# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Lyle Isaacs' _publ_contact_author_address ; Building 091 College Park Maryland United States MD 20742 ; _publ_contact_author_email LIsaacs@umd.edu loop_ _publ_author_name 'Li-Ping Cao.' 'Xiang-Gao Meng.' 'Jiao-Yang Ding.' 'Yunfeng Chen.' ; Meng Gao ; 'Yan-Dong Wu.' 'Yi-Tao Li.' 'An-Xin Wu.' L.Isaacs # Attachment '3-new.cif.txt' data_051212cm _database_code_depnum_ccdc_archive 'CCDC 756893' #TrackingRef '3-new.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H37 N5 O9, 1.16 (C H4 O)' _chemical_formula_sum 'C39.16 H41.64 N5 O10.16' _chemical_formula_weight 744.9071 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9808(16) _cell_length_b 12.1396(19) _cell_length_c 32.044(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.151(3) _cell_angle_gamma 90.00 _cell_volume 3852.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 5536 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 20.35 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1570 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9726 _exptl_absorpt_correction_T_max 0.9912 _exptl_absorpt_process_details 'SADABS, (Sheldrick,1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28041 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7122 _reflns_number_gt 4735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+1.3831P] 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 7122 _refine_ls_number_parameters 551 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.1846 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.048 _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 C1 C 0.3408(5) 0.2507(3) 0.15826(14) 0.0999(14) Uani 1 1 d . . . H1A H 0.2657 0.2009 0.1535 0.150 Uiso 1 1 calc R . . H1B H 0.4111 0.2177 0.1774 0.150 Uiso 1 1 calc R . . H1C H 0.3743 0.2662 0.1321 0.150 Uiso 1 1 calc R . . C2 C -0.1738(5) 0.5775(4) 0.05322(12) 0.1009(14) Uani 1 1 d . . . H2A H -0.1054 0.5796 0.0346 0.151 Uiso 1 1 calc R . . H2B H -0.2423 0.6310 0.0444 0.151 Uiso 1 1 calc R . . H2C H -0.2134 0.5054 0.0525 0.151 Uiso 1 1 calc R . . C3 C 0.1434(3) 0.4949(2) 0.17478(9) 0.0461(7) Uani 1 1 d . . . C4 C 0.1968(3) 0.4090(2) 0.15299(9) 0.0536(7) Uani 1 1 d . . . C5 C 0.1473(4) 0.3884(3) 0.11183(11) 0.0712(9) Uani 1 1 d . . . H5 H 0.1840 0.3316 0.0974 0.085 Uiso 1 1 calc R . . C6 C 0.0438(4) 0.4511(3) 0.09160(11) 0.0717(10) Uani 1 1 d . . . H6 H 0.0104 0.4357 0.0638 0.086 Uiso 1 1 calc R . . C7 C -0.0105(3) 0.5364(3) 0.11233(10) 0.0568(8) Uani 1 1 d . . . C8 C 0.0411(3) 0.5595(2) 0.15400(8) 0.0472(7) Uani 1 1 d . . . C9 C 0.1942(3) 0.5138(2) 0.22061(8) 0.0472(7) Uani 1 1 d . . . H9A H 0.1207 0.5009 0.2372 0.057 Uiso 1 1 calc R . . H9B H 0.2644 0.4604 0.2293 0.057 Uiso 1 1 calc R . . C10 C -0.0224(3) 0.6526(2) 0.17654(9) 0.0516(7) Uani 1 1 d . . . H10A H -0.0919 0.6870 0.1570 0.062 Uiso 1 1 calc R . . H10B H -0.0660 0.6215 0.1993 0.062 Uiso 1 1 calc R . . C11 C 0.3811(3) 0.6509(2) 0.23346(7) 0.0392(6) Uani 1 1 d . A . C12 C 0.1219(3) 0.8155(2) 0.16929(8) 0.0426(6) Uani 1 1 d . A . C13 C 0.1611(3) 0.7178(2) 0.23179(8) 0.0421(6) Uani 1 1 d . . . C14 C 0.0807(3) 0.7132(3) 0.26983(9) 0.0574(8) Uani 1 1 d D . . C15 C 0.0657(18) 0.6288(15) 0.3359(4) 0.107(5) Uani 0.52 1 d PD A 1 H15A H 0.0168 0.5597 0.3355 0.129 Uiso 0.52 1 calc PR A 1 H15B H 0.0036 0.6890 0.3388 0.129 Uiso 0.52 1 calc PR A 1 C16 C 0.1845(17) 0.6306(19) 0.3715(5) 0.161(6) Uani 0.52 1 d PD A 1 H16A H 0.2491 0.5753 0.3663 0.241 Uiso 0.52 1 calc PR A 1 H16B H 0.1516 0.6158 0.3979 0.241 Uiso 0.52 1 calc PR A 1 H16C H 0.2267 0.7017 0.3726 0.241 Uiso 0.52 1 calc PR A 1 O6 O 0.1317(12) 0.6415(8) 0.2979(3) 0.077(3) Uani 0.52 1 d PD A 1 O5 O -0.0143(11) 0.7706(13) 0.2745(5) 0.097(5) Uani 0.52 1 d PD A 1 C15' C 0.101(2) 0.6767(13) 0.3423(4) 0.093(5) Uani 0.48 1 d PD A 2 H15C H 0.0056 0.6948 0.3372 0.112 Uiso 0.48 1 calc PR A 2 H15D H 0.1447 0.7286 0.3627 0.112 Uiso 0.48 1 calc PR A 2 C16' C 0.119(3) 0.5606(14) 0.3589(9) 0.188(9) Uani 0.48 1 d PD A 2 H16D H 0.0670 0.5109 0.3401 0.282 Uiso 0.48 1 calc PR A 2 H16E H 0.0900 0.5564 0.3863 0.282 Uiso 0.48 1 calc PR A 2 H16F H 0.2131 0.5407 0.3608 0.282 Uiso 0.48 1 calc PR A 2 O5' O -0.0369(9) 0.7375(16) 0.2661(6) 0.093(4) Uani 0.48 1 d PD A 2 O6' O 0.1615(12) 0.6824(9) 0.3032(3) 0.073(3) Uani 0.48 1 d PD A 2 C17 C 0.2636(3) 0.8166(2) 0.23318(8) 0.0414(6) Uani 1 1 d . . . C18 C 0.2448(3) 0.9039(3) 0.26694(10) 0.0556(7) Uani 1 1 d D A . C19 C 0.3164(9) 0.9859(7) 0.3305(2) 0.0503(17) Uani 0.51 1 d PD A 1 H19A H 0.2258 0.9854 0.3385 0.060 Uiso 0.51 1 calc PR A 1 H19B H 0.3344 1.0580 0.3194 0.060 Uiso 0.51 1 calc PR A 1 C20 C 0.4187(19) 0.9577(15) 0.3673(5) 0.126(8) Uani 0.51 1 d PD A 1 H20A H 0.4127 0.8806 0.3735 0.190 Uiso 0.51 1 calc PR A 1 H20B H 0.4012 1.0001 0.3913 0.190 Uiso 0.51 1 calc PR A 1 H20C H 0.5076 0.9742 0.3606 0.190 Uiso 0.51 1 calc PR A 1 O7 O 0.1482(12) 0.9637(10) 0.2630(8) 0.078(4) Uani 0.51 1 d PD A 1 O8 O 0.3320(12) 0.9001(9) 0.2996(3) 0.054(2) Uani 0.51 1 d PD A 1 C19' C 0.2919(12) 0.9273(11) 0.3429(3) 0.099(3) Uani 0.49 1 d PD A 2 H19C H 0.2856 0.8746 0.3653 0.119 Uiso 0.49 1 calc PR A 2 H19D H 0.2096 0.9706 0.3393 0.119 Uiso 0.49 1 calc PR A 2 C20' C 0.411(2) 1.0015(15) 0.3543(7) 0.121(6) Uani 0.49 1 d PD A 2 H20D H 0.4927 0.9591 0.3559 0.181 Uiso 0.49 1 calc PR A 2 H20E H 0.4045 1.0352 0.3811 0.181 Uiso 0.49 1 calc PR A 2 H20F H 0.4122 1.0576 0.3333 0.181 Uiso 0.49 1 calc PR A 2 O7' O 0.1855(13) 0.9889(10) 0.2585(8) 0.072(3) Uani 0.49 1 d PD A 2 O8' O 0.3071(15) 0.8686(10) 0.3036(3) 0.085(5) Uani 0.49 1 d PD A 2 C21 C 0.5148(3) 0.8231(2) 0.23278(9) 0.0475(7) Uani 1 1 d . . . H21A H 0.5926 0.7824 0.2459 0.057 Uiso 1 1 calc R A . H21B H 0.5138 0.8937 0.2469 0.057 Uiso 1 1 calc R . . C22 C 0.3134(3) 0.9481(2) 0.17599(9) 0.0517(7) Uani 1 1 d . . . H22A H 0.3395 1.0016 0.1980 0.062 Uiso 1 1 calc R A . H22B H 0.2602 0.9863 0.1530 0.062 Uiso 1 1 calc R . . C23 C 0.4383(3) 0.9034(2) 0.16062(9) 0.0497(7) Uani 1 1 d . A . C24 C 0.5322(3) 0.8433(2) 0.18713(9) 0.0521(7) Uani 1 1 d . A . C25 C 0.6473(3) 0.8041(3) 0.17230(12) 0.0740(10) Uani 1 1 d . . . H25 H 0.7109 0.7650 0.1902 0.089 Uiso 1 1 calc R A . C26 C 0.6686(4) 0.8223(4) 0.13140(14) 0.1015(14) Uani 1 1 d . A . H26 H 0.7469 0.7958 0.1219 0.122 Uiso 1 1 calc R . . C27 C 0.5768(4) 0.8786(4) 0.10447(13) 0.0887(12) Uani 1 1 d . . . H27 H 0.5910 0.8884 0.0766 0.106 Uiso 1 1 calc R A . C28 C 0.4616(3) 0.9215(3) 0.11880(10) 0.0657(9) Uani 1 1 d . A . C29 C 0.3652(4) 0.9790(3) 0.08974(11) 0.0674(9) Uani 1 1 d . . . C30 C 0.2868(4) 1.0241(3) 0.06491(11) 0.0718(9) Uani 1 1 d . A . C31 C 0.1872(4) 1.0800(3) 0.03551(10) 0.0642(8) Uani 1 1 d . . . C32 C 0.1872(4) 1.0725(3) -0.00764(11) 0.0750(10) Uani 1 1 d . A . H32 H 0.2534 1.0311 -0.0184 0.090 Uiso 1 1 calc R . . C33 C 0.0860(4) 1.1410(3) 0.04986(11) 0.0758(10) Uani 1 1 d . A . H33 H 0.0828 1.1459 0.0787 0.091 Uiso 1 1 calc R . . C34 C 0.0917(4) 1.1248(3) -0.03458(10) 0.0717(10) Uani 1 1 d . . . H34 H 0.0938 1.1186 -0.0634 0.086 Uiso 1 1 calc R A . C35 C -0.0099(4) 1.1944(3) 0.02323(10) 0.0719(9) Uani 1 1 d . . . H35 H -0.0761 1.2358 0.0340 0.086 Uiso 1 1 calc R A . C36 C -0.0088(3) 1.1871(3) -0.01971(9) 0.0581(8) Uani 1 1 d . A . C37 C -0.2012(4) 1.3112(3) -0.04365(13) 0.0774(10) Uani 1 1 d . A . C38 C -0.2943(4) 1.3407(3) -0.08152(14) 0.0899(12) Uani 1 1 d . . . H38A H -0.3809 1.3077 -0.0799 0.135 Uiso 1 1 calc R . . H38B H -0.2586 1.3141 -0.1061 0.135 Uiso 1 1 calc R . . H38C H -0.3038 1.4193 -0.0832 0.135 Uiso 1 1 calc R . . N1 N 0.2478(2) 0.62389(16) 0.22978(7) 0.0403(5) Uani 1 1 d . . . N2 N 0.0718(2) 0.73712(18) 0.19382(7) 0.0449(5) Uani 1 1 d . . . N3 N 0.3930(2) 0.76277(16) 0.23938(6) 0.0396(5) Uani 1 1 d . A . N4 N 0.2301(2) 0.86384(17) 0.19222(7) 0.0442(5) Uani 1 1 d . A . N5 N -0.1065(3) 1.2352(2) -0.04942(8) 0.0678(7) Uani 1 1 d . . . H5A H -0.1060 1.2132 -0.0749 0.081 Uiso 1 1 calc R A . O1 O 0.2988(2) 0.34883(17) 0.17554(7) 0.0693(6) Uani 1 1 d . . . O2 O -0.1149(2) 0.6018(2) 0.09479(7) 0.0766(7) Uani 1 1 d . . . O3 O 0.47484(19) 0.58801(15) 0.23279(6) 0.0543(5) Uani 1 1 d . . . O4 O 0.0760(2) 0.83903(17) 0.13353(6) 0.0603(6) Uani 1 1 d . . . O9 O -0.2078(4) 1.3530(3) -0.00978(11) 0.1312(13) Uani 1 1 d . . . 