Supplementary Material (ESI) for Organic and Biomolecular Chemistry This journal is (C) The Royal Society of Chemistry 2006 Compound 7k data_f31114a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H30 I2 N2 O2' _chemical_formula_weight 584.26 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' 'I' 'I' -0.4742 1.8119 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 26.338(13) _cell_length_b 9.477(5) _cell_length_c 32.834(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.759(6) _cell_angle_gamma 90.00 _cell_volume 8121(7) _cell_formula_units_Z 14 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4004 _exptl_absorpt_coefficient_mu 2.726 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5489 _exptl_absorpt_correction_T_max 0.7722 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17376 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 26.01 _reflns_number_total 12349 _reflns_number_gt 7989 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of 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^)+(0.0699P)^2^+13.4691P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(4) _refine_ls_number_reflns 12349 _refine_ls_number_parameters 847 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1598 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.004 _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 I1 I 0.69604(4) 0.29659(11) 0.12448(3) 0.0483(3) Uani 1 1 d . . . I2 I 0.42161(6) 0.82179(17) 0.27646(4) 0.0890(5) Uani 1 1 d . . . I3 I 0.12871(5) 0.78529(19) 0.41381(4) 0.0894(5) Uani 1 1 d . . . I4 I 0.0000 0.2773(2) 0.0000 0.0713(5) Uani 1 2 d S . . I5 I 0.66144(5) 0.77385(13) 0.44676(3) 0.0646(4) Uani 1 1 d . . . I6 I 0.23466(4) 0.31380(11) 0.16211(3) 0.0496(3) Uani 1 1 d . . . I7 I 0.43315(5) 0.3292(2) 0.29084(4) 0.0958(6) Uani 1 1 d . . . I8 I 0.5000 0.26021(17) 0.0000 0.0479(4) Uani 1 2 d S . . N1 N 0.1682(5) 0.4928(17) 0.0222(4) 0.044(4) Uani 1 1 d . . . N2 N 0.5588(5) 0.5664(15) 0.1263(3) 0.040(3) Uani 1 1 d . . . O1 O 0.2485(5) 0.492(2) -0.0555(3) 0.074(5) Uani 1 1 d . . . H1 H 0.2632 0.4462 -0.0717 0.112 Uiso 1 1 calc R . . O2 O 0.4791(4) 0.6246(18) 0.2031(3) 0.072(4) Uani 1 1 d . . . H2 H 0.4628 0.6423 0.2221 0.108 Uiso 1 1 calc R . . C1 C 0.2046(7) 0.601(2) 0.0129(6) 0.062(5) Uani 1 1 d . . . H1A H 0.2041 0.6785 0.0323 0.074 Uiso 1 1 calc R . . H1B H 0.1938 0.6382 -0.0144 0.074 Uiso 1 1 calc R . . C2 C 0.2598(6) 0.544(3) 0.0152(5) 0.069(6) Uani 1 1 d . . . C3 C 0.2797(5) 0.512(2) -0.0216(5) 0.042(4) Uani 1 1 d . . . C4 C 0.3349(6) 0.477(2) -0.0135(5) 0.062(6) Uani 1 1 d . . . H4 H 0.3504 0.4440 -0.0355 0.074 Uiso 1 1 calc R . . C5 C 0.3634(6) 0.4896(18) 0.0218(4) 0.042(4) Uani 1 1 d . . . H5 H 0.3977 0.4634 0.0237 0.050 Uiso 1 1 calc R . . C6 C 0.3445(6) 0.5421(17) 0.0582(4) 0.034(3) Uani 1 1 d . . . C7 C 0.2937(5) 0.5711(13) 0.0520(3) 0.025(3) Uani 1 1 d . . . H7 H 0.2798 0.6120 0.0738 0.030 Uiso 1 1 calc R . . C8 C 0.3815(6) 0.5613(16) 0.0960(4) 0.043(4) Uani 1 1 d . . . C9 C 0.4299(6) 0.6045(14) 0.0939(4) 0.040(3) Uani 1 1 d . . . H9 H 0.4407 0.6321 0.0693 0.048 Uiso 1 1 calc R . . C10 C 0.4630(6) 0.605(2) 0.1312(4) 0.066(6) Uani 1 1 d . . . C11 C 0.4444(7) 0.587(2) 0.1673(4) 0.060(5) Uani 1 1 d . . . C12 C 0.3951(7) 0.561(2) 0.1712(4) 0.053(5) Uani 1 1 d . . . H12 H 0.3838 0.5549 0.1968 0.064 Uiso 1 1 calc R . . C13 C 0.3616(6) 0.5440(18) 0.1348(4) 0.042(4) Uani 1 1 d . . . H13 H 0.3273 0.5219 0.1354 0.050 Uiso 1 1 calc R . . C14 C 0.5179(6) 0.6740(19) 0.1287(5) 0.054(4) Uani 1 1 d . . . H14A H 0.5156 0.7343 0.1047 0.065 Uiso 1 1 calc R . . H14B H 0.5273 0.7325 0.1528 