2583 0.033 Uiso 1 1 calc R . .
C6 C 0.59143(11) 1.31365(12) 0.26437(12) 0.0220(3) Uani 1 1 d . . .
H6A H 0.6283 1.2325 0.2493 0.033 Uiso 1 1 calc R . .
H6B H 0.6366 1.3766 0.3562 0.033 Uiso 1 1 calc R . .
H6C H 0.6136 1.3625 0.2021 0.033 Uiso 1 1 calc R . .
C7 C 0.22896(11) 0.95974(11) 0.31330(11) 0.0170(2) Uani 1 1 d . . .
C8 C 0.30688(11) 0.89024(11) 0.37841(12) 0.0190(2) Uani 1 1 d . . .
H8 H 0.4063 0.9055 0.3846 0.023 Uiso 1 1 calc R . .
C9 C 0.23985(12) 0.79903(11) 0.43408(12) 0.0204(3) Uani 1 1 d . . .
H9 H 0.2928 0.7503 0.4769 0.024 Uiso 1 1 calc R . .
C10 C 0.09516(12) 0.77836(11) 0.42765(12) 0.0200(3) Uani 1 1 d . . .
C11 C 0.01758(12) 0.85007(11) 0.36497(12) 0.0213(3) Uani 1 1 d . . .
H11 H -0.0809 0.8377 0.3620 0.026 Uiso 1 1 calc R . .
C12 C 0.08480(12) 0.93976(11) 0.30685(12) 0.0200(3) Uani 1 1 d . . .
H12 H 0.0318 0.9875 0.2626 0.024 Uiso 1 1 calc R . .
C13 C -0.10898(13) 0.66188(14) 0.48281(15) 0.0350(3) Uani 1 1 d . . .
H13A H -0.1233 0.7490 0.5333 0.052 Uiso 1 1 calc R . .
H13B H -0.1365 0.5908 0.5237 0.052 Uiso 1 1 calc R . .
H13C H -0.1683 0.6304 0.3904 0.052 Uiso 1 1 calc R . .
C14 C 0.36312(11) 1.18053(11) -0.02115(12) 0.0170(2) Uani 1 1 d . . .
C15 C 0.35451(13) 1.07189(12) -0.13469(13) 0.0263(3) Uani 1 1 d . . .
H15 H 0.3425 0.9801 -0.1315 0.032 Uiso 1 1 calc R . .
C16 C 0.36348(13) 1.09804(13) -0.25101(13) 0.0296(3) Uani 1 1 d . . .
H16 H 0.3548 1.0242 -0.3292 0.036 Uiso 1 1 calc R . .
C17 C 0.38535(12) 1.23313(14) -0.25299(13) 0.0269(3) Uani 1 1 d . . .
H17 H 0.3910 1.2544 -0.3320 0.032 Uiso 1 1 calc R . .
C18 C 0.39851(13) 1.33533(13) -0.13583(13) 0.0251(3) Uani 1 1 d . . .
H18 H 0.4168 1.4286 -0.1358 0.030 Uiso 1 1 calc R . .
C19 C 0.17906(11) 0.91365(11) 0.01681(12) 0.0165(2) Uani 1 1 d . . .
C20 C 0.17732(11) 0.77554(11) -0.00205(11) 0.0162(2) Uani 1 1 d . . .
C21 C 0.25422(12) 0.70011(11) 0.05938(12) 0.0202(3) Uani 1 1 d . . .
H21 H 0.3306 0.7469 0.1386 0.024 Uiso 1 1 calc R . .
C22 C 0.21697(13) 0.55962(12) 0.00317(13) 0.0247(3) Uani 1 1 d . . .
H22 H 0.2682 0.5078 0.0433 0.030 Uiso 1 1 calc R . .
C23 C 0.10271(13) 0.48912(12) -0.11457(13) 0.0262(3) Uani 1 1 d . . .
H23 H 0.0765 0.3905 -0.1510 0.031 Uiso 1 1 calc R . .
C24 C 0.03082(13) 0.56030(12) -0.17550(13) 0.0251(3) Uani 1 1 d . . .
H24 H -0.0445 0.5136 -0.2555 0.030 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
N1 0.0212(5) 0.0175(5) 0.0135(5) 0.0068(4) 0.0031(4) 0.0013(4)
N2 0.0279(5) 0.0212(5) 0.0188(6) 0.0106(4) 0.0098(4) 0.0092(4)
N3 0.0193(5) 0.0185(5) 0.0169(5) 0.0032(4) 0.0020(4) 0.0050(4)
N4 0.0235(5) 0.0220(5) 0.0148(5) 0.0048(4) 0.0025(4) 0.0072(4)
N5 0.0254(5) 0.0223(5) 0.0196(6) 0.0055(4) 0.0002(4) 0.0095(4)
O1 0.0300(5) 0.0274(5) 0.0139(5) 0.0067(4) 0.0026(3) -0.0012(3)
O2 0.0299(5) 0.0301(5) 0.0284(6) 0.0175(4) 0.0077(4) -0.0019(4)
C1 0.0189(5) 0.0185(5) 0.0161(6) 0.0065(5) 0.0052(4) 0.0035(4)
C2 0.0206(5) 0.0157(5) 0.0133(6) 0.0052(5) 0.0051(4) 0.0024(4)
C3 0.0209(5) 0.0152(5) 0.0142(6) 0.0039(4) 0.0054(4) 0.0061(4)
C4 0.0186(5) 0.0172(5) 0.0130(6) 0.0055(5) 0.0040(4) 0.0069(4)
C5 0.0272(6) 0.0191(6) 0.0180(7) 0.0032(5) 0.0056(5) 0.0072(5)
C6 0.0216(6) 0.0222(6) 0.0212(7) 0.0092(5) 0.0048(5) 0.0026(4)
C7 0.0223(5) 0.0139(5) 0.0130(6) 0.0041(4) 0.0048(4) 0.0022(4)
C8 0.0182(5) 0.0217(6) 0.0167(6) 0.0068(5) 0.0038(4) 0.0054(4)
C9 0.0249(6) 0.0190(6) 0.0164(6) 0.0079(5) 0.0016(4) 0.0055(4)
C10 0.0259(6) 0.0158(5) 0.0143(6) 0.0051(5) 0.0044(5) -0.0009(4)
C11 0.0175(5) 0.0204(6) 0.0231(7) 0.0055(5) 0.0052(5) 0.0023(4)
C12 0.0218(6) 0.0184(5) 0.0193(6) 0.0076(5) 0.0027(4) 0.0058(4)
C13 0.0306(7) 0.0400(8) 0.0292(8) 0.0159(6) 0.0091(6) -0.0062(5)
C14 0.0185(5) 0.0175(5) 0.0146(6) 0.0054(5) 0.0044(4) 0.0042(4)
C15 0.0338(7) 0.0192(6) 0.0229(7) 0.0020(5) 0.0143(5) 0.0023(5)
C16 0.0266(6) 0.0347(7) 0.0168(7) -0.0027(6) 0.0097(5) -0.0013(5)
C17 0.0216(6) 0.0461(8) 0.0166(6) 0.0157(6) 0.0071(5) 0.0089(5)
C18 0.0283(6) 0.0323(7) 0.0255(7) 0.0192(6) 0.0127(5) 0.0132(5)
C19 0.0187(5) 0.0172(5) 0.0150(6) 0.0069(5) 0.0048(4) 0.0058(4)
C20 0.0159(5) 0.0169(5) 0.0142(6) 0.0034(4) 0.0042(4) 0.0034(4)
C21 0.0223(6) 0.0204(6) 0.0170(6) 0.0057(5) 0.0036(4) 0.0069(4)
C22 0.0312(6) 0.0216(6) 0.0256(7) 0.0097(5) 0.0096(5) 0.0123(5)
C23 0.0337(7) 0.0152(6) 0.0260(7) 0.0015(5) 0.0088(5) 0.0060(5)
C24 0.0262(6) 0.0181(6) 0.0215(7) -0.0027(5) 0.0036(5) 0.0019(5)

_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 C1 1.3770(16) . ?
