 
data_01src496 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C54 H61 N4 O6' 
_chemical_formula_weight          862.07 
 
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    C2/c 
 
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' 
 '-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                    20.5733(4) 
_cell_length_b                    17.9742(3) 
_cell_length_c                    25.3788(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  101.582(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      9193.7(3) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     49691 
_cell_measurement_theta_min       1.00 
_cell_measurement_theta_max       27.48 
 
_exptl_crystal_description        'square plate' 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.05 
_exptl_crystal_size_mid           0.05 
_exptl_crystal_size_min           0.01 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.246 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3688 
_exptl_absorpt_coefficient_mu     0.081 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.9960 
_exptl_absorpt_correction_T_max   0.9992 
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       120(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             53571 
_diffrn_reflns_av_R_equivalents   0.2019 
_diffrn_reflns_av_sigmaI/netI     0.1536 
_diffrn_reflns_limit_h_min        -24 
_diffrn_reflns_limit_h_max        24 
_diffrn_reflns_limit_k_min        -21 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -30 
_diffrn_reflns_limit_l_max        30 
_diffrn_reflns_theta_min          3.04 
_diffrn_reflns_theta_max          25.03 
_reflns_number_total              8120 
_reflns_number_gt                 3337 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' 
_computing_cell_refinement        'DENZO & COLLECT'
_computing_data_reduction         'DENZO & COLLECT' 
_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)+(0.0777P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          8120 
_refine_ls_number_parameters      577 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.2027 
_refine_ls_R_factor_gt            0.0692 
_refine_ls_wR_factor_ref          0.1866 
_refine_ls_wR_factor_gt           0.1389 
_refine_ls_goodness_of_fit_ref    0.942 
_refine_ls_restrained_S_all       0.942 
_refine_ls_shift/su_max           0.027 
_refine_ls_shift/su_mean          0.005 
 
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 0.06627(16) 0.57708(17) 0.00444(13) 0.0297(9) Uani 1 1 d . . . 
H1 H 0.0233 0.5829 0.0020 0.036 Uiso 1 1 calc R . . 
N2 N 0.08704(16) 0.41945(18) 0.02397(13) 0.0278(9) Uani 1 1 d . . . 
O1 O -0.12986(12) 0.82563(13) 0.18907(10) 0.0274(7) Uani 1 1 d . . . 
O2 O 0.02467(12) 0.80627(14) 0.19165(10) 0.0279(7) Uani 1 1 d . . . 
O3 O 0.17004(14) 0.60734(15) 0.04527(11) 0.0375(8) Uani 1 1 d . . . 
C1 C -0.19470(18) 0.8505(2) 0.16257(17) 0.0325(11) Uani 1 1 d . . . 
H1A H -0.2288 0.8305 0.1812 0.039 Uiso 1 1 calc R . . 
H1B H -0.2046 0.8327 0.1249 0.039 Uiso 1 1 calc R . . 
C2 C -0.1954(2) 0.9341(2) 0.16389(17) 0.0353(12) Uani 1 1 d . . . 
H2A H -0.1634 0.9529 0.1426 0.042 Uiso 1 1 calc R . . 
H2B H -0.1799 0.9506 0.2015 0.042 Uiso 1 1 calc R . . 
C3 C -0.2621(2) 0.9688(2) 0.14242(18) 0.0498(14) Uani 1 1 d . . . 
H3A H -0.2583 1.0231 0.1449 0.075 Uiso 1 1 calc R . . 
H3B H -0.2940 0.9516 0.1637 0.075 Uiso 1 1 calc R . . 
H3C H -0.2774 0.9542 0.1047 0.075 Uiso 1 1 calc R . . 
C4 C 0.0168(2) 0.8827(2) 0.17316(18) 0.0395(12) Uani 1 1 d . . . 
H4A H -0.0096 0.9101 0.1954 0.047 Uiso 1 1 calc R . . 
H4B H -0.0082 0.8833 0.1355 0.047 Uiso 1 1 calc R . . 
C5 C 0.0816(2) 0.9220(2) 0.17583(18) 0.0427(13) Uani 1 1 d . . . 