0.065 Uiso 1 1 calc R . . C15 C 0.1785(9) 0.423(3) 0.0569(8) 0.174(15) Uani 1 1 d . . . H15A H 0.1832 0.4891 0.0794 0.260 Uiso 1 1 calc R . . H15B H 0.2092 0.3691 0.0566 0.260 Uiso 1 1 calc R . . H15C H 0.1505 0.3614 0.0602 0.260 Uiso 1 1 calc R . . C16 C 0.1167(7) 0.559(2) 0.0169(6) 0.075(6) Uani 1 1 d . . . H16A H 0.1091 0.5949 -0.0105 0.113 Uiso 1 1 calc R . . H16B H 0.1162 0.6345 0.0363 0.113 Uiso 1 1 calc R . . H16C H 0.0916 0.4894 0.0216 0.113 Uiso 1 1 calc R . . C17 C 0.1604(8) 0.3790(18) -0.0146(4) 0.064(5) Uani 1 1 d . . . H17A H 0.1368 0.3075 -0.0084 0.096 Uiso 1 1 calc R . . H17B H 0.1927 0.3363 -0.0176 0.096 Uiso 1 1 calc R . . H17C H 0.1470 0.4253 -0.0398 0.096 Uiso 1 1 calc R . . C18 C 0.5466(9) 0.468(2) 0.0895(5) 0.081(6) Uani 1 1 d . . . H18A H 0.5196 0.4046 0.0943 0.122 Uiso 1 1 calc R . . H18B H 0.5766 0.4146 0.0858 0.122 Uiso 1 1 calc R . . H18C H 0.5360 0.5226 0.0652 0.122 Uiso 1 1 calc R . . C19 C 0.5669(7) 0.472(2) 0.1631(5) 0.071(6) Uani 1 1 d . . . H19A H 0.5808 0.5256 0.1868 0.107 Uiso 1 1 calc R . . H19B H 0.5903 0.3980 0.1584 0.107 Uiso 1 1 calc R . . H19C H 0.5347 0.4313 0.1676 0.107 Uiso 1 1 calc R . . C20 C 0.6060(7) 0.630(3) 0.1232(6) 0.099(8) Uani 1 1 d . . . H20A H 0.6029 0.6889 0.0991 0.149 Uiso 1 1 calc R . . H20B H 0.6313 0.5589 0.1212 0.149 Uiso 1 1 calc R . . H20C H 0.6161 0.6871 0.1472 0.149 Uiso 1 1 calc R . . N3 N 0.7649(5) 0.1040(17) 0.2689(3) 0.039(3) Uani 1 1 d . . . N4 N 0.3726(5) 0.0586(16) 0.1551(4) 0.052(4) Uani 1 1 d . . . O3 O 0.6782(4) 0.0810(15) 0.3419(2) 0.048(3) Uani 1 1 d . . . H3 H 0.6612 0.1042 0.3599 0.072 Uiso 1 1 calc R . . O4 O 0.4526(6) 0.025(2) 0.0779(3) 0.101(6) Uani 1 1 d . . . H4A H 0.4540 -0.0532 0.0672 0.151 Uiso 1 1 calc R . . C21 C 0.7216(5) -0.0074(16) 0.2734(4) 0.030(3) Uani 1 1 d . . . H21A H 0.7235 -0.0810 0.2532 0.036 Uiso 1 1 calc R . . H21B H 0.7290 -0.0506 0.3004 0.036 Uiso 1 1 calc R . . C22 C 0.6694(6) 0.0452(15) 0.2688(4) 0.036(4) Uani 1 1 d . . . C23 C 0.6473(7) 0.0895(19) 0.3029(4) 0.045(4) Uani 1 1 d . . . C24 C 0.5971(6) 0.1265(18) 0.3025(4) 0.036(4) Uani 1 1 d . . . H24 H 0.5844 0.1536 0.3265 0.044 Uiso 1 1 calc R . . C25 C 0.5646(7) 0.1218(19) 0.2633(4) 0.049(4) Uani 1 1 d . . . H25 H 0.5301 0.1459 0.2612 0.059 Uiso 1 1 calc R . . C26 C 0.5847(5) 0.0831(15) 0.2311(4) 0.030(3) Uani 1 1 d . . . C27 C 0.6378(6) 0.0478(17) 0.2330(5) 0.051(4) Uani 1 1 d . . . H27 H 0.6509 0.0261 0.2088 0.061 Uiso 1 1 calc R . . C28 C 0.5531(5) 0.0663(14) 0.1892(4) 0.027(3) Uani 1 1 d . . . C29 C 0.4996(5) 0.0228(16) 0.1867(3) 0.028(3) Uani 1 1 d . . . H29 H 0.4869 0.0077 0.2114 0.034 Uiso 1 1 calc R . . C30 C 0.4653(5) 0.0013(17) 0.1501(4) 0.037(4) Uani 1 1 d . . . C31 C 0.4837(6) 0.027(2) 0.1134(4) 0.062(6) Uani 1 1 d . . . C32 C 0.5359(7) 0.074(2) 0.1162(5) 0.062(6) Uani 1 1 d . . . H32 H 0.5481 0.0944 0.0916 0.075 Uiso 1 1 calc R . . C33 C 0.5683(8) 0.092(2) 0.1499(6) 0.059(5) Uani 1 1 d . . . H33 H 0.6016 0.1213 0.1481 0.071 Uiso 1 1 calc R . . C34 C 0.4154(6) -0.0516(18) 0.1529(5) 0.047(4) Uani 1 1 d . . . H34A H 0.4173 -0.1108 0.1772 0.056 Uiso 1 1 calc R . . H34B H 0.4053 -0.1117 0.1293 0.056 Uiso 1 1 calc R . . C35 C 0.7719(7) 0.195(2) 0.3036(5) 0.076(6) Uani 1 1 d . . . H35A H 0.8067 0.2272 0.3080 0.113 Uiso 1 1 calc R . . H35B H 0.7645 0.1439 0.3274 0.113 Uiso 1 1 calc R . . H35C H 0.7492 0.2739 0.2989 0.113 Uiso 1 1 calc R . . C36 C 0.8126(6) 0.008(2) 0.2675(5) 0.068(5) Uani 1 1 d . . . H36A H 0.8092 -0.0420 0.2419 0.102 Uiso 1 1 calc R . . H36B H 0.8150 -0.0582 0.2898 0.102 Uiso 1 1 calc R . . H36C H 0.8429 0.0653 0.2701 0.102 Uiso 