 
data_01sot013
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C26 H31 N3 O2' 
_chemical_formula_weight          417.54 
 
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    Cc
 
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                    25.5294(5) 
_cell_length_b                    18.9718(5) 
_cell_length_c                    9.7130(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  103.111(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      4581.75(18) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     14078 
_cell_measurement_theta_min       2.91 
_cell_measurement_theta_max       27.48 
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.211 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1792 
_exptl_absorpt_coefficient_mu     0.077 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.9847 
_exptl_absorpt_correction_T_max   0.9923 
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD' 
_diffrn_measurement_method        'Φ & ω scans' 
_diffrn_detector_area_resol_mean  9.091 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             18454 
_diffrn_reflns_av_R_equivalents   0.0810 
_diffrn_reflns_av_sigmaI/netI     0.0715 
_diffrn_reflns_limit_h_min        -28 
_diffrn_reflns_limit_h_max        28 
_diffrn_reflns_limit_k_min        -21 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        10 
_diffrn_reflns_theta_min          3.04 
_diffrn_reflns_theta_max          23.26 
_reflns_number_total              6361 
_reflns_number_gt                 5398 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'COLLECT (Hooft, 1998)' 
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'  
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'  
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0872P)²+2.6503P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0024(6) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.2(17) 
_refine_ls_number_reflns          6361 
_refine_ls_number_parameters      560 
_refine_ls_number_restraints      20 
_refine_ls_R_factor_all           0.0709 
_refine_ls_R_factor_gt            0.0567 
_refine_ls_wR_factor_ref          0.1555 
_refine_ls_wR_factor_gt           0.1438 
_refine_ls_goodness_of_fit_ref    1.082 
_refine_ls_restrained_S_all       1.099 
_refine_ls_shift/su_max           0.480 
_refine_ls_shift/su_mean          0.018 
 
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 0.1229(2) 1.5101(3) 0.1019(8) 0.0728(17) Uani 1 1 d . . . 
H1A H 0.1070 1.5260 0.1794 0.109 Uiso 1 1 calc R . . 
H1B H 0.0945 1.4921 0.0245 0.109 Uiso 1 1 calc R . . 
H1C H 0.1410 1.5498 0.0680 0.109 Uiso 1 1 calc R . . 
C2 C 0.1633(2) 1.4521(2) 0.1544(6) 0.0495(12) Uani 1 1 d . . . 
H2A H 0.1911 1.4701 0.2349 0.059 Uiso 1 1 calc R . . 
H2B H 0.1447 1.4123 0.1892 0.059 Uiso 1 1 calc R . . 
C3 C 0.1899(2) 1.4258(2) 0.0428(5) 0.0490(12) Uani 1 1 d . . . 
H3A H 0.2076 1.4660 0.0070 0.059 Uiso 1 1 calc R . . 
H3B H 0.1619 1.4075 -0.0369 0.059 Uiso 1 1 calc R . . 
C4 C 0.2309(2) 1.3690(2) 0.0899(6) 0.0451(13) Uani 1 1 d . . . 
H4A H 0.2486 1.3580 0.0119 0.054 Uiso 1 1 calc R . . 
H4B H 0.2588 1.3866 0.1707 0.054 Uiso 1 1 calc R . . 
C5 C 0.21834(17) 1.2394(2) 0.0932(4) 0.0236(10) Uani 1 1 d . . . 
C6 C 0.18620(17) 1.1825(2) 0.1327(4) 0.0218(10) Uani 1 1 d . . . 
C7 C 0.16413(18) 1.0697(2) 0.1518(4) 0.0234(10) Uani 1 1 d . . . 
C8 C 0.16879(17) 0.9917(2) 0.1368(4) 0.0213(9) Uani 1 1 d . . . 
C9 C 0.1578(2) 0.8774(2) 0.2438(5) 0.0363(12) Uani 1 1 d . . . 
H9A H 0.1855 0.8577 0.3226 0.044 Uiso 1 1 calc R . . 