H5A H 0.1099 0.8922 0.1565 0.051 Uiso 1 1 calc R . . 
H5B H 0.1048 0.9260 0.2139 0.051 Uiso 1 1 calc R . . 
C6 C 0.0724(2) 0.9992(2) 0.15131(19) 0.0558(15) Uani 1 1 d . . . 
H6A H 0.1158 1.0226 0.1534 0.084 Uiso 1 1 calc R . . 
H6B H 0.0456 1.0294 0.1711 0.084 Uiso 1 1 calc R . . 
H6C H 0.0497 0.9954 0.1136 0.084 Uiso 1 1 calc R . . 
C7 C -0.12503(17) 0.7482(2) 0.19144(16) 0.0209(10) Uani 1 1 d . . . 
C8 C -0.14034(18) 0.7109(2) 0.23584(16) 0.0224(10) Uani 1 1 d . . . 
C9 C -0.13781(19) 0.6337(2) 0.23613(17) 0.0309(11) Uani 1 1 d . . . 
H9 H -0.1498 0.6070 0.2650 0.037 Uiso 1 1 calc R . . 
C10 C -0.1179(2) 0.5949(2) 0.19466(17) 0.0329(12) Uani 1 1 d . . . 
H10 H -0.1162 0.5421 0.1953 0.040 Uiso 1 1 calc R . . 
C11 C -0.10057(19) 0.6335(2) 0.15253(16) 0.0281(11) Uani 1 1 d . . . 
H11 H -0.0869 0.6068 0.1244 0.034 Uiso 1 1 calc R . . 
C12 C -0.10272(18) 0.7107(2) 0.15044(16) 0.0209(10) Uani 1 1 d . . . 
C13 C -0.07692(18) 0.7508(2) 0.10629(15) 0.0248(10) Uani 1 1 d . . . 
H13A H -0.0832 0.8051 0.1095 0.030 Uiso 1 1 calc R . . 
H13B H -0.1021 0.7346 0.0707 0.030 Uiso 1 1 calc R . . 
C14 C -0.00392(19) 0.7337(2) 0.11078(15) 0.0254(11) Uani 1 1 d . . . 
C15 C 0.04367(19) 0.7586(2) 0.15503(16) 0.0236(10) Uani 1 1 d . . . 
C16 C 0.10926(19) 0.7325(2) 0.16501(15) 0.0216(10) Uani 1 1 d . . . 
C17 C 0.12799(19) 0.6856(2) 0.12718(16) 0.0258(11) Uani 1 1 d . . . 
H17A H 0.1460 0.6399 0.1465 0.031 Uiso 1 1 calc R . . 
H17B H 0.1654 0.7101 0.1149 0.031 Uiso 1 1 calc R . . 
C18 C 0.08302(18) 0.6628(2) 0.08091(15) 0.0227(10) Uani 1 1 d . . . 
C19 C 0.01796(19) 0.6867(2) 0.07408(15) 0.0236(10) Uani 1 1 d . . . 
H19 H -0.0130 0.6705 0.0433 0.028 Uiso 1 1 calc R . . 
C20 C 0.1099(2) 0.6137(2) 0.04245(16) 0.0269(11) Uani 1 1 d . . . 
C21 C 0.0911(2) 0.5280(2) -0.03232(15) 0.0303(11) Uani 1 1 d . . . 
H21A H 0.1247 0.5551 -0.0479 0.036 Uiso 1 1 calc R . . 
H21B H 0.0540 0.5149 -0.0622 0.036 Uiso 1 1 calc R . . 
C22 C 0.1218(2) 0.4572(2) -0.00671(16) 0.0274(11) Uani 1 1 d . . . 
C23 C 0.1814(2) 0.4307(2) -0.01710(16) 0.0308(11) Uani 1 1 d . . . 
H23 H 0.2052 0.4589 -0.0387 0.037 Uiso 1 1 calc R . . 
C24 C 0.2061(2) 0.3630(2) 0.00413(16) 0.0322(11) Uani 1 1 d . . . 
H24 H 0.2462 0.3435 -0.0033 0.039 Uiso 1 1 calc R . . 