1 1 calc R . . C37 C 0.7515(6) 0.1777(16) 0.2265(3) 0.043(3) Uani 1 1 d . . . H37A H 0.7439 0.1076 0.2055 0.064 Uiso 1 1 calc R . . H37B H 0.7800 0.2337 0.2208 0.064 Uiso 1 1 calc R . . H37C H 0.7221 0.2373 0.2271 0.064 Uiso 1 1 calc R . . C38 C 0.3853(6) 0.1418(19) 0.1943(4) 0.053(4) Uani 1 1 d . . . H38A H 0.3617 0.2189 0.1945 0.080 Uiso 1 1 calc R . . H38B H 0.4195 0.1780 0.1960 0.080 Uiso 1 1 calc R . . H38C H 0.3827 0.0816 0.2174 0.080 Uiso 1 1 calc R . . C39 C 0.3233(7) -0.034(2) 0.1575(7) 0.088(7) Uani 1 1 d . . . H39A H 0.3251 -0.0756 0.1844 0.132 Uiso 1 1 calc R . . H39B H 0.3215 -0.1080 0.1373 0.132 Uiso 1 1 calc R . . H39C H 0.2933 0.0238 0.1524 0.132 Uiso 1 1 calc R . . C40 C 0.3622(8) 0.153(2) 0.1179(5) 0.072(6) Uani 1 1 d . . . H40A H 0.3548 0.0960 0.0936 0.108 Uiso 1 1 calc R . . H40B H 0.3918 0.2101 0.1158 0.108 Uiso 1 1 calc R . . H40C H 0.3334 0.2126 0.1206 0.108 Uiso 1 1 calc R . . N5 N 0.9822(6) 0.4974(18) 0.4055(4) 0.056(4) Uani 1 1 d . . . N6 N 0.5913(5) 0.6040(18) 0.3030(3) 0.050(4) Uani 1 1 d . . . O5 O 0.9068(5) 0.450(2) 0.4877(4) 0.089(5) Uani 1 1 d . . . H5A H 0.8965 0.3822 0.4997 0.133 Uiso 1 1 calc R . . O6 O 0.6771(5) 0.605(2) 0.2303(3) 0.087(5) Uani 1 1 d . . . H6 H 0.6630 0.6822 0.2278 0.130 Uiso 1 1 calc R . . C41 C 0.9447(6) 0.3941(19) 0.4103(5) 0.068(4) Uani 1 1 d . . . H41A H 0.9560 0.3381 0.4345 0.081 Uiso 1 1 calc R . . H41B H 0.9412 0.3315 0.3867 0.081 Uiso 1 1 calc R . . C42 C 0.8926(5) 0.4588(14) 0.4144(4) 0.043(3) Uani 1 1 d . . . C43 C 0.8738(5) 0.4793(18) 0.4547(4) 0.045(4) Uani 1 1 d . . . C44 C 0.8228(8) 0.515(2) 0.4522(6) 0.075(7) Uani 1 1 d . . . H44 H 0.8090 0.5262 0.4767 0.090 Uiso 1 1 calc R . . C45 C 0.7891(7) 0.537(2) 0.4143(5) 0.071(6) Uani 1 1 d . . . H45 H 0.7541 0.5473 0.4153 0.085 Uiso 1 1 calc R . . C46 C 0.8052(5) 0.5427(19) 0.3799(4) 0.044(4) Uani 1 1 d . . . C47 C 0.8561(6) 0.527(3) 0.3811(4) 0.115(11) Uani 1 1 d . . . H47 H 0.8704 0.5630 0.3589 0.138 Uiso 1 1 calc R . . C48 C 0.7720(7) 0.573(2) 0.3405(4) 0.047(4) Uani 1 1 d . . . C49 C 0.7195(8) 0.570(3) 0.3401(5) 0.115(11) Uani 1 1 d . . . H49 H 0.7045 0.5825 0.3639 0.138 Uiso 1 1 calc R . . C50 C 0.6886(5) 0.5436(13) 0.3000(4) 0.039(3) Uani 1 1 d . . . C51 C 0.7108(8) 0.600(2) 0.2687(4) 0.067(6) Uani 1 1 d . . . C52 C 0.7592(7) 0.619(2) 0.2669(4) 0.057(5) Uani 1 1 d . . . H52 H 0.7710 0.6404 0.2422 0.068 Uiso 1 1 calc R . . C53 C 0.7922(8) 0.608(3) 0.3029(5) 0.082(7) Uani 1 1 d . . . H53 H 0.8272 0.6219 0.3031 0.099 Uiso 1 1 calc R . . C54 C 0.6325(5) 0.4931(16) 0.2973(4) 0.051(4) Uani 1 1 d . . . H54A H 0.6233 0.4491 0.2707 0.061 Uiso 1 1 calc R . . H54B H 0.6312 0.4205 0.3180 0.061 Uiso 1 1 calc R . . C55 C 1.0345(7) 0.426(2) 0.4035(7) 0.116(8) Uani 1 1 d . . . H55A H 1.0406 0.3567 0.4249 0.174 Uiso 1 1 calc R . . H55B H 1.0610 0.4962 0.4072 0.174 Uiso 1 1 calc R . . H55C H 1.0342 0.3816 0.3773 0.174 Uiso 1 1 calc R . . C56 C 0.9736(5) 0.6019(19) 0.3728(5) 0.079(5) Uani 1 1 d . . . H56A H 0.9411 0.6468 0.3735 0.119 Uiso 1 1 calc R . . H56B H 0.9738 0.5563 0.3467 0.119 Uiso 1 1 calc R . . H56C H 1.0003 0.6714 0.3766 0.119 Uiso 1 1 calc R . . C57 C 0.9941(9) 0.581(2) 0.4454(5) 0.116(10) Uani 1 1 d . . . H57A H 0.9647 0.6360 0.4498 0.173 Uiso 1 1 calc R . . H57B H 1.0225 0.6434 0.4434 0.173 Uiso 1 1 calc R . . H57C H 1.0027 0.5176 0.4680 0.173 Uiso 1 1 calc R . . C58 C 0.5899(6) 0.716(2) 0.2747(5) 0.082(5) Uani 1 1 d . . . H58A H 0.6219 0.7660 0.2787 0.122 Uiso 1 1 calc R . . H58B H 0.5626 0.7799 0.2788 0.122 Uiso 1 1 calc R . . H58C H 0.5841 0.6797 0.2472 0.122 Uiso 1 1 calc R . . C59 C 0.5450(6) 