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 C1 0.116(3) 0.063(2) 0.116(3) -0.024(2) -0.005(3) 0.025(2) C2 0.107(3) 0.106(3) 0.077(3) 0.004(2) -0.039(2) -0.007(3) C3 0.0431(15) 0.0367(15) 0.0581(16) 0.0000(12) 0.0044(13) -0.0099(12) C4 0.0568(18) 0.0414(16) 0.0624(18) -0.0065(14) 0.0064(15) -0.0054(14) C5 0.086(3) 0.056(2) 0.072(2) -0.0174(17) 0.0107(19) -0.0035(19) C6 0.086(3) 0.067(2) 0.0579(19) -0.0115(17) -0.0080(18) -0.011(2) C7 0.0526(18) 0.0525(18) 0.0628(19) -0.0016(15) -0.0033(15) -0.0097(15) C8 0.0428(15) 0.0444(16) 0.0523(16) -0.0015(12) -0.0025(13) -0.0096(13) C9 0.0501(16) 0.0348(14) 0.0564(16) 0.0033(12) 0.0048(13) -0.0008(13) C10 0.0377(15) 0.0508(17) 0.0642(18) -0.0003(14) -0.0024(13) -0.0017(13) C11 0.0430(15) 0.0352(14) 0.0389(13) 0.0013(10) 0.0033(11) 0.0061(13) C12 0.0416(15) 0.0407(15) 0.0443(15) -0.0019(12) 0.0001(12) 0.0108(12) C13 0.0416(15) 0.0386(14) 0.0459(14) 0.0003(11) 0.0049(12) 0.0045(12) C14 0.059(2) 0.056(2) 0.0588(19) -0.0047(15) 0.0143(16) 0.0025(16) C15 0.129(14) 0.118(14) 0.083(8) 0.012(8) 0.046(8) 0.008(10) C16 0.181(16) 0.222(19) 0.085(8) 0.027(11) 0.041(10) 0.043(14) O6 0.080(6) 0.097(7) 0.057(4) 0.023(5) 0.020(3) 0.005(5) O5 0.111(8) 0.111(9) 0.076(6) -0.002(6) 0.035(5) 0.047(7) C15' 0.107(10) 0.116(13) 0.061(7) 0.014(7) 0.026(7) -0.009(8) C16' 0.24(2) 0.169(18) 0.18(2) 0.058(16) 0.107(17) -0.016(16) O5' 0.060(5) 0.124(10) 0.101(9) -0.024(6) 0.040(4) 0.022(5) O6' 0.083(6) 0.091(7) 0.047(4) 0.008(4) 0.020(3) 0.000(5) C17 0.0439(15) 0.0347(14) 0.0443(14) -0.0030(11) 0.0009(11) 0.0039(12) C18 0.0515(19) 0.051(2) 0.063(2) -0.0127(15) -0.0014(15) 0.0065(16) C19 0.055(4) 0.047(4) 0.049(4) -0.021(3) 0.003(3) -0.002(4) C20 0.125(12) 0.145(16) 0.095(11) -0.063(11) -0.044(10) 0.053(11) O7 0.066(6) 0.066(6) 0.101(9) -0.033(6) 0.002(6) 0.020(5) O8 0.051(4) 0.055(4) 0.053(4) -0.017(3) -0.010(3) 0.007(3) C19' 0.114(9) 0.095(8) 0.087(7) -0.026(6) 0.012(6) 0.006(7) C20' 0.155(18) 0.093(11) 0.121(15) -0.027(8) 0.047(13) -0.011(11) O7' 0.079(7) 0.049(5) 0.088(5) -0.016(5) 0.014(7) 0.025(6) O8' 0.088(7) 0.108(10) 0.057(4) -0.037(5) 0.003(4) 0.015(6) C21 0.0404(15) 0.0394(15) 0.0601(17) -0.0016(12) -0.0045(13) 0.0004(12) C22 0.0554(18) 0.0351(15) 0.0624(17) 0.0077(12) -0.0016(14) 0.0014(13) C23 0.0448(16) 0.0377(15) 0.0658(18) 0.0092(13) 0.0033(14) -0.0041(13) C24 0.0479(17) 0.0427(16) 0.0663(18) 0.0035(13) 0.0092(14) -0.0052(13) C25 0.056(2) 0.082(2) 0.086(2) 0.0217(19) 0.0185(18) 0.0179(18) C26 0.084(3) 0.121(4) 0.108(3) 0.039(3) 0.044(3) 0.033(3) C27 0.088(3) 0.104(3) 0.080(2) 0.030(2) 0.034(2) 0.014(2) C28 0.066(2) 0.064(2) 0.067(2) 0.0153(16) 0.0095(17) -0.0051(17) C29 0.073(2) 0.068(2) 0.062(2) 0.0202(17) 0.0085(18) -0.0075(18) C30 0.080(2) 0.069(2) 0.066(2) 0.0169(18) 0.0060(19) -0.017(2) C31 0.072(2) 0.058(2) 0.061(2) 0.0076(16) 0.0022(17) -0.0123(17) C32 0.081(2) 0.081(2) 0.064(2) 0.0146(18) 0.0105(18) 0.013(2) C33 0.091(3) 0.086(3) 0.0491(19) 0.0034(17) 0.0036(19) -0.010(2) C34 0.082(2) 0.085(2) 0.0473(17) 0.0079(16) 0.0077(17) 0.012(2) C35 0.082(2) 0.076(2) 0.058(2) -0.0068(17) 0.0108(18) 0.003(2) C36 0.064(2) 0.0554(18) 0.0532(18) 0.0015(14) 0.0020(15) -0.0064(16) C37 0.083(3) 0.072(2) 0.077(3) 0.000(2) 0.008(2) 0.005(2) C38 0.073(2) 0.080(3) 0.114(3) 0.005(2) 0.000(2) 0.006(2) N1 0.0389(12) 0.0308(11) 0.0503(12) -0.0016(9) 0.0013(10) 0.0014(9) N2 0.0394(12) 0.0414(13) 0.0511(13) 0.0031(10) -0.0049(10) 0.0021(10) N3 0.0372(12) 0.0315(11) 0.0489(12) -0.0014(9) 0.0006(9) 0.0036(9) N4 0.0445(13) 0.0360(12) 0.0505(13) 0.0048(10) -0.0010(10) 0.0006(10) N5 0.0739(18) 0.0695(18) 0.0585(16) -0.0024(13) 0.0027(14) 0.0060(15) O1 0.0752(15) 0.0475(13) 0.0826(15) -0.0123(11) -0.0011(12) 0.0160(11) O2 0.0729(15) 0.0773(16) 0.0705(14) -0.0032(12) -0.0270(12) -0.0010(13) O3 0.0453(11) 0.0373(10) 0.0788(14) 0.0024(9) 0.0023(10) 0.0105(9) O4 0.0645(13) 0.0629(13) 0.0493(12) 0.0070(10) -0.0098(10) 0.0060(11) O9 0.152(3) 0.135(3) 0.104(2) -0.025(2) 0.006(2) 0.061(2) _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 O1 1.400(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O2 1.418(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C8 1.390(4) . ? C3 C4 1.397(4) . ? C3 C9 1.510(4) . ? C4 C5 1.373(4) . ? C4 O1 1.382(4) . ? C5 C6 1.378(5) . ? C5 H5 0.9300 . ? C6 C7 1.377(5) . ? C6 H6 0.9300 . ? C7 O2 1.374(4) . ? C7 C8 1.398(4) . ? C8 C10 1.521(4) . ? C9 N1 1.456(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.454(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O3 1.210(3) . ? C11 N1 1.361(3) . ? C11 N3 1.374(3) . ? C12 O4 1.214(3) . ? C12 N4 1.361(3) . ? C12 N2 1.367(3) . ? C13 N2 1.435(3) . ? C13 N1 1.437(3) . ? C13 C14 1.541(4) . ? C13 C17 1.574(4) . ? C14 O5 1.201(8) . ? C14 O5' 1.201(8) . ? C14 O6 1.308(8) . ? C14 O6' 1.312(8) . ? C15 O6 1.463(8) . ? C15 C16 1.541(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C15' O6' 1.459(8) . ? C15' C16' 1.509(10) . ? C15' H15C 0.9700 . ? C15' H15D 0.9700 . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17 N4 1.433(3) . ? C17 N3 1.439(3) . ? C17 C18 1.542(4) . ? C18 O7 1.201(8) . ? C18 O7' 1.204(8) . ? C18 O8 1.277(9) . ? C18 O8' 1.331(11) . ? C19 O8 1.458(8) . ? C19 C20 1.500(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C19' O8' 1.470(8) . ? C19' C20' 1.500(10) . ? C19' H19C 0.9700 . ? C19' H19D 0.9700 . ? C20' H20D 0.9600 . ? C20' H20E 0.9600 . ? C20' H20F 0.9600 . ? C21 N3 1.457(3) . ? C21 C24 1.514(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N4 1.455(3) . ? C22 C23 1.498(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.391(4) . ? C23 C28 1.405(4) . ? C24 C25 1.382(4) . ? C25 C26 1.372(5) . ? C25 H25 0.9300 . ? C26 C27 1.363(5) . ? C26 H26 0.9300 . ? C27 C28 1.391(5) . ? C27 H27 0.9300 . ? C28 C29 1.434(5) . ? C29 C30 1.179(5) . ? C30 C31 1.450(5) . ? C31 C33 1.377(5) . ? C31 C32 1.386(4) . ? C32 C34 1.361(5) . ? C32 H32 0.9300 . ? C33 C35 1.364(5) . ? C33 H33 0.9300 . ? C34 C36 1.388(5) . ? C34 H34 0.9300 . ? C35 C36 1.380(4) . ? C35 H35 0.9300 . ? C36 N5 1.402(4) . ? C37 O9 1.207(4) . ? C37 N5 1.350(5) . ? C37 C38 1.477(5) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? N5 H5A 0.8600 . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C8 C3 C4 119.0(3) . . ? C8 C3 C9 121.2(2) . . ? C4 C3 C9 119.7(3) . . ? C5 C4 O1 124.1(3) . . ? C5 C4 C3 120.1(3) . . ? O1 C4 C3 115.8(3) . . ? C4 C5 C6 120.7(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C7 C6 C5 120.3(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O2 C7 C6 124.1(3) . . ? O2 C7 C8 116.4(3) . . ? C6 C7 C8 119.4(3) . . ? C3 C8 C7 120.3(3) . . ? C3 C8 C10 121.1(2) . . ? C7 C8 C10 118.5(3) . . ? N1 C9 C3 114.0(2) . . ? N1 C9 H9A 108.8 . . ? C3 C9 H9A 108.8 . . ? N1 C9 H9B 108.8 . . ? C3 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N2 C10 C8 114.7(2) . . ? N2 C10 H10A 108.6 . . ? C8 C10 H10A 108.6 . . ? N2 C10 H10B 108.6 . . ? C8 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? O3 C11 N1 126.6(2) . . ? O3 C11 N3 124.9(2) . . ? N1 C11 N3 108.5(2) . . ? O4 C12 N4 126.0(3) . . ? O4 C12 N2 125.7(3) . . ? N4 C12 N2 108.2(2) . . ? N2 C13 N1 113.9(2) . . ? N2 C13 C14 110.3(2) . . ? N1 C13 C14 112.5(2) . . ? N2 C13 C17 103.4(2) . . ? N1 C13 C17 102.28(19) . . ? C14 C13 C17 113.9(2) . . ? O5 C14 O6 123.1(11) . . ? O5' C14 O6 121.6(13) . . ? O5 C14 O6' 118.6(11) . . ? O5' C14 O6' 130.1(12) . . ? O5 C14 C13 125.1(10) . . ? O5' C14 C13 120.7(10) . . ? O6 C14 C13 111.8(7) . . ? O6' C14 C13 109.2(7) . . ? O6 C15 C16 103.3(12) . . ? O6 C15 H15A 111.1 . . ? C16 C15 H15A 111.1 . . ? O6 C15 H15B 111.1 . . ? C16 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? C14 O6 C15 117.7(11) . . ? O6' C15' C16' 107.5(13) . . ? O6' C15' H15C 110.2 . . ? C16' C15' H15C 110.2 . . ? O6' C15' H15D 110.2 . . ? C16' C15' H15D 110.2 . . ? H15C C15' H15D 108.5 . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C14 O6' C15' 115.8(12) . . ? N4 C17 N3 114.3(2) . . ? N4 C17 C18 109.5(2) . . ? N3 C17 C18 113.6(2) . . ? N4 C17 C13 101.68(19) . . ? N3 C17 C13 103.10(19) . . ? C18 C17 C13 114.1(2) . . ? O7 C18 O8 124.4(14) . . ? O7' C18 O8 118.8(13) . . ? O7 C18 O8' 124.7(14) . . ? O7' C18 O8' 129.6(14) . . ? O7 C18 C17 120.5(13) . . ? O7' C18 C17 122.0(13) . . ? O8 C18 C17 114.9(5) . . ? O8' C18 C17 108.3(5) . . ? O8 C19 C20 104.5(10) . . ? O8 C19 H19A 110.9 . . ? C20 C19 H19A 110.9 . . ? O8 C19 H19B 110.9 . . ? C20 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? C18 O8 C19 114.3(8) . . ? O8' C19' C20' 109.6(14) . . ? O8' C19' H19C 109.7 . . ? C20' C19' H19C 109.7 . . ? O8' C19' H19D 109.7 . . ? C20' C19' H19D 109.7 . . ? H19C C19' H19D 108.2 . . ? C19' C20' H20D 109.5 . . ? C19' C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? C19' C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? C18 O8' C19' 120.9(11) . . ? N3 C21 C24 114.8(2) . . ? N3 C21 H21A 108.6 . . ? C24 C21 H21A 108.6 . . ? N3 C21 H21B 108.6 . . ? C24 C21 H21B 108.6 . . ? H21A C21 H21B 107.5 . . ? N4 C22 C23 113.5(2) . . ? N4 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? N4 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C28 119.0(3) . . ? C24 C23 C22 120.9(3) . . ? C28 C23 C22 120.0(3) . . ? C25 C24 C23 119.8(3) . . ? C25 C24 C21 118.5(3) . . ? C23 C24 C21 121.7(3) . . ? C26 C25 C24 120.5(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C27 C26 C25 120.9(4) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 119.8(3) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C23 119.9(3) . . ? C27 C28 C29 118.9(3) . . ? C23 C28 C29 121.2(3) . . ? C30 C29 C28 178.0(4) . . ? C29 C30 C31 178.0(4) . . ? C33 C31 C32 117.3(3) . . ? C33 C31 C30 120.4(3) . . ? C32 C31 C30 122.2(3) . . ? C34 C32 C31 121.0(3) . . ? C34 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C35 C33 C31 122.2(3) . . ? C35 C33 H33 118.9 . . ? C31 C33 H33 118.9 . . ? C32 C34 C36 121.1(3) . . ? C32 C34 H34 119.5 . . ? C36 C34 H34 119.5 . . ? C33 C35 C36 120.1(3) . . ? C33 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C34 118.2(3) . . ? C35 C36 N5 124.0(3) . . ? C34 C36 N5 117.7(3) . . ? O9 C37 N5 121.9(4) . . ? O9 C37 C38 122.5(4) . . ? N5 C37 C38 115.6(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C11 N1 C13 113.1(2) . . ? C11 N1 C9 124.7(2) . . ? C13 N1 C9 121.9(2) . . ? C12 N2 C13 111.6(2) . . ? C12 N2 C10 122.5(2) . . ? C13 N2 C10 120.7(2) . . ? C11 N3 C17 111.7(2) . . ? C11 N3 C21 122.4(2) . . ? C17 N3 C21 120.1(2) . . ? C12 N4 C17 113.6(2) . . ? C12 N4 C22 124.1(2) . . ? C17 N4 C22 122.0(2) . . ? C37 N5 C36 129.1(3) . . ? C37 N5 H5A 115.4 . . ? C36 N5 H5A 115.4 . . ? C4 O1 C1 118.7(3) . . ? C7 O2 C2 117.9(3) . . ? 