N1 C4 1.4264(15) . ?
N1 C7 1.4355(14) . ?
N2 C18 1.3403(15) . ?
N2 C14 1.3487(14) . ?
N3 N5 1.3612(13) . ?
N3 C20 1.3752(16) . ?
N3 C24 1.3766(14) . ?
N4 N5 1.3135(14) . ?
N4 C19 1.3562(15) . ?
O1 C1 1.2183(14) . ?
O2 C10 1.3667(13) . ?
O2 C13 1.4346(16) . ?
C1 C2 1.5263(16) . ?
C2 C3 1.5180(17) . ?
C2 C6 1.5341(15) . ?
C2 C5 1.5419(15) . ?
C3 C4 1.3504(15) . ?
C3 C14 1.4650(16) . ?
C4 C19 1.4635(17) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C12 1.3850(15) . ?
C7 C8 1.3911(15) . ?
C8 C9 1.3806(16) . ?
C8 H8 0.9500 . ?
C9 C10 1.3896(16) . ?
C9 H9 0.9500 . ?
C10 C11 1.3933(17) . ?
C11 C12 1.3897(16) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.3984(17) . ?
C15 C16 1.3754(18) . ?
C15 H15 0.9500 . ?
C16 C17 1.3852(18) . ?
C16 H16 0.9500 . ?
C17 C18 1.3768(18) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.3945(15) . ?
C20 C21 1.4133(15) . ?
C21 C22 1.3566(16) . ?
C21 H21 0.9500 . ?
C22 C23 1.4170(19) . ?
C22 H22 0.9500 . ?
C23 C24 1.3468(18) . ?
C23 H23 0.9500 . ?
C24 H24 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
C1 N1 C4 110.10(10) . . ?
C1 N1 C7 122.38(10) . . ?
C4 N1 C7 127.09(10) . . ?
C18 N2 C14 117.74(11) . . ?
N5 N3 C20 111.35(9) . . ?
N5 N3 C24 125.22(10) . . ?
C20 N3 C24 123.42(10) . . ?
N5 N4 C19 110.47(10) . . ?
N4 N5 N3 106.38(9) . . ?
C10 O2 C13 117.42(10) . . ?
O1 C1 N1 125.37(11) . . ?
O1 C1 C2 126.74(10) . . ?
N1 C1 C2 107.86(10) . . ?
C3 C2 C1 102.36(9) . . ?
C3 C2 C6 113.29(10) . . ?
C1 C2 C6 109.78(10) . . ?
C3 C2 C5 114.03(10) . . ?
C1 C2 C5 106.54(9) . . ?
C6 C2 C5 110.29(10) . . ?
C4 C3 C14 126.68(11) . . ?
C4 C3 C2 109.09(10) . . ?
C14 C3 C2 124.11(10) . . ?
C3 C4 N1 110.46(10) . . ?
C3 C4 C19 129.26(11) . . ?
N1 C4 C19 120.28(10) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C7 C8 119.99(10) . . ?
C12 C7 N1 120.48(10) . . ?
C8 C7 N1 119.50(10) . . ?
C9 C8 C7 120.03(10) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 120.21(11) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
O2 C10 C9 115.34(10) . . ?
O2 C10 C11 124.78(10) . . ?
C9 C10 C11 119.87(10) . . ?
C12 C11 C10 119.72(10) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C7 C12 C11 120.15(11) . . ?
C7 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
O2 C13 H13A 109.5 . . ?
O2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 C15 120.89(11) . . ?
N2 C14 C3 116.35(10) . . ?
C15 C14 C3 122.75(10) . . ?
C16 C15 C14 119.95(12) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 119.34(12) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C18 C17 C16 117.31(12) . . ?
C18 C17 H17 121.3 . . ?
C16 C17 H17 121.3 . . ?
N2 C18 C17 124.69(12) . . ?
N2 C18 H18 117.7 . . ?
C17 C18 H18 117.7 . . ?
N4 C19 C20 108.50(10) . . ?
N4 C19 C4 121.41(10) . . ?
C20 C19 C4 129.95(10) . . ?
N3 C20 C19 103.30(10) . . ?
N3 C20 C21 118.20(10) . . ?
C19 C20 C21 138.46(11) . . ?
C22 C21 C20 118.77(11) . . ?
C22 C21 H21 120.6 . . ?
C20 C21 H21 120.6 . . ?
C21 C22 C23 120.88(12) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C24 C23 C22 120.80(11) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 N3 117.89(11) . . ?
C23 C24 H24 121.1 . . ?
N3 C24 H24 121.1 . . ?

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
C19 N4 N5 N3 0.40(12) . . . . ?
C20 N3 N5 N4 -0.81(12) . . . . ?