H9B H 0.1652 0.8597 0.1542 0.044 Uiso 1 1 calc R . . 
C10 C 0.1027(2) 0.8511(2) 0.2566(5) 0.0447(13) Uani 1 1 d . . . 
H10A H 0.0760 0.8854 0.2055 0.054 Uiso 1 1 calc R . . 
H10B H 0.1018 0.8547 0.3578 0.054 Uiso 1 1 calc R . . 
C11 C 0.0811(3) 0.7771(4) 0.2070(8) 0.091(2) Uani 1 1 d U . . 
H11A H 0.0487 0.7664 0.2434 0.109 Uiso 1 1 calc R . . 
H11B H 0.0710 0.7753 0.1025 0.109 Uiso 1 1 calc R . . 
C12 C 0.1196(3) 0.7301(5) 0.2560(8) 0.098(2) Uani 1 1 d U . . 
H12A H 0.1066 0.6828 0.2251 0.146 Uiso 1 1 calc R . . 
H12B H 0.1290 0.7319 0.3596 0.146 Uiso 1 1 calc R . . 
H12C H 0.1514 0.7411 0.2195 0.146 Uiso 1 1 calc R . . 
C13 C 0.13871(16) 1.1812(2) 0.1791(4) 0.0202(9) Uani 1 1 d . . . 
C14 C 0.12497(17) 1.1093(2) 0.1927(4) 0.0240(10) Uani 1 1 d . . . 
C15 C 0.10347(17) 1.2430(2) 0.1956(4) 0.0237(10) Uani 1 1 d . . . 
C16 C 0.10610(19) 1.2764(2) 0.3242(5) 0.0303(10) Uani 1 1 d . . . 
H16 H 0.1318 1.2614 0.4057 0.036 Uiso 1 1 calc R . . 
C17 C 0.07162(19) 1.3312(2) 0.3348(5) 0.0381(12) Uani 1 1 d . . . 
H17 H 0.0734 1.3530 0.4238 0.046 Uiso 1 1 calc R . . 
C18 C 0.0346(2) 1.3545(2) 0.2174(5) 0.0388(12) Uani 1 1 d . . . 
H18 H 0.0113 1.3926 0.2250 0.047 Uiso 1 1 calc R . . 
C19 C 0.0317(2) 1.3220(2) 0.0883(5) 0.0400(12) Uani 1 1 d . . . 
H19 H 0.0063 1.3378 0.0070 0.048 Uiso 1 1 calc R . . 
C20 C 0.06568(19) 1.2665(2) 0.0774(5) 0.0326(11) Uani 1 1 d . . . 
H20 H 0.0633 1.2443 -0.0115 0.039 Uiso 1 1 calc R . . 
C21 C 0.07350(16) 1.0845(2) 0.2262(4) 0.0231(10) Uani 1 1 d . . . 
C22 C 0.04142(18) 1.0360(2) 0.1404(4) 0.0281(10) Uani 1 1 d . . . 
H22 H 0.0528 1.0163 0.0622 0.034 Uiso 1 1 calc R . . 
C23 C -0.0071(2) 1.0162(3) 0.1682(5) 0.0362(11) Uani 1 1 d . . . 
H23 H -0.0295 0.9837 0.1075 0.043 Uiso 1 1 calc R . . 
C24 C -0.02327(18) 1.0433(2) 0.2837(5) 0.0344(12) Uani 1 1 d . . . 
H24 H -0.0566 1.0291 0.3027 0.041 Uiso 1 1 calc R . . 
C25 C 0.00887(19) 1.0913(2) 0.3720(5) 0.0335(11) Uani 1 1 d . . . 
H25 H -0.0025 1.1109 0.4503 0.040 Uiso 1 1 calc R . . 
C26 C 0.05807(18) 1.1103(2) 0.3443(5) 0.0290(10) Uani 1 1 d . . . 
H26 H 0.0813 1.1412 0.4070 0.035 Uiso 1 1 calc R . . 
