data_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H23 N3 O7' _chemical_formula_sum 'C20 H23 N3 O7' _chemical_formula_weight 417.41 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 10.0906(17) _cell_length_b 10.702(2) _cell_length_c 19.365(3) _cell_angle_alpha 94.622(6) _cell_angle_beta 104.715(6) _cell_angle_gamma 95.703(7) _cell_volume 2000.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6245 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.106 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9719 _exptl_absorpt_correction_T_max 0.9822 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007-HF CCD(Saturn 724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24779 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.45 _reflns_number_total 9087 _reflns_number_gt 7939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.0441P)^2^+0.8487P] 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 9087 _refine_ls_number_parameters 574 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.123 _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 -0.00482(16) 1.11019(14) 0.24597(9) 0.0499(4) Uani 1 1 d . . . O2 O 0.18740(17) 1.22228(13) 0.30193(8) 0.0462(4) Uani 1 1 d . . . O3 O 0.43222(13) 0.33608(12) 0.45556(7) 0.0321(3) Uani 1 1 d . . . O4 O 0.09119(14) 0.39281(13) 0.60975(7) 0.0375(3) Uani 1 1 d . . . O5 O 0.14642(14) 0.59433(12) 0.59225(7) 0.0322(3) Uani 1 1 d . . . O6 O 0.34491(14) 0.25383(13) 0.59435(7) 0.0380(3) Uani 1 1 d . . . O7 O 0.19601(17) 0.09169(13) 0.52936(8) 0.0480(4) Uani 1 1 d . . . O8 O 0.37083(19) 1.26242(13) 0.19416(9) 0.0535(4) Uani 1 1 d . . . O9 O 0.49951(17) 1.17757(14) 0.28038(9) 0.0524(4) Uani 1 1 d . . . O10 O 0.07405(13) 0.26220(11) 0.05450(7) 0.0314(3) Uani 1 1 d . . . O11 O 0.29488(15) 0.57316(13) -0.09845(7) 0.0404(3) Uani 1 1 d . . . O12 O 0.41512(13) 0.40738(12) -0.09641(7) 0.0322(3) Uani 1 1 d . . . O13 O 0.16024(15) 0.20861(13) -0.10335(8) 0.0406(3) Uani 1 1 d . A . N1 N 0.11048(18) 1.12172(14) 0.28670(8) 0.0327(4) Uani 1 1 d . . . N2 N 0.26446(15) 0.57261(13) 0.36497(7) 0.0235(3) Uani 1 1 d . . . N3 N 0.27691(15) 0.47306(13) 0.41210(7) 0.0237(3) Uani 1 1 d . . . N4 N 0.40800(19) 1.17007(15) 0.22402(10) 0.0386(4) Uani 1 1 d . . . N5 N 0.18002(15) 0.57530(13) 0.13572(7) 0.0240(3) Uani 1 1 d . . . N6 N 0.17888(15) 0.46736(13) 0.08493(7) 0.0242(3) Uani 1 1 d . . . C1 C 0.16087(19) 1.01078(16) 0.31967(9) 0.0272(4) Uani 1 1 d . . . C2 C 0.08043(19) 0.89499(16) 0.29816(10) 0.0285(4) Uani 1 1 d . . . H2A H -0.0048 0.8871 0.2623 0.034 Uiso 1 1 calc R . . C3 C 0.12727(18) 0.79117(16) 0.33019(9) 0.0265(4) Uani 1 1 d . . . H3A H 0.0721 0.7113 0.3172 0.032 Uiso 1 1 calc R . . C4 C 0.25398(18) 0.80198(15) 0.38111(9) 0.0234(3) Uani 1 1 d . . . C5 C 0.33224(19) 0.92003(16) 0.40085(9) 0.0277(4) Uani 1 1 d . . . H5A H 0.4191 0.9279 0.4355 0.033 Uiso 1 1 calc R . . C6 C 0.2859(2) 1.02617(16) 0.37099(10) 0.0297(4) Uani 1 1 d . . . H6A H 0.3385 1.1070 0.3854 0.036 Uiso 1 1 calc R . . C7 C 0.30584(18) 0.68926(15) 