C24 N3 N5 N4 -179.63(10) . . . . ?
C4 N1 C1 O1 179.99(10) . . . . ?
C7 N1 C1 O1 7.09(17) . . . . ?
C4 N1 C1 C2 2.06(12) . . . . ?
C7 N1 C1 C2 -170.84(9) . . . . ?
O1 C1 C2 C3 178.75(11) . . . . ?
N1 C1 C2 C3 -3.36(11) . . . . ?
O1 C1 C2 C6 58.16(15) . . . . ?
N1 C1 C2 C6 -123.95(10) . . . . ?
O1 C1 C2 C5 -61.25(15) . . . . ?
N1 C1 C2 C5 116.64(10) . . . . ?
C1 C2 C3 C4 3.60(11) . . . . ?
C6 C2 C3 C4 121.73(10) . . . . ?
C5 C2 C3 C4 -111.03(11) . . . . ?
C1 C2 C3 C14 -172.66(10) . . . . ?
C6 C2 C3 C14 -54.54(14) . . . . ?
C5 C2 C3 C14 72.70(13) . . . . ?
C14 C3 C4 N1 173.55(10) . . . . ?
C2 C3 C4 N1 -2.59(12) . . . . ?
C14 C3 C4 C19 -6.52(18) . . . . ?
C2 C3 C4 C19 177.35(10) . . . . ?
C1 N1 C4 C3 0.32(12) . . . . ?
C7 N1 C4 C3 172.81(10) . . . . ?
C1 N1 C4 C19 -179.62(9) . . . . ?
C7 N1 C4 C19 -7.14(16) . . . . ?
C1 N1 C7 C12 104.63(13) . . . . ?
C4 N1 C7 C12 -67.00(15) . . . . ?
C1 N1 C7 C8 -73.38(14) . . . . ?
C4 N1 C7 C8 114.99(13) . . . . ?
C12 C7 C8 C9 1.41(17) . . . . ?
N1 C7 C8 C9 179.43(10) . . . . ?
C7 C8 C9 C10 -1.28(17) . . . . ?
C13 O2 C10 C9 178.64(10) . . . . ?
C13 O2 C10 C11 -2.18(17) . . . . ?
C8 C9 C10 O2 179.13(10) . . . . ?
C8 C9 C10 C11 -0.09(17) . . . . ?
O2 C10 C11 C12 -177.83(11) . . . . ?
C9 C10 C11 C12 1.31(17) . . . . ?
C8 C7 C12 C11 -0.18(17) . . . . ?
N1 C7 C12 C11 -178.18(10) . . . . ?
C10 C11 C12 C7 -1.17(18) . . . . ?
C18 N2 C14 C15 1.94(16) . . . . ?
C18 N2 C14 C3 -179.30(10) . . . . ?
C4 C3 C14 N2 152.78(11) . . . . ?
C2 C3 C14 N2 -31.63(15) . . . . ?
C4 C3 C14 C15 -28.48(17) . . . . ?
C2 C3 C14 C15 147.11(11) . . . . ?
N2 C14 C15 C16 -3.32(18) . . . . ?
C3 C14 C15 C16 178.00(11) . . . . ?
C14 C15 C16 C17 1.92(18) . . . . ?
C15 C16 C17 C18 0.66(18) . . . . ?
C14 N2 C18 C17 0.82(17) . . . . ?
C16 C17 C18 N2 -2.13(18) . . . . ?
N5 N4 C19 C20 0.13(13) . . . . ?
N5 N4 C19 C4 176.19(9) . . . . ?
C3 C4 C19 N4 -46.14(17) . . . . ?
N1 C4 C19 N4 133.79(11) . . . . ?
C3 C4 C19 C20 128.99(14) . . . . ?
N1 C4 C19 C20 -51.08(16) . . . . ?
N5 N3 C20 C19 0.86(12) . . . . ?
C24 N3 C20 C19 179.70(10) . . . . ?
N5 N3 C20 C21 -176.99(10) . . . . ?
C24 N3 C20 C21 1.86(16) . . . . ?
N4 C19 C20 N3 -0.59(12) . . . . ?
C4 C19 C20 N3 -176.21(11) . . . . ?
N4 C19 C20 C21 176.55(13) . . . . ?
C4 C19 C20 C21 0.9(2) . . . . ?
N3 C20 C21 C22 -1.42(16) . . . . ?
C19 C20 C21 C22 -178.26(13) . . . . ?
C20 C21 C22 C23 -0.31(18) . . . . ?
C21 C22 C23 C24 1.77(19) . . . . ?
C22 C23 C24 N3 -1.38(19) . . . . ?
N5 N3 C24 C23 178.25(11) . . . . ?
C20 N3 C24 C23 -0.44(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        27.85
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.044

# Attachment '8i-CCDC.cif'

data_shelxl2
_database_code_depnum_ccdc_archive 'CCDC 844399'
#TrackingRef '8i-CCDC.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40.50 H44 N4 O4.50'
_chemical_formula_sum            'C40.50 H44 N4 O4.50'
_chemical_formula_weight         658.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   11.7220(17)
_cell_length_b                   11.8090(18)
_cell_length_c                   14.7910(18)
_cell_angle_alpha                96.802(8)
_cell_angle_beta                 93.368(2)
_cell_angle_gamma                119.634(9)
_cell_volume                     1750.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    5968
_cell_measurement_theta_min      1.40
_cell_measurement_theta_max      28.00

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             702
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9742
_exptl_absorpt_correction_T_max  0.9854
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD camera'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22069
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         27.91
_reflns_number_total             8303
_reflns_number_gt                4625
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r2'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r2'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'

_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^)+(0.0833P)^2^+0.0000P] 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         8303
_refine_ls_number_parameters     459
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1633
_refine_ls_wR_factor_gt          0.1545
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.060
_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 0.79733(14) 1.21865(14) 0.31422(11) 0.0367(4) Uani 1 1 d . . .
O2 O -0.11875(15) 0.21857(14) 0.01310(10) 0.0348(4) Uani 1 1 d . . .
O3 O 1.03525(15) 1.14651(16) 0.68080(11) 0.0444(4) Uani 1 1 d . . .
O4 O -0.45159(14) 0.53439(15) 0.14608(10) 0.0354(4) Uani 1 1 d . . .
N1 N 0.67089(15) 1.02877(15) 0.37380(11) 0.0248(4) Uani 1 1 d . . .
