# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email icpg@iacs.res.in _publ_contact_author_name 'Pradyut Ghosh' loop_ _publ_author_name 'Pradyut Ghosh' 'M. Arunachalam' data_COMPLEX_1 _database_code_depnum_ccdc_archive 'CCDC 812289' #TrackingRef '- COMPLEX_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H128 F2 N14 O24' _chemical_formula_weight 1804.04 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.7347(17) _cell_length_b 17.1841(18) _cell_length_c 19.617(2) _cell_angle_alpha 101.428(3) _cell_angle_beta 109.835(2) _cell_angle_gamma 99.502(3) _cell_volume 4732.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5120 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9794 _exptl_absorpt_correction_T_max 0.9850 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38293 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 23.26 _reflns_number_total 13536 _reflns_number_gt 8002 _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 PLATON _computing_publication_material 'MERCURY 2.3' _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^)+(0.1103P)^2^+3.5134P] 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 13536 _refine_ls_number_parameters 1211 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1236 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.2304 _refine_ls_wR_factor_gt 0.1985 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.041 _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 C1A C 1.0138(7) 0.5738(6) 0.9798(6) 0.070(3) Uiso 0.587(12) 1 d PD A 1 C2A C 0.9173(9) 0.5125(9) 0.9571(8) 0.096(4) Uiso 0.587(12) 1 d PD . 1 O6A O 1.0757(6) 0.5297(6) 0.9828(5) 0.104(3) Uiso 0.587(12) 1 d P . 1 C1B C 0.9660(8) 0.5176(7) 0.9264(7) 0.051(4) Uiso 0.413(12) 1 d PD A 2 C2B C 0.9019(15) 0.4628(16) 0.9443(14) 0.128(8) Uiso 0.413(12) 1 d PD A 2 O6B O 1.024(2) 0.4818(16) 0.9377(16) 0.219(10) Uiso 0.413(12) 1 d P A 2 F1 F 0.34856(17) 0.78736(14) 0.98272(13) 0.0474(6) Uani 1 1 d D . . F2 F 0.62925(18) 0.80986(14) 0.02683(14) 0.0541(7) Uani 1 1 d D . . O1 O 0.5126(3) 0.8637(2) 0.08975(19) 0.0546(8) Uani 1 1 d D . . H1A H 0.551(2) 0.8493(19) 0.0632(17) 0.015(9) Uiso 1 1 d D . . H1B H 0.462(3) 0.838(3) 0.049(2) 0.09(2) Uiso 1 1 d D . . O2 O 0.4659(3) 0.75880(19) 0.9107(2) 0.0537(8) Uani 1 1 d D . . H2A H 0.521(2) 0.781(4) 0.946(3) 0.12(3) Uiso 1 1 d D . . H2B H 0.429(3) 0.7676(14) 0.934(3) 0.14(3) Uiso 1 1 d D . . O3 O 0.3157(3) 0.9183(2) 0.9327(2) 0.0680(10) Uani 1 1 d D . . H3A H 0.332(4) 0.881(3) 0.954(3) 0.09(2) Uiso 1 1 d D . . H3B H 0.340(5) 0.964(3) 0.968(3) 0.15(3) Uiso 1 1 d D . . O4 O 0.4529(4) 0.9614(2) 0.8771(3) 0.1030(15) Uani 1 1 d . . . O5 O 0.6340(3) 0.9368(2) 0.9583(3) 0.0919(13) Uani 1 1 d D . . H5A H 0.623(5) 0.893(3) 0.977(3) 0.12(2) Uiso 1 1 d D . . C6 C 0.3720(3) 0.6027(2) 0.9951(2) 0.0335(10) Uani 1 1 d . . . C7 C 0.2695(3) 0.5802(3) 0.9425(2) 0.0389(10) Uani 1 1 d . . . H7A H 0.2502 0.5226 0.9150 0.047 Uiso 1 1 calc R . . H7B H 0.2312 0.5895 0.9715 0.047 Uiso 1 1 calc R . . N8 N 0.2570(3) 0.6306(2) 0.8896(2) 0.0407(9) Uani 1 1 d . . . H8 H 0.287(3) 0.683(3) 0.909(2) 0.037(12) Uiso 1 1 d . . . C9 C 0.2170(3) 0.5989(3) 0.8142(3) 0.0417(11) Uani 1 1 d . . . O10 O 0.1814(2) 0.52538(19) 0.78316(17) 0.0530(8) Uani 1 1 d . . . C11 C 0.2227(3) 0.6585(3) 0.7680(2) 0.0405(11) Uani 1 1 d . . . C12 C 0.2377(3) 0.7427(3) 0.7947(3) 0.0527(13) Uani 1 1 d . . . H12 H 0.2420 0.7648 0.8434 0.063 Uiso 1 1 calc R . . C13 C 0.2463(4) 0.7944(3) 0.7505(3) 0.0602(14) Uani 1 1 d . . . H13 H 0.2563 0.8506 0.7694 0.072 Uiso 1 1 calc R . . C14 C 0.2402(4) 0.7625(3) 0.6781(3) 0.0590(14) Uani 1 1 d . . . H14 H 0.2468 0.7968 0.6480 0.071 Uiso 1 1 calc R . . C15 C 0.2239(3) 0.6789(3) 0.6515(2) 0.0495(12) Uani 1 1 d . . . C16 C 0.2146(3) 0.6262(3) 0.6947(2) 0.0479(12) Uani 1 1 d . . . H16 H 0.2030 0.5699 0.6750 0.058 Uiso 1 1 calc R . . N17 N 0.2197(4) 0.6450(3) 0.5749(2) 0.0716(13) Uani 1 1 d . . . O18 O 0.2007(4) 0.5713(3) 0.5504(2) 0.1057(16) Uani 1 1 d . . . O19 O 0.2387(3) 0.6920(3) 0.5397(2) 0.0863(12) Uani 1 1 d . . . C20 C 0.4394(3) 0.5858(2) 0.9668(2) 0.0336(10) Uani 1 1 d . . . C21 C 0.4086(3) 0.5368(2) 0.8852(2) 0.0365(10) Uani 1 1 d . . . H21A H 0.4391 0.4922 0.8831 0.044 Uiso 1 1 calc R . . H21B H 0.3417 0.5130 0.8646 