0.41627(9) 0.0233(3) Uani 1 1 d . . . H7A H 0.4086 0.7040 0.4351 0.028 Uiso 1 1 calc R . . C8 C 0.36259(19) 0.54838(17) 0.32116(9) 0.0291(4) Uani 1 1 d . . . H8A H 0.4116 0.6290 0.3138 0.035 Uiso 1 1 calc R . . H8B H 0.3126 0.5032 0.2736 0.035 Uiso 1 1 calc R . . C9 C 0.46436(19) 0.46809(17) 0.36241(9) 0.0282(4) Uani 1 1 d . . . H9A H 0.4824 0.3996 0.3298 0.034 Uiso 1 1 calc R . . H9B H 0.5529 0.5202 0.3873 0.034 Uiso 1 1 calc R . . C10 C 0.39551(18) 0.41492(16) 0.41545(9) 0.0249(4) Uani 1 1 d . . . C11 C 0.23035(17) 0.51246(16) 0.47223(9) 0.0228(3) Uani 1 1 d . . . C12 C 0.23949(18) 0.65512(15) 0.47675(9) 0.0243(3) Uani 1 1 d . . . H12A H 0.2977 0.6946 0.5241 0.029 Uiso 1 1 calc R . . H12B H 0.1466 0.6830 0.4689 0.029 Uiso 1 1 calc R . . C13 C 0.18431(17) 0.43026(16) 0.51227(9) 0.0249(4) Uani 1 1 d . . . C14 C 0.13705(18) 0.46906(17) 0.57611(9) 0.0278(4) Uani 1 1 d . . . C15 C 0.0955(2) 0.6364(2) 0.65300(10) 0.0352(4) Uani 1 1 d . . . H15A H 0.0116 0.5797 0.6529 0.042 Uiso 1 1 calc R . . H15B H 0.0696 0.7227 0.6480 0.042 Uiso 1 1 calc R . . C16 C 0.2011(2) 0.6367(2) 0.72244(11) 0.0471(5) Uani 1 1 d . . . H16A H 0.1703 0.6791 0.7613 0.071 Uiso 1 1 calc R . . H16B H 0.2889 0.6817 0.7199 0.071 Uiso 1 1 calc R . . H16C H 0.2138 0.5495 0.7319 0.071 Uiso 1 1 calc R . . C17 C 0.16179(19) 0.28973(16) 0.49202(10) 0.0293(4) Uani 1 1 d . . . H17A H 0.1830 0.2721 0.4453 0.035 Uiso 1 1 calc R . . H17B H 0.0629 0.2597 0.4853 0.035 Uiso 1 1 calc R . . C18 C 0.2467(2) 0.21447(17) 0.54562(10) 0.0304(4) Uani 1 1 d . . . C19 C 0.2606(3) 0.0043(2) 0.57690(14) 0.0543(6) Uani 1 1 d . . . H19A H 0.3610 0.0325 0.5948 0.065 Uiso 1 1 calc R . . H19B H 0.2480 -0.0807 0.5501 0.065 Uiso 1 1 calc R . . C20 C 0.1994(3) -0.0022(3) 0.63805(16) 0.0653(7) Uani 1 1 d . . . H20A H 0.2406 -0.0646 0.6684 0.098 Uiso 1 1 calc R . . H20B H 0.0995 -0.0270 0.6202 0.098 Uiso 1 1 calc R . . H20C H 0.2171 0.0809 0.6663 0.098 Uiso 1 1 calc R . . C21 C 0.3395(2) 1.04379(16) 0.19158(10) 0.0307(4) Uani 1 1 d . . . C22 C 0.3927(2) 0.93978(17) 0.22087(10) 0.0311(4) Uani 1 1 d . . . H22A H 0.4704 0.9496 0.2615 0.037 Uiso 1 1 calc R . . C23 C 0.32960(19) 0.82142(16) 0.18932(10) 0.0292(4) Uani 1 1 d . . . H23A H 0.3639 0.7486 0.2087 0.035 Uiso 1 1 calc R . . C24 C 0.21667(18) 0.80711(16) 0.12965(9) 0.0247(4) Uani 1 1 d . . . C25 C 0.1638(2) 0.91367(17) 0.10312(10) 0.0317(4) Uani 1 1 d . . . H25A H 0.0841 0.9042 0.0635 0.038 Uiso 1 1 calc R . . C26 C 0.2256(2) 1.03355(17) 0.13359(10) 0.0335(4) Uani 1 1 d . . . H26A H 0.1904 1.1066 0.1150 0.040 Uiso 1 1 calc R . . C27 C 0.15748(18) 0.67899(15) 0.08937(9) 0.0240(3) Uani 1 1 d . . . H27A H 0.0564 0.6778 0.0670 0.029 Uiso 1 1 calc R . . C28 C 0.06342(19) 0.53818(17) 0.16665(10) 0.0295(4) Uani 1 1 d . . . H28A H -0.0220 0.5695 0.1402 0.035 Uiso 1 1 calc R . . H28B H 0.0849 0.5719 0.2179 0.035 Uiso 1 1 calc R . . C29 C 0.0477(2) 0.39460(17) 0.15818(10) 0.0315(4) Uani 1 1 d . . . H29A H 0.1043 0.3625 0.2011 0.038 Uiso 1 1 calc R . . H29B H -0.0500 0.3591 0.1504 0.038 Uiso 