0.525(2) 0.3057(5) 0.091(6) Uani 1 1 d . . . H59A H 0.5172 0.5884 0.3078 0.136 Uiso 1 1 calc R . . H59B H 0.5499 0.4651 0.3296 0.136 Uiso 1 1 calc R . . H59C H 0.5372 0.4672 0.2816 0.136 Uiso 1 1 calc R . . C60 C 0.6103(7) 0.6761(19) 0.3463(3) 0.081(5) Uani 1 1 d . . . H60A H 0.6402 0.7323 0.3441 0.122 Uiso 1 1 calc R . . H60B H 0.6187 0.6043 0.3667 0.122 Uiso 1 1 calc R . . H60C H 0.5836 0.7351 0.3541 0.122 Uiso 1 1 calc R . . N7 N 0.1976(6) 0.0136(17) 0.5570(4) 0.048(3) Uani 1 1 d . . . O7 O 0.1130(5) 0.035(2) 0.6325(3) 0.092(5) Uani 1 1 d . . . H7A H 0.0975 0.0559 0.6517 0.138 Uiso 1 1 calc R . . C61 C 0.1563(6) 0.1196(19) 0.5615(5) 0.051(4) Uani 1 1 d . . . H61A H 0.1568 0.1894 0.5400 0.061 Uiso 1 1 calc R . . H61B H 0.1655 0.1680 0.5875 0.061 Uiso 1 1 calc R . . C62 C 0.0990(5) 0.0648(18) 0.5601(4) 0.034(4) Uani 1 1 d . . . C63 C 0.0788(5) 0.0233(18) 0.5970(4) 0.039(3) Uani 1 1 d . . . C64 C 0.0286(7) -0.008(2) 0.5936(5) 0.062(5) Uani 1 1 d . . . H64 H 0.0140 -0.0311 0.6170 0.074 Uiso 1 1 calc R . . C65 C -0.0009(6) -0.0078(19) 0.5567(5) 0.045(4) Uani 1 1 d . . . H65 H -0.0352 -0.0326 0.5554 0.054 Uiso 1 1 calc R . . C66 C 0.0188(7) 0.030(2) 0.5189(4) 0.057(5) Uani 1 1 d . . . C67 C 0.0671(6) 0.0649(16) 0.5204(4) 0.036(4) Uani 1 1 d . . . H67 H 0.0807 0.0891 0.4966 0.043 Uiso 1 1 calc R . . C68 C 0.2019(8) -0.091(2) 0.5922(4) 0.068(6) Uani 1 1 d . . . H68A H 0.1683 -0.1218 0.5965 0.102 Uiso 1 1 calc R . . H68B H 0.2186 -0.0474 0.6167 0.102 Uiso 1 1 calc R . . H68C H 0.2216 -0.1714 0.5855 0.102 Uiso 1 1 calc R . . C69 C 0.2448(6) 0.093(2) 0.5568(5) 0.056(4) Uani 1 1 d . . . H69A H 0.2723 0.0297 0.5537 0.084 Uiso 1 1 calc R . . H69B H 0.2524 0.1438 0.5823 0.084 Uiso 1 1 calc R . . H69C H 0.2407 0.1590 0.5344 0.084 Uiso 1 1 calc R . . C70 C 0.1864(7) -0.074(2) 0.5213(4) 0.061(5) Uani 1 1 d . . . H70A H 0.2135 -0.1412 0.5206 0.091 Uiso 1 1 calc R . . H70B H 0.1836 -0.0160 0.4971 0.091 Uiso 1 1 calc R . . H70C H 0.1547 -0.1225 0.5223 0.091 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 I1 0.0438(5) 0.0606(7) 0.0411(4) 0.0036(5) 0.0079(4) 0.0010(5) I2 0.1230(12) 0.0641(9) 0.0940(8) -0.0038(7) 0.0660(8) -0.0048(8) I3 0.0602(7) 0.1204(13) 0.0914(7) -0.0529(9) 0.0240(6) -0.0030(8) I4 0.0686(10) 0.0630(12) 0.0868(10) 0.000 0.0267(8) 0.000 I5 0.0630(7) 0.0763(10) 0.0588(5) -0.0051(6) 0.0231(5) -0.0046(7) I6 0.0422(5) 0.0615(8) 0.0452(4) 0.0055(5) 0.0067(4) 0.0021(6) I7 0.0675(9) 0.1210(16) 0.1014(9) -0.0488(9) 0.0204(7) 0.0033(8) I8 0.0526(8) 0.0455(8) 0.0432(5) 0.000 -0.0027(5) 0.000 N1 0.023(6) 0.058(9) 0.052(7) -0.015(7) 0.003(5) 0.013(6) N2 0.034(7) 0.051(7) 0.033(6) -0.007(5) -0.008(5) -0.007(5) O1 0.041(7) 0.121(13) 0.060(6) -0.029(8) 0.000(5) -0.002(8) O2 0.037(6) 0.141(11) 0.039(5) -0.030(6) 0.008(4) 0.015(7) C1 0.043(10) 0.060(11) 0.089(12) 0.009(10) 0.026(9) 0.031(9) C2 0.028(9) 0.139(19) 0.041(8) -0.013(10) 0.001(6) 0.004(10) C3 0.009(6) 0.062(9) 0.060(8) -0.014(8) 0.020(5) 0.001(7) C4 0.021(8) 0.101(16) 0.068(10) -0.020(10) 0.024(7) 0.001(9) C5 0.023(7) 0.050(9) 0.053(7) -0.015(7) 0.007(6) -0.010(7) C6 0.026(7) 0.024(7) 0.055(7) -0.014(5) 0.017(6) 0.000(5) C7 0.028(7) 0.019(5) 0.030(6) -0.013(4) 0.009(5) -0.013(4) C8 0.041(9) 0.043(8) 0.048(7) -0.014(6) 0.012(6) -0.026(7) C9 0.047(9) 0.023(6) 0.049(7) 0.004(5) 0.002(6) -0.004(6) C10 0.036(10) 0.138(17) 0.025(6) -0.016(8) 0.012(6) 0.000(10) C11 0.061(12) 0.088(13) 0.032(7) -0.020(7) 0.015(7) 0.017(10) C12 0.050(10) 0.092(13) 0.019(6) -0.009(6) 0.006(6) -0.007(9) C13 0.024(7) 0.069(11) 0.029(6) 0.011(6) -0.012(5) 0.004(6) C14 0.032(8) 0.063(10) 