0.044 Uiso 1 1 calc R . . N22 N 0.4311(3) 0.5877(3) 0.8391(2) 0.0397(9) Uani 1 1 d . . . H22 H 0.439(3) 0.635(3) 0.856(2) 0.036(14) Uiso 1 1 d . . . C23 C 0.4294(3) 0.5513(3) 0.7717(2) 0.0404(11) Uani 1 1 d . . . O24 O 0.4138(2) 0.47666(19) 0.74840(17) 0.0546(8) Uani 1 1 d . . . C25 C 0.4459(3) 0.6063(3) 0.7237(2) 0.0443(11) Uani 1 1 d . . . C26 C 0.4730(4) 0.6912(3) 0.7484(3) 0.0581(13) Uani 1 1 d . . . H26 H 0.4844 0.7178 0.7980 0.070 Uiso 1 1 calc R . . C27 C 0.4833(4) 0.7368(3) 0.6993(3) 0.0698(16) Uani 1 1 d . . . H27 H 0.5032 0.7937 0.7165 0.084 Uiso 1 1 calc R . . C28 C 0.4641(4) 0.6979(3) 0.6253(3) 0.0666(15) Uani 1 1 d . . . H28 H 0.4686 0.7279 0.5915 0.080 Uiso 1 1 calc R . . C29 C 0.4384(3) 0.6143(3) 0.6026(3) 0.0576(13) Uani 1 1 d . . . C30 C 0.4287(3) 0.5676(3) 0.6499(2) 0.0518(12) Uani 1 1 d . . . H30 H 0.4108 0.5106 0.6325 0.062 Uiso 1 1 calc R . . N31 N 0.4174(4) 0.5716(4) 0.5232(2) 0.0836(16) Uani 1 1 d . . . O32 O 0.4301(3) 0.6144(3) 0.4828(2) 0.0994(15) Uani 1 1 d . . . O33 O 0.3894(4) 0.4973(3) 0.5021(2) 0.129(2) Uani 1 1 d . . . C34 C 0.5344(3) 0.6097(2) 1.0138(2) 0.0343(10) Uani 1 1 d . . . C35 C 0.6054(3) 0.5874(2) 0.9822(2) 0.0412(11) Uani 1 1 d . . . H35A H 0.6510 0.5690 1.0186 0.049 Uiso 1 1 calc R . . H35B H 0.5740 0.5421 0.9369 0.049 Uiso 1 1 calc R . . N36 N 0.6540(2) 0.6561(2) 0.9644(2) 0.0430(9) Uani 1 1 d . . . H36 H 0.646(3) 0.715(3) 0.985(2) 0.053(13) Uiso 1 1 d . . . C37 C 0.7124(3) 0.6412(3) 0.9304(3) 0.0513(12) Uani 1 1 d . . . O38 O 0.7261(3) 0.5727(2) 0.9150(2) 0.0690(10) Uani 1 1 d . . . C39 C 0.7627(3) 0.7123(3) 0.9123(3) 0.0574(14) Uani 1 1 d . . . C40 C 0.7397(4) 0.7865(3) 0.9148(3) 0.0686(15) Uani 1 1 d . . . H40 H 0.6906 0.7951 0.9291 0.082 Uiso 1 1 calc R . . C41 C 0.7881(5) 0.8486(4) 0.8964(4) 0.0848(19) Uani 1 1 d . . . H41 H 0.7719 0.8983 0.8986 0.102 Uiso 1 1 calc R . . C42 C 0.8596(5) 0.8362(4) 0.8752(3) 0.0775(17) Uani 1 1 d . . . H42 H 0.8913 0.8774 0.8617 0.093 Uiso 1 1 calc R . . C43 C 0.8851(4) 0.7646(4) 0.8734(3) 0.0691(16) Uani 1 1 d . . . C44 C 0.8370(4) 0.6996(3) 0.8921(3) 0.0666(15) Uani 1 1 d . . . H44 H 0.8546 0.6504 0.8908 0.080 Uiso 1 1 calc R . . N45 N 0.9606(5) 0.7498(4) 0.8502(3) 0.0996(19) Uani 1 1 d . . . O46 O 0.9854(4) 0.6860(4) 0.8530(3) 0.125(2) Uani 1 1 d . . . O47 O 0.9983(4) 0.8034(3) 0.8291(3) 0.1206(19) Uani 1 1 d . . . C48 C 0.5619(3) 0.6529(2) 1.0901(2) 0.0367(10) Uani 1 1 d . . . C49 C 0.6644(3) 0.6780(2) 1.1417(3) 0.0481(12) Uani 1 1 d . . . H49A H 0.6707 0.6639 1.1884 0.058 Uiso 1 1 calc R . . H49B H 0.6980 0.6469 1.1181 0.058 Uiso 1 1 calc R . . N50 N 0.7070(3) 0.7648(2) 1.1591(2) 0.0447(10) Uani 1 1 d . . . H50 H 0.696(3) 0.785(3) 1.125(3) 0.047(15) Uiso 1 1 d . . . C51 C 0.7761(3) 0.8066(3) 1.2250(3) 0.0449(11) Uani 1 1 d . . . O52 O 0.8019(2) 0.77525(19) 1.27730(18) 0.0675(10) Uani 1 1 d . . . C53 C 0.8226(3) 0.8936(2) 1.2338(2) 0.0400(10) Uani 1 1 d . . . C54 C 0.7938(3) 0.9363(3) 1.1808(2) 0.0441(11) Uani 1 1 d . . . H54 H 0.7431 0.9100 1.1358 0.053 Uiso 1 1 calc R . . C55 C 0.8387(3) 1.0171(3) 1.1932(3) 0.0493(12) Uani 1 1 d . . . H55 H 0.8177 1.0445 1.1568 0.059 Uiso 1 1 calc R . . C56 C 0.9143(3) 1.0572(3) 1.2593(3) 0.0476(12) Uani 1 1 d . . . H56 H 0.9448 1.1117 1.2683 0.057 Uiso 1 1 calc R . . C57 C 0.9433(3) 1.0140(3) 1.3116(2) 0.0438(11) Uani 1 1 d . . . C58 C 0.8999(3) 0.9335(3) 1.3002(2) 0.0421(11) Uani 1 1 d . . . H58 H 0.9218 0.9060 1.3364 0.050 Uiso 1 1 calc R . . N59 N 1.0246(3) 1.0553(3) 1.3824(2) 0.0549(10) Uani 1 1 d . . . O60 O 1.0582(2) 1.1291(2) 1.3940(2) 0.0676(10) Uani 1 1 d . . . O61 O 1.0548(3) 1.0161(2) 1.4262(2) 0.0754(11) Uani 1 1 d . . . C62 C 0.4946(3) 0.6703(2) 1.1183(2) 0.0376(10) Uani 1 1 d . . . C63 C 0.5247(3) 0.7181(3) 1.2007(2) 0.0467(12) Uani 1 1 d . . . H63A H 0.5000 0.6837 1.2268 0.056 Uiso 1 1 calc R . . H63B H 0.5922 0.7328 1.2248 0.056 Uiso 1 1 calc R . . N64 N 0.4904(3) 0.7935(2) 1.2064(2) 0.0513(11) Uani 1 1 d . . . H64 H 0.511(3) 0.820(3) 1.179(3) 0.056(15) Uiso 1 1 d . . . C65 C 0.4481(3) 0.8141(3) 1.2532(3) 0.0494(12) Uani 1 1 d . . . O66 O 0.4388(2) 0.7748(2) 1.29723(17) 0.0601(9) Uani 1 1 d . . . C67 C 0.4061(4) 0.8866(3) 1.2480(3) 0.0545(13) Uani 1 1 d . . . C68 C 0.4258(4) 0.9429(3) 1.2110(3) 0.0685(15) Uani 1 1 