1 1 calc R . . C30 C 0.09802(18) 0.36151(16) 0.09334(9) 0.0261(4) Uani 1 1 d . . . C31 C 0.23380(18) 0.50444(15) 0.02945(9) 0.0242(3) Uani 1 1 d . . . C32 C 0.23021(19) 0.64540(16) 0.03101(9) 0.0260(4) Uani 1 1 d . . . H32A H 0.1780 0.6673 -0.0161 0.031 Uiso 1 1 calc R . . H32B H 0.3249 0.6909 0.0432 0.031 Uiso 1 1 calc R . . C33 C 0.29220(18) 0.42919(16) -0.01016(9) 0.0250(4) Uani 1 1 d . . . C34 C 0.33174(18) 0.48008(16) -0.07185(9) 0.0269(4) Uani 1 1 d . . . C35 C 0.4403(2) 0.4314(2) -0.16501(10) 0.0360(4) Uani 1 1 d . . . H35A H 0.5380 0.4243 -0.1634 0.043 Uiso 1 1 calc R . . H35B H 0.4214 0.5179 -0.1754 0.043 Uiso 1 1 calc R . . C36 C 0.3475(2) 0.3366(2) -0.22260(11) 0.0467(5) Uani 1 1 d . . . H36A H 0.3674 0.3490 -0.2687 0.070 Uiso 1 1 calc R . . H36B H 0.2510 0.3479 -0.2259 0.070 Uiso 1 1 calc R . . H36C H 0.3635 0.2511 -0.2108 0.070 Uiso 1 1 calc R . . C37 C 0.32730(19) 0.30008(16) 0.00640(10) 0.0287(4) Uani 1 1 d . A . H37A H 0.3065 0.2831 0.0523 0.034 Uiso 1 1 calc R . . H37B H 0.4276 0.2986 0.0129 0.034 Uiso 1 1 calc R . . C38 C 0.2499(2) 0.19666(18) -0.05111(11) 0.0342(4) Uani 1 1 d D . . O14 O 0.2854(9) 0.0842(6) -0.0280(4) 0.0426(13) Uani 0.538(16) 1 d PDU A 1 C39 C 0.2306(10) -0.0294(8) -0.0778(5) 0.054(2) Uani 0.538(16) 1 d PDU A 1 H39A H 0.1434 -0.0156 -0.1120 0.065 Uiso 0.538(16) 1 calc PR A 1 H39B H 0.2104 -0.1006 -0.0509 0.065 Uiso 0.538(16) 1 calc PR A 1 C40 C 0.3331(10) -0.0613(12) -0.1181(7) 0.096(3) Uani 0.538(16) 1 d PDU A 1 H40A H 0.3383 0.0005 -0.1524 0.145 Uiso 0.538(16) 1 calc PR A 1 H40B H 0.3042 -0.1460 -0.1442 0.145 Uiso 0.538(16) 1 calc PR A 1 H40C H 0.4241 -0.0592 -0.0843 0.145 Uiso 0.538(16) 1 calc PR A 1 O14' O 0.3122(10) 0.0935(8) -0.0466(6) 0.050(2) Uani 0.462(16) 1 d PDU A 2 C39' C 0.2514(12) -0.0131(9) -0.0999(7) 0.064(3) Uani 0.462(16) 1 d PDU A 2 H39C H 0.2369 0.0121 -0.1490 0.077 Uiso 0.462(16) 1 calc PR A 2 H39D H 0.1617 -0.0499 -0.0936 0.077 Uiso 0.462(16) 1 calc PR A 2 C40' C 0.3546(9) -0.1044(6) -0.0863(6) 0.063(2) Uani 0.462(16) 1 d PDU A 2 H40D H 0.4411 -0.0673 -0.0946 0.094 Uiso 0.462(16) 1 calc PR A 2 H40E H 0.3192 -0.1822 -0.1188 0.094 Uiso 0.462(16) 1 calc PR A 2 H40F H 0.3714 -0.1239 -0.0364 0.094 Uiso 0.462(16) 1 calc PR A 2 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 0.0472(9) 0.0400(8) 0.0567(10) 0.0149(7) -0.0034(8) 0.0151(7) O2 0.0618(10) 0.0251(7) 0.0469(9) 0.0092(6) 0.0046(7) 0.0041(7) O3 0.0321(7) 0.0311(7) 0.0336(7) 0.0099(5) 0.0049(5) 0.0119(5) O4 0.0394(8) 0.0402(8) 0.0367(8) 0.0114(6) 0.0164(6) -0.0001(6) O5 0.0420(8) 0.0313(7) 0.0273(7) 0.0040(5) 0.0152(6) 0.0078(6) O6 0.0359(8) 0.0380(8) 0.0386(8) 0.0125(6) 0.0051(6) 0.0026(6) O7 0.0681(11) 0.0240(7) 0.0499(9) 0.0061(6) 0.0127(8) 0.0019(7) O8 0.0833(12) 0.0230(7) 0.0540(10) 0.0042(7) 0.0207(9) -0.0006(7) O9 0.0500(10) 0.0361(8) 0.0600(11) -0.0111(7) 0.0025(8) -0.0022(7) O10 0.0350(7) 0.0225(6) 0.0334(7) 0.0029(5) 0.0038(6) 0.0017(5) O11 0.0529(9) 0.0414(8) 0.0381(8) 0.0153(6) 0.0236(7) 0.0205(7) O12 0.0321(7) 0.0385(7) 0.0300(7) 