N2 N -0.07057(15) 0.38227(15) 0.14082(11) 0.0225(3) Uani 1 1 d . . .
N3 N 0.14500(15) 0.55778(15) 0.22337(11) 0.0221(3) Uani 1 1 d . . .
N4 N 0.5329(3) 0.61513(19) 0.59453(14) 0.0524(6) Uani 1 1 d . . .
C1 C 0.6950(2) 1.11255(19) 0.30995(14) 0.0278(4) Uani 1 1 d . . .
C2 C 0.57458(19) 1.05413(18) 0.23493(13) 0.0256(4) Uani 1 1 d . . .
C3 C 0.48312(19) 0.92676(18) 0.26657(13) 0.0227(4) Uani 1 1 d . . .
C4 C 0.54398(18) 0.91490(18) 0.34717(13) 0.0225(4) Uani 1 1 d . . .
C5 C 0.46533(18) 0.79622(18) 0.37804(13) 0.0214(4) Uani 1 1 d . . .
C6 C 0.34798(18) 0.72924(17) 0.31008(13) 0.0198(4) Uani 1 1 d . . .
C7 C 0.36287(18) 0.81199(18) 0.24042(13) 0.0212(4) Uani 1 1 d . . .
C8 C 0.26063(19) 0.75998(18) 0.16526(13) 0.0239(4) Uani 1 1 d . . .
H8 H 0.2653 0.8122 0.1199 0.029 Uiso 1 1 calc R . .
C9 C 0.15659(19) 0.63640(19) 0.15807(13) 0.0232(4) Uani 1 1 d . . .
H9 H 0.0894 0.6023 0.1068 0.028 Uiso 1 1 calc R . .
C10 C 0.23893(18) 0.60412(18) 0.29850(13) 0.0211(4) Uani 1 1 d . . .
H10 H 0.2289 0.5495 0.3432 0.025 Uiso 1 1 calc R . .
C11 C 0.76186(18) 1.06059(18) 0.45434(14) 0.0256(4) Uani 1 1 d . . .
C12 C 0.7218(2) 1.05587(19) 0.54030(14) 0.0270(4) Uani 1 1 d . . .
H12 H 0.6332 1.0333 0.5464 0.032 Uiso 1 1 calc R . .
C13 C 0.8099(2) 1.08376(19) 0.61813(14) 0.0289(5) Uani 1 1 d . . .
H13 H 0.7811 1.0781 0.6770 0.035 Uiso 1 1 calc R . .
C14 C 0.9401(2) 1.1198(2) 0.60925(15) 0.0335(5) Uani 1 1 d . . .
C15 C 0.9808(2) 1.1281(3) 0.52296(17) 0.0489(7) Uani 1 1 d . . .
H15 H 1.0707 1.1555 0.5171 0.059 Uiso 1 1 calc R . .
C16 C 0.8928(2) 1.0972(2) 0.44568(16) 0.0424(6) Uani 1 1 d . . .
H16 H 0.9212 1.1008 0.3867 0.051 Uiso 1 1 calc R . .
C17 C 0.5249(2) 1.15418(19) 0.24020(15) 0.0324(5) Uani 1 1 d . . .
H17A H 0.5034 1.1666 0.3030 0.039 Uiso 1 1 calc R . .
H17B H 0.5984 1.2404 0.2307 0.039 Uiso 1 1 calc R . .
C18 C 0.4045(2) 1.1163(2) 0.17195(17) 0.0413(6) Uani 1 1 d . . .
H18A H 0.4239 1.1034 0.1093 0.062 Uiso 1 1 calc R . .
H18B H 0.3832 1.1871 0.1794 0.062 Uiso 1 1 calc R . .
H18C H 0.3289 1.0342 0.1832 0.062 Uiso 1 1 calc R . .
C19 C 0.6174(2) 1.0353(2) 0.14019(14) 0.0314(5) Uani 1 1 d . . .
H19A H 0.5414 1.0056 0.0921 0.038 Uiso 1 1 calc R . .
H19B H 0.6892 1.1220 0.1298 0.038 Uiso 1 1 calc R . .
C20 C 0.6656(2) 0.9366(2) 0.12875(16) 0.0369(5) Uani 1 1 d . . .
H20A H 0.7369 0.9614 0.1785 0.055 Uiso 1 1 calc R . .
H20B H 0.6989 0.9370 0.0695 0.055 Uiso 1 1 calc R . .
H20C H 0.5920 0.8479 0.1310 0.055 Uiso 1 1 calc R . .
C21 C 0.9996(2) 1.1441(2) 0.77129(15) 0.0404(6) Uani 1 1 d . . .
H21A H 0.9759 1.2121 0.7869 0.061 Uiso 1 1 calc R . .
H21B H 1.0747 1.1615 0.8151 0.061 Uiso 1 1 calc R . .
H21C H 0.9237 1.0570 0.7741 0.061 Uiso 1 1 calc R . .
C22 C -0.05460(19) 0.29104(19) 0.08367(13) 0.0251(4) Uani 1 1 d . . .
C23 C 0.06681(19) 0.31574(18) 0.14714(13) 0.0232(4) Uani 1 1 d . . .
C24 C 0.04120(18) 0.41752(18) 0.20904(13) 0.0222(4) Uani 1 1 d . . .
H24 H 0.0118 0.3878 0.2683 0.027 Uiso 1 1 calc R . .
C25 C -0.16819(18) 0.41967(18) 0.14409(13) 0.0226(4) Uani 1 1 d . . .
C26 C -0.16314(19) 0.50240(18) 0.22083(13) 0.0256(4) Uani 1 1 d . . .
H26 H -0.0951 0.5328 0.2712 0.031 Uiso 1 1 calc R . .
C27 C -0.2585(2) 0.54132(19) 0.22426(14) 0.0270(4) Uani 1 1 d . . .
H27 H -0.2554 0.5973 0.2772 0.032 Uiso 1 1 calc R . .
C28 C -0.35680(19) 0.49834(19) 0.15064(14) 0.0259(4) Uani 1 1 d . . .
C29 C -0.3614(2) 0.4153(2) 0.07396(14) 0.0287(5) Uani 1 1 d . . .
H29 H -0.4292 0.3854 0.0235 0.034 Uiso 1 1 calc R . .
C30 C -0.26826(19) 0.37568(19) 0.07014(14) 0.0255(4) Uani 1 1 d . . .