C25 C 0.1709(2) 0.3247(2) 0.03643(17) 0.0327(12) Uani 1 1 d . . . 
H25 H 0.1867 0.2785 0.0522 0.039 Uiso 1 1 calc R . . 
C26 C 0.1124(2) 0.3545(2) 0.04539(16) 0.0315(11) Uani 1 1 d . . . 
H26 H 0.0888 0.3280 0.0679 0.038 Uiso 1 1 calc R . . 
C27 C -0.15712(19) 0.7516(2) 0.28307(15) 0.0255(10) Uani 1 1 d . . . 
H27A H -0.2028 0.7384 0.2866 0.031 Uiso 1 1 calc R . . 
H27B H -0.1558 0.8058 0.2767 0.031 Uiso 1 1 calc R . . 
N3 N 0.42954(16) 0.42058(17) -0.00521(12) 0.0277(9) Uani 1 1 d . . . 
H3 H 0.4722 0.4132 -0.0032 0.033 Uiso 1 1 calc R . . 
N4 N 0.41613(16) 0.58151(19) -0.01851(13) 0.0293(9) Uani 1 1 d . . . 
O4 O 0.46669(12) 0.19962(14) -0.19714(10) 0.0257(7) Uani 1 1 d . . . 
O5 O 0.36034(12) 0.18046(13) -0.31472(10) 0.0252(7) Uani 1 1 d . . . 
O6 O 0.32499(14) 0.39686(16) -0.04681(12) 0.0426(9) Uani 1 1 d . . . 
C28 C 0.4424(2) 0.1243(2) -0.20017(17) 0.0337(11) Uani 1 1 d . . . 
H28A H 0.4421 0.1044 -0.2366 0.040 Uiso 1 1 calc R . . 
H28B H 0.3960 0.1243 -0.1947 0.040 Uiso 1 1 calc R . . 
C29 C 0.48285(19) 0.0747(2) -0.15971(16) 0.0331(11) Uani 1 1 d . . . 
H29A H 0.4833 0.0943 -0.1232 0.040 Uiso 1 1 calc R . . 
H29B H 0.5291 0.0738 -0.1653 0.040 Uiso 1 1 calc R . . 
C30 C 0.4547(2) -0.0046(2) -0.16432(18) 0.0480(14) Uani 1 1 d . . . 
H30A H 0.4823 -0.0365 -0.1375 0.072 Uiso 1 1 calc R . . 
H30B H 0.4546 -0.0241 -0.2004 0.072 Uiso 1 1 calc R . . 
H30C H 0.4092 -0.0039 -0.1580 0.072 Uiso 1 1 calc R . . 
C31 C 0.30087(18) 0.1656(2) -0.35460(16) 0.0315(11) Uani 1 1 d . . . 
H31A H 0.3075 0.1805 -0.3907 0.038 Uiso 1 1 calc R . . 
H31B H 0.2632 0.1944 -0.3463 0.038 Uiso 1 1 calc R . . 
C32 C 0.2863(2) 0.0830(2) -0.35375(17) 0.0378(12) Uani 1 1 d . . . 
H32A H 0.2484 0.0713 -0.3834 0.045 Uiso 1 1 calc R . . 
H32B H 0.3253 0.0550 -0.3604 0.045 Uiso 1 1 calc R . . 
C33 C 0.2701(2) 0.0569(2) -0.30139(18) 0.0435(13) Uani 1 1 d . . . 
H33A H 0.2613 0.0033 -0.3033 0.065 Uiso 1 1 calc R . . 
H33B H 0.2307 0.0833 -0.2950 0.065 Uiso 1 1 calc R . . 
H33C H 0.3077 0.0673 -0.2719 0.065 Uiso 1 1 calc R . . 
C34 C 0.37403(18) 0.2564(2) -0.31011(17) 0.0232(11) Uani 1 1 d . . . 
C35 C 0.40665(19) 0.2904(2) -0.34724(16) 0.0255(11) Uani 1 1 d . . . 
C36 C 0.41909(19) 0.3661(2) -0.34195(17) 0.0317(11) Uani 1 1 d . . . 