0.0041(5) 0.0122(5) 0.0128(6) O13 0.0372(8) 0.0385(8) 0.0395(8) -0.0024(6) 0.0004(6) 0.0037(6) N1 0.0438(10) 0.0272(8) 0.0303(8) 0.0056(6) 0.0121(7) 0.0110(7) N2 0.0292(8) 0.0222(7) 0.0201(7) 0.0047(5) 0.0066(6) 0.0065(6) N3 0.0262(8) 0.0220(7) 0.0234(7) 0.0056(5) 0.0057(6) 0.0057(6) N4 0.0463(10) 0.0277(9) 0.0426(10) -0.0031(7) 0.0173(8) 0.0003(7) N5 0.0303(8) 0.0204(7) 0.0217(7) 0.0012(5) 0.0074(6) 0.0052(6) N6 0.0303(8) 0.0195(7) 0.0235(7) 0.0015(5) 0.0082(6) 0.0041(6) C1 0.0341(10) 0.0244(8) 0.0269(9) 0.0059(7) 0.0113(7) 0.0110(7) C2 0.0272(9) 0.0284(9) 0.0299(9) 0.0030(7) 0.0058(7) 0.0073(7) C3 0.0270(9) 0.0246(8) 0.0280(9) 0.0022(7) 0.0075(7) 0.0036(7) C4 0.0278(9) 0.0238(8) 0.0209(8) 0.0032(6) 0.0094(7) 0.0063(7) C5 0.0279(9) 0.0279(9) 0.0260(9) 0.0035(7) 0.0050(7) 0.0024(7) C6 0.0383(10) 0.0222(9) 0.0287(9) 0.0027(7) 0.0097(8) 0.0020(7) C7 0.0245(8) 0.0223(8) 0.0223(8) 0.0028(6) 0.0043(6) 0.0039(6) C8 0.0328(10) 0.0331(9) 0.0238(9) 0.0037(7) 0.0095(7) 0.0098(8) C9 0.0283(9) 0.0290(9) 0.0277(9) 0.0000(7) 0.0080(7) 0.0057(7) C10 0.0249(9) 0.0229(8) 0.0239(8) -0.0014(6) 0.0017(7) 0.0038(7) C11 0.0201(8) 0.0252(8) 0.0213(8) 0.0025(6) 0.0018(6) 0.0043(6) C12 0.0265(9) 0.0227(8) 0.0245(8) 0.0031(6) 0.0078(7) 0.0046(7) C13 0.0234(9) 0.0256(9) 0.0248(8) 0.0050(7) 0.0036(7) 0.0037(7) C14 0.0212(9) 0.0336(10) 0.0275(9) 0.0064(7) 0.0036(7) 0.0029(7) C15 0.0375(11) 0.0427(11) 0.0294(10) 0.0033(8) 0.0142(8) 0.0106(9) C16 0.0429(12) 0.0652(15) 0.0315(11) 0.0000(10) 0.0086(9) 0.0064(11) C17 0.0291(9) 0.0272(9) 0.0304(9) 0.0050(7) 0.0069(7) -0.0009(7) C18 0.0356(10) 0.0256(9) 0.0331(10) 0.0058(7) 0.0149(8) 0.0017(8) C19 0.0722(17) 0.0309(11) 0.0706(17) 0.0164(11) 0.0313(14) 0.0167(11) C20 0.0725(18) 0.0590(16) 0.0782(19) 0.0293(14) 0.0358(15) 0.0145(14) C21 0.0387(11) 0.0223(9) 0.0334(10) -0.0034(7) 0.0168(8) 0.0009(7) C22 0.0327(10) 0.0304(9) 0.0294(9) -0.0006(7) 0.0072(8) 0.0054(8) C23 0.0359(10) 0.0241(9) 0.0286(9) 0.0037(7) 0.0076(8) 0.0097(7) C24 0.0287(9) 0.0222(8) 0.0254(9) 0.0015(6) 0.0106(7) 0.0060(7) C25 0.0359(10) 0.0275(9) 0.0318(10) 0.0064(7) 0.0061(8) 0.0081(8) C26 0.0430(11) 0.0232(9) 0.0365(10) 0.0070(7) 0.0124(9) 0.0076(8) C27 0.0271(9) 0.0227(8) 0.0222(8) 0.0032(6) 0.0051(7) 0.0070(7) C28 0.0327(10) 0.0300(9) 0.0292(9) 0.0061(7) 0.0128(8) 0.0060(7) C29 0.0339(10) 0.0334(10) 0.0281(9) 0.0078(7) 0.0092(8) 0.0020(8) C30 0.0265(9) 0.0241(9) 0.0264(9) 0.0075(7) 0.0020(7) 0.0054(7) C31 0.0264(9) 0.0227(8) 0.0225(8) 0.0036(6) 0.0040(7) 0.0035(7) C32 0.0321(9) 0.0236(8) 0.0240(9) 0.0042(6) 0.0092(7) 0.0062(7) C33 0.0247(9) 0.0242(8) 0.0239(8) 0.0005(6) 0.0029(7) 0.0032(7) C34 0.0245(9) 0.0278(9) 0.0267(9) -0.0009(7) 0.0048(7) 0.0041(7) C35 0.0363(11) 0.0449(11) 0.0316(10) 0.0029(8) 0.0156(8) 0.0114(9) C36 0.0481(13) 0.0591(14) 0.0331(11) -0.0010(10) 0.0120(10) 0.0094(11) C37 0.0303(10) 0.0256(9) 0.0307(9) 0.0027(7) 0.0069(7) 0.0087(7) C38 0.0357(11) 0.0274(9) 0.0400(11) 0.0006(8) 0.0104(9) 0.0080(8) O14 0.069(3) 0.0225(16) 0.037(3) -0.0014(15) 0.0146(19) 