H30 H -0.2724 0.3187 0.0174 0.031 Uiso 1 1 calc R . .
C31 C -0.4529(2) 0.6140(2) 0.22670(16) 0.0377(5) Uani 1 1 d . . .
H31A H -0.4708 0.5648 0.2780 0.056 Uiso 1 1 calc R . .
H31B H -0.5222 0.6360 0.2150 0.056 Uiso 1 1 calc R . .
H31C H -0.3666 0.6955 0.2422 0.056 Uiso 1 1 calc R . .
C32 C 0.0377(2) 0.19585(19) 0.19262(14) 0.0263(4) Uani 1 1 d . . .
H32A H -0.0501 0.1610 0.2141 0.032 Uiso 1 1 calc R . .
H32B H 0.0332 0.1256 0.1462 0.032 Uiso 1 1 calc R . .
C33 C 0.1406(2) 0.2274(2) 0.27323(15) 0.0349(5) Uani 1 1 d . . .
H33A H 0.2267 0.2559 0.2517 0.052 Uiso 1 1 calc R . .
H33B H 0.1145 0.1483 0.3012 0.052 Uiso 1 1 calc R . .
H33C H 0.1472 0.2983 0.3189 0.052 Uiso 1 1 calc R . .
C34 C 0.1969(2) 0.3752(2) 0.10511(15) 0.0314(5) Uani 1 1 d . . .
H34A H 0.2068 0.4509 0.0767 0.038 Uiso 1 1 calc R . .
H34B H 0.2720 0.4094 0.1548 0.038 Uiso 1 1 calc R . .
C35 C 0.2038(2) 0.2760(2) 0.03260(16) 0.0411(6) Uani 1 1 d . . .
H35A H 0.2010 0.2041 0.0612 0.062 Uiso 1 1 calc R . .
H35B H 0.2865 0.3206 0.0060 0.062 Uiso 1 1 calc R . .
H35C H 0.1283 0.2397 -0.0160 0.062 Uiso 1 1 calc R . .
C36 C 0.4903(2) 0.73793(18) 0.45347(13) 0.0249(4) Uani 1 1 d . . .
C37 C 0.3911(2) 0.6687(2) 0.50693(14) 0.0330(5) Uani 1 1 d . . .
H37 H 0.3071 0.6622 0.4969 0.040 Uiso 1 1 calc R . .
C38 C 0.4174(3) 0.6101(2) 0.57453(16) 0.0452(6) Uani 1 1 d . . .
H38 H 0.3484 0.5628 0.6094 0.054 Uiso 1 1 calc R . .
C39 C 0.6264(3) 0.6807(2) 0.54289(17) 0.0449(6) Uani 1 1 d . . .
H39 H 0.7093 0.6854 0.5547 0.054 Uiso 1 1 calc R . .
C40 C 0.6104(2) 0.7423(2) 0.47340(15) 0.0340(5) Uani 1 1 d . . .
H40 H 0.6811 0.7875 0.4392 0.041 Uiso 1 1 calc R . .
O5 O 1.0160(5) 0.4307(5) 0.4332(3) 0.111(2) Uani 0.50 1 d PDU A -1
H5 H 0.9432 0.3612 0.4139 0.166 Uiso 0.50 1 calc PR A -1
C41 C 0.9925(10) 0.5309(8) 0.4776(5) 0.107(4) Uani 0.50 1 d PDU A -1
H41A H 1.0271 0.5526 0.5431 0.160 Uiso 0.50 1 calc PR A -1
H41B H 0.8970 0.4980 0.4707 0.160 Uiso 0.50 1 calc PR A -1
H41C H 1.0372 0.6103 0.4494 0.160 Uiso 0.50 1 calc PR A -1

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 0.0278(8) 0.0260(8) 0.0401(9) 0.0069(6) 0.0030(7) 0.0015(7)
O2 0.0399(9) 0.0397(9) 0.0275(8) -0.0049(7) -0.0071(7) 0.0256(8)
O3 0.0314(9) 0.0605(11) 0.0332(9) -0.0027(8) -0.0075(7) 0.0206(8)
O4 0.0351(9) 0.0464(9) 0.0366(9) 0.0042(7) 0.0068(7) 0.0298(8)
N1 0.0198(8) 0.0206(8) 0.0260(9) 0.0033(7) 0.0016(7) 0.0045(7)
N2 0.0206(8) 0.0233(8) 0.0232(8) 0.0019(6) 0.0005(6) 0.0115(7)
N3 0.0207(8) 0.0198(8) 0.0234(8) 0.0039(6) 0.0025(6) 0.0085(7)
N4 0.0851(18) 0.0313(11) 0.0340(12) 0.0004(9) -0.0163(11) 0.0280(12)
C1 0.0267(11) 0.0265(11) 0.0275(11) 0.0036(8) 0.0056(8) 0.0114(9)
C2 0.0249(10) 0.0230(10) 0.0251(10) 0.0050(8) 0.0034(8) 0.0092(9)
C3 0.0244(10) 0.0206(9) 0.0227(10) 0.0040(7) 0.0045(8) 0.0109(8)
C4 0.0207(10) 0.0231(10) 0.0226(10) 0.0006(8) 0.0028(7) 0.0111(8)
C5 0.0198(9) 0.0217(9) 0.0212(10) 0.0022(7) 0.0013(7) 0.0099(8)
C6 0.0189(9) 0.0193(9) 0.0214(9) 0.0029(7) 0.0035(7) 0.0099(8)
C7 0.0219(10) 0.0232(10) 0.0215(10) 0.0039(7) 0.0038(7) 0.0136(8)
C8 0.0276(10) 0.0227(10) 0.0228(10) 0.0053(8) 0.0034(8) 0.0135(9)
C9 0.0239(10) 0.0286(10) 0.0200(10) 0.0053(8) 0.0005(7) 0.0155(9)
C10 0.0230(10) 0.0228(10) 0.0187(9) 0.0037(7) 0.0027(7) 0.0123(8)
C11 0.0184(10) 0.0239(10) 0.0270(11) 0.0005(8) -0.0005(8) 0.0063(8)
C12 0.0252(10) 0.0262(11) 0.0305(11) 0.0012(8) 0.0039(8) 0.0145(9)
C13 0.0294(11) 0.0279(11) 0.0277(11) -0.0016(8) 0.0032(8) 0.0146(9)
C14 0.0276(11) 0.0341(12) 0.0300(12) -0.0017(9) -0.0052(9) 0.0114(10)
C15 0.0220(12) 0.0737(18) 0.0398(14) 0.0094(13) 0.0030(10) 0.0162(12)
C16 0.0224(11) 0.0630(16) 0.0303(12) 0.0053(11) 0.0054(9) 0.0134(11)
C17 0.0354(12) 0.0219(10) 0.0384(13) 0.0061(9) 0.0074(10) 0.0130(10)
C18 0.0416(14) 0.0338(12) 0.0537(16) 0.0125(11) 0.0055(11) 0.0220(11)