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 C8 C3 C4 C5 -0.8(4) . . . . ? C9 C3 C4 C5 177.4(3) . . . . ? C8 C3 C4 O1 179.5(2) . . . . ? C9 C3 C4 O1 -2.4(4) . . . . ? O1 C4 C5 C6 179.0(3) . . . . ? C3 C4 C5 C6 -0.7(5) . . . . ? C4 C5 C6 C7 0.8(5) . . . . ? C5 C6 C7 O2 -179.0(3) . . . . ? C5 C6 C7 C8 0.5(5) . . . . ? C4 C3 C8 C7 2.1(4) . . . . ? C9 C3 C8 C7 -176.0(2) . . . . ? C4 C3 C8 C10 178.8(2) . . . . ? C9 C3 C8 C10 0.7(4) . . . . ? O2 C7 C8 C3 177.6(2) . . . . ? C6 C7 C8 C3 -2.0(4) . . . . ? O2 C7 C8 C10 0.8(4) . . . . ? C6 C7 C8 C10 -178.8(3) . . . . ? C8 C3 C9 N1 -59.0(3) . . . . ? C4 C3 C9 N1 122.9(3) . . . . ? C3 C8 C10 N2 59.0(3) . . . . ? C7 C8 C10 N2 -124.3(3) . . . . ? N2 C13 C14 O5 -38.0(10) . . . . ? N1 C13 C14 O5 -166.4(10) . . . . ? C17 C13 C14 O5 77.8(10) . . . . ? N2 C13 C14 O5' -8.6(11) . . . . ? N1 C13 C14 O5' -137.0(11) . . . . ? C17 C13 C14 O5' 107.2(11) . . . . ? N2 C13 C14 O6 144.7(5) . . . . ? N1 C13 C14 O6 16.3(6) . . . . ? C17 C13 C14 O6 -99.6(5) . . . . ? N2 C13 C14 O6' 172.5(5) . . . . ? N1 C13 C14 O6' 44.1(6) . . . . ? C17 C13 C14 O6' -71.8(6) . . . . ? O5 C14 O6 C15 2.4(16) . . . . ? O5' C14 O6 C15 -27.2(15) . . . . ? O6' C14 O6 C15 90(3) . . . . ? C13 C14 O6 C15 179.8(9) . . . . ? C16 C15 O6 C14 -133.3(14) . . . . ? O5 C14 O6' C15' 26.7(16) . . . . ? O5' C14 O6' C15' -0.3(18) . . . . ? O6 C14 O6' C15' -81(3) . . . . ? C13 C14 O6' C15' 178.5(9) . . . . ? C16' C15' O6' C14 122.2(17) . . . . ? N2 C13 C17 N4 -9.9(2) . . . . ? N1 C13 C17 N4 108.6(2) . . . . ? C14 C13 C17 N4 -129.7(2) . . . . ? N2 C13 C17 N3 -128.5(2) . . . . ? N1 C13 C17 N3 -10.0(2) . . . . ? C14 C13 C17 N3 111.7(2) . . . . ? N2 C13 C17 C18 107.8(2) . . . . ? N1 C13 C17 C18 -133.7(2) . . . . ? C14 C13 C17 C18 -12.0(3) . . . . ? N4 C17 C18 O7 42.4(9) . . . . ? N3 C17 C18 O7 171.5(8) . . . . ? C13 C17 C18 O7 -70.8(9) . . . . ? N4 C17 C18 O7' 13.3(8) . . . . ? N3 C17 C18 O7' 142.4(8) . . . . ? C13 C17 C18 O7' -99.8(8) . . . . ? N4 C17 C18 O8 -143.0(7) . . . . ? N3 C17 C18 O8 -13.9(7) . . . . ? C13 C17 C18 O8 103.9(7) . . . . ? N4 C17 C18 O8' -164.7(7) . . . . ? N3 C17 C18 O8' -35.6(8) . . . . ? C13 C17 C18 O8' 82.2(7) . . . . ? O7 C18 O8 C19 -8.1(16) . . . . ? O7' C18 O8 C19 20.4(16) . . . . ? O8' C18 O8 C19 -106(3) . . . . ? C17 C18 O8 C19 177.5(7) . . . . ? C20 C19 O8 C18 174.2(12) . . . . ? O7 C18 O8' C19' -20.3(18) . . . . ? O7' C18 O8' C19' 10.3(19) . . . . ? O8 C18 O8' C19' 76(2) . . . . ? C17 C18 O8' C19' -171.9(10) . . . . ? C20' C19' O8' C18 -98.5(16) . . . . ? N4 C22 C23 C24 -57.6(4) . . . . ? N4 C22 C23 C28 122.0(3) . . . . ? C28 C23 C24 C25 1.2(4) . . . . ? C22 C23 C24 C25 -179.2(3) . . . . ? C28 C23 C24 C21 178.6(3) . . . . ? C22 C23 C24 C21 -1.8(4) . . . . ? N3 C21 C24 C25 -121.9(3) . . . . ? N3 C21 C24 C23 60.7(3) . . . . ? C23 C24 C25 C26 -1.2(5) . . . . ? C21 C24 C25 C26 -178.7(4) . . . . ? C24 C25 C26 C27 -0.4(7) . . . . ? C25 C26 C27 C28 2.0(7) . . . . ? C26 C27 C28 C23 -2.0(6) . . . . ? C26 C27 C28 C29 -179.0(4) . . . . ? C24 C23 C28 C27 0.5(5) . . . . ? C22 C23 C28 C27 -179.2(3) . . . . ? C24 C23 C28 C29 177.4(3) . . . . ? C22 C23 C28 C29 -2.2(5) . . . . ? C33 C31 C32 C34 0.9(5) . . . . ? C30 C31 C32 C34 179.2(3) . . . . ? C32 C31 C33 C35 -1.4(5) . . . . ? C30 C31 C33 C35 -179.7(3) . . . . ? C31 C32 C34 C36 -0.1(6) . . . . ? C31 C33 C35 C36 1.0(6) . . . . ? C33 C35 C36 C34 -0.1(5) . . . . ? C33 C35 C36 N5 177.1(3) . . . . ? C32 C34 C36 C35 -0.3(5) . . . . ? C32 C34 C36 N5 -177.7(3) . . . . ? O3 C11 N1 C13 -180.0(2) . . . . ? N3 C11 N1 C13 1.8(3) . . . . ? O3 C11 N1 C9 -5.7(4) . . . . ? N3 C11 N1 C9 176.0(2) . . . . ? N2 C13 N1 C11 116.2(2) . . . . ? C14 C13 N1 C11 -117.3(2) . . . . ? C17 C13 N1 C11 5.4(3) . . . . ? N2 C13 N1 C9 -58.2(3) . . . . ? C14 C13 N1 C9 68.3(3) . . . . ? C17 C13 N1 C9 -169.0(2) . . . . ? C3 C9 N1 C11 -97.4(3) . . . . ? C3 C9 N1 C13 76.4(3) . . . . ? O4 C12 N2 C13 171.0(2) . . . . ? N4 C12 N2 C13 -10.3(3) . . . . ? O4 C12 N2 C10 16.2(4) . . . . ? N4 C12 N2 C10 -165.1(2) . . . . ? N1 C13 N2 C12 -97.5(3) . . . . ? C14 C13 N2 C12 134.9(2) . . . . ? C17 C13 N2 C12 12.7(3) . . . . ? N1 C13 N2 C10 57.8(3) . . . . ? C14 C13 N2 C10 -69.9(3) . . . . ? C17 C13 N2 C10 167.9(2) . . . . ? C8 C10 N2 C12 76.1(3) . . . . ? C8 C10 N2 C13 -76.4(3) . . . . ? O3 C11 N3 C17 172.5(2) . . . . ? N1 C11 N3 C17 -9.2(3) . . . . ? O3 C11 N3 C21 19.4(4) . . . . ? N1 C11 N3 C21 -162.3(2) . . . . ? N4 C17 N3 C11 -97.5(2) . . . . ? C18 C17 N3 C11 135.9(2) . . . . ? C13 C17 N3 C11 11.9(3) . . . . ? N4 C17 N3 C21 56.4(3) . . . . ? C18 C17 N3 C21 -70.2(3) . . . . ? C13 C17 N3 C21 165.8(2) . . . . ? C24 C21 N3 C11 76.4(3) . . . . ? C24 C21 N3 C17 -74.6(3) . . . . ? O4 C12 N4 C17 -178.3(2) . . . . ? N2 C12 N4 C17 3.0(3) . . . . ? O4 C12 N4 C22 -4.0(4) . . . . ? N2 C12 N4 C22 177.3(2) . . . . ? N3 C17 N4 C12 114.9(2) . . . . ? C18 C17 N4 C12 -116.4(2) . . . . ? C13 C17 N4 C12 4.6(3) . . . . ? N3 C17 N4 C22 -59.5(3) . . . . ? C18 C17 N4 C22 69.2(3) . . . . ? C13 C17 N4 C22 -169.8(2) . . . . ? C23 C22 N4 C12 -96.0(3) . . . . ? C23 C22 N4 C17 77.9(3) . . . . ? O9 C37 N5 C36 3.9(6) . . . . ? C38 C37 N5 C36 -176.8(3) . . . . ? C35 C36 N5 C37 13.5(5) . . . . ? C34 C36 N5 C37 -169.3(3) . . . . ? C5 C4 O1 C1 -10.5(5) . . . . ? C3 C4 O1 C1 169.2(3) . . . . ? C6 C7 O2 C2 2.4(5) . . . . ? C8 C7 O2 C2 -177.1(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 N5 H5A O4 0.86 2.04 2.894(3) 171.9 3_575 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.209 _refine_diff_density_min -0.169 _refine_diff_density_rms 0.043 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.407 0.000 229 42 ' ' 2 0.500 0.067 0.500 229 42 ' ' _platon_squeeze_details ; During the refinement, the methanol molecules are seriously disordered. During the final refinement, the contribution of the solvent molecules to the crystal structure is treated by using the Platon/SQUEEZE procedure. Check using platon shows that there are 458\%A^3^ volumes in the unit cell (approximately 84 electrons, i.e. ca. 4.66 methanol molecules based on the solvents we have used and each host molecule was distributed 1.16 methanol molecules). So the suitable formula should be C~38~H~37~N~5~O~9~.(MeOH)~1.16~. Some related items have been corrected in the cif file. ; # start Validation Reply Form _vrf_PLAT220_051212cm ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.85 Ratio RESPONSE: This is due to the disorder of the ethyl groups. ; _vrf_PLAT222_051212cm ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.95 Ratio RESPONSE: This is due to the disorder of the ethyl groups. ; _vrf_PLAT043_051212cm ; PROBLEM: Check Reported Molecular Weight ................ 744.91 RESPONSE: This is due to the serious disorders of the methanol solvent, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000. ; _vrf_ABSMU01_051212cm ; PROBLEM: The ratio of given/expected absorption coefficient lies outside the range 0.95 <> 1.05 Calculated value of mu = 0.094 Value of mu given = 0.088 RESPONSE: This is due to the serious disorders of the methanol solvent, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000. ; _vrf_CHEMW03_051212cm ; PROBLEM: WARNING: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 744.91 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 38.00 456.42 H 1.01 37.00 37.30 N 14.01 5.00 70.04 O 16.00 9.00 143.99 Calculated formula weight 707.74 RESPONSE: This is due to the serious disorders of the methanol solvent, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000. ; _vrf_DENSD01_051212cm ; PROBLEM: The ratio of the submitted crystal density and that calculated from the formula is outside the range 0.95 <> 1.05 Crystal density given = 1.220 Calculated crystal density = 1.284 RESPONSE: This is due to the serious disorders of the methanol solvent, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000. ; _vrf_PLAT046_051212cm ; PROBLEM: Reported Z, MW and D(calc) are Inconsistent .... 1.28 RESPONSE: This is due to the serious disorders of the methanol solvent, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000. ; _vrf_PLAT242_051212cm ; PROBLEM: Check Low Ueq as Compared to Neighbors for C19 RESPONSE: This is due to the disorder of the ethyl groups. ; _vrf_PLAT068_051212cm ; PROBLEM: Reported F000 Differs from Calcd (or Missing)... ? RESPONSE: This is due to the serious disorders of the methanol solvent, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000. ; data_090618cm _database_code_depnum_ccdc_archive 'CCDC 756894' #TrackingRef '2-new.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H35 N5 O9' _chemical_formula_sum 'C35 H35 N5 O9' _chemical_formula_weight 669.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9776(9) _cell_length_b 18.8944(16) _cell_length_c 16.5449(14) _cell_angle_alpha 90.00 _cell_angle_beta 106.843(2) _cell_angle_gamma 90.00 _cell_volume 3284.