0.0079(17) C39 0.080(4) 0.030(3) 0.050(4) -0.005(2) 0.018(3) -0.002(2) C40 0.097(5) 0.090(6) 0.093(6) -0.040(5) 0.027(5) 0.002(5) O14' 0.056(4) 0.031(3) 0.052(4) -0.011(2) -0.004(3) 0.021(2) C39' 0.077(5) 0.033(4) 0.067(6) -0.019(4) -0.004(4) 0.017(4) C40' 0.085(5) 0.028(3) 0.071(5) -0.011(3) 0.014(4) 0.016(3) _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 N1 1.217(2) . ? O2 N1 1.230(2) . ? O3 C10 1.214(2) . ? O4 C14 1.212(2) . ? O5 C14 1.340(2) . ? O5 C15 1.456(2) . ? O6 C18 1.195(2) . ? O7 C18 1.344(2) . ? O7 C19 1.450(3) . ? O8 N4 1.228(2) . ? O9 N4 1.229(2) . ? O10 C30 1.217(2) . ? O11 C34 1.206(2) . ? O12 C34 1.347(2) . ? O12 C35 1.452(2) . ? O13 C38 1.199(2) . ? N1 C1 1.467(2) . ? N2 N3 1.4522(18) . ? N2 C7 1.485(2) . ? N2 C8 1.487(2) . ? N3 C10 1.392(2) . ? N3 C11 1.412(2) . ? N4 C21 1.468(2) . ? N5 N6 1.4528(19) . ? N5 C27 1.482(2) . ? N5 C28 1.485(2) . ? N6 C30 1.374(2) . ? N6 C31 1.395(2) . ? C1 C6 1.379(3) . ? C1 C2 1.383(3) . ? C2 C3 1.382(2) . ? C2 H2A 0.9500 . ? C3 C4 1.390(2) . ? C3 H3A 0.9500 . ? C4 C5 1.392(2) . ? C4 C7 1.507(2) . ? C5 C6 1.385(2) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.540(2) . ? C7 H7A 1.0000 . ? C8 C9 1.517(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.496(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C13 1.343(2) . ? C11 C12 1.514(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.478(2) . ? C13 C17 1.503(2) . ? C15 C16 1.488(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.510(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.472(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.376(3) . ? C21 C22 1.384(3) . ? C22 C23 1.379(3) . ? C22 H22A 0.9500 . ? C23 C24 1.387(2) . ? C23 H23A 0.9500 . ? C24 C25 1.388(2) . ? C24 C27 1.508(2) . ? C25 C26 1.384(3) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C32 1.534(2) . ? C27 H27A 1.0000 . ? C28 C29 1.520(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.500(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 C33 1.345(2) . ? C31 C32 1.511(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.479(2) . ? C33 C37 1.499(2) . ? C35 C36 1.499(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.504(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 O14' 1.322(7) . ? C38 O14 1.367(7) . ? O14 C39 1.456(8) . ? C39 C40 1.494(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? O14' C39' 1.447(9) . ? C39' C40' 1.487(10) . ? C39' H39C 0.9900 . ? C39' H39D 0.9900 . ? C40' H40D 0.9800 . ? C40' H40E 0.9800 . ? C40' H40F 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 O5 C15 116.19(14) . . ? C18 O7 C19 117.13(18) . . ? C34 O12 C35 116.91(14) . . ? O1 N1 O2 123.23(16) . . ? O1 N1 C1 118.73(16) . . ? O2 N1 C1 118.04(16) . . ? N3 N2 C7 102.79(12) . . ? N3 N2 C8 103.99(12) . . ? C7 N2 C8 114.59(14) . . ? C10 N3 C11 124.68(14) . . ? C10 N3 N2 112.65(13) . . ? C11 N3 N2 108.20(12) . . ? O8 N4 O9 123.36(17) . . ? O8 N4 C21 118.86(18) . . ? O9 N4 C21 117.78(17) . . ? N6 N5 C27 102.78(12) . . ? N6 N5 C28 103.95(12) . . ? C27 