C27 C 0.3329(3) 0.4381(4) 0.8852(6) 0.0809(19) Uani 1 1 d . . . 
H27A H 0.3687 0.4598 0.9042 0.121 Uiso 1 1 calc R . . 
H27B H 0.3341 0.3954 0.9427 0.121 Uiso 1 1 calc R . . 
H27C H 0.3071 0.4714 0.9091 0.121 Uiso 1 1 calc R . . 
C28 C 0.3158(2) 0.4188(3) 0.7296(5) 0.0556(13) Uani 1 1 d . . . 
H28A H 0.3427 0.3863 0.7053 0.067 Uiso 1 1 calc R . . 
H28B H 0.3151 0.4620 0.6719 0.067 Uiso 1 1 calc R . . 
C29 C 0.26038(17) 0.3838(2) 0.6929(4) 0.0410(11) Uani 1 1 d . . . 
H29A H 0.2342 0.4155 0.7227 0.049 Uiso 1 1 calc R . . 
H29B H 0.2619 0.3396 0.7478 0.049 Uiso 1 1 calc R . . 
C30 C 0.2399(2) 0.3667(2) 0.5355(5) 0.0392(12) Uani 1 1 d . . . 
H30A H 0.2011 0.3553 0.5176 0.047 Uiso 1 1 calc R . . 
H30B H 0.2439 0.4090 0.4792 0.047 Uiso 1 1 calc R . . 
C31 C 0.25118(18) 0.2407(2) 0.4999(4) 0.0247(10) Uani 1 1 d . . . 
C32 C 0.28383(17) 0.1846(2) 0.4541(4) 0.0235(10) Uani 1 1 d . . . 
C33 C 0.30433(17) 0.07141(19) 0.4271(4) 0.0189(9) Uani 1 1 d . . . 
C34 C 0.29838(17) -0.0054(2) 0.4384(4) 0.0204(9) Uani 1 1 d . . . 
C35 C 0.30540(18) -0.1203(2) 0.3280(4) 0.0277(10) Uani 1 1 d . . . 
H35A H 0.2825 -0.1388 0.2393 0.033 Uiso 1 1 calc R . . 
H35B H 0.2908 -0.1379 0.4077 0.033 Uiso 1 1 calc R . . 
C36 C 0.36236(18) -0.1473(2) 0.3436(5) 0.0308(10) Uani 1 1 d . . . 
H36A H 0.3760 -0.1331 0.2600 0.037 Uiso 1 1 calc R . . 
H36B H 0.3860 -0.1260 0.4284 0.037 Uiso 1 1 calc R . . 
C37 C 0.36387(17) -0.22657(18) 0.3571(4) 0.0270(9) Uani 1 1 d . . . 
H37A H 0.3467 -0.2475 0.2645 0.032 Uiso 1 1 calc R . . 
H37B H 0.3424 -0.2408 0.4256 0.032 Uiso 1 1 calc R . . 
C38 C 0.42128(17) -0.2570(2) 0.4060(5) 0.0370(10) Uani 1 1 d U . . 
H38A H 0.4194 -0.3085 0.4109 0.055 Uiso 1 1 calc R . . 
H38B H 0.4380 -0.2382 0.4997 0.055 Uiso 1 1 calc R . . 
H38C H 0.4428 -0.2435 0.3385 0.055 Uiso 1 1 calc R . . 
C39 C 0.33128(18) 0.1840(2) 0.4081(4) 0.0242(10) Uani 1 1 d . . . 
C40 C 0.34441(16) 0.1124(2) 0.3908(4) 0.0223(10) Uani 1 1 d . . . 
C41 C 0.36616(17) 0.2451(2) 0.3965(4) 0.0257(10) Uani 1 1 d . . . 
C42 C 0.3592(2) 0.2858(2) 0.2743(5) 0.0355(12) Uani 1 1 d . . . 
H42 H 0.3311 0.2749 0.1949 0.043 Uiso 1 1 calc R . . 