C19 0.0341(12) 0.0291(11) 0.0272(11) 0.0076(9) 0.0085(9) 0.0123(10)
C20 0.0359(13) 0.0320(12) 0.0381(13) 0.0021(10) 0.0108(10) 0.0140(10)
C21 0.0456(14) 0.0393(13) 0.0304(12) 0.0006(10) -0.0075(10) 0.0195(11)
C22 0.0262(10) 0.0273(10) 0.0233(10) 0.0049(8) 0.0027(8) 0.0147(9)
C23 0.0232(10) 0.0228(10) 0.0229(10) 0.0030(8) 0.0015(8) 0.0115(8)
C24 0.0191(9) 0.0213(10) 0.0221(10) 0.0034(7) -0.0001(7) 0.0075(8)
C25 0.0203(10) 0.0215(10) 0.0255(10) 0.0072(8) 0.0059(8) 0.0092(8)
C26 0.0255(10) 0.0237(10) 0.0248(10) 0.0029(8) 0.0008(8) 0.0108(9)
C27 0.0299(11) 0.0256(10) 0.0268(11) 0.0016(8) 0.0053(8) 0.0154(9)
C28 0.0228(10) 0.0267(10) 0.0328(11) 0.0093(8) 0.0092(8) 0.0145(9)
C29 0.0257(11) 0.0344(11) 0.0268(11) 0.0060(9) 0.0019(8) 0.0157(9)
C30 0.0253(10) 0.0257(10) 0.0243(10) 0.0030(8) 0.0056(8) 0.0118(9)
C31 0.0391(13) 0.0387(13) 0.0434(14) 0.0022(10) 0.0093(10) 0.0264(11)
C32 0.0263(11) 0.0231(10) 0.0281(11) 0.0038(8) -0.0001(8) 0.0119(9)
C33 0.0373(13) 0.0352(12) 0.0342(12) 0.0096(9) -0.0004(10) 0.0197(10)
C34 0.0306(11) 0.0328(12) 0.0338(12) 0.0081(9) 0.0092(9) 0.0172(10)
C35 0.0452(14) 0.0459(14) 0.0404(14) 0.0079(11) 0.0163(11) 0.0279(12)
C36 0.0286(11) 0.0181(9) 0.0228(10) -0.0008(7) -0.0032(8) 0.0095(8)
C37 0.0403(13) 0.0255(11) 0.0252(11) 0.0023(8) 0.0016(9) 0.0113(10)
C38 0.0665(18) 0.0271(12) 0.0254(12) 0.0026(9) -0.0001(11) 0.0124(12)
C39 0.0557(16) 0.0342(13) 0.0411(14) -0.0029(11) -0.0204(12) 0.0248(12)
C40 0.0347(12) 0.0264(11) 0.0359(12) -0.0015(9) -0.0100(9) 0.0147(10)
O5 0.101(4) 0.084(3) 0.033(2) -0.011(2) 0.023(2) -0.036(3)
C41 0.079(4) 0.115(7) 0.051(5) -0.009(4) 0.021(4) -0.003(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 1.224(2) . ?
O2 C22 1.203(2) . ?
O3 C14 1.378(2) . ?
O3 C21 1.425(3) . ?
O4 C28 1.373(2) . ?
O4 C31 1.434(2) . ?
N1 C1 1.388(3) . ?
N1 C4 1.416(2) . ?
N1 C11 1.430(2) . ?
N2 C22 1.383(2) . ?
N2 C25 1.417(2) . ?
N2 C24 1.454(2) . ?
N3 C10 1.365(2) . ?
N3 C9 1.384(2) . ?
N3 C24 1.471(2) . ?
N4 C39 1.335(4) . ?
N4 C38 1.340(3) . ?
C1 C2 1.540(3) . ?
C2 C3 1.504(3) . ?
C2 C19 1.544(3) . ?
C2 C17 1.551(3) . ?
C3 C7 1.377(3) . ?
C3 C4 1.410(3) . ?
C4 C5 1.395(3) . ?
C5 C6 1.450(3) . ?
C5 C36 1.465(3) . ?
C6 C10 1.376(3) . ?
C6 C7 1.462(3) . ?
C7 C8 1.415(3) . ?
C8 C9 1.348(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.379(3) . ?
C11 C16 1.392(3) . ?
C12 C13 1.391(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(3) . ?
C15 C16 1.376(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.520(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.524(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.536(3) . ?
C23 C32 1.532(3) . ?
C23 C34 1.536(3) . ?
C23 C24 1.582(3) . ?
C24 H24 1.0000 . ?
C25 C26 1.385(3) . ?
C25 C30 1.398(3) . ?
C26 C27 1.404(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.384(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.388(3) . ?
C29 C30 1.386(3) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.516(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.528(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C40 1.396(3) . ?
C36 C37 1.403(3) . ?
C37 C38 1.383(3) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.381(3) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
O5 C41 1.439(8) . ?
O5 H5 0.8400 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 O3 C21 117.74(17) . . ?
C28 O4 C31 116.58(17) . . ?
C1 N1 C4 109.11(16) . . ?
C1 N1 C11 123.10(16) . . ?
C4 N1 C11 127.75(16) . . ?
C22 N2 C25 135.11(16) . . ?
C22 N2 C24 94.92(14) . . ?
C25 N2 C24 129.42(15) . . ?
C10 N3 C9 120.67(16) . . ?
C10 N3 C24 117.47(15) . . ?
C9 N3 C24 121.44(15) . . ?
C39 N4 C38 115.6(2) . . ?
O1 C1 N1 124.19(19) . . ?
O1 C1 C2 125.35(19) . . ?
N1 C1 C2 110.44(16) . . ?
C3 C2 C1 100.59(16) . . ?
C3 C2 C19 113.97(16) . . ?
C1 C2 C19 109.38(16) . . ?