N5 C28 114.32(13) . . ? C30 N6 C31 133.95(15) . . ? C30 N6 N5 113.15(14) . . ? C31 N6 N5 110.89(13) . . ? C6 C1 C2 122.69(16) . . ? C6 C1 N1 118.80(16) . . ? C2 C1 N1 118.51(16) . . ? C3 C2 C1 118.30(17) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 120.88(16) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C3 C4 C5 118.98(15) . . ? C3 C4 C7 121.23(15) . . ? C5 C4 C7 119.78(15) . . ? C6 C5 C4 121.25(17) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C1 C6 C5 117.86(16) . . ? C1 C6 H6A 121.1 . . ? C5 C6 H6A 121.1 . . ? N2 C7 C4 111.01(13) . . ? N2 C7 C12 102.17(13) . . ? C4 C7 C12 113.37(14) . . ? N2 C7 H7A 110.0 . . ? C4 C7 H7A 110.0 . . ? C12 C7 H7A 110.0 . . ? N2 C8 C9 106.78(14) . . ? N2 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? N2 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? C10 C9 C8 104.70(14) . . ? C10 C9 H9A 110.8 . . ? C8 C9 H9A 110.8 . . ? C10 C9 H9B 110.8 . . ? C8 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? O3 C10 N3 123.90(16) . . ? O3 C10 C9 128.43(16) . . ? N3 C10 C9 107.67(14) . . ? C13 C11 N3 122.37(15) . . ? C13 C11 C12 131.10(16) . . ? N3 C11 C12 106.49(13) . . ? C11 C12 C7 104.05(13) . . ? C11 C12 H12A 110.9 . . ? C7 C12 H12A 110.9 . . ? C11 C12 H12B 110.9 . . ? C7 C12 H12B 110.9 . . ? H12A C12 H12B 109.0 . . ? C11 C13 C14 123.45(16) . . ? C11 C13 C17 123.03(16) . . ? C14 C13 C17 113.23(15) . . ? O4 C14 O5 123.38(17) . . ? O4 C14 C13 122.09(17) . . ? O5 C14 C13 114.52(15) . . ? O5 C15 C16 111.55(16) . . ? O5 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? O5 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 C18 115.17(15) . . ? C13 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? C13 C17 H17B 108.5 . . ? C18 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? O6 C18 O7 123.84(18) . . ? O6 C18 C17 127.24(17) . . ? O7 C18 C17 108.91(16) . . ? O7 C19 C20 110.3(2) . . ? O7 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? O7 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? 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 . . ? C26 C21 C22 122.75(17) . . ? C26 C21 N4 118.95(17) . . ? C22 C21 N4 118.30(18) . . ? C23 C22 C21 118.06(17) . . ? C23 C22 H22A 121.0 . . ? C21 C22 H22A 121.0 . . ? C22 C23 C24 120.92(16) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? C23 C24 C25 119.32(16) . . ? C23 C24 C27 121.37(15) . . ? C25 C24 C27 119.12(16) . . ? C26 C25 C24 120.86(18) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C21 C26 C25 118.04(17) . . ? C21 C26 H26A 121.0 . . ? C25 C26 H26A 121.0 . . ? N5 C27 C24 112.68(13) . . ? N5 C27 C32 103.66(13) . . ? C24 C27 C32 111.33(14) . . ? N5 C27 H27A 109.7 . . ? C24 C27 H27A 109.7 . . ? C32 C27 H27A 109.7 . . ? N5 C28 C29 104.30(14) . . ? N5 C28 H28A 110.9 . . ? C29 C28 H28A 110.9 . . ? N5 C28 H28B 110.9 . . ? C29 C28 H28B 110.9 . . ? H28A C28 H28B 108.9 . . ? C30 C29 C28 104.00(14) . . ? C30 C29 H29A 111.0 . . ? C28 C29 H29A 111.0 . . ? C30 C29 H29B 111.0 . . ? C28 C29 H29B 111.0 . . ? H29A C29 H29B 109.0 . . ? O10 