d . . . H68 H 0.4672 0.9373 1.1871 0.082 Uiso 1 1 calc R . . C69 C 0.3833(5) 1.0096(3) 1.2093(4) 0.0806(18) Uani 1 1 d . . . H69 H 0.3960 1.0472 1.1836 0.097 Uiso 1 1 calc R . . C70 C 0.3228(4) 1.0185(3) 1.2460(3) 0.0726(16) Uani 1 1 d . . . H70 H 0.2943 1.0618 1.2453 0.087 Uiso 1 1 calc R . . C71 C 0.3060(4) 0.9625(3) 1.2833(3) 0.0659(15) Uani 1 1 d . . . C72 C 0.3462(4) 0.8968(3) 1.2856(3) 0.0641(15) Uani 1 1 d . . . H72 H 0.3335 0.8599 1.3119 0.077 Uiso 1 1 calc R . . N73 N 0.2451(4) 0.9730(4) 1.3245(3) 0.0961(18) Uani 1 1 d . . . O74 O 0.2095(4) 1.0306(3) 1.3230(3) 0.1062(15) Uani 1 1 d . . . O75 O 0.2310(6) 0.9241(5) 1.3575(5) 0.197(4) Uani 1 1 d . . . C76 C 0.3999(3) 0.6430(2) 1.0717(2) 0.0378(10) Uani 1 1 d . . . C77 C 0.3257(3) 0.6551(3) 1.1039(2) 0.0440(11) Uani 1 1 d . . . H77A H 0.2782 0.6039 1.0868 0.053 Uiso 1 1 calc R . . H77B H 0.3543 0.6693 1.1584 0.053 Uiso 1 1 calc R . . N78 N 0.2818(3) 0.7194(2) 1.0811(2) 0.0450(10) Uani 1 1 d . . . H78 H 0.307(3) 0.747(2) 1.058(2) 0.038(12) Uiso 1 1 d . . . C79 C 0.2194(3) 0.7416(3) 1.1083(3) 0.0497(12) Uani 1 1 d . . . O80 O 0.1977(3) 0.7100(2) 1.1532(2) 0.0649(10) Uani 1 1 d . . . C81 C 0.1760(3) 0.8076(3) 1.0821(3) 0.0502(12) Uani 1 1 d . . . C82 C 0.1831(4) 0.8357(3) 1.0231(3) 0.0681(15) Uani 1 1 d . . . H82 H 0.2163 0.8131 0.9966 0.082 Uiso 1 1 calc R . . C83 C 0.1416(4) 0.8972(4) 1.0021(4) 0.0742(17) Uani 1 1 d . . . H83 H 0.1484 0.9156 0.9623 0.089 Uiso 1 1 calc R . . C84 C 0.0916(4) 0.9306(3) 1.0385(3) 0.0675(15) Uani 1 1 d . . . H84 H 0.0634 0.9715 1.0244 0.081 Uiso 1 1 calc R . . C85 C 0.0843(4) 0.9018(3) 1.0971(3) 0.0664(15) Uani 1 1 d . . . C86 C 0.1245(3) 0.8405(3) 1.1192(3) 0.0594(14) Uani 1 1 d . . . H86 H 0.1168 0.8218 1.1586 0.071 Uiso 1 1 calc R . . N87 N 0.0322(4) 0.9383(3) 1.1384(4) 0.0972(19) Uani 1 1 d . . . O88 O -0.0157(4) 0.9832(3) 1.1102(4) 0.144(2) Uani 1 1 d . . . N90 N 0.1003(2) 0.6176(2) 0.3085(2) 0.0464(9) Uani 1 1 d . . . C91 C 0.1429(3) 0.7038(3) 0.3606(3) 0.0498(12) Uani 1 1 d . . . H91A H 0.1560 0.7406 0.3317 0.060 Uiso 1 1 calc R . . H91B H 0.2018 0.7050 0.3989 0.060 Uiso 1 1 calc R . . C92 C 0.0808(3) 0.7358(3) 0.3995(3) 0.0574(13) Uani 1 1 d . . . H92A H 0.0218 0.7348 0.3612 0.069 Uiso 1 1 calc R . . H92B H 0.0676 0.6991 0.4284 0.069 Uiso 1 1 calc R . . C93 C 0.1244(4) 0.8225(3) 0.4516(3) 0.0697(15) Uani 1 1 d . . . H93A H 0.1865 0.8254 0.4866 0.084 Uiso 1 1 calc R . . H93B H 0.1304 0.8606 0.4221 0.084 Uiso 1 1 calc R . . C94 C 0.0662(4) 0.8468(3) 0.4951(4) 0.0832(19) Uani 1 1 d . . . H94A H 0.0039 0.8412 0.4606 0.125 Uiso 1 1 calc R . . H94B H 0.0930 0.9028 0.5249 0.125 Uiso 1 1 calc R . . H94C H 0.0645 0.8120 0.5275 0.125 Uiso 1 1 calc R . . C95 C 0.0039(3) 0.6095(3) 0.2490(3) 0.0527(12) Uani 1 1 d . . . H95A H -0.0164 0.5556 0.2135 0.063 Uiso 1 1 calc R . . H95B H -0.0399 0.6125 0.2737 0.063 Uiso 1 1 calc R . . C96 C -0.0008(3) 0.6729(3) 0.2057(3) 0.0551(13) Uani 1 1 d . . . H96A H 0.0198 0.7273 0.2405 0.066 Uiso 1 1 calc R . . H96B H 0.0407 0.6692 0.1789 0.066 Uiso 1 1 calc R . . C97 C -0.0984(3) 0.6604(3) 0.1506(3) 0.0673(15) Uani 1 1 d . . . H97A H -0.1402 0.6612 0.1773 0.081 Uiso 1 1 calc R . . H97B H -0.1177 0.6069 0.1146 0.081 Uiso 1 1 calc R . . C99 C 0.0905(3) 0.5588(3) 0.3561(3) 0.0502(12) Uani 1 1 d . . . H99A H 0.1496 0.5709 0.3984 0.060 Uiso 1 1 calc R . . H99B H 0.0444 0.5707 0.3765 0.060 Uiso 1 1 calc R . . O89 O 0.0352(4) 0.9204(3) 1.1967(3) 0.1115(17) Uani 1 1 d . . . C98 C -0.1067(4) 0.7255(4) 0.1087(3) 0.0783(17) Uani 1 1 d . . . H98A H -0.0836 0.7788 0.1442 0.118 Uiso 1 1 calc R . . H98B H -0.1710 0.7180 0.0774 0.118 Uiso 1 1 calc R . . H98C H -0.0707 0.7209 0.0778 0.118 Uiso 1 1 calc R . . C100 C 0.0629(3) 0.4678(3) 0.3174(3) 0.0514(12) Uani 1 1 d . . . H10I H 0.1094 0.4535 0.2986 0.062 Uiso 1 1 calc R . . H10J H 0.0034 0.4536 0.2751 0.062 Uiso 1 1 calc R . . C101 C 0.0554(4) 0.4210(3) 0.3741(3) 0.0671(15) Uani 1 1 d . . . H10P H 0.0075 0.4351 0.3913 0.081 Uiso 1 1 calc R . . H10Q H 0.1141 0.4387 0.4174 0.081 Uiso 1 1 calc R . . C102 C 0.0321(4) 0.3284(3) 0.3434(3) 0.0791(17) Uani 1 1 d . . . H10R H -0.0290 0.3095 0.3040 0.119 Uiso 1 1 calc R . . H10S H 0.0334 0.3033 0.3832 0.119 Uiso 1 1 calc R . . H10T H 0.0773 0.3139 0.3238 0.119 Uiso 