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3418 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 21.39 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9743 _exptl_absorpt_correction_T_max 0.9901 _exptl_absorpt_process_details 'SADABS, Sheldrick,1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19350 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5766 _reflns_number_gt 3984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+0.3925P] 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_number_reflns 5766 _refine_ls_number_parameters 489 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.1246 _refine_ls_R_factor_gt 0.0864 _refine_ls_wR_factor_ref 0.2095 _refine_ls_wR_factor_gt 0.1888 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.153 _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 C1 C 0.8241(5) -0.1313(3) 0.9653(4) 0.120(2) Uani 1 1 d . . . H1A H 0.7844 -0.1288 1.0098 0.180 Uiso 1 1 calc R . . H1B H 0.9077 -0.1513 0.9868 0.180 Uiso 1 1 calc R . . H1C H 0.7738 -0.1605 0.9205 0.180 Uiso 1 1 calc R . . C2 C 0.2823(4) 0.0591(3) 0.7592(4) 0.122(2) Uani 1 1 d . . . H2A H 0.2739 0.0140 0.7316 0.183 Uiso 1 1 calc R . . H2B H 0.2191 0.0910 0.7264 0.183 Uiso 1 1 calc R . . H2C H 0.2709 0.0536 0.8142 0.183 Uiso 1 1 calc R . . C3 C 0.7238(4) -0.0292(2) 0.8929(3) 0.0659(11) Uani 1 1 d . . . C4 C 0.7352(3) 0.03915(19) 0.8630(2) 0.0526(9) Uani 1 1 d . . . C5 C 0.6261(3) 0.07674(19) 0.8216(2) 0.0538(9) Uani 1 1 d . . . C6 C 0.5064(3) 0.0461(2) 0.8084(3) 0.0641(11) Uani 1 1 d . . . C7 C 0.4972(4) -0.0210(2) 0.8365(3) 0.0851(15) Uani 1 1 d . . . H7 H 0.4176 -0.0419 0.8272 0.102 Uiso 1 1 calc R . . C8 C 0.6051(4) -0.0581(2) 0.8786(3) 0.0833(14) Uani 1 1 d . . . H8 H 0.5970 -0.1037 0.8977 0.100 Uiso 1 1 calc R . . C9 C 0.6332(3) 0.15220(19) 0.7930(2) 0.0543(10) Uani 1 1 d . . . H9A H 0.5479 0.1684 0.7640 0.065 Uiso 1 1 calc R . . H9B H 0.6659 0.1819 0.8423 0.065 Uiso 1 1 calc R . . C10 C 0.8674(3) 0.0722(2) 0.8835(2) 0.0572(10) Uani 1 1 d . . . H10A H 0.8721 0.1100 0.9240 0.069 Uiso 1 1 calc R . . H10B H 0.9293 0.0366 0.9108 0.069 Uiso 1 1 calc R . . C11 C 0.8489(3) 0.16393(16) 0.7697(2) 0.0407(8) Uani 1 1 d . . . C12 C 0.8900(3) 0.23032(18) 0.8261(2) 0.0486(9) Uani 1 1 d . A . C13 C 0.8596(10) 0.3561(4) 0.8236(7) 0.060(3) Uani 0.56 1 d PDU A 1 H13A H 0.9172 0.3808 0.7986 0.072 Uiso 0.56 1 calc PR A 1 H13B H 0.8969 0.3539 0.8844 0.072 Uiso 0.56 1 calc PR A 1 C14 C 0.7311(10) 0.3907(6) 0.8007(8) 0.091(3) Uani 0.56 1 d PDU A 1 H14A H 0.7021 0.3984 0.7408 0.136 Uiso 0.56 1 calc PR A 1 H14B H 0.7371 0.4353 0.8295 0.136 Uiso 0.56 1 calc PR A 1 H14C H 0.6720 0.3606 0.8172 0.136 Uiso 0.56 1 calc PR A 1 C15 C 0.8891(3) 0.16395(16) 0.6865(2) 0.0420(8) Uani 1 1 d . . . C16 C 0.9821(3) 0.22381(19) 0.6817(3) 0.0523(9) Uani 1 1 d . B . C17 C 1.1760(6) 0.2778(4) 0.7520(5) 0.087(2) Uani 0.83 1 d PDU B 1 H17A H 1.1367 0.3203 0.7660 0.104 Uiso 0.83 1 calc PR B 1 H17B H 1.2000 0.2863 0.7008 0.104 Uiso 0.83 1 calc PR B 1 C18 C 1.2905(7) 0.2571(5) 0.8237(5) 0.129(3) Uani 0.83 1 d PDU B 1 H18A H 1.2636 0.2438 0.8718 0.193 Uiso 0.83 1 calc PR B 1 H18B H 1.3480 0.2965 0.8382 0.193 Uiso 0.83 1 calc PR B 1 H18C H 1.3328 0.2179 0.8067 0.193 Uiso 0.83 1 calc PR B 1 C19 C 0.6689(3) 0.16320(16) 0.6524(2) 0.0460(9) Uani 1 1 d . . . C20 C 0.9509(3) 0.05813(18) 0.7604(2) 0.0482(9) Uani 1 1 d . . . C21 C 0.7588(4) 0.15640(18) 0.5325(2) 0.0581(10) Uani 1 1 d . . . H21A H 0.8310 0.1768 0.5181 0.070 Uiso 1 1 calc R . . H21B H 0.6822 0.1783 0.4967 0.070 Uiso 1 1 calc R . . C22 C 0.9746(3) 0.06420(19) 0.6160(2) 0.0517(9) Uani 1 1 d . . . H22A H 1.0369 0.0268 0.6349 0.062 Uiso 1 1 calc R . . H22B H 1.0118 0.0999 0.5882 0.062 Uiso 1 1 calc R . . C23 C 0.7542(4) 0.07770(19) 0.5148(2) 0.0526(9) Uani 1 1 d . . . C24 C 0.8577(3) 0.03396(18) 0.5530(2) 0.0479(9) Uani 1 1 d . . . C25 C 0.8518(3) -0.03795(18) 0.5353(2) 0.0486(9) Uani 1 1 d . . . H25 H 0.9214 -0.0666 0.5603 0.058 Uiso 1 1 calc R . . C26 C 0.7432(3) -0.06748(19) 0.4810(2) 0.0514(9) Uani 1 1 d . . . C27 C 0.6413(4) -0.0244(2) 0.4441(2) 0.0660(11) Uani 1 1 d . . . H27 H 0.5677 -0.0437 0.4078 0.079 Uiso 1 1 calc R . . C28 C 0.6474(4) 0.0469(2) 0.4606(2) 0.0680(12) Uani 1 1 d . . . H28 H 0.5777 0.0752 0.4346 0.082 Uiso 1 1 calc R . . C29 C 0.8171(4) -0.1926(2) 0.4867(3) 0.0599(10) Uani 1 1 d . . . C30 C 0.7739(3) -0.26735(19) 0.4628(2) 0.0550(10) Uani 1 1 d . . . C31 C 0.8640(4) -0.3200(2) 0.4874(3) 0.0652(11) Uani 1 1 d . . . H31 H 0.9465 -0.3085 0.5187 0.078 Uiso 1 1 calc R . . C32 C 0.8329(5) -0.3893(2) 0.4661(3) 0.0754(13) Uani 1 1 d . . . H32 H 0.8941 -0.4245 0.4837 0.090 Uiso 1 1 calc R . . C33 C 0.7131(5) -0.4065(2) 0.4195(3) 0.0814(14) Uani 1 1 d . . . H33 H 0.6929 -0.4535 0.4047 0.098 Uiso 1 1 calc R . . C34 C 0.6238(4) -0.3562(2) 0.3947(3) 0.0844(14) Uani 1 1 d . . . H34 H 0.5419 -0.3685 0.3627 0.101 Uiso 1 1 calc R . . C35 C 0.6531(4) -0.2862(2) 0.4166(3) 0.0755(13) Uani 1 1 d . . . H35 H 0.5904 -0.2517 0.3998 0.091 Uiso 1 1 calc R . . N1 N 0.7123(2) 0.16116(14) 0.73779(19) 0.0453(7) Uani 1 1 d . . . N2 N 0.9048(2) 0.10098(14) 0.81240(18) 0.0455(7) Uani 1 1 d . . . N3 N 0.7697(3) 0.17248(14) 0.62087(18) 0.0466(7) Uani 1 1 d . . . N4 N 0.9475(2) 0.09569(14) 0.68909(18) 0.0446(7) Uani 1 1 d . . . N5 N 0.7296(3) -0.14104(16) 0.4626(2) 0.0579(9) Uani 1 1 d . . . H5 H 0.659(4) -0.152(2) 0.434(3) 0.070 Uiso 1 1 d . . . O1 O 0.8335(3) -0.06339(15) 0.9344(2) 0.0855(10) Uani 1 1 d . . . O2 O 0.4031(2) 0.08656(16) 0.7673(2) 0.0865(10) Uani 1 1 d . . . O3 O 0.9664(3) 0.23089(15) 0.89187(19) 0.0902(10) Uani 1 1 d . . . O4 O 0.8294(3) 0.28538(14) 0.78740(18) 0.0821(10) Uani 1 1 d D . . O5 O 0.9577(3) 0.26978(16) 0.6300(2) 0.0971(11) Uani 1 1 d . . . O6 O 1.0886(3) 0.21709(16) 0.74116(19) 0.0817(9) Uani 1 1 d D . . O7 O 0.5580(2) 0.15873(13) 0.60974(17) 0.0650(8) Uani 1 1 d . . . O8 O 0.9922(2) -0.00131(13) 0.77590(18) 0.0691(8) Uani 1 1 d . . . O9 O 0.9270(3) -0.18039(15) 0.5256(3) 0.1047(13) Uani 1 1 d . . . C13' C 0.840(2) 0.3444(7) 0.8463(10) 0.119(9) Uani 0.44 1 d PDU A 2 H13C H 0.9287 0.3509 0.8789 0.143 Uiso 0.44 1 calc PR A 2 H13D H 0.7911 0.3347 0.8851 0.143 Uiso 0.44 1 calc PR A 2 C14' C 0.7923(19) 0.4087(10) 0.7966(13) 0.129(7) Uani 0.44 1 d PDU A 2 H14D H 0.8521 0.4237 0.7677 0.193 Uiso 0.44 1 calc PR A 2 H14E H 0.7815 0.4457 0.8337 0.193 Uiso 0.44 1 calc PR A 2 H14F H 0.7119 0.3986 0.7561 0.193 Uiso 0.44 1 calc PR A 2 C18' C 1.230(4) 0.3005(18) 0.817(2) 0.102(10) Uani 0.17 1 d PDU B 2 H18D H 1.1521 0.3269 0.8064 0.153 Uiso 0.17 1 calc PR B 2 H18E H 1.2982 0.3320 0.8160 0.153 Uiso 0.17 1 calc PR B 2 H18F H 1.2482 0.2779 0.8709 0.153 Uiso 0.17 1 calc PR B 2 C17' C 1.2157(17) 0.2451(16) 0.749(2) 0.083(11) Uani 0.17 1 d PDU B 2 H17C H 1.2203 0.2660 0.6963 0.099 Uiso 0.17 1 calc PR B 2 H17D H 1.2802 0.2086 0.7662 0.099 Uiso 0.17 1 calc PR B 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 C1 0.098(4) 0.081(4) 0.159(6) 0.056(4) 0.004(4) -0.011(3) C2 0.045(3) 0.117(4) 0.194(6) 0.004(4) 0.018(3) -0.013(3) C3 0.055(2) 0.059(2) 0.082(3) 0.007(2) 0.017(2) -0.013(2) C4 0.048(2) 0.052(2) 0.057(2) 0.0011(18) 0.0143(17) -0.0101(17) C5 0.046(2) 0.054(2) 0.062(2) -0.0066(18) 0.0173(18) -0.0045(17) C6 0.045(2) 0.061(3) 0.086(3) -0.004(2) 0.017(2) -0.0105(19) C7 0.054(3) 0.073(3) 0.128(4) 0.002(3) 0.027(3) -0.023(2) C8 0.071(3) 0.057(3) 0.122(4) 0.017(3) 0.027(3) -0.017(2) C9 0.042(2) 0.058(2) 0.064(2) -0.0041(18) 0.0164(18) -0.0006(16) C10 0.047(2) 0.058(2) 0.060(2) 0.0098(18) 0.0044(18) -0.0123(17) C11 0.0306(16) 0.0411(18) 0.047(2) -0.0015(15) 0.0057(14) -0.0036(13) C12 0.043(2) 0.050(2) 0.050(2) -0.0013(17) 0.0099(17) -0.0050(16) C13 0.095(6) 0.025(4) 0.052(4) -0.008(3) 0.012(4) -0.004(4) C14 0.099(7) 0.077(6) 0.102(7) -0.014(5) 0.037(6) 0.020(5) C15 0.0369(18) 0.0381(18) 0.049(2) -0.0014(15) 0.0090(15) -0.0002(14) C16 0.056(2) 0.042(2) 0.064(3) -0.0048(19) 0.025(2) -0.0024(17) C17 0.070(4) 0.085(4) 0.104(5) -0.026(4) 0.023(3) -0.042(3) C18 0.088(5) 0.141(6) 0.138(6) -0.035(5) 0.000(4) -0.040(4) C19 0.039(2) 0.0360(18) 0.055(2) -0.0043(15) 0.0010(18) 0.0035(14) C20 0.0288(17) 0.039(2) 0.070(3) 0.0002(19) 0.0029(16) -0.0007(15) C21 0.066(2) 0.053(2) 0.049(2) 0.0038(17) 0.0069(18) 0.0073(18) C22 0.043(2) 0.050(2) 0.063(2) -0.0124(18) 0.0166(17) -0.0023(16) C23 0.061(2) 0.051(2) 0.042(2) 0.0012(16) 0.0088(18) 0.0038(17) C24 0.044(2) 0.048(2) 0.053(2) -0.0056(17) 0.0172(17) -0.0014(16) C25 0.0424(19) 0.051(2) 0.052(2) -0.0061(17) 0.0145(17) 0.0023(16) C26 0.051(2) 0.052(2) 0.052(2) -0.0079(17) 0.0144(18) 0.0000(17) C27 0.062(3) 0.062(3) 0.059(3) -0.012(2) -0.006(2) 0.002(2) C28 0.067(3) 0.062(3) 0.057(3) -0.003(2) -0.012(2) 0.015(2) C29 0.047(2) 0.059(2) 0.071(3) -0.015(2) 0.013(2) -0.0007(19) C30 0.053(2) 0.053(2) 0.063(2) -0.0098(18) 0.0235(19) -0.0045(18) C31 0.065(3) 0.060(3) 0.072(3) -0.007(2) 0.023(2) 0.001(2) C32 0.089(3) 0.056(3) 0.087(3) -0.005(2) 0.033(3) 0.010(2) C33 0.092(4) 0.061(3) 0.099(4) -0.019(3) 0.038(3) -0.015(3) C34 0.066(3) 0.068(3) 0.115(4) -0.030(3) 0.020(3) -0.013(2) C35 0.056(3) 0.066(3) 0.102(3) -0.021(2) 0.017(2) -0.006(2) N1 0.0337(15) 0.0485(17) 0.0525(19) 0.0003(13) 0.0102(13) -0.0003(12) N2 0.0371(15) 0.0449(16) 0.0526(18) 0.0104(14) 0.0100(13) -0.0028(12) N3 0.0458(17) 0.0417(16) 0.0487(19) -0.0010(13) 0.0080(14) -0.0002(12) N4 0.0363(15) 0.0416(16) 0.0519(19) -0.0033(14) 0.0061(13) 0.0014(12) N5 0.0443(18) 0.0514(19) 0.071(2) -0.0149(16) 0.0049(16) -0.0063(15) O1 0.0653(19) 0.0647(19) 0.115(3) 0.0339(17) 0.0087(17) -0.0086(15) O2 0.0345(15) 0.089(2) 0.132(3) 0.0079(19) 0.0175(16) -0.0049(14) O3 0.105(2) 0.0699(19) 0.066(2) -0.0123(15) -0.0214(18) -0.0050(16) O4 0.099(2) 0.0472(16) 0.077(2) -0.0171(14) -0.0116(16) 0.0102(15) O5 0.086(2) 0.0623(19) 0.140(3) 0.029(2) 0.028(2) -0.0127(16) O6 0.0550(17) 0.100(2) 0.079(2) 0.0039(16) 