0.071(9) -0.031(8) 0.015(7) -0.012(7) C15 0.053(13) 0.24(3) 0.22(3) 0.13(3) 0.005(15) -0.053(18) C16 0.032(9) 0.082(13) 0.109(13) -0.029(11) -0.001(9) 0.003(9) C17 0.098(14) 0.048(9) 0.044(7) -0.016(7) -0.002(8) -0.013(10) C18 0.120(18) 0.072(12) 0.053(9) -0.024(8) 0.014(10) -0.014(12) C19 0.052(10) 0.099(14) 0.061(9) 0.004(9) 0.006(8) 0.042(9) C20 0.051(12) 0.123(19) 0.126(15) -0.066(14) 0.021(11) -0.017(12) N3 0.029(6) 0.072(9) 0.014(4) -0.004(5) -0.007(4) -0.011(6) N4 0.026(7) 0.077(10) 0.051(7) -0.022(6) -0.005(5) 0.030(6) O3 0.034(6) 0.087(8) 0.024(4) -0.012(4) 0.006(4) 0.016(6) O4 0.069(9) 0.202(18) 0.029(5) -0.002(8) -0.005(5) 0.028(11) C21 0.015(6) 0.047(8) 0.027(6) -0.019(6) 0.002(5) -0.018(6) C22 0.050(9) 0.023(7) 0.038(7) -0.011(5) 0.015(7) -0.004(6) C23 0.054(10) 0.052(9) 0.028(6) -0.007(6) 0.002(6) -0.021(8) C24 0.036(8) 0.047(9) 0.026(6) -0.009(6) 0.002(6) 0.001(7) C25 0.037(8) 0.057(10) 0.050(8) -0.006(7) -0.005(7) 0.012(8) C26 0.022(6) 0.026(7) 0.041(6) -0.003(5) -0.002(5) -0.005(5) C27 0.024(8) 0.045(9) 0.089(11) 0.002(8) 0.030(7) 0.000(6) C28 0.009(5) 0.029(6) 0.042(6) 0.011(5) 0.000(5) 0.003(5) C29 0.018(6) 0.045(8) 0.023(5) -0.010(5) 0.010(4) 0.003(6) C30 0.025(7) 0.037(8) 0.047(7) -0.006(6) 0.002(6) 0.008(6) C31 0.021(7) 0.130(17) 0.032(7) -0.006(9) -0.008(5) 0.008(10) C32 0.047(11) 0.101(15) 0.044(8) 0.015(8) 0.021(8) 0.026(10) C33 0.055(11) 0.056(10) 0.076(11) 0.022(9) 0.040(9) 0.000(8) C34 0.035(8) 0.056(9) 0.047(7) -0.009(6) -0.004(6) 0.027(7) C35 0.038(9) 0.068(12) 0.127(14) -0.032(11) 0.036(9) -0.021(9) C36 0.023(8) 0.100(15) 0.083(10) -0.024(11) 0.014(7) 0.003(10) C37 0.058(8) 0.055(8) 0.012(4) 0.012(5) -0.005(5) -0.011(7) C38 0.031(8) 0.061(10) 0.068(9) -0.008(8) 0.009(7) 0.019(7) C39 0.026(8) 0.063(12) 0.18(2) 0.002(12) 0.029(10) 0.007(8) C40 0.076(13) 0.082(13) 0.057(9) -0.013(9) 0.006(9) -0.012(10) N5 0.045(8) 0.071(10) 0.054(7) 0.005(7) 0.013(6) -0.003(7) N6 0.052(8) 0.074(10) 0.019(5) 0.000(5) -0.014(5) 0.030(8) O5 0.054(8) 0.137(13) 0.073(7) 0.055(8) -0.005(6) -0.019(8) O6 0.047(7) 0.183(16) 0.024(4) 0.016(7) -0.015(5) -0.034(9) C41 0.044(9) 0.073(11) 0.087(10) 0.001(9) 0.012(8) -0.010(8) C42 0.029(7) 0.037(7) 0.062(8) 0.011(6) 0.003(6) 0.007(5) C43 0.024(6) 0.069(9) 0.038(7) 0.036(6) -0.007(5) -0.016(6) C44 0.069(13) 0.091(14) 0.079(11) 0.016(11) 0.059(10) 0.020(11) C45 0.056(11) 0.092(14) 0.072(10) 0.055(10) 0.031(8) 0.044(10) C46 0.021(7) 0.062(11) 0.048(7) 0.000(7) 0.008(6) -0.017(7) C47 0.024(8) 0.29(3) 0.029(7) 0.037(12) 0.002(6) -0.036(14) C48 0.050(10) 0.065(11) 0.027(6) -0.004(5) 0.004(6) -0.006(7) C49 0.056(12) 0.26(3) 0.034(8) -0.011(12) 0.010(8) -0.047(16) C50 0.030(7) 0.031(7) 0.058(7) 0.007(6) 0.018(6) 0.005(6) C51 0.097(15) 0.085(12) 0.010(5) 0.008(6) -0.031(7) -0.028(11) C52 0.054(10) 0.079(12) 0.035(7) 0.031(7) 0.001(7) 0.018(9) C53 0.050(11) 0.131(19) 0.070(11) 0.046(12) 0.024(8) -0.008(12) C54 0.032(7) 0.071(10) 0.046(7) 0.000(7) -0.009(6) 0.016(7) C55 0.046(10) 0.112(16) 0.20(2) -0.041(15) 0.034(12) 0.017(10) C56 0.028(7) 0.108(14) 0.101(12) 0.036(10) 0.010(7) -0.021(8) C57 0.14(2) 0.16(2) 0.042(9) 0.034(10) -0.012(10) -0.077(16) C58 0.052(9) 0.101(15) 0.094(11) -0.002(11) 0.017(8) 0.008(10) C59 0.034(8) 0.138(18) 0.102(12) 0.031(13) 0.016(8) -0.010(11) C60 0.105(13) 0.102(13) 0.025(6) -0.027(7) -0.030(7) 0.011(10) N7 0.040(8) 0.047(7) 0.061(7) 0.002(7) 0.023(6) -0.003(7) O7 0.038(6) 0.184(16) 0.052(6) 0.017(8) -0.002(5) 0.008(9) C61 0.036(9) 0.050(9) 0.069(9) -0.001(8) 0.016(7) -0.015(8) C62 0.021(7) 0.048(9) 0.036(6) -0.007(5) 0.012(5) -0.006(6) C63 