1 1 calc R . . C103 C 0.1626(3) 0.5963(3) 0.2671(2) 0.0480(12) Uani 1 1 d . . . H10A H 0.1321 0.5424 0.2319 0.058 Uiso 1 1 calc R . . H10B H 0.1662 0.6350 0.2376 0.058 Uiso 1 1 calc R . . C104 C 0.2611(3) 0.5958(3) 0.3136(3) 0.0492(12) Uani 1 1 d . . . H10C H 0.2971 0.6512 0.3425 0.059 Uiso 1 1 calc R . . H10D H 0.2603 0.5630 0.3484 0.059 Uiso 1 1 calc R . . C105 C 0.3050(3) 0.5601(3) 0.2612(3) 0.0554(13) Uani 1 1 d . . . H10K H 0.2719 0.5029 0.2367 0.066 Uiso 1 1 calc R . . H10L H 0.2969 0.5886 0.2223 0.066 Uiso 1 1 calc R . . C106 C 0.4066(4) 0.5651(3) 0.2987(3) 0.0657(15) Uani 1 1 d . . . H10M H 0.4412 0.6216 0.3179 0.099 Uiso 1 1 calc R . . H10N H 0.4278 0.5367 0.2628 0.099 Uiso 1 1 calc R . . H10O H 0.4161 0.5402 0.3395 0.099 Uiso 1 1 calc R . . N107 N 0.6701(2) 0.7861(2) 0.48272(19) 0.0441(9) Uani 1 1 d . . . C108 C 0.7197(3) 0.7845(3) 0.5645(2) 0.0456(11) Uani 1 1 d . . . H10G H 0.7862 0.7945 0.5757 0.055 Uiso 1 1 calc R . . H10H H 0.7104 0.8295 0.5974 0.055 Uiso 1 1 calc R . . C109 C 0.6894(3) 0.7070(3) 0.5833(2) 0.0505(12) Uani 1 1 d . . . H10E H 0.7124 0.6641 0.5606 0.061 Uiso 1 1 calc R . . H10F H 0.6217 0.6895 0.5626 0.061 Uiso 1 1 calc R . . C110 C 0.7260(4) 0.7197(3) 0.6681(3) 0.0615(14) Uani 1 1 d . . . H11E H 0.7933 0.7412 0.6890 0.074 Uiso 1 1 calc R . . H11F H 0.6996 0.7601 0.6901 0.074 Uiso 1 1 calc R . . C111 C 0.7028(4) 0.6420(3) 0.6893(3) 0.0764(17) Uani 1 1 d . . . H11M H 0.6364 0.6195 0.6674 0.115 Uiso 1 1 calc R . . H11N H 0.7243 0.6537 0.7431 0.115 Uiso 1 1 calc R . . H11O H 0.7327 0.6032 0.6709 0.115 Uiso 1 1 calc R . . C112 C 0.5681(3) 0.7829(3) 0.4670(3) 0.0500(12) Uani 1 1 d . . . H11C H 0.5392 0.7308 0.4715 0.060 Uiso 1 1 calc R . . H11D H 0.5381 0.7837 0.4151 0.060 Uiso 1 1 calc R . . C113 C 0.5481(3) 0.8508(3) 0.5169(3) 0.0591(13) Uani 1 1 d . . . H11G H 0.5694 0.8457 0.5680 0.071 Uiso 1 1 calc R . . H11H H 0.5825 0.9035 0.5177 0.071 Uiso 1 1 calc R . . C114 C 0.4458(4) 0.8477(4) 0.4898(3) 0.0756(17) Uani 1 1 d . . . H11I H 0.4113 0.7939 0.4865 0.091 Uiso 1 1 calc R . . H11J H 0.4253 0.8553 0.4396 0.091 Uiso 1 1 calc R . . C115 C 0.4232(5) 0.9131(5) 0.5416(4) 0.114(3) Uani 1 1 d . . . H11U H 0.4418 0.9049 0.5910 0.171 Uiso 1 1 calc R . . H11V H 0.3574 0.9089 0.5217 0.171 Uiso 1 1 calc R . . H11W H 0.4565 0.9666 0.5445 0.171 Uiso 1 1 calc R . . C116 C 0.6745(3) 0.7128(3) 0.4285(3) 0.0521(12) Uani 1 1 d . . . H11A H 0.6391 0.7137 0.3775 0.062 Uiso 1 1 calc R . . H11B H 0.6444 0.6634 0.4365 0.062 Uiso 1 1 calc R . . C117 C 0.7723(4) 0.7079(3) 0.4350(3) 0.0652(15) Uani 1 1 d . . . H11K H 0.7937 0.7438 0.4084 0.078 Uiso 1 1 calc R . . H11L H 0.8141 0.7274 0.4876 0.078 Uiso 1 1 calc R . . C118 C 0.7766(4) 0.6248(4) 0.4041(4) 0.100(2) Uani 1 1 d . . . H11S H 0.7303 0.6035 0.3530 0.120 Uiso 1 1 calc R . . H11T H 0.7606 0.5901 0.4337 0.120 Uiso 1 1 calc R . . C119 C 0.8710(5) 0.6197(4) 0.4034(5) 0.123(3) Uani 1 1 d . . . H11P H 0.8878 0.6544 0.3748 0.184 Uiso 1 1 calc R . . H11Q H 0.8687 0.5641 0.3808 0.184 Uiso 1 1 calc R . . H11R H 0.9167 0.6374 0.4541 0.184 Uiso 1 1 calc R . . C120 C 0.7205(3) 0.8658(3) 0.4754(3) 0.0494(12) Uani 1 1 d . . . H12A H 0.7241 0.9107 0.5159 0.059 Uiso 1 1 calc R . . H12B H 0.7839 0.8633 0.4821 0.059 Uiso 1 1 calc R . . C121 C 0.6760(4) 0.8851(3) 0.4015(3) 0.0557(13) Uani 1 1 d . . . H12E H 0.6151 0.8940 0.3963 0.067 Uiso 1 1 calc R . . H12F H 0.6677 0.8392 0.3600 0.067 Uiso 1 1 calc R . . C122 C 0.7384(4) 0.9618(3) 0.3993(3) 0.0578(13) Uani 1 1 d . . . H12C H 0.7518 1.0057 0.4440 0.069 Uiso 1 1 calc R . . H12D H 0.7972 0.9506 0.4003 0.069 Uiso 1 1 calc R . . C123 C 0.6945(4) 0.9902(3) 0.3299(3) 0.0697(16) Uani 1 1 d . . . H12G H 0.6787 0.9463 0.2855 0.105 Uiso 1 1 calc R . . H12H H 0.7379 1.0363 0.3296 0.105 Uiso 1 1 calc R . . H12I H 0.6390 1.0059 0.3308 0.105 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0574(16) 0.0389(14) 0.0528(16) 0.0194(12) 0.0244(13) 0.0148(12) F2 0.0635(17) 0.0390(14) 0.0492(15) 0.0160(12) 0.0100(13) 0.0060(12) O1 0.063(2) 0.054(2) 0.044(2) 0.0146(17) 0.018(2) 0.0102(18) O2 0.066(2) 0.0399(19) 0.051(2) 0.0134(16) 0.021(2) 0.0043(18) O3 0.078(3) 0.049(2) 0.073(3) 0.030(2) 0.015(2) 0.015(2) O4 0.144(4) 0.066(3) 0.105(3) 0.021(2) 0.068(3) 0.000(3) O5 0.137(4) 