C30 N6 125.22(17) . . ? O10 C30 C29 128.41(16) . . ? N6 C30 C29 106.36(15) . . ? C33 C31 N6 124.99(15) . . ? C33 C31 C32 128.59(16) . . ? N6 C31 C32 105.97(14) . . ? C31 C32 C27 104.81(13) . . ? C31 C32 H32A 110.8 . . ? C27 C32 H32A 110.8 . . ? C31 C32 H32B 110.8 . . ? C27 C32 H32B 110.8 . . ? H32A C32 H32B 108.9 . . ? C31 C33 C34 117.73(15) . . ? C31 C33 C37 124.46(16) . . ? C34 C33 C37 117.71(15) . . ? O11 C34 O12 122.98(17) . . ? O11 C34 C33 125.98(17) . . ? O12 C34 C33 111.04(15) . . ? O12 C35 C36 108.88(17) . . ? O12 C35 H35A 109.9 . . ? C36 C35 H35A 109.9 . . ? O12 C35 H35B 109.9 . . ? C36 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C37 C38 113.40(15) . . ? C33 C37 H37A 108.9 . . ? C38 C37 H37A 108.9 . . ? C33 C37 H37B 108.9 . . ? C38 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? O13 C38 O14' 121.0(4) . . ? O13 C38 O14 125.5(4) . . ? O14' C38 O14 21.8(5) . . ? O13 C38 C37 126.26(17) . . ? O14' C38 C37 111.2(4) . . ? O14 C38 C37 107.6(3) . . ? C38 O14 C39 117.3(6) . . ? O14 C39 C40 110.0(7) . . ? O14 C39 H39A 109.7 . . ? C40 C39 H39A 109.7 . . ? O14 C39 H39B 109.7 . . ? C40 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? C38 O14' C39' 117.4(7) . . ? O14' C39' C40' 103.9(7) . . ? O14' C39' H39C 111.0 . . ? C40' C39' H39C 111.0 . . ? O14' C39' H39D 111.0 . . ? C40' C39' H39D 111.0 . . ? H39C C39' H39D 109.0 . . ? C39' C40' H40D 109.5 . . ? C39' C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C39' C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N2 N3 C10 -103.19(15) . . . . ? C8 N2 N3 C10 16.57(17) . . . . ? C7 N2 N3 C11 38.65(16) . . . . ? C8 N2 N3 C11 158.41(13) . . . . ? C27 N5 N6 C30 -133.16(14) . . . . ? C28 N5 N6 C30 -13.72(17) . . . . ? C27 N5 N6 C31 33.05(17) . . . . ? C28 N5 N6 C31 152.49(14) . . . . ? O1 N1 C1 C6 -173.89(17) . . . . ? O2 N1 C1 C6 5.9(2) . . . . ? O1 N1 C1 C2 5.8(3) . . . . ? O2 N1 C1 C2 -174.38(17) . . . . ? C6 C1 C2 C3 0.7(3) . . . . ? N1 C1 C2 C3 -178.97(16) . . . . ? C1 C2 C3 C4 -2.0(3) . . . . ? C2 C3 C4 C5 1.5(3) . . . . ? C2 C3 C4 C7 -179.97(16) . . . . ? C3 C4 C5 C6 0.3(3) . . . . ? C7 C4 C5 C6 -178.26(16) . . . . ? C2 C1 C6 C5 1.0(3) . . . . ? N1 C1 C6 C5 -179.31(16) . . . . ? C4 C5 C6 C1 -1.5(3) . . . . ? N3 N2 C7 C4 -160.15(13) . . . . ? C8 N2 C7 C4 87.73(17) . . . . ? N3 N2 C7 C12 -38.98(15) . . . . ? C8 N2 C7 C12 -151.10(13) . . . . ? C3 C4 C7 N2 35.4(2) . . . . ? C5 C4 C7 N2 -146.04(15) . . . . ? C3 C4 C7 C12 -78.9(2) . . . . ? C5 C4 C7 C12 99.63(18) . . . . ? N3 N2 C8 C9 -20.62(17) . . . . ? C7 N2 C8 C9 90.79(16) . . . . ? N2 C8 C9 C10 17.75(18) . . . . ? C11 N3 C10 O3 39.7(3) . . . . ? N2 N3 C10 O3 174.17(15) . . . . ? C11 N3 C10 C9 -139.94(16) . . . . ? N2 N3 C10 C9 -5.48(18) . . . . ? C8 C9 C10 O3 172.58(17) . . . . ? C8 C9 C10 N3 -7.79(18) . . . . ? C10 N3 C11 C13 -67.2(2) . . . . ? N2 N3 C11 C13 156.67(15) . . . . ? C10 N3 C11 C12 114.94(17) . . . . ? N2 N3 C11 C12 -21.16(17) . . . . ? C13 C11 C12 C7 178.39(17) . . . . ? N3 C11 C12 C7 -4.04(17) . . . . ? N2 C7 C12 C11 