H36 H 0.4404 0.3903 -0.3672 0.038 Uiso 1 1 calc R . . 
C37 C 0.4014(2) 0.4074(2) -0.30100(18) 0.0380(12) Uani 1 1 d . . . 
H37 H 0.4095 0.4595 -0.2985 0.046 Uiso 1 1 calc R . . 
C38 C 0.37162(19) 0.3713(2) -0.26366(17) 0.0306(11) Uani 1 1 d . . . 
H38 H 0.3601 0.3991 -0.2351 0.037 Uiso 1 1 calc R . . 
C39 C 0.35836(18) 0.2957(2) -0.26709(15) 0.0223(10) Uani 1 1 d . . . 
C40 C 0.33322(19) 0.2584(2) -0.22136(15) 0.0278(11) Uani 1 1 d . . . 
H40A H 0.2892 0.2790 -0.2192 0.033 Uiso 1 1 calc R . . 
H40B H 0.3279 0.2044 -0.2286 0.033 Uiso 1 1 calc R . . 
C41 C 0.38080(19) 0.2704(2) -0.16805(15) 0.0222(10) Uani 1 1 d . . . 
C42 C 0.4464(2) 0.2440(2) -0.15916(15) 0.0242(10) Uani 1 1 d . . . 
C43 C 0.49387(18) 0.2658(2) -0.11414(15) 0.0207(10) Uani 1 1 d . . . 
C44 C 0.47345(19) 0.3117(2) -0.07661(16) 0.0264(11) Uani 1 1 d . . . 
H44 H 0.5048 0.3266 -0.0456 0.032 Uiso 1 1 calc R . . 
C45 C 0.40864(19) 0.3366(2) -0.08307(16) 0.0261(10) Uani 1 1 d . . . 
C46 C 0.36309(19) 0.3159(2) -0.12870(15) 0.0247(10) Uani 1 1 d . . . 
H46 H 0.3187 0.3332 -0.1333 0.030 Uiso 1 1 calc R . . 
C47 C 0.3844(2) 0.3864(2) -0.04401(16) 0.0278(11) Uani 1 1 d . . . 
C48 C 0.4069(2) 0.4695(2) 0.03302(15) 0.0318(11) Uani 1 1 d . . . 
H48A H 0.4447 0.4795 0.0631 0.038 Uiso 1 1 calc R . . 
H48B H 0.3724 0.4432 0.0480 0.038 Uiso 1 1 calc R . . 
C49 C 0.3788(2) 0.5433(2) 0.00988(15) 0.0256(11) Uani 1 1 d . . . 
C50 C 0.3196(2) 0.5704(2) 0.01934(16) 0.0319(11) Uani 1 1 d . . . 
H50 H 0.2942 0.5419 0.0395 0.038 Uiso 1 1 calc R . . 
C51 C 0.2973(2) 0.6392(2) -0.00071(17) 0.0343(12) Uani 1 1 d . . . 
H51 H 0.2572 0.6593 0.0063 0.041 Uiso 1 1 calc R . . 
C52 C 0.3344(2) 0.6784(2) -0.03103(16) 0.0287(11) Uani 1 1 d . . . 
H52 H 0.3200 0.7255 -0.0460 0.034 Uiso 1 1 calc R . . 
C53 C 0.3924(2) 0.6476(2) -0.03895(16) 0.0283(11) Uani 1 1 d . . . 
H53 H 0.4175 0.6744 -0.0602 0.034 Uiso 1 1 calc R . . 
C54 C 0.56631(18) 0.2461(2) -0.11088(15) 0.0271(11) Uani 1 1 d . . . 
H54A H 0.5706 0.1922 -0.1174 0.033 Uiso 1 1 calc R . . 
H54B H 0.5921 0.2577 -0.0745 0.033 Uiso 1 1 calc R . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
N1 C20 1.350(5) . ? 
N1 C21 1.449(5) . ? 
N2 C22 1.343(5) . ? 
N2 C26 1.348(5) . ? 
O1 C7 1.395(4) . ? 
O1 C1 1.439(4) . ? 