0.050(2) 0.118(4) 0.034(2) 0.079(3) 0.023(2) C6 0.042(3) 0.026(2) 0.036(2) 0.0182(19) 0.013(2) 0.0098(19) C7 0.048(3) 0.036(2) 0.038(2) 0.021(2) 0.018(2) 0.011(2) N8 0.047(2) 0.030(2) 0.041(2) 0.0136(18) 0.0096(18) 0.0078(18) C9 0.038(3) 0.038(3) 0.045(3) 0.017(2) 0.008(2) 0.009(2) O10 0.054(2) 0.0380(19) 0.0500(19) 0.0142(16) 0.0053(16) -0.0023(16) C11 0.040(3) 0.040(3) 0.034(3) 0.014(2) 0.001(2) 0.012(2) C12 0.074(3) 0.041(3) 0.038(3) 0.013(2) 0.012(2) 0.017(2) C13 0.089(4) 0.039(3) 0.045(3) 0.015(2) 0.013(3) 0.018(3) C14 0.073(4) 0.056(3) 0.050(3) 0.030(3) 0.016(3) 0.021(3) C15 0.062(3) 0.046(3) 0.032(3) 0.011(2) 0.006(2) 0.015(2) C16 0.051(3) 0.036(3) 0.040(3) 0.010(2) -0.001(2) 0.008(2) N17 0.108(4) 0.056(3) 0.044(3) 0.016(2) 0.020(3) 0.020(3) O18 0.189(5) 0.066(3) 0.049(2) 0.007(2) 0.040(3) 0.020(3) O19 0.132(4) 0.082(3) 0.052(2) 0.031(2) 0.035(2) 0.030(3) C20 0.042(3) 0.021(2) 0.040(2) 0.0187(19) 0.013(2) 0.0074(18) C21 0.046(3) 0.030(2) 0.035(2) 0.0142(19) 0.015(2) 0.0061(19) N22 0.053(2) 0.028(2) 0.040(2) 0.0153(19) 0.0182(19) 0.0082(19) C23 0.040(3) 0.041(3) 0.040(3) 0.017(2) 0.013(2) 0.007(2) O24 0.076(2) 0.039(2) 0.052(2) 0.0103(16) 0.0337(18) 0.0069(17) C25 0.044(3) 0.045(3) 0.042(3) 0.015(2) 0.016(2) 0.002(2) C26 0.077(4) 0.051(3) 0.047(3) 0.021(2) 0.027(3) 0.005(3) C27 0.097(4) 0.050(3) 0.069(4) 0.026(3) 0.042(3) 0.001(3) C28 0.080(4) 0.071(4) 0.052(3) 0.032(3) 0.029(3) 0.003(3) C29 0.057(3) 0.063(4) 0.036(3) 0.008(3) 0.012(2) -0.008(3) C30 0.056(3) 0.053(3) 0.040(3) 0.012(2) 0.019(2) -0.003(2) N31 0.100(4) 0.091(4) 0.040(3) 0.011(3) 0.028(3) -0.020(3) O32 0.115(4) 0.121(4) 0.044(2) 0.027(2) 0.029(2) -0.019(3) O33 0.200(6) 0.089(4) 0.057(3) -0.010(2) 0.058(3) -0.052(4) C34 0.042(3) 0.022(2) 0.042(3) 0.0192(19) 0.015(2) 0.0071(19) C35 0.042(3) 0.032(2) 0.048(3) 0.019(2) 0.013(2) 0.005(2) N36 0.045(2) 0.039(2) 0.045(2) 0.0157(18) 0.0180(19) 0.0036(18) C37 0.060(3) 0.038(3) 0.046(3) 0.008(2) 0.016(3) -0.002(2) O38 0.079(3) 0.052(2) 0.085(3) 0.0090(19) 0.053(2) 0.0037(19) C39 0.056(3) 0.066(4) 0.038(3) 0.003(2) 0.020(2) -0.006(3) C40 0.079(4) 0.053(3) 0.074(4) 0.026(3) 0.031(3) 0.002(3) C41 0.094(5) 0.073(4) 0.098(5) 0.034(4) 0.051(4) 0.005(4) C42 0.105(5) 0.061(4) 0.061(4) 0.016(3) 0.037(4) -0.003(4) C43 0.074(4) 0.080(4) 0.046(3) 0.002(3) 0.037(3) -0.014(3) C44 0.082(4) 0.061(3) 0.048(3) 0.002(3) 0.031(3) -0.003(3) N45 0.123(5) 0.088(4) 0.093(4) 0.011(4) 0.071(4) -0.009(4) O46 0.153(5) 0.110(4) 0.174(5) 0.052(4) 0.131(5) 0.035(4) O47 0.153(5) 0.094(3) 0.130(4) 0.014(3) 0.106(4) -0.021(3) C48 0.042(3) 0.025(2) 0.036(3) 0.0176(19) 0.003(2) 0.0047(19) C49 0.056(3) 0.027(2) 0.056(3) 0.016(2) 0.012(2) 0.010(2) N50 0.047(2) 0.033(2) 0.041(2) 0.013(2) 0.003(2) 0.0028(18) C51 0.049(3) 0.038(3) 0.039(3) 0.011(2) 0.008(2) 0.008(2) O52 0.078(3) 0.048(2) 0.049(2) 0.0205(17) -0.0043(18) -0.0039(18) C53 0.039(3) 0.034(2) 0.040(3) 0.009(2) 0.009(2) 0.005(2) C54 0.045(3) 0.036(3) 0.040(3) 0.006(2) 0.009(2) 0.003(2) C55 0.056(3) 0.041(3) 0.051(3) 0.016(2) 0.021(3) 0.009(2) C56 0.051(3) 0.033(3) 0.053(3) 0.006(2) 0.021(3) 0.001(2) C57 0.038(3) 0.041(3) 0.045(3) 0.004(2) 0.014(2) 0.003(2) C58 0.046(3) 0.037(3) 0.042(3) 0.013(2) 0.014(2) 0.012(2) N59 0.042(2) 0.050(3) 0.055(3) 0.002(2) 0.012(2) -0.003(2) O60 0.053(2) 0.048(2) 0.076(3) 0.0011(18) 0.0117(19) -0.0070(17) O61 0.066(3) 0.067(2) 0.061(2) 0.014(2) -0.0067(19) 0.002(2) C62 0.054(3) 0.027(2) 0.035(2) 0.0179(19) 0.016(2) 0.012(2) C63 0.061(3) 0.038(3) 0.039(3) 0.017(2) 0.012(2) 0.018(2) N64 0.071(3) 0.044(2) 0.038(2) 0.016(2) 0.019(2) 0.014(2) C65 0.074(3) 0.042(3) 0.034(3) 0.012(2) 0.023(3) 0.014(2) O66 0.089(3) 0.056(2) 0.0402(19) 0.0173(17) 0.0256(18) 0.0242(19) C67 0.074(4) 0.050(3) 0.035(3) 0.009(2) 0.017(3) 0.015(3) C68 0.099(4) 0.053(3) 0.071(4) 0.026(3) 0.046(3) 0.026(3) C69 0.115(5) 0.061(4) 0.092(5) 0.038(3) 0.054(4) 0.037(4) C70 0.101(5) 0.051(3) 0.071(4) 0.015(3) 0.036(4) 0.029(3) C71 0.087(4) 0.062(4) 0.053(3) 0.012(3) 0.031(3) 0.023(3) C72 0.097(4) 0.056(3) 0.043(3) 0.010(2) 0.032(3) 0.023(3) N73 0.142(5) 0.072(4) 0.114(5) 0.027(3) 0.084(4) 0.052(4) O74 0.127(4) 0.065(3) 0.137(4) 0.002(3) 0.074(3) 0.033(3) O75 0.334(10) 0.194(7) 0.279(9) 0.169(7) 0.268(9) 0.180(7) C76 0.052(3) 0.029(2) 