C43 C 0.3933(2) 0.3424(3) 0.2679(5) 0.0460(13) Uani 1 1 d . . . 
H43 H 0.3881 0.3700 0.1843 0.055 Uiso 1 1 calc R . . 
C44 C 0.4347(2) 0.3589(3) 0.3826(5) 0.0446(13) Uani 1 1 d . . . 
H44 H 0.4582 0.3970 0.3767 0.054 Uiso 1 1 calc R . . 
C45 C 0.4416(2) 0.3206(2) 0.5033(5) 0.0400(12) Uani 1 1 d . . . 
H45 H 0.4693 0.3326 0.5828 0.048 Uiso 1 1 calc R . . 
C46 C 0.40794(19) 0.2637(2) 0.5102(4) 0.0332(11) Uani 1 1 d . . . 
H46 H 0.4136 0.2367 0.5947 0.040 Uiso 1 1 calc R . . 
C47 C 0.39401(16) 0.0869(2) 0.3551(4) 0.0222(10) Uani 1 1 d . . . 
C48 C 0.42532(19) 0.0340(2) 0.4337(5) 0.0301(10) Uani 1 1 d . . . 
H48 H 0.4137 0.0132 0.5106 0.036 Uiso 1 1 calc R . . 
C49 C 0.47301(18) 0.0109(2) 0.4024(5) 0.0332(11) Uani 1 1 d . . . 
H49 H 0.4930 -0.0262 0.4553 0.040 Uiso 1 1 calc R . . 
C50 C 0.4910(2) 0.0428(2) 0.2932(5) 0.0369(12) Uani 1 1 d . . . 
H50 H 0.5240 0.0285 0.2724 0.044 Uiso 1 1 calc R . . 
C51 C 0.46122(19) 0.0949(3) 0.2160(5) 0.0350(12) Uani 1 1 d . . . 
H51 H 0.4737 0.1163 0.1410 0.042 Uiso 1 1 calc R . . 
C52 C 0.41345(18) 0.1171(2) 0.2446(4) 0.0280(10) Uani 1 1 d . . . 
H52 H 0.3934 0.1533 0.1888 0.034 Uiso 1 1 calc R . . 
N1 N 0.20738(16) 1.30476(18) 0.1320(4) 0.0356(10) Uani 1 1 d . . . 
H1 H 0.1844 1.3091 0.1866 0.043 Uiso 1 1 calc R . . 
N2 N 0.20018(14) 1.11417(18) 0.1157(3) 0.0240(8) Uani 1 1 d . . . 
H2 H 0.2287 1.1009 0.0855 0.029 Uiso 1 1 calc R . . 
N3 N 0.16205(14) 0.95437(17) 0.2466(3) 0.0265(9) Uani 1 1 d . . . 
H3 H 0.1600 0.9768 0.3246 0.032 Uiso 1 1 calc R . . 
N4 N 0.26817(16) 0.30776(19) 0.4877(4) 0.0347(9) Uani 1 1 d . . . 
H4 H 0.2961 0.3158 0.4511 0.042 Uiso 1 1 calc R . . 
N5 N 0.26782(13) 0.11566(17) 0.4663(3) 0.0205(8) Uani 1 1 d . . . 
H5 H 0.2389 0.1024 0.4945 0.025 Uiso 1 1 calc R . . 
N6 N 0.30320(15) -0.04305(17) 0.3258(3) 0.0249(8) Uani 1 1 d . . . 
H6 H 0.3051 -0.0208 0.2476 0.030 Uiso 1 1 calc R . . 
O1 O 0.25431(12) 1.22776(16) 0.0299(3) 0.0350(8) Uani 1 1 d . . . 
O2 O 0.17801(11) 0.96614(14) 0.0272(3) 0.0261(7) Uani 1 1 d . . . 
O3 O 0.21383(12) 0.22643(16) 0.5512(3) 0.0321(8) Uani 1 1 d . . . 