0.0023(15) -0.0381(15) O7 0.0384(14) 0.0659(17) 0.0761(19) -0.0070(13) -0.0062(13) 0.0062(12) O8 0.0612(17) 0.0450(15) 0.094(2) 0.0119(14) 0.0112(15) 0.0143(12) O9 0.0557(19) 0.0603(19) 0.173(3) -0.030(2) -0.006(2) 0.0041(14) C13' 0.136(12) 0.093(11) 0.128(12) 0.003(8) 0.036(8) -0.014(7) C14' 0.149(11) 0.113(10) 0.128(10) -0.002(7) 0.044(8) 0.006(8) C18' 0.106(13) 0.100(13) 0.095(13) -0.010(9) 0.022(9) 0.003(9) C17' 0.085(14) 0.076(13) 0.083(13) 0.002(9) 0.016(9) -0.010(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 C1 O1 1.396(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O2 1.394(5) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 O1 1.364(5) . ? C3 C8 1.368(5) . ? C3 C4 1.402(5) . ? C4 C5 1.389(5) . ? C4 C10 1.526(5) . ? C5 C6 1.395(5) . ? C5 C9 1.512(5) . ? C6 C7 1.364(6) . ? C6 O2 1.373(5) . ? C7 C8 1.379(6) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 N1 1.440(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.458(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.428(4) . ? C11 N1 1.439(4) . ? C11 C12 1.550(5) . ? C11 C15 1.564(5) . ? C12 O3 1.166(4) . ? C12 O4 1.299(4) . ? C13 O4 1.462(6) . ? C13 C14 1.500(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N4 1.435(4) . ? C15 N3 1.449(4) . ? C15 C16 1.541(5) . ? C16 O5 1.194(4) . ? C16 O6 1.297(4) . ? C17 O6 1.473(5) . ? C17 C18 1.508(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O7 1.221(4) . ? C19 N1 1.354(4) . ? C19 N3 1.364(4) . ? C20 O8 1.211(4) . ? C20 N4 1.368(4) . ? C20 N2 1.380(4) . ? C21 N3 1.464(5) . ? C21 C23 1.514(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N4 1.454(4) . ? C22 C24 1.512(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C28 1.381(5) . ? C23 C24 1.399(5) . ? C24 C25 1.387(5) . ? C25 C26 1.385(5) . ? C25 H25 0.9300 . ? C26 C27 1.375(5) . ? C26 N5 1.421(4) . ? C27 C28 1.372(5) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 O9 1.213(4) . ? C29 N5 1.345(5) . ? C29 C30 1.506(5) . ? C30 C35 1.371(5) . ? C30 C31 1.379(5) . ? C31 C32 1.372(6) . ? C31 H31 0.9300 . ? C32 C33 1.357(6) . ? C32 H32 0.9300 . ? C33 C34 1.342(6) . ? C33 H33 0.9300 . ? C34 C35 1.386(6) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? N5 H5 0.81(4) . ? O4 C13' 1.462(9) . ? O6 C17' 1.463(10) . ? C13' C14' 1.477(10) . ? C13' H13C 0.9700 . ? C13' H13D 0.9700 . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C18' C17' 1.509(10) . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C18' H18F 0.9600 . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 C8 123.8(4) . . ? O1 C3 C4 117.2(3) . . ? C8 C3 C4 119.0(4) . . ? C5 C4 C3 119.5(3) . . ? C5 C4 C10 121.9(3) . . ? C3 C4 C10 118.4(3) . . ? C4 C5 C6 120.2(3) . . ? C4 C5 C9 121.4(3) . . ? C6 C5 C9 118.3(3) . . ? C7 C6 O2 123.7(3) . . ? C7 C6 C5 119.4(4) . . ? O2 C6 C5 116.8(4) . . ? C6 C7 C8 120.5(4) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C3 C8 C7 121.3(4) . . ? C3 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? N1 C9 C5 113.9(3) . . ? N1 C9 H9A 108.8 . . ? C5 C9 H9A 108.8 . . ? N1 C9 H9B 108.8 . . ? C5 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N2 C10 C4 116.5(3) . . ? N2 C10 H10A 108.2 . . ? C4 C10 H10A 108.2 . . ? N2 C10 H10B 108.2 . . ? C4 C10 H10B 108.2 . . ? H10A C10 H10B 107.3 . . ? N2 C11 N1 113.9(2) . . ? N2 C11 C12 111.6(3) . . ? N1 C11 C12 109.9(3) . . ? N2 C11 C15 104.2(3) . . ? N1 C11 C15 101.9(2) . . ? C12 C11 C15 115.0(3) . . ? O3 C12 O4 125.4(3) . . ? O3 C12 C11 125.1(3) . . ? O4 C12 C11 109.5(3) . . ? O4 C13 C14 102.1(7) . . ? O4 C13 H13A 111.3 . . ? C14 C13 H13A 111.3 . . ? O4 C13 H13B 111.3 . . ? C14 C13 H13B 111.3 . . ? H13A C13 H13B 109.2 . . ? N4 C15 N3 114.9(3) . . ? N4 C15 C16 111.4(3) . . ? N3 C15 C16 110.4(3) . . ? N4 C15 C11 102.2(3) . . ? N3 C15 C11 103.6(2) . . ? C16 C15 C11 113.9(3) . . ? O5 C16 O6 125.5(4) . . ? O5 C16 C15 123.8(3) . . ? O6 C16 C15 110.7(3) . . ? O6 C17 C18 105.0(5) . . ? O6 C17 H17A 110.7 . . ? C18 C17 H17A 110.7 . . ? O6 C17 H17B 110.7 . . ? C18 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? O7 C19 N1 126.2(4) . . ? O7 C19 N3 124.8(3) . . ? N1 C19 N3 108.9(3) . . ? O8 C20 N4 125.4(4) . . ? O8 C20 N2 126.5(4) . . ? N4 C20 N2 108.1(3) . . ? N3 C21 C23 112.7(3) . . ? N3 C21 H21A 109.1 . . ? C23 C21 H21A 109.1 . . ? N3 C21 H21B 109.1 . . ? C23 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? N4 C22 C24 113.0(3) . . ? N4 C22 H22A 109.0 . . ? C24 C22 H22A 109.0 . . ? N4 C22 H22B 109.0 . . ? C24 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C28 C23 C24 118.0(3) . . ? C28 C23 C21 121.0(3) . . ? C24 C23 C21 121.0(3) . . ? C25 C24 C23 120.1(3) . . ? C25 C24 C22 119.6(3) . . ? C23 C24 C22 120.3(3) . . ? C26 C25 C24 120.7(3) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 C25 119.1(3) . . ? C27 C26 N5 117.5(3) . . ? C25 C26 N5 123.4(3) . . ? C28 C27 C26 120.4(3) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C23 121.8(3) . . ? C27 C28 H28 119.1 . . ? C23 C28 H28 119.1 . . ? O9 C29 N5 122.2(4) . . ? O9 C29 C30 120.5(3) . . ? N5 C29 C30 117.3(3) . . ? C35 C30 C31 118.2(4) . . ? C35 C30 C29 124.7(3) . . ? C31 C30 C29 117.0(3) . . ? C32 C31 C30 120.6(4) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 120.1(4) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.4(4) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.2(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C30 C35 C34 120.5(4) . . ? C30 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C19 N1 C11 113.3(3) . . ? C19 N1 C9 124.8(3) . . ? C11 N1 C9 121.8(3) . . ? C20 N2 C11 111.3(3) . . ? C20 N2 C10 121.6(3) . . ? C11 N2 C10 121.8(3) . . ? C19 N3 C15 110.9(3) . . ? C19 N3 C21 121.0(3) . . ? C15 N3 C21 121.3(3) . . ? C20 N4 C15 113.1(3) . . ? C20 N4 C22 123.0(3) . . ? C15 N4 C22 122.7(3) . . ? C29 N5 C26 128.6(3) . . ? C29 N5 H5 118(3) . . ? C26 N5 H5 114(3) . . ? C3 O1 C1 118.1(3) . . ? C6 O2 C2 117.8(4) . . ? C12 O4 C13' 110.5(8) . . ? C12 O4 C13 120.4(4) . . ? C16 O6 C17' 131.1(15) . . ? C16 O6 C17 115.4(4) . . ? O4 C13' C14' 108.0(13) . . ? O4 C13' H13C 110.1 . . ? C14' C13' H13C 110.1 . . ? O4 C13' H13D 110.1 . . ? C14' C13' H13D 110.1 . . ? H13C C13' H13D 108.4 . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C17' C18' H18D 109.5 . . ? C17' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? O6 C17' C18' 102(2) . . ? O6 C17' H17C 111.4 . . ? C18' C17' H17C 111.4 . . ? O6 C17' H17D 111.4 . . ? C18' C17' H17D 111.4 . . ? H17C C17' H17D 109.3 . . ? 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 O1 C3 C4 C5 -178.8(4) . . . . ? C8 C3 C4 C5 1.7(6) . . . . ? O1 C3 C4 C10 -3.8(6) . . . . ? C8 C3 C4 C10 176.7(4) . . . . ? C3 C4 C5 C6 -1.4(6) . . . . ? C10 C4 C5 C6 -176.3(4) . . . . ? C3 C4 C5 C9 176.2(4) . . . . ? C10 C4 C5 C9 1.4(5) . . . . ? C4 C5 C6 C7 0.2(6) . . . . ? C9 C5 C6 C7 -177.5(4) . . . . ? C4 C5 C6 O2 179.8(3) . . . . ? C9 C5 C6 O2 2.1(5) . . . . ? O2 C6 C7 C8 -178.9(4) . . . . ? C5 C6 C7 C8 0.7(7) . . . . ? O1 C3 C8 C7 179.7(4) . . . . ? C4 C3 C8 C7 -0.8(7) . . . . ? C6 C7 C8 C3 -0.4(8) . . . . ? C4 C5 C9 N1 56.5(5) . . . . ? C6 C5 C9 N1 -125.7(4) . . . . ? C5 C4 C10 N2 -56.6(5) . . . . ? C3 C4 C10 N2 128.6(4) . . . . ? N2 C11 C12 O3 7.1(5) . . . . ? N1 C11 C12 O3 134.4(4) . . . . ? C15 C11 C12 O3 -111.3(4) . . . . ? N2 C11 C12 O4 -175.1(3) . . . . ? N1 C11 C12 O4 -47.8(4) . . . . ? C15 C11 C12 O4 66.6(4) . . . . ? N2 C11 C15 N4 7.6(3) . . . . ? N1 C11 C15 N4 -111.0(2) . . . . ? C12 C11 C15 N4 130.1(3) . . . . ? N2 C11 C15 N3 127.4(2) . . . . ? N1 C11 C15 N3 8.7(3) . . . . ? C12 C11 C15 N3 -110.2(3) . . . . ? N2 C11 C15 C16 -112.6(3) . . . . ? N1 C11 C15 C16 128.7(3) . . . . ? C12 C11 C15 C16 9.8(4) . . . . ? N4 C15 C16 O5 128.1(4) . . . . ? N3 C15 C16 O5 -0.9(5) . . . . ? C11 C15 C16 O5 -116.9(4) . . . . ? N4 C15 C16 O6 -52.0(4) . . . . ? N3 C15 C16 O6 179.0(3) . . . . ? C11 C15 C16 O6 62.9(4) . . . . ? N3 C21 C23 C28 115.9(4) . . . . ? N3 C21 C23 C24 -63.9(5) . . . . ? C28 C23 C24 C25 0.7(5) . . . . ? C21 C23 C24 C25 -179.5(3) . . . . ? C28 C23 C24 C22 -177.1(4) . . . . ? C21 C23 C24 C22 2.7(5) . . . . ? N4 C22 C24 C25 -117.9(3) . . . . ? N4 C22 C24 C23 59.9(4) . . . . ? C23 C24 C25 C26 -1.0(5) . . . . ? C22 C24 C25 C26 176.9(3) . . . . ? C24 C25 C26 C27 0.4(5) . . . . ? C24 C25 C26 N5 -177.8(3) . . . . ? C25 C26 C27 C28 0.4(6) . . . . ? N5 C26 C27 C28 178.7(4) . . . . ? C26 C27 C28 C23 -0.7(7) . . . . ? C24 C23 C28 C27 0.1(6) . . . . ? C21 C23 C28 C27 -179.7(4) . . . . ? O9 C29 C30 C35 -177.8(4) . . . . ? N5 C29 C30 C35 1.7(6) . . . . ? O9 C29 C30 C31 0.3(6) . . . . ? N5 C29 C30 C31 179.8(4) . . . . ? C35 C30 C31 C32 -0.1(6) . . . . ? C29 C30 C31 C32 -178.3(4) . . . . ? C30 C31 C32 C33 0.8(7) . . . . ? C31 C32 C33 C34 -0.8(7) . . . . ? C32 C33 C34 C35 -0.1(8) . . . . ? C31 C30 C35 C34 -0.8(7) . . . . ? C29 C30 C35 C34 177.3(4) . . . . ? C33 C34 C35 C30 0.9(7) . . . . ? O7 C19 N1 C11 176.8(3) . . . . ? N3 C19 N1 C11 -4.3(4) . . . . ? O7 C19 N1 C9 1.0(5) . . . . ? N3 C19 N1 C9 179.8(3) . . . . ? N2 C11 N1 C19 -114.6(3) . . . . ? C12 C11 N1 C19 119.3(3) . . . . ? C15 C11 N1 C19 -3.1(3) . . . . ? N2 C11 N1 C9 61.4(4) . . . . ? C12 C11 N1 C9 -64.7(4) . . . . ? C15 C11 N1 C9 172.9(3) . . . . ? C5 C9 N1 C19 96.8(4) . . . . ? C5 C9 N1 C11 -78.8(4) . . . . ? O8 C20 N2 C11 -172.5(3) . . . . ? N4 C20 N2 C11 10.3(3) . . . . ? O8 C20 N2 C10 -17.7(5) . . . . ? N4 C20 N2 C10 165.1(3) . . . . ? N1 C11 N2 C20 