0.039(3) 0.023(2) 0.016(2) 0.013(2) C77 0.059(3) 0.043(3) 0.041(3) 0.021(2) 0.025(2) 0.018(2) N78 0.057(3) 0.043(2) 0.052(2) 0.027(2) 0.031(2) 0.0180(19) C79 0.059(3) 0.044(3) 0.056(3) 0.018(2) 0.031(3) 0.017(2) O80 0.092(3) 0.065(2) 0.073(2) 0.038(2) 0.058(2) 0.033(2) C81 0.055(3) 0.050(3) 0.060(3) 0.019(2) 0.035(3) 0.019(2) C82 0.070(4) 0.078(4) 0.091(4) 0.048(3) 0.047(3) 0.044(3) C83 0.074(4) 0.084(4) 0.099(5) 0.054(4) 0.050(4) 0.041(3) C84 0.064(4) 0.059(3) 0.098(4) 0.034(3) 0.040(3) 0.028(3) C85 0.068(4) 0.056(3) 0.102(5) 0.025(3) 0.055(3) 0.032(3) C86 0.063(3) 0.053(3) 0.078(4) 0.021(3) 0.042(3) 0.019(3) N87 0.106(4) 0.065(4) 0.165(6) 0.038(4) 0.095(5) 0.038(3) O88 0.173(5) 0.125(4) 0.261(7) 0.115(5) 0.166(5) 0.113(4) N90 0.042(2) 0.048(2) 0.047(2) 0.0176(19) 0.0150(19) 0.0057(18) C91 0.049(3) 0.041(3) 0.055(3) 0.015(2) 0.018(2) 0.004(2) C92 0.055(3) 0.058(3) 0.057(3) 0.016(3) 0.020(3) 0.010(3) C93 0.074(4) 0.043(3) 0.093(4) 0.011(3) 0.039(3) 0.009(3) C94 0.091(4) 0.054(4) 0.111(5) 0.004(3) 0.060(4) 0.012(3) C95 0.042(3) 0.059(3) 0.053(3) 0.017(3) 0.014(2) 0.006(2) C96 0.048(3) 0.062(3) 0.054(3) 0.021(3) 0.014(3) 0.013(2) C97 0.047(3) 0.080(4) 0.066(4) 0.025(3) 0.009(3) 0.014(3) C99 0.051(3) 0.053(3) 0.053(3) 0.024(2) 0.024(2) 0.009(2) O89 0.148(5) 0.094(4) 0.132(4) 0.026(3) 0.095(4) 0.050(3) C98 0.061(4) 0.104(5) 0.068(4) 0.036(4) 0.014(3) 0.023(3) C100 0.048(3) 0.047(3) 0.055(3) 0.017(2) 0.014(2) 0.008(2) C101 0.079(4) 0.051(3) 0.070(4) 0.021(3) 0.030(3) 0.008(3) C102 0.086(4) 0.057(4) 0.091(4) 0.028(3) 0.026(4) 0.016(3) C103 0.048(3) 0.051(3) 0.042(3) 0.016(2) 0.015(2) 0.006(2) C104 0.053(3) 0.046(3) 0.049(3) 0.014(2) 0.022(2) 0.005(2) C105 0.067(4) 0.061(3) 0.056(3) 0.029(3) 0.032(3) 0.028(3) C106 0.067(4) 0.067(4) 0.080(4) 0.030(3) 0.040(3) 0.024(3) N107 0.044(2) 0.042(2) 0.038(2) 0.0144(18) 0.0078(17) 0.0003(17) C108 0.038(3) 0.051(3) 0.038(3) 0.014(2) 0.006(2) 0.001(2) C109 0.057(3) 0.045(3) 0.044(3) 0.014(2) 0.015(2) 0.005(2) C110 0.062(3) 0.063(3) 0.047(3) 0.026(3) 0.007(3) -0.001(3) C111 0.080(4) 0.082(4) 0.055(3) 0.038(3) 0.010(3) 0.003(3) C112 0.040(3) 0.060(3) 0.044(3) 0.023(2) 0.009(2) 0.004(2) C113 0.050(3) 0.065(3) 0.064(3) 0.024(3) 0.021(3) 0.015(3) C114 0.065(4) 0.101(5) 0.080(4) 0.047(4) 0.032(3) 0.035(3) C115 0.088(5) 0.131(6) 0.140(7) 0.032(5) 0.055(5) 0.056(5) C116 0.058(3) 0.043(3) 0.048(3) 0.012(2) 0.017(2) 0.002(2) C117 0.071(4) 0.059(3) 0.068(4) 0.012(3) 0.038(3) 0.004(3) C118 0.068(4) 0.069(4) 0.145(6) -0.008(4) 0.050(4) -0.004(3) C119 0.103(5) 0.061(4) 0.200(8) -0.022(5) 0.099(6) -0.008(4) C120 0.053(3) 0.045(3) 0.047(3) 0.020(2) 0.016(2) 0.003(2) C121 0.065(3) 0.050(3) 0.050(3) 0.020(2) 0.019(3) 0.010(3) C122 0.074(4) 0.050(3) 0.062(3) 0.024(3) 0.036(3) 0.016(3) C123 0.090(4) 0.069(4) 0.079(4) 0.042(3) 0.051(3) 0.031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A O6A 1.323(11) . ? C1A C2A 1.562(15) . ? C2A O6A 1.486(15) 2_767 ? O6A C2A 1.486(15) 2_767 ? C1B O6B 1.16(2) . ? C1B C2B 1.444(19) . ? F1 F1 0.000(5) 1 ? F2 F2 0.000(6) 1 ? O1 H1A 0.958(18) . ? O1 H1B 0.89(2) . ? O2 O2 0.0000 1 ? O2 H2A 0.87(2) . ? O2 H2B 0.86(2) . ? O3 H3A 0.86(2) . ? O3 H3B 0.86(2) . ? O5 H5A 0.91(2) . ? C6 C20 1.398(6) . ? C6 C76 1.402(6) . ? C6 C7 1.524(6) . ? C7 N8 1.461(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? N8 C9 1.349(6) . ? N8 H8 0.89(4) . ? C9 O10 1.229(5) . ? C9 C11 1.507(6) . ? C11 C12 1.388(6) . ? C11 C16 1.390(6) . ? C12 C13 1.381(6) . ? C12 H12 0.9300 . ? C13 C14 1.381(7) . ? C13 H13 0.9300 . ? C14 C15 1.377(6) . ? C14 H14 0.9300 . ? C15 C16 1.378(6) . ? C15 N17 1.475(6) . ? C16 H16 0.9300 . ? N17 O18 1.209(5) . ? N17 O19 1.224(5) . ? C20 C34 1.402(6) . ? C20 C21 1.521(5) . ? C21 N22 1.461(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? N22 C23 1.336(6) . ? N22 H22 0.78(4) . ? C23 O24 1.225(5) . ? C23 C25 1.511(6) . ? C25 C30 1.381(6) . ? C25 C26 1.386(6) . ? C26 C27 1.390(6) . ? C26 H26 0.9300 . ? C27 C28 1.378(7) . ? C27 H27 0.9300 . ? C28 C29 1.363(7) . ? C28 H28 0.9300 . ? C29 C30 1.371(6) . ? C29 N31 1.481(6) . ? C30 H30 0.9300 . ? N31 O33 1.215(6) . ? N31 O32 1.224(5) . ? C34 C48 1.412(6) . ? C34 C35 1.515(6) . ? C35 N36 1.466(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? N36 C37 