0.031(7) 0.061(9) 0.026(5) 0.003(6) 0.007(5) -0.006(7) C64 0.045(10) 0.085(13) 0.061(9) 0.030(9) 0.029(8) 0.007(9) C65 0.022(6) 0.061(10) 0.054(8) 0.010(7) 0.008(6) -0.004(7) C66 0.052(10) 0.065(11) 0.060(9) 0.003(9) 0.026(8) -0.001(9) C67 0.039(8) 0.042(8) 0.023(5) 0.003(5) -0.004(5) -0.006(6) C68 0.073(12) 0.087(14) 0.041(7) 0.032(8) -0.004(8) 0.021(11) C69 0.043(9) 0.061(10) 0.062(8) -0.002(7) 0.000(7) -0.003(8) C70 0.053(10) 0.085(12) 0.044(7) -0.018(8) 0.006(7) 0.004(9) _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 C15 1.31(2) . ? N1 C1 1.46(2) . ? N1 C16 1.48(2) . ? N1 C17 1.612(19) . ? N2 C20 1.40(2) . ? N2 C14 1.49(2) . ? N2 C19 1.49(2) . ? N2 C18 1.528(18) . ? O1 C3 1.305(17) . ? O1 H1 0.8200 . ? O2 C11 1.430(18) . ? O2 H2 0.8200 . ? C1 C2 1.54(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.41(2) . ? C2 C7 1.426(17) . ? C3 C4 1.48(2) . ? C4 C5 1.30(2) . ? C4 H4 0.9300 . ? C5 C6 1.44(2) . ? C5 H5 0.9300 . ? C6 C7 1.353(19) . ? C6 C8 1.481(19) . ? C7 H7 0.9300 . ? C8 C9 1.35(2) . ? C8 C13 1.45(2) . ? C9 C10 1.40(2) . ? C9 H9 0.9300 . ? C10 C11 1.35(2) . ? C10 C14 1.60(2) . ? C11 C12 1.35(3) . ? C12 C13 1.395(18) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? N3 C35 1.42(2) . ? N3 C37 1.553(15) . ? N3 C36 1.55(2) . ? N3 C21 1.575(19) . ? N4 C40 1.51(2) . ? N4 C38 1.509(18) . ? N4 C34 1.545(19) . ? N4 C39 1.58(2) . ? O3 C23 1.424(16) . ? O3 H3 0.8200 . ? O4 C31 1.331(15) . ? O4 H4A 0.8200 . ? C21 C22 1.45(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.346(19) . ? C22 C23 1.39(2) . ? C23 C24 1.37(2) . ? C24 C25 1.449(18) . ? C24 H24 0.9300 . ? C25 C26 1.30(2) . ? C25 H25 0.9300 . ? C26 C27 1.43(2) . ? C26 C28 1.517(16) . ? C27 H27 0.9300 . ? C28 C33 1.42(2) . ? C28 C29 1.459(18) . ? C29 C30 1.418(16) . ? C29 H29 0.9300 . ? C30 C31 1.38(2) . ? C30 C34 1.42(2) . ? C31 C32 1.44(2) . ? C32 C33 1.31(3) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? N5 C41 1.41(2) . ? N5 C56 1.46(2) . ? N5 C57 1.53(2) . ? N5 C55 1.54(2) . ? N6 C58 1.41(2) . ? N6 C59 1.45(2) . ? N6 C54 1.540(19) . ? N6 C60 1.595(15) . ? O5 C43 1.323(15) . ? O5 H5A 0.8200 . ? O6 C51 1.442(14) . ? O6 H6 0.8200 . ? C41 C42 1.53(2) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.49(2) . ? C42 C47 1.50(2) . ? C43 C44 1.38(2) . ? C44 C45 1.44(2) . ? C44 H44 0.9300 . ? C45 C46 1.26(2) . ? C45 H45 0.9300 . ? C46 C47 1.34(2) . ? C46 C48 1.489(15) . ? C47 H47 0.9300 . ? C48 C49 1.38(2) . ? C48 C53 1.44(2) . ? C49 C50 1.47(2) . ? C49 H49 0.9300 . ? C50 C51 1.36(2) . ? C50 C54 1.543(18) . ? C51 C52 1.30(3) . ? C52 C53 1.38(2) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? N7 C70 1.433(19) . ? N7 C69 1.45(2) . ? N7 C61 1.50(2) . ? N7 C68 1.515(19) . ? O7 C63 1.379(15) . ? O7 H7A 0.8200 . ? C61 C62 1.59(2) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.444(19) . ? C62 C67 1.450(17) . ? C63 C64 1.35(2) . ? C64 C65 1.35(2) . ? C64 H64 0.9300 . ? C65 C66 1.45(2) . ? C65 H65 0.9300 . ? C66 C67 1.31(2) . ? C66 C66 1.48(3) 2_556 ? C67 H67 0.9300 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? 