O2 C15 1.378(4) . ? 
O2 C4 1.451(5) . ? 
O3 C20 1.230(4) . ? 
C1 C2 1.503(5) . ? 
C2 C3 1.506(5) . ? 
C4 C5 1.497(5) . ? 
C5 C6 1.517(6) . ? 
C7 C8 1.401(5) . ? 
C7 C12 1.393(5) . ? 
C8 C9 1.388(5) . ? 
C8 C27 1.502(5) . ? 
C9 C10 1.391(5) . ? 
C10 C11 1.381(5) . ? 
C11 C12 1.388(5) . ? 
C12 C13 1.516(5) . ? 
C13 C14 1.515(5) . ? 
C14 C19 1.398(5) . ? 
C14 C15 1.406(5) . ? 
C15 C16 1.403(5) . ? 
C16 C17 1.389(5) . ? 
C16 C27 1.517(5) 2 ? 
C17 C18 1.402(5) . ? 
C18 C19 1.383(5) . ? 
C18 C20 1.502(5) . ? 
C21 C22 1.510(5) . ? 
C22 C23 1.389(5) . ? 
C23 C24 1.385(5) . ? 
C24 C25 1.383(5) . ? 
C25 C26 1.376(6) . ? 
C27 C16 1.517(5) 2 ? 
N3 C47 1.357(4) . ? 
N3 C48 1.453(5) . ? 
N4 C49 1.342(5) . ? 
N4 C53 1.348(5) . ? 
O4 C42 1.378(4) . ? 
O4 C28 1.440(4) . ? 
O5 C34 1.393(4) . ? 
O5 C31 1.448(4) . ? 
O6 C47 1.225(4) . ? 
C28 C29 1.483(5) . ? 
C29 C30 1.535(5) . ? 
C31 C32 1.517(5) . ? 
C32 C33 1.508(6) . ? 
C34 C39 1.392(5) . ? 
C34 C35 1.403(5) . ? 
C35 C36 1.386(5) . ? 
C35 C54 1.520(5) 2_654 ? 
C36 C37 1.384(6) . ? 
C37 C38 1.389(6) . ? 
C38 C39 1.385(5) . ? 
C39 C40 1.518(5) . ? 
C40 C41 1.518(5) . ? 
C41 C46 1.395(5) . ? 
C41 C42 1.406(5) . ? 
C42 C43 1.401(5) . ? 
C43 C44 1.389(5) . ? 
C43 C54 1.517(5) . ? 
C44 C45 1.384(5) . ? 
C45 C46 1.386(5) . ? 
C45 C47 1.494(5) . ? 
C48 C49 1.518(5) . ? 
C49 C50 1.377(5) . ? 
C50 C51 1.381(5) . ? 
C51 C52 1.380(5) . ? 
C52 C53 1.366(5) . ? 
C54 C35 1.520(5) 2_654 ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C20 N1 C21 119.1(3) . . ? 
C22 N2 C26 117.5(4) . . ? 
C7 O1 C1 112.4(3) . . ? 
C15 O2 C4 113.5(3) . . ? 
O1 C1 C2 108.2(3) . . ? 
C1 C2 C3 114.7(3) . . ? 
O2 C4 C5 113.1(3) . . ? 
C4 C5 C6 112.1(4) . . ? 
O1 C7 C8 119.1(4) . . ? 
O1 C7 C12 118.8(4) . . ? 
C8 C7 C12 122.0(4) . . ? 
C9 C8 C7 118.0(4) . . ? 
C9 C8 C27 119.8(4) . . ? 
C7 C8 C27 122.2(4) . . ? 
C8 C9 C10 120.9(4) . . ? 
C11 C10 C9 119.6(4) . . ? 
C10 C11 C12 121.4(4) . . ? 
C11 C12 C7 117.9(4) . . ? 
C11 C12 C13 119.4(4) . . ? 
C7 C12 C13 122.6(4) . . ? 
C12 C13 C14 109.7(3) . . ? 
C19 C14 C15 117.3(4) . . ? 
C19 C14 C13 121.3(3) . . ? 