1.334(6) . ? N36 H36 1.06(5) . ? C37 O38 1.229(6) . ? C37 C39 1.513(7) . ? C39 C40 1.379(7) . ? C39 C44 1.391(7) . ? C40 C41 1.385(7) . ? C40 H40 0.9300 . ? C41 C42 1.358(8) . ? C41 H41 0.9300 . ? C42 C43 1.354(8) . ? C42 H42 0.9300 . ? C43 C44 1.423(7) . ? C43 N45 1.450(8) . ? C44 H44 0.9300 . ? N45 O46 1.228(7) . ? N45 O47 1.229(6) . ? C48 C62 1.398(6) . ? C48 C49 1.517(6) . ? C49 N50 1.450(5) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? N50 C51 1.338(6) . ? N50 H50 0.79(4) . ? C51 O52 1.231(5) . ? C51 C53 1.500(6) . ? C53 C54 1.385(6) . ? C53 C58 1.393(6) . ? C54 C55 1.383(6) . ? C54 H54 0.9300 . ? C55 C56 1.378(6) . ? C55 H55 0.9300 . ? C56 C57 1.382(6) . ? C56 H56 0.9300 . ? C57 C58 1.377(6) . ? C57 N59 1.474(6) . ? C58 H58 0.9300 . ? N59 O61 1.214(5) . ? N59 O60 1.235(5) . ? C62 C76 1.397(6) . ? C62 C63 1.529(6) . ? C63 N64 1.483(6) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? N64 C65 1.332(6) . ? N64 H64 0.87(5) . ? C65 O66 1.228(5) . ? C65 C67 1.510(7) . ? C67 C68 1.374(7) . ? C67 C72 1.392(7) . ? C68 C69 1.420(7) . ? C68 H68 0.9300 . ? C69 C70 1.385(8) . ? C69 H69 0.9300 . ? C70 C71 1.363(7) . ? C70 H70 0.9300 . ? C71 C72 1.384(7) . ? C71 N73 1.458(7) . ? C72 H72 0.9300 . ? N73 O75 1.195(7) . ? N73 O74 1.217(6) . ? C76 C77 1.528(6) . ? C77 N78 1.461(5) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? N78 C79 1.339(6) . ? N78 H78 0.87(4) . ? C79 O80 1.233(5) . ? C79 C81 1.505(6) . ? C81 C82 1.370(6) . ? C81 C86 1.376(6) . ? C82 C83 1.389(7) . ? C82 H82 0.9300 . ? C83 C84 1.352(7) . ? C83 H83 0.9300 . ? C84 C85 1.369(7) . ? C84 H84 0.9300 . ? C85 C86 1.382(7) . ? C85 N87 1.463(7) . ? C86 H86 0.9300 . ? N87 O89 1.231(7) . ? N87 O88 1.244(7) . ? N90 C91 1.515(6) . ? N90 C103 1.515(6) . ? N90 C99 1.529(5) . ? N90 C95 1.531(6) . ? C91 C92 1.535(7) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 C93 1.523(7) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C93 C94 1.502(7) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? C95 C96 1.505(6) . ? C95 H95A 0.9700 . ? C95 H95B 0.9700 . ? C96 C97 1.499(6) . ? C96 H96A 0.9700 . ? C96 H96B 0.9700 . ? C97 C98 1.511(7) . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C99 C100 1.514(6) . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? C100 C101 1.518(6) . ? C100 H10I 0.9700 . ? C100 H10J 0.9700 . ? C101 C102 1.519(7) . ? C101 H10P 0.9700 . ? C101 H10Q 0.9700 . ? C102 H10R 0.9600 . ? C102 H10S 0.9600 . ? C102 H10T 0.9600 . ? C103 C104 1.511(6) . ? C103 H10A 0.9700 . ? C103 H10B 0.9700 . ? C104 C105 1.511(6) . ? C104 H10C 0.9700 . ? C104 H10D 0.9700 . ? C105 C106 1.496(7) . ? C105 H10K 0.9700 . ? C105 H10L 0.9700 . ? C106 H10M 0.9600 . ? C106 H10N 0.9600 . ? C106 H10O 0.9600 . ? N107 C116 1.507(6) . ? N107 C112 1.516(6) . ? N107 C120 1.525(5) . ? N107 C108 1.536(5) . ? C108 C109 1.497(6) . ? C108 H10G 0.9700 . ? C108 H10H 0.9700 . ? C109 C110 1.520(6) . ? C109 H10E 0.9700 . ? C109 H10F 0.9700 . ? C110 C111 1.500(7) . ? C110 H11E 0.9700 . ? C110 H11F 0.9700 . ? C111 H11M 0.9600 . ? C111 H11N 0.9600 . ? C111 H11O 0.9600 . ? C112 C113 1.517(7) . ? C112 H11C 0.9700 . ? C112 H11D 0.9700 . ? C113 C114 1.502(7) . ? C113 H11G 0.9700 . ? C113 H11H 0.9700 . ? C114 C115 1.531(8) . ? C114 H11I 0.9700 . ? C114 H11J 0.9700 . ? C115 H11U 0.9600 . ? C115 H11V 0.9600 . ? C115 H11W 0.9600 . ? C116 C117 1.518(7) . ? C116 H11A 0.9700 . ? C116 H11B 0.9700 . ? C117 C118 1.459(7) . ? C117 H11K 0.9700 . ? C117 H11L 0.9700 . ? C118 C119 1.507(8) . ? C118 H11S 0.9700 . ? C118 H11T 0.9700 . ? C119 H11P 0.9600 . ? C119 H11Q 0.9600 . ? C119 H11R 0.9600 . ? C120 C121 1.510(6) . ? C120 H12A 0.9700 . ? C120 H12B 0.9700 . ? C121 C122 1.526(6) . ? C121 H12E 0.9700 . ? C121 H12F 0.9700 . ? C122 C123 1.518(7) . ? C122 H12C 0.9700 . ? C122 H12D 0.9700 . ? C123 H12G 0.9600 . ? C123 H12H 0.9600 . ? C123 H12I 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6A C1A C2A 107.0(10) . . ? O6A C2A C1A 107.9(10) 2_767 . ? C1A O6A C2A 109.3(9) . 