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 C15 N1 C1 117.9(15) . . ? C15 N1 C16 112.9(17) . . ? C1 N1 C16 107.1(15) . . ? C15 N1 C17 107.9(19) . . ? C1 N1 C17 109.6(13) . . ? C16 N1 C17 99.9(12) . . ? C20 N2 C14 111.3(15) . . ? C20 N2 C19 106.7(14) . . ? C14 N2 C19 113.1(13) . . ? C20 N2 C18 107.4(14) . . ? C14 N2 C18 112.5(12) . . ? C19 N2 C18 105.3(13) . . ? C3 O1 H1 109.5 . . ? C11 O2 H2 109.5 . . ? N1 C1 C2 112.4(16) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C3 C2 C7 120.0(15) . . ? C3 C2 C1 119.3(13) . . ? C7 C2 C1 117.3(16) . . ? O1 C3 C2 119.9(13) . . ? O1 C3 C4 127.5(14) . . ? C2 C3 C4 111.4(14) . . ? C5 C4 C3 125.1(16) . . ? C5 C4 H4 117.4 . . ? C3 C4 H4 117.4 . . ? C4 C5 C6 123.1(15) . . ? C4 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C7 C6 C5 113.1(12) . . ? C7 C6 C8 128.6(13) . . ? C5 C6 C8 118.3(14) . . ? C6 C7 C2 125.7(14) . . ? C6 C7 H7 117.1 . . ? C2 C7 H7 117.1 . . ? C9 C8 C13 122.2(13) . . ? C9 C8 C6 120.9(14) . . ? C13 C8 C6 116.7(14) . . ? C8 C9 C10 116.0(14) . . ? C8 C9 H9 122.0 . . ? C10 C9 H9 122.0 . . ? C11 C10 C9 120.5(16) . . ? C11 C10 C14 122.2(16) . . ? C9 C10 C14 114.7(15) . . ? C12 C11 C10 125.0(16) . . ? C12 C11 O2 119.0(13) . . ? C10 C11 O2 115.0(17) . . ? C11 C12 C13 116.5(15) . . ? C11 C12 H12 121.7 . . ? C13 C12 H12 121.7 . . ? C12 C13 C8 118.6(15) . . ? C12 C13 H13 120.7 . . ? C8 C13 H13 120.7 . . ? N2 C14 C10 112.9(15) . . ? N2 C14 H14A 109.0 . . ? C10 C14 H14A 109.0 . . ? N2 C14 H14B 109.0 . . ? C10 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C35 N3 C37 115.9(15) . . ? C35 N3 C36 111.0(12) . . ? C37 N3 C36 109.0(11) . . ? C35 N3 C21 110.2(11) . . ? C37 N3 C21 107.8(9) . . ? C36 N3 C21 102.0(14) . . ? C40 N4 C38 112.1(14) . . ? C40 N4 C34 114.7(14) . . ? C38 N4 C34 108.3(11) . . ? C40 N4 C39 108.1(13) . . ? C38 N4 C39 109.7(14) . . ? C34 N4 C39 103.6(14) . . ? C23 O3 H3 109.5 . . ? C31 O4 H4A 109.5 . . ? C22 C21 N3 116.6(13) . . ? C22 C21 H21A 108.1 . . ? N3 C21 H21A 108.1 . . ? C22 C21 H21B 108.1 . . ? N3 C21 H21B 108.1 . . ? H21A C21 H21B 107.3 . . ? C27 C22 C23 114.9(16) . . ? C27 C22 C21 124.3(13) . . ? C23 C22 C21 120.7(13) . . ? C24 C23 C22 125.4(13) . . ? C24 C23 O3 117.2(14) . . ? C22 C23 O3 117.1(16) . . ? C23 C24 C25 117.0(14) . . ? C23 C24 H24 121.5 . . ? C25 C24 H24 121.5 . . ? C26 C25 C24 118.4(16) . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 120.8 . . ? C25 C26 C27 122.3(14) . . ? C25 C26 C28 122.3(14) . . ? C27 C26 C28 115.4(14) . . ? C22 C27 C26 121.8(16) . . ? C22 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C33 C28 C29 112.7(12) . . ? C33 C28 C26 128.1(14) . . ? C29 C28 C26 119.2(12) . . ? C30 C29 C28 126.1(12) . . ? C30 C29 H29 117.0 . . ? C28 C29 H29 117.0 . . ? C31 C30 C29 117.1(13) . . ? C31 C30 C34 123.7(13) . . ? C29 C30 C34 119.1(14) . . ? O4 C31 C30 121.0(15) . . ? O4 C31 C32 122.0(16) . . ? C30 C31 C32 116.4(12) . . ? C33 C32 C31 126.9(17) . . ? C33 C32 H32 116.6 . . ? C31 C32 H32 116.6 . . ? C32 C33 C28 120.8(18) . . ? C32 C33 H33 119.6 . . ? C28 C33 H33 119.6 . . ? C30 C34 N4 116.8(15) . . ? C30 C34 H34A 108.1 . . ? N4 C34 H34A 108.1 . . ? C30 C34 H34B 108.1 . . ? N4 C34 H34B 108.1 . . ? H34A C34 H34B 107.3 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 H37A 109.5 . . ? N3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 H38A 109.5 . . ? N4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N4 C39 H39A 109.5 . . ? N4 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N4 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N4 C40 H40A 109.5 . . ? N4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C41 N5 C56 120.8(13) . . ? C41 N5 C57 109.4(14) . . ? C56 N5 C57 105.7(15) . . ? C41 N5 C55 110.0(16) . . ? C56 N5 C55 108.4(14) . . ? C57 N5 C55 100.5(15) . . ? C58 N6 C59 119.1(13) . . ? C58 N6 C54 113.0(13) . . ? C59 N6 C54 105.4(15) . . ? C58 N6 C60 104.0(14) . . ? C59 N6 C60 109.6(13) . . ? C54 N6 C60 105.0(10) . . ? C43 O5 H5A 109.5 . . ? C51 O6 H6 109.5 . . ? N5 C41 C42 112.4(15) . . ? N5 C41 H41A 109.1 . . ? C42 C41 H41A 109.1 . . ? N5 C41 H41B 109.1 . . ? C42 C41 H41B 109.1 . . ? H41A