O4 O 0.29126(12) -0.03201(14) 0.5506(2) 0.0253(7) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
C1 C2 1.516(7) . ? 
C2 C3 1.490(7) . ? 
C3 C4 1.499(7) . ? 
C4 N1 1.457(5) . ? 
C5 O1 1.235(5) . ? 
C5 N1 1.344(5) . ? 
C5 C6 1.459(6) . ? 
C6 N2 1.364(5) . ? 
C6 C13 1.386(6) . ? 
C7 N2 1.353(5) . ? 
C7 C14 1.380(6) . ? 
C7 C8 1.494(6) . ? 
C8 O2 1.239(5) . ? 
C8 N3 1.324(5) . ? 
C9 N3 1.465(5) . ? 
C9 C10 1.524(7) . ? 
C10 C11 1.544(9) . ? 
C11 C12 1.332(10) . ? 
C13 C14 1.422(5) . ? 
C13 C15 1.508(6) . ? 
C14 C21 1.499(6) . ? 
C15 C16 1.389(6) . ? 
C15 C20 1.395(6) . ? 
C16 C17 1.381(6) . ? 
C17 C18 1.378(7) . ? 
C18 C19 1.384(7) . ? 
C19 C20 1.382(6) . ? 
C21 C22 1.379(6) . ? 
C21 C26 1.384(6) . ? 
C22 C23 1.379(6) . ? 
C23 C24 1.379(7) . ? 
C24 C25 1.384(7) . ? 
C25 C26 1.391(6) . ? 
C27 C28 1.520(7) . ? 
C28 C29 1.530(6) . ? 
C29 C30 1.534(6) . ? 
C30 N4 1.463(6) . ? 
C31 O3 1.203(5) . ? 
C31 N4 1.358(6) . ? 
C31 C32 1.480(6) . ? 
C32 C39 1.383(6) . ? 
C32 N5 1.384(5) . ? 
C33 N5 1.371(5) . ? 
C33 C40 1.393(6) . ? 
C33 C34 1.471(5) . ? 
C34 O4 1.252(5) . ? 
C34 N6 1.336(5) . ? 
C35 N6 1.466(5) . ? 
C35 C36 1.517(6) . ? 
C36 C37 1.510(5) . ? 
C37 C38 1.546(6) . ? 
C39 C40 1.418(6) . ? 
C39 C41 1.482(6) . ? 
C40 C47 1.468(6) . ? 
C41 C42 1.393(6) . ? 
C41 C46 1.396(6) . ? 
C42 C43 1.392(6) . ? 
C43 C44 1.386(7) . ? 
C44 C45 1.356(7) . ? 
C45 C46 1.391(6) . ? 
C47 C48 1.398(6) . ? 
C47 C52 1.403(6) . ? 
C48 C49 1.391(6) . ? 
C49 C50 1.387(7) . ? 
C50 C51 1.363(7) . ? 
C51 C52 1.377(6) . ? 
 
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 
C3 C2 C1 112.7(5) . . ? 
C2 C3 C4 114.9(4) . . ? 
N1 C4 C3 112.6(4) . . ? 
O1 C5 N1 122.0(4) . . ? 
O1 C5 C6 121.6(4) . . ? 
N1 C5 C6 116.3(4) . . ? 
N2 C6 C13 107.1(4) . . ? 
N2 C6 C5 119.5(4) . . ? 
C13 C6 C5 133.2(4) . . ? 
N2 C7 C14 108.3(3) . . ? 
N2 C7 C8 121.3(4) . . ? 
C14 C7 C8 130.3(4) . . ? 
O2 C8 N3 124.6(4) . . ? 
O2 C8 C7 120.4(4) . . ? 
N3 C8 C7 115.0(3) . . ? 
N3 C9 C10 113.0(4) . . ? 
C9 C10 C11 122.9(5) . . ? 
C12 C11 C10 108.3(7) . . ? 
C6 C13 C14 107.5(4) . . ? 
C6 C13 C15 127.4(4) . . ? 