26.53(16) . . . . ? C4 C7 C12 C11 146.06(14) . . . . ? N3 C11 C13 C14 179.02(15) . . . . ? C12 C11 C13 C14 -3.7(3) . . . . ? N3 C11 C13 C17 -7.6(3) . . . . ? C12 C11 C13 C17 169.61(17) . . . . ? C15 O5 C14 O4 -1.1(3) . . . . ? C15 O5 C14 C13 177.51(14) . . . . ? C11 C13 C14 O4 177.22(17) . . . . ? C17 C13 C14 O4 3.3(2) . . . . ? C11 C13 C14 O5 -1.4(2) . . . . ? C17 C13 C14 O5 -175.30(15) . . . . ? C14 O5 C15 C16 83.0(2) . . . . ? C11 C13 C17 C18 119.65(19) . . . . ? C14 C13 C17 C18 -66.4(2) . . . . ? C19 O7 C18 O6 3.8(3) . . . . ? C19 O7 C18 C17 -177.42(17) . . . . ? C13 C17 C18 O6 -14.6(3) . . . . ? C13 C17 C18 O7 166.71(15) . . . . ? C18 O7 C19 C20 85.3(3) . . . . ? O8 N4 C21 C26 -7.4(3) . . . . ? O9 N4 C21 C26 172.03(18) . . . . ? O8 N4 C21 C22 172.56(18) . . . . ? O9 N4 C21 C22 -8.0(3) . . . . ? C26 C21 C22 C23 1.2(3) . . . . ? N4 C21 C22 C23 -178.73(16) . . . . ? C21 C22 C23 C24 0.4(3) . . . . ? C22 C23 C24 C25 -2.3(3) . . . . ? C22 C23 C24 C27 172.58(16) . . . . ? C23 C24 C25 C26 2.6(3) . . . . ? C27 C24 C25 C26 -172.38(17) . . . . ? C22 C21 C26 C25 -0.9(3) . . . . ? N4 C21 C26 C25 179.03(17) . . . . ? C24 C25 C26 C21 -1.0(3) . . . . ? N6 N5 C27 C24 -153.79(13) . . . . ? C28 N5 C27 C24 94.26(17) . . . . ? N6 N5 C27 C32 -33.31(16) . . . . ? C28 N5 C27 C32 -145.26(14) . . . . ? C23 C24 C27 N5 28.2(2) . . . . ? C25 C24 C27 N5 -156.86(16) . . . . ? C23 C24 C27 C32 -87.73(19) . . . . ? C25 C24 C27 C32 87.18(19) . . . . ? N6 N5 C28 C29 25.63(16) . . . . ? C27 N5 C28 C29 136.88(14) . . . . ? N5 C28 C29 C30 -28.52(18) . . . . ? C31 N6 C30 O10 13.2(3) . . . . ? N5 N6 C30 O10 175.22(15) . . . . ? C31 N6 C30 C29 -166.57(17) . . . . ? N5 N6 C30 C29 -4.59(18) . . . . ? C28 C29 C30 O10 -159.25(18) . . . . ? C28 C29 C30 N6 20.55(18) . . . . ? C30 N6 C31 C33 -42.8(3) . . . . ? N5 N6 C31 C33 154.97(16) . . . . ? C30 N6 C31 C32 144.43(18) . . . . ? N5 N6 C31 C32 -17.84(18) . . . . ? C33 C31 C32 C27 -176.65(17) . . . . ? N6 C31 C32 C27 -4.19(18) . . . . ? N5 C27 C32 C31 23.53(17) . . . . ? C24 C27 C32 C31 144.92(14) . . . . ? N6 C31 C33 C34 173.65(15) . . . . ? C32 C31 C33 C34 -15.2(3) . . . . ? N6 C31 C33 C37 -10.0(3) . . . . ? C32 C31 C33 C37 161.15(17) . . . . ? C35 O12 C34 O11 -11.0(3) . . . . ? C35 O12 C34 C33 168.29(15) . . . . ? C31 C33 C34 O11 -14.4(3) . . . . ? C37 C33 C34 O11 168.96(18) . . . . ? C31 C33 C34 O12 166.35(15) . . . . ? C37 C33 C34 O12 -10.3(2) . . . . ? C34 O12 C35 C36 -98.96(19) . . . . ? C31 C33 C37 C38 117.5(2) . . . . ? C34 C33 C37 C38 -66.1(2) . . . . ? C33 C37 C38 O13 -5.7(3) . . . . ? C33 C37 C38 O14' 160.2(6) . . . . ? C33 C37 C38 O14 -176.9(4) . . . . ? O13 C38 O14 C39 13.3(8) . . . . ? O14' C38 O14 C39 -72.2(16) . . . . ? C37 C38 O14 C39 -175.4(5) . . . . ? C38 O14 C39 C40 94.6(14) . . . . ? O13 C38 O14' C39' -11.6(9) . . . . ? O14 C38 O14' C39' 97(2) . . . . ? C37 C38 O14' C39' -178.3(6) . . . . ? C38 O14' C39' C40' 172.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.423 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.047