C3 C2 C17 114.13(16) . . ?
C1 C2 C17 106.45(15) . . ?
C19 C2 C17 111.40(17) . . ?
C7 C3 C4 107.90(17) . . ?
C7 C3 C2 141.58(18) . . ?
C4 C3 C2 110.30(17) . . ?
C5 C4 C3 112.87(17) . . ?
C5 C4 N1 137.60(18) . . ?
C3 C4 N1 109.53(16) . . ?
C4 C5 C6 103.22(16) . . ?
C4 C5 C36 132.02(18) . . ?
C6 C5 C36 124.51(17) . . ?
C10 C6 C5 131.17(17) . . ?
C10 C6 C7 119.20(17) . . ?
C5 C6 C7 109.35(16) . . ?
C3 C7 C8 135.70(18) . . ?
C3 C7 C6 106.62(16) . . ?
C8 C7 C6 117.66(16) . . ?
C9 C8 C7 120.01(18) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 N3 121.81(17) . . ?
C8 C9 H9 119.1 . . ?
N3 C9 H9 119.1 . . ?
N3 C10 C6 120.60(17) . . ?
N3 C10 H10 119.7 . . ?
C6 C10 H10 119.7 . . ?
C12 C11 C16 119.61(19) . . ?
C12 C11 N1 120.96(17) . . ?
C16 C11 N1 119.44(18) . . ?
C11 C12 C13 120.67(19) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C14 C13 C12 119.55(19) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
O3 C14 C13 124.8(2) . . ?
O3 C14 C15 115.6(2) . . ?
C13 C14 C15 119.6(2) . . ?
C16 C15 C14 120.9(2) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C11 119.7(2) . . ?
C15 C16 H16 120.2 . . ?
C11 C16 H16 120.2 . . ?
C18 C17 C2 115.85(17) . . ?
C18 C17 H17A 108.3 . . ?
C2 C17 H17A 108.3 . . ?
C18 C17 H17B 108.3 . . ?
C2 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C2 114.74(18) . . ?
C20 C19 H19A 108.6 . . ?
C2 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C2 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 H21A 109.5 . . ?
O3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O2 C22 N2 131.27(18) . . ?
O2 C22 C23 136.00(17) . . ?
N2 C22 C23 92.68(14) . . ?
C32 C23 C22 111.81(15) . . ?
C32 C23 C34 114.61(16) . . ?
C22 C23 C34 114.76(17) . . ?
C32 C23 C24 111.85(15) . . ?
C22 C23 C24 84.22(13) . . ?
C34 C23 C24 116.01(15) . . ?
N2 C24 N3 114.23(15) . . ?
N2 C24 C23 88.19(13) . . ?
N3 C24 C23 117.41(15) . . ?
N2 C24 H24 111.7 . . ?
N3 C24 H24 111.7 . . ?
C23 C24 H24 111.7 . . ?
C26 C25 C30 119.66(18) . . ?
C26 C25 N2 119.60(17) . . ?
C30 C25 N2 120.73(17) . . ?
C25 C26 C27 120.03(19) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 120.14(18) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
O4 C28 C27 124.53(18) . . ?
O4 C28 C29 115.90(19) . . ?
C27 C28 C29 119.56(18) . . ?
C30 C29 C28 120.75(19) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C25 119.86(18) . . ?
C29 C30 H30 120.1 . . ?
C25 C30 H30 120.1 . . ?
O4 C31 H31A 109.5 . . ?
O4 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O4 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C23 113.25(16) . . ?
C33 C32 H32A 108.9 . . ?
C23 C32 H32A 108.9 . . ?
C33 C32 H32B 108.9 . . ?
C23 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C23 113.19(17) . . ?
C35 C34 H34A 108.9 . . ?
C23 C34 H34A 108.9 . . ?
C35 C34 H34B 108.9 . . ?
C23 C34 H34B 108.9 . . ?
H34A C34 H34B 107.8 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C40 C36 C37 116.4(2) . . ?
C40 C36 C5 122.46(19) . . ?
C37 C36 C5 121.09(19) . . ?
C38 C37 C36 119.0(2) . . ?
C38 C37 H37 120.5 . . ?
C36 C37 H37 120.5 . . ?
N4 C38 C37 124.9(2) . . ?
N4 C38 H38 117.6 . . ?
C37 C38 H38 117.6 . . ?
N4 C39 C40 124.3(2) . . ?
N4 C39 H39 117.9 . . ?
C40 C39 H39 117.9 . . ?
C39 C40 C36 119.9(2) . . ?
C39 C40 H40 120.0 . . ?
C36 C40 H40 120.0 . . ?

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
C4 N1 C1 O1 -179.41(18) . . . . ?
C11 N1 C1 O1 2.8(3) . . . . ?
C4 N1 C1 C2 1.5(2) . . . . ?
C11 N1 C1 C2 -176.24(16) . . . . ?
O1 C1 C2 C3 -179.67(19) . . . . ?
N1 C1 C2 C3 -0.6(2) . . . . ?
O1 C1 C2 C19 60.1(3) . . . . ?
N1 C1 C2 C19 -120.89(17) . . . . ?
O1 C1 C2 C17 -60.4(2) . . . . ?
N1 C1 C2 C17 118.64(18) . . . . ?
C1 C2 C3 C7 -174.1(2) . . . . ?
C19 C2 C3 C7 -57.2(3) . . . . ?
C17 C2 C3 C7 72.4(3) . . . . ?
C1 C2 C3 C4 -0.51(19) . . . . ?
C19 C2 C3 C4 116.40(19) . . . . ?
C17 C2 C3 C4 -114.05(18) . . . . ?
C7 C3 C4 C5 -2.1(2) . . . . ?
C2 C3 C4 C5 -177.93(15) . . . . ?
C7 C3 C4 N1 177.28(15) . . . . ?
C2 C3 C4 N1 1.5(2) . . . . ?
C1 N1 C4 C5 177.3(2) . . . . ?
C11 N1 C4 C5 -5.0(4) . . . . ?
C1 N1 C4 C3 -1.9(2) . . . . ?
C11 N1 C4 C3 175.78(17) . . . . ?
C3 C4 C5 C6 1.0(2) . . . . ?
N1 C4 C5 C6 -178.2(2) . . . . ?
C3 C4 C5 C36 175.23(19) . . . . ?
N1 C4 C5 C36 -3.9(4) . . . . ?
C4 C5 C6 C10 174.22(19) . . . . ?