C14 C13 C15 124.7(4) . . ? 
C7 C14 C13 106.6(4) . . ? 
C7 C14 C21 128.3(4) . . ? 
C13 C14 C21 124.6(4) . . ? 
C16 C15 C20 118.5(4) . . ? 
C16 C15 C13 122.8(4) . . ? 
C20 C15 C13 118.6(4) . . ? 
C17 C16 C15 120.6(4) . . ? 
C18 C17 C16 120.6(4) . . ? 
C17 C18 C19 119.5(4) . . ? 
C20 C19 C18 120.2(4) . . ? 
C19 C20 C15 120.6(4) . . ? 
C22 C21 C26 119.6(4) . . ? 
C22 C21 C14 120.6(4) . . ? 
C26 C21 C14 119.8(4) . . ? 
C21 C22 C23 120.1(4) . . ? 
C22 C23 C24 120.3(5) . . ? 
C23 C24 C25 120.3(4) . . ? 
C24 C25 C26 119.0(4) . . ? 
C21 C26 C25 120.5(4) . . ? 
C27 C28 C29 112.2(4) . . ? 
C28 C29 C30 114.4(4) . . ? 
N4 C30 C29 113.4(4) . . ? 
O3 C31 N4 123.1(4) . . ? 
O3 C31 C32 121.1(4) . . ? 
N4 C31 C32 115.7(4) . . ? 
C39 C32 N5 108.5(4) . . ? 
C39 C32 C31 134.2(4) . . ? 
N5 C32 C31 117.2(4) . . ? 
N5 C33 C40 108.2(3) . . ? 
N5 C33 C34 119.8(4) . . ? 
C40 C33 C34 131.8(4) . . ? 
O4 C34 N6 123.7(3) . . ? 
O4 C34 C33 120.2(3) . . ? 
N6 C34 C33 116.0(3) . . ? 
N6 C35 C36 111.8(4) . . ? 
C37 C36 C35 110.5(4) . . ? 
C36 C37 C38 113.7(4) . . ? 
C32 C39 C40 107.1(4) . . ? 
C32 C39 C41 127.1(4) . . ? 
C40 C39 C41 125.3(4) . . ? 
C33 C40 C39 107.3(4) . . ? 
C33 C40 C47 126.7(4) . . ? 
C39 C40 C47 125.7(4) . . ? 
C42 C41 C46 117.5(4) . . ? 
C42 C41 C39 122.4(4) . . ? 
C46 C41 C39 120.1(4) . . ? 
C43 C42 C41 120.3(4) . . ? 
C44 C43 C42 120.6(4) . . ? 
C45 C44 C43 120.0(5) . . ? 
C44 C45 C46 119.8(4) . . ? 
C45 C46 C41 121.8(4) . . ? 
C48 C47 C52 117.0(4) . . ? 
C48 C47 C40 121.6(4) . . ? 
C52 C47 C40 121.3(4) . . ? 
C49 C48 C47 121.8(4) . . ? 
C50 C49 C48 119.3(4) . . ? 
C51 C50 C49 119.7(5) . . ? 
C50 C51 C52 121.4(5) . . ? 
C51 C52 C47 120.9(4) . . ? 
C5 N1 C4 124.6(4) . . ? 
C7 N2 C6 110.5(3) . . ? 
C8 N3 C9 122.8(3) . . ? 
C31 N4 C30 119.8(4) . . ? 
C33 N5 C32 108.8(3) . . ? 
C34 N6 C35 122.2(3) . . ? 
 
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 H2 O4  0.88 2.15 2.984(4) 157.8 2_564 
N3 H3 O2  0.88 2.20 3.060(4) 165.0 2_575 
N5 H5 O2  0.88 2.11 2.938(4) 157.5 2_565 
N6 H6 O4  0.88 2.12 2.982(4) 167.5 2_554 
 
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              23.26 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    0.667 
_refine_diff_density_min   -0.410 
_refine_diff_density_rms    0.056 