C41 H41B 107.9 . . ? C43 C42 C47 109.5(12) . . ? C43 C42 C41 122.9(12) . . ? C47 C42 C41 127.1(14) . . ? O5 C43 C44 129.0(16) . . ? O5 C43 C42 116.1(14) . . ? C44 C43 C42 114.7(12) . . ? C43 C44 C45 124.7(16) . . ? C43 C44 H44 117.6 . . ? C45 C44 H44 117.6 . . ? C46 C45 C44 122.5(17) . . ? C46 C45 H45 118.8 . . ? C44 C45 H45 118.8 . . ? C45 C46 C47 115.0(15) . . ? C45 C46 C48 123.9(13) . . ? C47 C46 C48 121.0(12) . . ? C46 C47 C42 127.4(15) . . ? C46 C47 H47 116.3 . . ? C42 C47 H47 116.3 . . ? C49 C48 C53 118.9(15) . . ? C49 C48 C46 118.1(12) . . ? C53 C48 C46 122.9(14) . . ? C48 C49 C50 116.2(15) . . ? C48 C49 H49 121.9 . . ? C50 C49 H49 121.9 . . ? C51 C50 C49 111.6(14) . . ? C51 C50 C54 125.9(13) . . ? C49 C50 C54 120.6(13) . . ? C52 C51 C50 128.1(14) . . ? C52 C51 O6 116.6(15) . . ? C50 C51 O6 113.3(16) . . ? C51 C52 C53 117.4(16) . . ? C51 C52 H52 121.3 . . ? C53 C52 H52 121.3 . . ? C52 C53 C48 119.2(18) . . ? C52 C53 H53 120.4 . . ? C48 C53 H53 120.4 . . ? N6 C54 C50 117.8(13) . . ? N6 C54 H54A 107.8 . . ? C50 C54 H54A 107.8 . . ? N6 C54 H54B 107.8 . . ? C50 C54 H54B 107.8 . . ? H54A C54 H54B 107.2 . . ? N5 C55 H55A 109.5 . . ? N5 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N5 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N5 C56 H56A 109.5 . . ? N5 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N5 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N5 C57 H57A 109.5 . . ? N5 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N5 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N6 C58 H58A 109.5 . . ? N6 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? N6 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N6 C59 H59A 109.5 . . ? N6 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N6 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N6 C60 H60A 109.5 . . ? N6 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N6 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C70 N7 C69 112.2(14) . . ? C70 N7 C61 113.3(13) . . ? C69 N7 C61 106.4(14) . . ? C70 N7 C68 103.3(14) . . ? C69 N7 C68 111.6(13) . . ? C61 N7 C68 110.2(13) . . ? C63 O7 H7A 109.5 . . ? N7 C61 C62 118.4(14) . . ? N7 C61 H61A 107.7 . . ? C62 C61 H61A 107.7 . . ? N7 C61 H61B 107.7 . . ? C62 C61 H61B 107.7 . . ? H61A C61 H61B 107.1 . . ? C63 C62 C67 121.4(13) . . ? C63 C62 C61 121.3(12) . . ? C67 C62 C61 117.3(13) . . ? C64 C63 O7 127.8(14) . . ? C64 C63 C62 117.4(12) . . ? O7 C63 C62 114.5(13) . . ? C63 C64 C65 120.9(16) . . ? C63 C64 H64 119.6 . . ? C65 C64 H64 119.6 . . ? C64 C65 C66 122.8(16) . . ? C64 C65 H65 118.6 . . ? C66 C65 H65 118.6 . . ? C67 C66 C65 119.1(14) . . ? C67 C66 C66 124.7(19) . 2_556 ? C65 C66 C66 116(2) . 2_556 ? C66 C67 C62 118.4(14) . . ? C66 C67 H67 120.8 . . ? C62 C67 H67 120.8 . . ? N7 C68 H68A 109.5 . . ? N7 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? N7 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N7 C69 H69A 109.5 . . ? N7 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N7 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N7 C70 H70A 109.5 . . ? N7 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N7 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 I1 0.82 2.58 3.401(14) 176.4 2_655 O2 H2 I2 0.82 2.79 3.545(11) 154.0 . O3 H3 I3 0.82 2.69 3.444(10) 154.3 3_545 O4 H4A I4 0.82 3.10 3.802(15) 144.5 3_545 O5 H5A I5 0.82 2.68 3.420(13) 150.3 4_646 O6 H6 I6 0.82 3.30 3.486(14) 96.6 3 O7 H7A I7 0.82 3.04 3.529(15) 120.8 4_546 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.163 _refine_diff_density_min -1.861 _refine_diff_density_rms 0.133