C36 C5 C6 C10 -0.6(3) . . . . ?
C4 C5 C6 C7 0.45(19) . . . . ?
C36 C5 C6 C7 -174.37(16) . . . . ?
C4 C3 C7 C8 -175.8(2) . . . . ?
C2 C3 C7 C8 -2.2(4) . . . . ?
C4 C3 C7 C6 2.2(2) . . . . ?
C2 C3 C7 C6 175.9(2) . . . . ?
C10 C6 C7 C3 -176.34(16) . . . . ?
C5 C6 C7 C3 -1.7(2) . . . . ?
C10 C6 C7 C8 2.1(2) . . . . ?
C5 C6 C7 C8 176.77(16) . . . . ?
C3 C7 C8 C9 175.6(2) . . . . ?
C6 C7 C8 C9 -2.3(3) . . . . ?
C7 C8 C9 N3 0.9(3) . . . . ?
C10 N3 C9 C8 0.8(3) . . . . ?
C24 N3 C9 C8 -171.66(16) . . . . ?
C9 N3 C10 C6 -1.0(3) . . . . ?
C24 N3 C10 C6 171.77(15) . . . . ?
C5 C6 C10 N3 -173.79(18) . . . . ?
C7 C6 C10 N3 -0.5(3) . . . . ?
C1 N1 C11 C12 126.4(2) . . . . ?
C4 N1 C11 C12 -51.0(3) . . . . ?
C1 N1 C11 C16 -53.4(3) . . . . ?
C4 N1 C11 C16 129.2(2) . . . . ?
C16 C11 C12 C13 -1.8(3) . . . . ?
N1 C11 C12 C13 178.40(17) . . . . ?
C11 C12 C13 C14 1.6(3) . . . . ?
C21 O3 C14 C13 -3.6(3) . . . . ?
C21 O3 C14 C15 177.7(2) . . . . ?
C12 C13 C14 O3 -178.33(19) . . . . ?
C12 C13 C14 C15 0.3(3) . . . . ?
O3 C14 C15 C16 176.7(2) . . . . ?
C13 C14 C15 C16 -2.0(4) . . . . ?
C14 C15 C16 C11 1.8(4) . . . . ?
C12 C11 C16 C15 0.1(3) . . . . ?
N1 C11 C16 C15 179.9(2) . . . . ?
C3 C2 C17 C18 -69.6(2) . . . . ?
C1 C2 C17 C18 -179.65(18) . . . . ?
C19 C2 C17 C18 61.2(2) . . . . ?
C3 C2 C19 C20 -48.2(2) . . . . ?
C1 C2 C19 C20 63.5(2) . . . . ?
C17 C2 C19 C20 -179.07(17) . . . . ?
C25 N2 C22 O2 5.5(4) . . . . ?
C24 N2 C22 O2 177.1(2) . . . . ?
C25 N2 C22 C23 -172.1(2) . . . . ?
C24 N2 C22 C23 -0.42(15) . . . . ?
O2 C22 C23 C32 -65.7(3) . . . . ?
N2 C22 C23 C32 111.64(16) . . . . ?
O2 C22 C23 C34 67.1(3) . . . . ?
N2 C22 C23 C34 -115.63(17) . . . . ?
O2 C22 C23 C24 -176.9(3) . . . . ?
N2 C22 C23 C24 0.39(14) . . . . ?
C22 N2 C24 N3 119.81(16) . . . . ?
C25 N2 C24 N3 -67.8(2) . . . . ?
C22 N2 C24 C23 0.41(14) . . . . ?
C25 N2 C24 C23 172.77(18) . . . . ?
C10 N3 C24 N2 166.91(15) . . . . ?
C9 N3 C24 N2 -20.4(2) . . . . ?
C10 N3 C24 C23 -91.9(2) . . . . ?
C9 N3 C24 C23 80.8(2) . . . . ?
C32 C23 C24 N2 -111.58(16) . . . . ?
C22 C23 C24 N2 -0.37(13) . . . . ?
C34 C23 C24 N2 114.40(18) . . . . ?
C32 C23 C24 N3 131.93(17) . . . . ?
C22 C23 C24 N3 -116.86(17) . . . . ?
C34 C23 C24 N3 -2.1(2) . . . . ?
C22 N2 C25 C26 169.6(2) . . . . ?
C24 N2 C25 C26 0.4(3) . . . . ?
C22 N2 C25 C30 -11.4(3) . . . . ?
C24 N2 C25 C30 179.44(17) . . . . ?
C30 C25 C26 C27 0.2(3) . . . . ?
N2 C25 C26 C27 179.22(17) . . . . ?
C25 C26 C27 C28 -0.7(3) . . . . ?
C31 O4 C28 C27 -4.9(3) . . . . ?
C31 O4 C28 C29 176.58(18) . . . . ?
C26 C27 C28 O4 -177.70(18) . . . . ?
C26 C27 C28 C29 0.7(3) . . . . ?
O4 C28 C29 C30 178.23(17) . . . . ?
C27 C28 C29 C30 -0.3(3) . . . . ?
C28 C29 C30 C25 -0.1(3) . . . . ?
C26 C25 C30 C29 0.2(3) . . . . ?
N2 C25 C30 C29 -178.80(17) . . . . ?
C22 C23 C32 C33 -165.04(16) . . . . ?
C34 C23 C32 C33 62.2(2) . . . . ?
C24 C23 C32 C33 -72.5(2) . . . . ?
C32 C23 C34 C35 57.9(2) . . . . ?
C22 C23 C34 C35 -73.5(2) . . . . ?
C24 C23 C34 C35 -169.35(17) . . . . ?
C4 C5 C36 C40 -41.7(3) . . . . ?
C6 C5 C36 C40 131.5(2) . . . . ?
C4 C5 C36 C37 141.4(2) . . . . ?
C6 C5 C36 C37 -45.4(3) . . . . ?
C40 C36 C37 C38 -0.1(3) . . . . ?
C5 C36 C37 C38 176.96(18) . . . . ?
C39 N4 C38 C37 -1.1(3) . . . . ?
C36 C37 C38 N4 0.8(3) . . . . ?
C38 N4 C39 C40 0.7(3) . . . . ?
N4 C39 C40 C36 -0.1(3) . . . . ?
C37 C36 C40 C39 -0.2(3) . . . . ?
C5 C36 C40 C39 -177.25(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.91
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.050