99.0(3) . . . . ? C12 C11 N2 C20 -135.8(3) . . . . ? C15 C11 N2 C20 -11.1(3) . . . . ? N1 C11 N2 C10 -55.7(4) . . . . ? C12 C11 N2 C10 69.5(4) . . . . ? C15 C11 N2 C10 -165.9(3) . . . . ? C4 C10 N2 C20 -81.3(4) . . . . ? C4 C10 N2 C11 70.9(4) . . . . ? O7 C19 N3 C15 -170.5(3) . . . . ? N1 C19 N3 C15 10.6(3) . . . . ? O7 C19 N3 C21 -19.1(5) . . . . ? N1 C19 N3 C21 162.0(3) . . . . ? N4 C15 N3 C19 98.6(3) . . . . ? C16 C15 N3 C19 -134.3(3) . . . . ? C11 C15 N3 C19 -12.0(3) . . . . ? N4 C15 N3 C21 -52.7(4) . . . . ? C16 C15 N3 C21 74.3(4) . . . . ? C11 C15 N3 C21 -163.3(3) . . . . ? C23 C21 N3 C19 -72.6(4) . . . . ? C23 C21 N3 C15 75.9(4) . . . . ? O8 C20 N4 C15 177.9(3) . . . . ? N2 C20 N4 C15 -4.8(3) . . . . ? O8 C20 N4 C22 10.4(5) . . . . ? N2 C20 N4 C22 -172.3(3) . . . . ? N3 C15 N4 C20 -113.4(3) . . . . ? C16 C15 N4 C20 120.1(3) . . . . ? C11 C15 N4 C20 -2.0(3) . . . . ? N3 C15 N4 C22 54.2(4) . . . . ? C16 C15 N4 C22 -72.4(4) . . . . ? C11 C15 N4 C22 165.6(3) . . . . ? C24 C22 N4 C20 89.4(4) . . . . ? C24 C22 N4 C15 -77.0(4) . . . . ? O9 C29 N5 C26 -4.5(7) . . . . ? C30 C29 N5 C26 176.0(4) . . . . ? C27 C26 N5 C29 175.8(4) . . . . ? C25 C26 N5 C29 -6.0(6) . . . . ? C8 C3 O1 C1 -1.0(7) . . . . ? C4 C3 O1 C1 179.5(5) . . . . ? C7 C6 O2 C2 4.6(7) . . . . ? C5 C6 O2 C2 -175.0(4) . . . . ? O3 C12 O4 C13' -16.8(11) . . . . ? C11 C12 O4 C13' 165.4(10) . . . . ? O3 C12 O4 C13 3.5(8) . . . . ? C11 C12 O4 C13 -174.3(7) . . . . ? C14 C13 O4 C12 -143.4(7) . . . . ? C14 C13 O4 C13' -77(3) . . . . ? O5 C16 O6 C17' -21.1(16) . . . . ? C15 C16 O6 C17' 159.0(15) . . . . ? O5 C16 O6 C17 10.1(7) . . . . ? C15 C16 O6 C17 -169.8(4) . . . . ? C18 C17 O6 C16 180.0(6) . . . . ? C18 C17 O6 C17' -51(3) . . . . ? C12 O4 C13' C14' 169.1(13) . . . . ? C13 O4 C13' C14' 46(2) . . . . ? C16 O6 C17' C18' 109(2) . . . . ? C17 O6 C17' C18' 40(2) . . . . ? 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 N5 H5 O7 0.81(4) 2.29(4) 3.053(4) 159(4) 3_656 C25 H25 O9 0.93 2.23 2.833(4) 121.8 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.269 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.055 # Attachment '- 1.cif' data_i:\081225bpub-1\t _database_code_depnum_ccdc_archive 'CCDC 756895' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H37 N5 O10, 0.18(C H2 Cl2), 3(C H4 O), H2 O' _chemical_formula_sum 'C39.17 H51.33 Cl0.33 N5 O14' _chemical_formula_weight 828.29 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 36.4925(4) _cell_length_b 36.4925(4) _cell_length_c 16.5404(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 19075.8(5) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3500 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 23.59 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7904.4 _exptl_absorpt_coefficient_mu 0.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9747 _exptl_absorpt_correction_T_max 0.9882 _exptl_absorpt_process_details 'SADABS, (Sheldrick,1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15964 _diffrn_reflns_av_R_equivalents 0.0938 _diffrn_reflns_av_sigmaI/netI 0.1025 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7380 _reflns_number_gt 4656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1366P)^2^?] 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_number_reflns 7380 _refine_ls_number_parameters 638 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1128 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2262 _refine_ls_wR_factor_gt 0.2046 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.978 _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 C1 C 0.82364(13) 0.10890(13) 0.48211(19) 0.0437(10) Uani 1 1 d . . . H1A H 0.8228 0.1353 0.4829 0.051(12) Uiso 1 1 calc R . . H1B H 0.8024 0.0891 0.4440 0.106(19) Uiso 1 1 calc R . . H1C H 0.8518 0.1148 0.4652 0.062(13) Uiso 1 1 calc R . . C2 C 0.83976(10) 0.11576(11) 0.62322(18) 0.0290(8) Uani 1 1 d . . . C3 C 0.87250(11) 0.15683(11) 0.6146(2) 0.0359(8) Uani 1 1 d . . . H3 H 0.8788 0.1697 0.5627 0.035(9) Uiso 1 1 calc R . . C4 C 0.89614(11) 0.17936(11) 0.6804(2) 0.0362(9) Uani 1 1 d . . . H4 H 0.9187 0.2076 0.6737 0.039(10) Uiso 1 1 calc R . . C5 C 0.88713(11) 0.16102(10) 0.75626(18) 0.0309(8) Uani 1 1 d . . . C6 C 0.85390(10) 0.11933(10) 0.76729(18) 0.0278(7) Uani 1 1 d . . . C7 C 0.83004(10) 0.09628(10) 0.70019(17) 0.0271(7) Uani 1 1 d . . . C8 C 0.94167(13) 0.22454(12) 0.8157(2) 0.0506(11) Uani 1 1 d . . . H8A H 0.9632 0.2264 0.7777 0.070(14) Uiso 1 1 calc R . . H8B H 0.9549 0.2361 0.8682 0.065(13) Uiso 1 1 calc R . . H8C H 0.9290 0.2408 0.7947 0.052(12) Uiso 1 1 calc R . . C9 C 0.79619(10) 0.05007(10) 0.70504(17) 0.0296(8) Uani 1 1 d . . . H9A H 0.7835 0.0406 0.6507 0.034(9) Uiso 1 1 calc R . . H9B H 0.8098 0.0334 0.7198 0.030(9) Uiso 1 1 calc R . . C10 C 0.84612(10) 0.10016(11) 0.85150(17) 0.0286(8) Uani 1 1 d . . . H10A H 0.8551 0.0787 0.8523 0.025(7) Uiso 1 1 calc R . . H10B H 0.8643 0.1227 0.8902 0.033(9) Uiso 1 1 calc R . . C11 C 0.76948(10) 0.04028(10) 0.84927(16) 0.0243(7) Uani 1 1 d . . . C12 C 0.77602(11) 0.00255(11) 0.86781(18) 0.0291(8) Uani 1 1 d . A . C13 C 0.8173(3) -0.0199(3) 0.9419(5) 0.038(2) Uani 0.646(17) 1 d PD A 1 H13A H 0.8465 -0.0051 0.9639 0.27(13) Uiso 0.646(17) 1 calc PR A 1 H13B H 0.8173 -0.0337 0.8903 0.036(15) Uiso 0.646(17) 1 calc PR A 1 C14 C 0.7873(2) -0.0518(3) 1.0010(5) 0.057(3) Uani 0.646(17) 1 d PD A 1 H14A H 0.7856 -0.0373 1.0495 0.054(15) Uiso 0.646(17) 1 calc PR A 1 H14B H 0.7973 -0.0713 1.0159 0.055(19) Uiso 0.646(17) 1 calc PR A 1 H14C H 0.7591 -0.0678 0.9764 0.07(2) Uiso 0.646(17) 1 calc PR A 1 C15 C 0.72751(10) 0.04456(10) 0.74617(17) 0.0265(7) Uani 1 1 d . . . C16 C 0.78681(10) 0.10004(10) 0.92823(16) 0.0253(7) Uani 1 1 d . . . C17 C 0.72831(10) 0.03689(10) 0.88717(16) 0.0241(7) Uani 1 1 d . . . C18 C 0.70027(10) -0.00448(10) 0.93382(18) 0.0281(7) Uani 1 1 d . . . C19 C 0.64473(12) -0.07555(11) 0.9210(2) 0.0450(10) Uani 1 1 d . . . H19A H 0.6221 -0.0929 0.8818 0.050(11) Uiso 1 1 calc R . . H19B H 0.6312 -0.0714 0.9694 0.047(8) Uiso 1 1 calc R . . C20 C 0.66753(15) -0.09893(13) 0.9451(3) 0.0582(12) Uani 1 1 d . . . H20A H 0.6830 -0.1009 0.8984 0.066(13) Uiso 1 1 calc R . . H20B H 0.6469 -0.1274 0.9636 0.083(15) Uiso 1 1 calc R . . H20C H 0.6875 -0.0836 0.9888 0.11(2) Uiso 1 1 calc R . . C21 C 0.67185(10) 0.04935(10) 0.82368(18) 0.0298(8) Uani 1 1 d . . . H21A H 0.6525 0.0314 0.8671 0.026(8) Uiso 1 1 calc R . . H21B H 0.6558 0.0413 0.7723 0.026(8) Uiso 1 1 calc R . . C22 C 0.71705(10) 0.08702(10) 0.97278(17) 0.0274(7) Uani 1 1 d . . . H22A H 0.7293 0.1035 1.0229 0.025(7) Uiso 1 1 calc R . . H22B H 0.6895 0.0621 0.9869 0.024(8) Uiso 1 1 calc R . . C23 C 0.68647(10) 0.09551(10) 0.84199(18) 0.0273(7) Uani 1 1 d . . . C24 C 0.70969(10) 0.11410(10) 0.91342(17) 0.0274(8) Uani 1 1 d . . . C25 C 0.72524(10) 0.15704(10) 0.92689(17) 0.0283(8) Uani 1 1 d . . . C26 C 0.71688(11) 0.18100(12) 0.8733(2) 0.0371(9) Uani 1 1 d . . . H26 H 0.7278 0.2103 0.8834 0.031(9) Uiso 1 1 calc R . . C27 C 0.69282(12) 0.16257(11) 0.8053(2) 0.0366(9) Uani 1 1 d . . . H27 H 0.6864 0.1789 0.7695 0.039(10) Uiso 1 1 calc R . . C28 C 0.67800(11) 0.12018(11) 0.78912(19) 0.0308(8) Uani 1 1 d . . . C29 C 0.64411(16) 0.12444(14) 0.6686(2) 0.0557(12) Uani 1 1 d . . . H29A H 0.6281 0.1349 0.6989 0.049(11) Uiso 1 1 calc R . . H29B H 0.6268 0.1066 0.6238 0.052(11) Uiso 1 1 calc R . . H29C H 0.6700 0.1485 0.6471 0.054(13) Uiso 1 1 calc R . . C30 C 0.74402(11) 0.20035(11) 1.04963(19) 0.0337(8) Uani 1 1 d . . . C31 C 0.77539(11) 0.21954(11) 1.11731(18) 0.0343(9) Uani 1 1 d . . . C32 C 0.79819(12) 0.20192(12) 1.1465(2) 0.0429(9) Uani 1 1 d . . . H32 H 0.7946 0.1765 1.1234 0.044(10) Uiso 1 1 calc R . . C33 C 0.82668(16) 0.22110(14) 1.2101(2) 0.0574(12) Uani 1 1 d . . . H33 H 0.8424 0.2087 1.2302 0.069(14) Uiso 1 1 calc R . . C34 C 0.83198(16) 0.25732(14) 1.2431(2) 0.0600(13) Uani 1 1 d . . . H34 H 0.8515 0.2705 1.2860 0.059(12) Uiso 1 1 calc R . . C35 C 0.80900(16) 0.27494(14) 1.2142(2) 0.0614(13) Uani 1 1 d . . . H35 H 0.8128 0.3004 1.2374 0.093(17) Uiso 1 1 calc R . . C36 C 0.78043(13) 0.25615(12) 1.1520(2) 0.0458(10) Uani 1 1 d . . . H36 H 0.7643 0.2683 1.1332 0.036(10) Uiso 1 1 calc R . . C37 C 0.8907(2) 0.0561(2) 0.5947(5) 0.0950(18) Uani 1 1 d D . . H37A H 0.8809 0.0401 0.6453 0.16(3) Uiso 1 1 calc R . . H37B H 0.8667 0.0470 0.5577 0.30(7) Uiso 1 1 calc R . . H37C H 0.9030 0.0864 0.6062 0.25(5) Uiso 1 1 calc R . . O12 O 0.9282(4) 0.0750(3) 0.8425(7) 0.227(4) Uani 1 1 d D . . H12 H 0.935(7) 0.057(5) 0.832(12) 0.341 Uiso 1 1 d D . . C40 C 0.9379(5) 0.0328(7) 0.3692(11) 0.366(12) Uani 1 1 d D . . H40A H 0.9634 0.0337 0.3909 0.549 Uiso 1 1 calc R . . H40B H 0.9408 0.0609 0.3731 0.549 Uiso 1 1 calc R . . H40C H 0.9343 0.0240 0.3124 0.549 Uiso 1 1 calc R . . C13' C 0.7965(6) -0.0291(4) 0.9682(10) 0.051(5) Uani 0.354(17) 1 d PD A 2 H13C H 0.7937 -0.0296 1.0278 0.08(6) Uiso 0.354(17) 1 calc PR A 2 H13D H 0.7737 -0.0555 0.9440 0.11(6) Uiso 0.354(17) 1 calc PR A 2 C14' C 0.8398(8) -0.0181(8) 0.9404(12) 0.084(7) Uani 0.354(17) 1 d PD A 2 H14D H 0.8416 -0.0145 0.8815 2(4) Uiso 0.354(17) 1 calc PR A 2 H14E H 0.8453 -0.0410 0.9550 0.08(4) Uiso 0.354(17) 1 calc PR A 2 H14F H 0.8609 0.0082 0.9663 0.08(4) Uiso 0.354(17) 1 calc PR A 2 C41 C 0.9195(10) -0.0973(9) 0.9465(16) 0.082(9) Uani 0.17 1 d PD A -1 H41A H 0.9246 -0.1124 0.9020 0.098 Uiso 0.17 1 calc PR A -1 H41B H 0.8892 -0.1153 