C15 C14 C13 121.1(4) . . ? 
O2 C15 C16 118.6(3) . . ? 
O2 C15 C14 119.4(4) . . ? 
C16 C15 C14 121.9(4) . . ? 
C17 C16 C15 117.9(4) . . ? 
C17 C16 C27 121.0(4) . 2 ? 
C15 C16 C27 120.9(4) . 2 ? 
C16 C17 C18 121.9(4) . . ? 
C19 C18 C17 118.3(4) . . ? 
C19 C18 C20 125.0(3) . . ? 
C17 C18 C20 116.7(4) . . ? 
C18 C19 C14 122.5(4) . . ? 
O3 C20 N1 120.9(4) . . ? 
O3 C20 C18 121.0(4) . . ? 
N1 C20 C18 118.2(4) . . ? 
N1 C21 C22 114.0(3) . . ? 
N2 C22 C23 122.1(4) . . ? 
N2 C22 C21 116.7(4) . . ? 
C23 C22 C21 121.1(4) . . ? 
C24 C23 C22 119.7(4) . . ? 
C25 C24 C23 118.2(4) . . ? 
C26 C25 C24 118.9(4) . . ? 
N2 C26 C25 123.5(4) . . ? 
C8 C27 C16 111.7(3) . 2 ? 
C47 N3 C48 119.6(3) . . ? 
C49 N4 C53 117.1(4) . . ? 
C42 O4 C28 115.5(3) . . ? 
C34 O5 C31 111.6(3) . . ? 
O4 C28 C29 112.8(3) . . ? 
C28 C29 C30 110.8(3) . . ? 
O5 C31 C32 108.2(3) . . ? 
C33 C32 C31 113.3(4) . . ? 
O5 C34 C39 119.3(4) . . ? 
O5 C34 C35 119.1(4) . . ? 
C39 C34 C35 121.5(4) . . ? 
C36 C35 C34 117.9(4) . . ? 
C36 C35 C54 119.7(4) . 2_654 ? 
C34 C35 C54 122.2(4) . 2_654 ? 
C35 C36 C37 121.9(4) . . ? 
C36 C37 C38 118.7(4) . . ? 
C39 C38 C37 121.6(4) . . ? 
C38 C39 C34 118.3(4) . . ? 
C38 C39 C40 118.6(4) . . ? 
C34 C39 C40 122.9(4) . . ? 
C41 C40 C39 111.2(3) . . ? 
C46 C41 C42 117.6(3) . . ? 
C46 C41 C40 120.5(3) . . ? 
C42 C41 C40 121.5(4) . . ? 
O4 C42 C41 119.9(3) . . ? 
O4 C42 C43 118.2(4) . . ? 
C41 C42 C43 121.7(4) . . ? 
C44 C43 C42 117.9(4) . . ? 
C44 C43 C54 122.0(3) . . ? 
C42 C43 C54 119.7(4) . . ? 
C43 C44 C45 121.8(4) . . ? 
C46 C45 C44 119.1(4) . . ? 
C46 C45 C47 117.1(4) . . ? 
C44 C45 C47 123.8(4) . . ? 
C45 C46 C41 121.7(4) . . ? 
O6 C47 N3 120.2(4) . . ? 
O6 C47 C45 121.0(4) . . ? 
N3 C47 C45 118.8(4) . . ? 
N3 C48 C49 114.7(3) . . ? 
N4 C49 C50 122.3(4) . . ? 
N4 C49 C48 116.1(4) . . ? 
C50 C49 C48 121.6(4) . . ? 
C49 C50 C51 119.5(4) . . ? 
C52 C51 C50 118.9(4) . . ? 
C53 C52 C51 118.1(4) . . ? 
N4 C53 C52 124.1(4) . . ? 
C43 C54 C35 109.5(3) . 2_654 ? 
 
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 
N1 H1 N2  0.88 2.23 3.092(4) 164.9 5_565 
N3 H3 N4  0.88 2.25 3.111(4) 164.6 5_665 
 
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              25.03 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    0.406 
_refine_diff_density_min   -0.468 
_refine_diff_density_rms    0.057 