0.9604 0.098 Uiso 0.17 1 calc PR A -1 Cl1 Cl 0.9216(9) -0.0540(8) 0.8990(15) 0.241(10) Uani 0.17 1 d PD A -1 Cl2 Cl 0.9454(9) -0.1040(11) 1.0281(18) 0.283(13) Uani 0.17 1 d PD A -1 N1 N 0.76213(8) 0.04056(8) 0.76320(14) 0.0259(6) Uani 1 1 d . . . N2 N 0.80242(8) 0.08036(8) 0.87973(14) 0.0264(6) Uani 1 1 d . . . N3 N 0.70693(8) 0.04148(8) 0.81732(14) 0.0250(6) Uani 1 1 d . . . N4 N 0.74522(8) 0.07241(8) 0.94206(13) 0.0236(6) Uani 1 1 d . . . N5 N 0.75136(9) 0.17659(9) 0.99580(15) 0.0304(7) Uani 1 1 d D . . H5 H 0.7731(7) 0.1734(11) 1.000(2) 0.037 Uiso 1 1 d D . . O1 O 0.81480(8) 0.09079(7) 0.56079(12) 0.0388(6) Uani 1 1 d . . . O2 O 0.90982(7) 0.18165(7) 0.82511(13) 0.0389(6) Uani 1 1 d . . . O3 O 0.71653(7) 0.04921(7) 0.67926(11) 0.0317(6) Uani 1 1 d . . . O4 O 0.80705(7) 0.13583(7) 0.95657(12) 0.0304(6) Uani 1 1 d . . . O5 O 0.75990(8) -0.02922(8) 0.83002(14) 0.0430(7) Uani 1 1 d . . . O6 O 0.80151(11) 0.01026(9) 0.92966(16) 0.0659(10) Uani 1 1 d D . . O7 O 0.70396(9) -0.00828(8) 1.00496(13) 0.0451(7) Uani 1 1 d . . . O8 O 0.67349(7) -0.03433(7) 0.88473(13) 0.0358(6) Uani 1 1 d . . . O9 O 0.65493(8) 0.10012(7) 0.72130(13) 0.0385(6) Uani 1 1 d . . . O10 O 0.71418(9) 0.20632(9) 1.04290(16) 0.0548(8) Uani 1 1 d . . . O11 O 0.92097(19) 0.0489(2) 0.5595(6) 0.190(3) Uani 1 1 d D . . H11 H 0.9418 0.0721 0.5451 0.228 Uiso 1 1 calc R . . C38 C 0.95156(19) 0.1113(2) 0.7985(4) 0.095(2) Uani 1 1 d . . . H38A H 0.9797 0.1151 0.7879 0.143 Uiso 1 1 calc R . . H38B H 0.9544 0.1356 0.8290 0.143 Uiso 1 1 calc R . . H38C H 0.9373 0.1091 0.7471 0.143 Uiso 1 1 calc R . . O13 O 0.9030(2) 0.0042(3) 0.4129(7) 0.195(3) Uani 1 1 d D . . H13 H 0.902(3) 0.0144(19) 0.457(4) 0.233 Uiso 1 1 d D . . O14 O 0.9007(3) 0.0056(5) 0.7876(8) 0.313(6) Uani 1 1 d D . . H14H H 0.883(4) 0.003(6) 0.754(8) 0.375 Uiso 1 1 d D . . H14G H 0.887(6) -0.018(4) 0.820(10) 0.375 Uiso 1 1 d D . . 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 C1 0.049(3) 0.047(2) 0.0231(17) 0.0069(16) 0.0055(17) 0.015(2) C2 0.0309(19) 0.032(2) 0.0237(16) -0.0019(14) 0.0017(14) 0.0160(17) C3 0.040(2) 0.035(2) 0.0281(17) 0.0038(15) 0.0056(15) 0.0150(18) C4 0.036(2) 0.030(2) 0.0340(18) 0.0004(15) 0.0078(15) 0.0093(17) C5 0.0300(19) 0.0286(19) 0.0317(17) -0.0008(14) 0.0029(14) 0.0128(16) C6 0.0289(19) 0.0307(19) 0.0244(15) -0.0022(14) 0.0025(13) 0.0153(16) C7 0.0275(18) 0.0287(18) 0.0228(15) -0.0008(13) 0.0061(13) 0.0122(15) C8 0.050(3) 0.040(2) 0.042(2) -0.0102(18) -0.002(2) 0.008(2) C9 0.0322(19) 0.0313(19) 0.0201(15) -0.0042(13) 0.0029(14) 0.0119(17) C10 0.0279(19) 0.0324(19) 0.0245(16) -0.0026(14) -0.0004(14) 0.0143(16) C11 0.0278(18) 0.0276(18) 0.0147(14) -0.0047(12) -0.0031(12) 0.0118(15) C12 0.036(2) 0.031(2) 0.0203(15) -0.0030(14) 0.0027(14) 0.0159(17) C13 0.039(7) 0.043(5) 0.042(4) -0.008(3) -0.006(4) 0.028(5) C14 0.070(6) 0.047(6) 0.051(4) 0.013(4) -0.012(4) 0.027(4) C15 0.0325(19) 0.0204(17) 0.0214(16) -0.0026(13) -0.0019(14) 0.0095(15) C16 0.032(2) 0.0296(19) 0.0147(14) 0.0013(13) -0.0025(13) 0.0160(16) C17 0.0277(18) 0.0228(17) 0.0185(14) -0.0026(12) -0.0014(12) 0.0103(15) C18 0.0303(19) 0.0271(18) 0.0272(17) 0.0002(14) 0.0048(14) 0.0146(16) C19 0.046(2) 0.028(2) 0.044(2) 0.0009(17) 0.0122(18) 0.0063(19) C20 0.073(3) 0.035(2) 0.054(3) 0.004(2) 0.011(2) 0.018(2) C21 0.0302(19) 0.033(2) 0.0229(15) 0.0005(14) -0.0027(14) 0.0129(16) C22 0.0311(19) 0.0302(19) 0.0177(14) -0.0007(13) 0.0040(13) 0.0128(16) C23 0.0227(17) 0.0313(19) 0.0253(15) 0.0011(13) 0.0035(13) 0.0116(15) C24 0.0296(18) 0.0307(19) 0.0202(15) 0.0007(13) 0.0071(13) 0.0136(16) C25 0.0303(19) 0.0312(19) 0.0226(15) -0.0026(14) 0.0020(13) 0.0146(16) C26 0.045(2) 0.031(2) 0.0350(18) -0.0018(15) 0.0000(16) 0.0193(18) C27 0.044(2) 0.039(2) 0.0336(18) 0.0022(16) -0.0044(16) 0.0262(19) C28 0.0299(19) 0.036(2) 0.0268(16) 0.0001(14) -0.0011(14) 0.0171(17) C29 0.080(3) 0.057(3) 0.042(2) -0.007(2) -0.027(2) 0.043(3) C30 0.037(2) 0.034(2) 0.0305(17) -0.0017(15) 0.0026(15) 0.0175(18) C31 0.042(2) 0.033(2) 0.0229(16) 0.0004(14) 0.0084(15) 0.0153(18) C32 0.058(3) 0.046(2) 0.0288(18) -0.0048(17) -0.0048(17) 0.029(2) C33 0.084(3) 0.063(3) 0.032(2) -0.011(2) -0.016(2) 0.042(3) C34 0.089(4) 0.056(3) 0.0277(19) -0.0113(19) -0.017(2) 0.031(3) C35 0.095(4) 0.047(3) 0.039(2) -0.015(2) -0.008(2) 0.032(3) C36 0.060(3) 0.041(2) 0.0353(19) -0.0082(17) -0.0043(18) 0.024(2) C37 0.074(4) 0.085(5) 0.124(5) 0.000(4) 0.018(4) 0.038(4) O12 0.258(10) 0.224(10) 0.245(9) -0.039(8) -0.018(7) 0.155(8) C40 0.36(3) 0.40(3) 0.33(3) 0.04(2) -0.04(2) 0.18(3) C13' 0.056(12) 0.049(13) 0.051(12) 0.004(10) -0.009(8) 0.028(11) C14' 0.073(15) 0.102(15) 0.103(13) -0.022(11) -0.027(12) 0.064(13) C41 0.07(2) 0.09(2) 0.08(2) -0.008(18) 0.015(17) 0.032(19) Cl1 0.24(2) 0.24(2) 0.26(3) -0.03(2) -0.01(2) 0.13(2) Cl2 0.26(3) 0.29(3) 0.34(4) 0.03(3) 0.03(3) 0.17(3) N1 0.0292(16) 0.0311(16) 0.0137(12) -0.0022(11) 0.0017(10) 0.0124(13) N2 0.0287(15) 0.0273(15) 0.0199(12) -0.0039(11) -0.0017(11) 0.0116(13) N3 0.0305(16) 0.0315(16) 0.0164(12) -0.0018(11) -0.0017(11) 0.0180(13) N4 0.0283(15) 0.0240(14) 0.0157(12) -0.0018(10) 0.0017(10) 0.0108(13) N5 0.0352(17) 0.0315(16) 0.0259(13) -0.0032(12) 0.0004(12) 0.0177(14) O1 0.0496(16) 0.0379(14) 0.0174(11) 0.0005(10) 0.0033(10) 0.0132(12) O2 0.0374(14) 0.0295(14) 0.0335(12) -0.0071(10) -0.0070(11) 0.0046(12) O3 0.0400(14) 0.0341(13) 0.0172(10) -0.0025(9) -0.0065(10) 0.0156(11) O4 0.0362(14) 0.0256(13) 0.0222(10) -0.0068(9) -0.0040(9) 0.0099(11) O5 0.0598(18) 0.0346(15) 0.0371(13) -0.0123(12) -0.0149(12) 0.0255(14) O6 0.117(3) 0.0524(18) 0.0520(16) -0.0251(14) -0.0498(17) 0.0604(19) O7 0.0634(18) 0.0388(15) 0.0244(12) 0.0054(11) -0.0059(11) 0.0191(14) O8 0.0377(14) 0.0273(13) 0.0278(11) -0.0047(10) 0.0017(10) 0.0051(11) O9 0.0497(16) 0.0376(15) 0.0318(12) -0.0040(10) -0.0123(11) 0.0244(13) O10 0.0598(19) 0.073(2) 0.0493(16) -0.0190(14) -0.0056(14) 0.0464(17) O11 0.116(5) 0.152(5) 0.317(9) -0.052(6) 0.021(5) 0.078(4) C38 0.068(4) 0.066(4) 0.123(5) 0.004(4) -0.001(3) 0.011(3) O13 0.117(5) 0.195(8) 0.266(11) -0.005(6) 0.024(5) 0.073(5) O14 0.170(8) 0.348(15) 0.262(12) -0.021(9) -0.118(8) 0.011(8) _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 O1 1.422(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.377(4) . ? C2 C3 1.380(5) . ? C2 C7 1.414(4) . ? C3 C4 1.377(5) . ? C3 H3 0.9500 . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 O2 1.388(4) . ? C5 C6 1.405(5) . ? C6 C7 1.402(4) . ? C6 C10 1.520(4) . ? C7 C9 1.514(4) . ? C8 O2 1.416(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.470(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.460(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N2 1.442(4) . ? C11 N1 1.450(3) . ? C11 C12 1.541(5) . ? C11 C17 1.574(4) . ? C12 O5 1.183(4) . ? C12 O6 1.315(4) . ? C13 O6 1.490(7) . ? C13 C14 1.496(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 O3 1.217(3) . ? C15 N3 1.370(4) . ? C15 N1 1.372(4) . ? C16 O4 1.227(4) . ? C16 N4 1.357(4) . ? C16 N2 1.376(4) . ? C17 N4 1.444(4) . ? C17 N3 1.450(4) . ? C17 C18 1.542(4) . ? C18 O7 1.200(4) . ? C18 O8 1.318(4) . ? C19 O8 1.465(4) . ? C19 C20 1.513(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N3 1.449(4) . ? C21 C23 1.522(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N4 1.465(4) . ? C22 C24 1.510(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.396(4) . ? C23 C24 1.414(4) . ? C24 C25 1.392(4) . ? C25 C26 1.382(5) . ? C25 N5 1.427(4) . ? C26 C27 1.377(5) . ? C26 H26 0.9500 . ? C27 C28 1.386(5) . ? C27 H27 0.9500 . ? C28 O9 1.373(4) . ? C29 O9 1.433(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 O10 1.218(4) . ? C30 N5 1.359(4) . ? C30 C31 1.501(5) . ? C31 C32 1.369(5) . ? C31 C36 1.379(5) . ? C32 C33 1.395(5) . ? C32 H32 0.9500 . ? C33 C34 1.351(6) . ? C33 H33 0.9500 . ? C34 C35 1.373(6) . ? C34 H34 0.9500 . ? C35 C36 1.378(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 O11 1.386(6) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? O12 C38 1.371(12) . ? O12 H12 0.8(2) . ? C40 O13 1.380(10) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C13' C14' 1.495(11) . ? C13' O6 1.498(10) . ? C13' H13C 0.9900 . ? C13' H13D 0.9900 . ? C14' H14D 0.9800 . ? C14' H14E 0.9800 . ? C14' H14F 0.9800 . ? C41 Cl1 1.731(2) . ? C41 Cl2 1.732(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? N5 H5 0.86(3) . ? O11 H11 0.8400 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O13 H13 0.83(7) . ? O14 H14H 0.82(15) . ? O14 H14G 0.92(15) . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.7(3) . . ? O1 C2 C7 115.2(3) . . ? C3 C2 C7 120.2(3) . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.1(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 O2 123.3(3) . . ? C4 C5 C6 120.7(3) . . ? O2 C5 C6 116.0(3) . . ? C7 C6 C5 119.2(3) . . ? C7 C6 C10 122.2(3) . . ? C5 C6 C10 118.6(3) . . ? C6 C7 C2 119.1(3) . . ? C6 C7 C9 122.8(3) . . ? C2 C7 C9 117.9(3) . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C7 114.9(2) . . ? N1 C9 H9A 108.6 . . ? C7 C9 H9A 108.6 . . ? N1 C9 H9B 108.6 . . ? C7 C9 H9B 108.6 . . ? H9A C9 H9B 107.5 . . ? N2 C10 C6 115.3(3) . . ? N2 C10 H10A 108.5 . . ? C6 C10 H10A 108.5 . . ? N2 C10 H10B 108.5 . . ? C6 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? N2 C11 N1 113.5(2) . . ? N2 C11 C12 114.4(2) . . ? N1 C11 C12 108.3(2) . . ? N2 C11 C17 102.7(2) . . ? N1 C11 C17 102.6(2) . . ? C12 C11 C17 114.7(2) . . ? O5 C12 O6 125.0(3) . . ? O5 C12 C11 123.2(3) . . ? O6 C12 C11 111.9(3) . . ? O6 C13 C14 105.1(8) . . ? O6 C13 H13A 110.7 . . ? C14 C13 H13A 110.7 . . ? O6 C13 H13B 110.7 . . ? C14 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? O3 C15 N3 126.0(3) . . ? O3 C15 N1 125.9(3) . . ? N3 C15 N1 108.1(3) . . ? O4 C16 N4 125.5(3) . . ? O4 C16 N2 126.3(3) . . ? N4 C16 N2 108.2(3) . . ? N4 C17 N3 114.2(3) . . ? N4 C17 C18 109.9(2) . . ? N3 C17 C18 112.3(3) . . ? N4 C17 C11 102.5(2) . . ? N3 C17 C11 102.8(2) . . ? C18 C17 C11 114.6(2) . . ? O7 C18 O8 126.0(3) . . ? O7 C18 C17 123.1(3) . . ? O8 C18 C17 110.8(2) . . ? O8 C19 C20 111.9(3) . . ? O8 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? O8 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? 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 . . ? N3 C21 C23 112.2(3) . . ? N3 C21 H21A 109.2 . . ? C23 C21 H21A 109.2 . . ? N3 C21 H21B 109.2 . . ? C23 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N4 C22 C24 113.5(2) . . ? N4 C22 H22A 108.9 . . ? C24 C22 H22A 108.9 . . ? N4 C22 H22B 108.9 . . ? C24 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C28 C23 C24 119.1(3) . . ? C28 C23 C21 121.4(3) . . ? C24 C23 C21 119.5(3) . . ? C25 C24 C23 118.9(3) . . ? C25 C24 C22 121.8(3) . . ? C23 C24 C22 119.3(3) . . ? C26 C25 C24 121.0(3) . . ? C26 C25 N5 120.0(3) . . ? C24 C25 N5 119.0(3) . . ? C27 C26 C25 120.2(3) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.0(3) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? O9 C28 C27 123.1(3) . . ? O9 C28 C23 116.3(3) . . ? C27 C28 C23 120.7(3) . . ? O9 C29 H29A 109.5 . . ? O9 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O9 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O10 C30 N5 122.2(3) . . ? O10 C30 C31 121.7(3) . . ? N5 C30 C31 116.0(3) . . ? C32 C31 C36 119.3(3) . . ? C32 C31 C30 123.0(3) . . ? C36 C31 C30 117.6(3) . . ? C31 C32 C33 120.4(4) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C32 120.1(4) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 119.7(4) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C36 120.9(4) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 119.6(4) . . ? C35 C36 H36 120.2 . . ? C31 C36 H36 120.2 . . ? O11 C37 H37A 109.5 . . ? O11 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O11 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C38 O12 H12 112(10) . . ? O13 C40 H40A 109.5 . . ? O13 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O13 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C14' C13' O6 90.3(13) . . ? C14' C13' H13C 113.6 . . ? O6 C13' H13C 113.6 . . ? C14' C13' H13D 113.6 . . ? O6 C13' H13D 113.6 . . ? H13C C13' H13D 110.9 . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? Cl1 C41 Cl2 135(2) . . ? Cl1 C41 H41A 103.5 . . ? Cl2 C41 H41A 103.5 . . ? Cl1 C41 H41B 103.5 . . ? Cl2 C41 H41B 103.5 . . ? H41A C41 H41B 105.3 . . ? C41 Cl1 H14G 152(3) . . ? H14G Cl1 H14E 52.2 . . ? C15 N1 C11 112.7(2) . . ? C15 N1 C9 123.8(2) . . ? C11 N1 C9 120.5(3) . . ? C16 N2 C11 112.4(3) . . ? C16 N2 C10 124.3(3) . . ? C11 N2 C10 122.7(2) . . ? C15 N3 C21 123.2(3) . . ? C15 N3 C17 112.9(3) . . ? C21 N3 C17 123.0(2) . . ? C16 N4 C17 112.2(2) . . ? C16 N4 C22 121.0(3) . . ? C17 N4 C22 118.8(2) . . ? C30 N5 C25 123.1(3) . . ? C30 N5 H5 121(2) . . ? C25 N5 H5 116(2) . . ? C2 O1 C1 117.2(3) . . ? C5 O2 C8 116.5(3) . . ? C12 O6 C13 116.2(4) . . ? C12 O6 C13' 113.1(7) . . ? C13 O6 C13' 30.6(6) . . ? C18 O8 C19 116.8(3) . . ? C28 O9 C29 116.9(3) . . ? C37 O11 H11 109.5 . . ? O12 C38 H38A 109.5 . . ? O12 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O12 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 O13 H13 111(6) . . ? H14H O14 H12 119(10) . . ? H14G O14 H12 120(10) . . ? H12 O14 H14H 119(10) . . ? H14H O14 H14G 105(18) . . ? H12 O14 H14G 120(10) . . ? 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 O1 C2 C3 C4 -179.3(3) . . . . ? C7 C2 C3 C4 0.1(5) . . . . ? C2 C3 C4 C5 -0.3(5) . . . . ? C3 C4 C5 O2 179.4(3) . . . . ? C3 C4 C5 C6 0.0(5) . . . . ? C4 C5 C6 C7 0.4(5) . . . . ? O2 C5 C6 C7 -179.0(3) . . . . ? C4 C5 C6 C10 178.2(3) . . . . ? O2 C5 C6 C10 -1.2(4) . . . . ? C5 C6 C7 C2 -0.6(5) . . . . ? C10 C6 C7 C2 -178.3(3) . . . . ? C5 C6 C7 C9 174.6(3) . . . . ? C10 C6 C7 C9 -3.1(5) . . . . ? O1 C2 C7 C6 179.8(3) . . . . ? C3 C2 C7 C6 0.4(5) . . . . ? O1 C2 C7 C9 4.4(4) . . . . ? C3 C2 C7 C9 -175.1(3) . . . . ? C6 C7 C9 N1 57.8(4) . . . . ? C2 C7 C9 N1 -126.9(3) . . . . ? C7 C6 C10 N2 -52.3(4) . . . . ? C5 C6 C10 N2 130.0(3) . . . . ? N2 C11 C12 O5 -158.0(3) . . . . ? N1 C11 C12 O5 -30.2(4) . . . . ? C17 C11 C12 O5 83.7(4) . . . . ? N2 C11 C12 O6 21.8(4) . . . . ? N1 C11 C12 O6 149.5(3) . . . . ? C17 C11 C12 O6 -96.5(3) . . . . ? N2 C11 C17 N4 -8.1(3) . . . . ? N1 C11 C17 N4 -126.1(2) . . . . ? C12 C11 C17 N4 116.7(3) . . . . ? N2 C11 C17 N3 110.7(2) . . . . ? N1 C11 C17 N3 -7.3(3) . . . . ? C12 C11 C17 N3 -124.5(3) . . . . ? N2 C11 C17 C18 -127.1(3) . . . . ? N1 C11 C17 C18 114.8(3) . . . . ? C12 C11 C17 C18 -2.4(3) . . . . ? N4 C17 C18 O7 -23.8(4) . . . . ? N3 C17 C18 O7 -152.1(3) . . . . ? C11 C17 C18 O7 91.1(4) . . . . ? N4 C17 C18 O8 158.2(3) . . . . ? N3 C17 C18 O8 29.8(4) . . . . ? C11 C17 C18 O8 -87.0(3) . . . . ? N3 C21 C23 C28 119.4(3) . . . . ? N3 C21 C23 C24 -59.7(4) . . . . ? C28 C23 C24 C25 -3.2(5) . . . . ? C21 C23 C24 C25 175.9(3) . . . . ? C28 C23 C24 C22 177.0(3) . . . . ? C21 C23 C24 C22 -4.0(4) . . . . ? N4 C22 C24 C25 -111.8(3) . . . . ? N4 C22 C24 C23 68.0(4) . . . . ? C23 C24 C25 C26 2.5(5) . . . . ? C22 C24 C25 C26 -177.6(3) . . . . ? C23 C24 C25 N5 -175.3(3) . . . . ? C22 C24 C25 N5 4.5(5) . . . . ? C24 C25 C26 C27 0.1(5) . . . . ? N5 C25 C26 C27 177.9(3) . . . . ? C25 C26 C27 C28 -2.0(5) . . . . ? C26 C27 C28 O9 -178.0(3) . . . . ? C26 C27 C28 C23 1.3(5) . . . . ? C24 C23 C28 O9 -179.3(3) . . . . ? C21 C23 C28 O9 1.6(4) . . . . ? C24 C23 C28 C27 1.3(5) . . . . ? C21 C23 C28 C27 -177.7(3) . . . . ? O10 C30 C31 C32 153.4(4) . . . . ? N5 C30 C31 C32 -27.7(5) . . . . ? O10 C30 C31 C36 -25.3(5) . . . . ? N5 C30 C31 C36 153.6(3) . . . . ? C36 C31 C32 C33 -0.9(6) . . . . ? C30 C31 C32 C33 -179.5(3) . . . . ? C31 C32 C33 C34 -0.1(6) . . . . ? C32 C33 C34 C35 0.5(7) . . . . ? C33 C34 C35 C36 0.2(7) . . . . ? C34 C35 C36 C31 -1.2(6) . . . . ? C32 C31 C36 C35 1.5(6) . . . . ? C30 C31 C36 C35 -179.8(3) . . . . ? Cl2 C41 Cl1 H14G -148(11) . . . . ? Cl2 C41 Cl1 H14E -100.4 . . . . ? O3 C15 N1 C11 173.4(3) . . . . ? N3 C15 N1 C11 -7.9(3) . . . . ? O3 C15 N1 C9 13.3(5) . . . . ? N3 C15 N1 C9 -168.1(3) . . . . ? N2 C11 N1 C15 -100.5(3) . . . . ? C12 C11 N1 C15 131.2(3) . . . . ? C17 C11 N1 C15 9.5(3) . . . . ? N2 C11 N1 C9 60.4(4) . . . . ? C12 C11 N1 C9 -67.9(3) . . . . ? C17 C11 N1 C9 170.4(2) . . . . ? C7 C9 N1 C15 83.8(4) . . . . ? C7 C9 N1 C11 -74.9(4) . . . . ? O4 C16 N2 C11 -173.4(3) . . . . ? N4 C16 N2 C11 8.8(3) . . . . ? O4 C16 N2 C10 -2.5(5) . . . . ? N4 C16 N2 C10 179.8(2) . . . . ? N1 C11 N2 C16 110.1(3) . . . . ? C12 C11 N2 C16 -125.0(3) . . . . ? C17 C11 N2 C16 0.0(3) . . . . ? N1 C11 N2 C10 -61.1(4) . . . . ? C12 C11 N2 C10 63.9(3) . . . . ? C17 C11 N2 C10 -171.1(2) . . . . ? C6 C10 N2 C16 -96.5(3) . . . . ? C6 C10 N2 C11 73.6(4) . . . . ? O3 C15 N3 C21 -9.0(5) . . . . ? N1 C15 N3 C21 172.3(3) . . . . ? O3 C15 N3 C17 -178.9(3) . . . . ? N1 C15 N3 C17 2.4(3) . . . . ? C23 C21 N3 C15 -89.9(3) . . . . ? C23 C21 N3 C17 79.0(3) . . . . ? N4 C17 N3 C15 113.6(3) . . . . ? C18 C17 N3 C15 -120.4(3) . . . . ? C11 C17 N3 C15 3.3(3) . . . . ? N4 C17 N3 C21 -56.3(4) . . . . ? C18 C17 N3 C21 69.7(3) . . . . ? C11 C17 N3 C21 -166.6(3) . . . . ? O4 C16 N4 C17 167.4(3) . . . . ? N2 C16 N4 C17 -14.9(3) . . . . ? O4 C16 N4 C22 18.8(4) . . . . ? N2 C16 N4 C22 -163.4(2) . . . . ? N3 C17 N4 C16 -96.2(3) . . . . ? C18 C17 N4 C16 136.5(3) . . . . ? C11 C17 N4 C16 14.2(3) . . . . ? N3 C17 N4 C22 53.1(3) . . . . ? C18 C17 N4 C22 -74.2(3) . . . . ? C11 C17 N4 C22 163.5(2) . . . . ? C24 C22 N4 C16 67.3(3) . . . . ? C24 C22 N4 C17 -79.2(3) . . . . ? O10 C30 N5 C25 0.6(5) . . . . ? C31 C30 N5 C25 -178.3(3) . . . . ? C26 C25 N5 C30 53.4(4) . . . . ? C24 C25 N5 C30 -128.7(3) . . . . ? C3 C2 O1 C1 0.0(5) . . . . ? C7 C2 O1 C1 -179.5(3) . . . . ? C4 C5 O2 C8 4.4(5) . . . . ? C6 C5 O2 C8 -176.2(3) . . . . ? O5 C12 O6 C13 12.3(7) . . . . ? C11 C12 O6 C13 -167.4(5) . . . . ? O5 C12 O6 C13' -21.3(10) . . . . ? C11 C12 O6 C13' 159.0(9) . . . . ? C14 C13 O6 C12 -94.1(6) . . . . ? C14 C13 O6 C13' -2.6(13) . . . . ? C14' C13' O6 C12 112.7(12) . . . . ? C14' C13' O6 C13 9.9(12) . . . . ? O7 C18 O8 C19 2.0(5) . . . . ? C17 C18 O8 C19 -180.0(3) . . . . ? C20 C19 O8 C18 -72.1(4) . . . . ? C27 C28 O9 C29 -3.8(5) . . . . ? C23 C28 O9 C29 176.8(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 O12 H12 O14 0.8(2) 1.80(17) 2.390(19) 126.0 . O14 H14H O10 0.82(15) 2.11(13) 2.764(8) 135(16) 9_654 C34 H34 O6 0.95 2.60 3.373(5) 138.8 13_657 C22 H22B O3 0.99 2.49 3.481(4) 175.3 5_545 C27 H27 O13 0.95 2.53 3.383(8) 150.1 5_545 C19 H19B O9 0.99 2.50 3.317(4) 139.5 5_545 C4 H4 O3 0.95 2.45 3.340(4) 155.2 13_656 N5 H5 O4 0.86(3) 2.37(2) 3.128(4) 147(3) . O13 H13 O11 0.83(7) 2.01(3) 2.811(13) 161(8) . O11 H11 O13 0.84 2.09 2.696(11) 128.5 11_666 O14 H14G Cl1 0.92(15) 2.58(16) 3.22(3) 127(16) . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.788 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.080