2_767 ? O6B C1B C2B 95.7(18) . . ? H1A O1 H1B 90(4) . . ? O2 O2 H2A 0(10) 1 . ? O2 O2 H2B 0(10) 1 . ? H2A O2 H2B 103(6) . . ? H3A O3 H3B 105(7) . . ? C20 C6 C76 119.5(4) . . ? C20 C6 C7 120.1(4) . . ? C76 C6 C7 120.4(4) . . ? N8 C7 C6 109.2(3) . . ? N8 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? N8 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? C9 N8 C7 123.2(4) . . ? C9 N8 H8 120(3) . . ? C7 N8 H8 116(3) . . ? O10 C9 N8 123.4(4) . . ? O10 C9 C11 120.4(4) . . ? N8 C9 C11 116.1(4) . . ? C12 C11 C16 118.7(4) . . ? C12 C11 C9 124.3(4) . . ? C16 C11 C9 117.0(4) . . ? C13 C12 C11 121.4(4) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 120.0(5) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 118.4(4) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C14 C15 C16 122.5(4) . . ? C14 C15 N17 118.4(4) . . ? C16 C15 N17 119.0(4) . . ? C15 C16 C11 119.1(4) . . ? C15 C16 H16 120.5 . . ? C11 C16 H16 120.5 . . ? O18 N17 O19 122.5(5) . . ? O18 N17 C15 118.2(4) . . ? O19 N17 C15 119.3(5) . . ? C6 C20 C34 120.8(4) . . ? C6 C20 C21 119.4(4) . . ? C34 C20 C21 119.7(4) . . ? N22 C21 C20 111.9(3) . . ? N22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? N22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C23 N22 C21 119.0(4) . . ? C23 N22 H22 126(3) . . ? C21 N22 H22 114(3) . . ? O24 C23 N22 122.3(4) . . ? O24 C23 C25 120.7(4) . . ? N22 C23 C25 117.0(4) . . ? C30 C25 C26 119.4(4) . . ? C30 C25 C23 116.3(4) . . ? C26 C25 C23 124.3(4) . . ? C25 C26 C27 120.2(5) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 120.1(5) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C27 118.5(5) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? C28 C29 C30 122.7(5) . . ? C28 C29 N31 119.1(5) . . ? C30 C29 N31 118.2(5) . . ? C29 C30 C25 119.1(4) . . ? C29 C30 H30 120.5 . . ? C25 C30 H30 120.5 . . ? O33 N31 O32 124.1(5) . . ? O33 N31 C29 119.0(5) . . ? O32 N31 C29 116.9(5) . . ? C20 C34 C48 119.2(4) . . ? C20 C34 C35 119.5(4) . . ? C48 C34 C35 121.3(4) . . ? N36 C35 C34 112.8(3) . . ? N36 C35 H35A 109.0 . . ? C34 C35 H35A 109.0 . . ? N36 C35 H35B 109.0 . . ? C34 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C37 N36 C35 117.6(4) . . ? C37 N36 H36 125(2) . . ? C35 N36 H36 117(2) . . ? O38 C37 N36 121.7(4) . . ? O38 C37 C39 120.7(5) . . ? N36 C37 C39 117.6(4) . . ? C40 C39 C44 119.6(5) . . ? C40 C39 C37 124.5(5) . . ? C44 C39 C37 116.0(5) . . ? C39 C40 C41 121.3(6) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C42 C41 C40 119.6(6) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C43 C42 C41 120.6(6) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 121.3(6) . . ? C42 C43 N45 121.5(6) . . ? C44 C43 N45 117.1(6) . . ? C39 C44 C43 117.6(5) . . ? C39 C44 H44 121.2 . . ? C43 C44 H44 121.2 . . ? O46 N45 O47 122.3(6) . . ? O46 N45 C43 120.1(6) . . ? O47 N45 C43 117.6(7) . . ? C62 C48 C34 120.0(4) . . ? C62 C48 C49 120.3(4) . . ? C34 C48 C49 119.7(4) . . ? N50 C49 C48 113.5(3) . . ? N50 C49 H49A 108.9 . . ? C48 C49 H49A 108.9 . . ? N50 C49 H49B 108.9 . . ? C48 C49 H49B 108.9 . . ? H49A C49 H49B 107.7 . . ? C51 N50 C49 122.5(4) . . ? C51 N50 H50 119(4) . . ? C49 N50 H50 117(3) . . ? O52 C51 N50 121.7(4) . . ? O52 C51 C53 120.3(4) . . ? N50 C51 C53 118.0(4) . . ? C54 C53 C58 118.4(4) . . ? C54 C53 C51 124.5(4) . . ? C58 C53 C51 117.1(4) . . ? C55 C54 C53 121.6(4) . . ? C55 C54 H54 119.2 . . ? C53 C54 H54 119.2 . . ? C56 C55 C54 120.3(4) . . ? C56 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C55 C56 C57 117.9(4) . . ? C55 C56 H56 121.0 . . ? C57 C56 H56 121.0 . . ? C58 C57 C56 122.8(4) . . ? C58 C57 N59 118.3(4) . . ? C56 C57 N59 119.0(4) . . ? C57 C58 C53 119.1(4) . . ? C57 C58 H58 120.4 . . ? C53 C58 H58 120.4 . . ? O61 N59 O60 123.4(4) . . ? O61 N59 C57 119.4(4) . . ? O60 N59 C57 117.2(4) . . ? C76 C62 C48 120.1(4) . . ? C76 C62 C63 120.0(4) . . ? C48 C62 C63 119.9(4) . . ? N64 C63 C62 110.8(3) . . ? N64 C63 H63A 109.5 . . ? C62 C63 H63A 109.5 . . ? N64 C63 H63B 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 108.1 . . ? C65 N64 C63 121.8(4) . . ? C65 N64 H64 132(3) . . ? C63 N64 H64 105(3) . . ? O66 C65 N64 123.0(4) . . ? O66 C65 C67 119.6(4) . . ? N64 C65 C67 117.4(4) . . ? C68 C67 C72 119.5(5) . . ? C68 C67 C65 124.1(5) . . ? C72 C67 C65 116.3(4) . . ? C67 C68 C69 120.3(5) . . ? C67 C68 H68 119.8 . . ? C69 C68 H68 119.8 . . ? C70 C69 C68 119.7(5) . . ? C70 C69 H69 120.2 . . ? C68 C69 H69 120.2 . . ? C71 C70 C69 118.6(5) . . ? C71 C70 H70 120.7 . . ? C69 C70 H70 120.7 . . ? C70 C71 C72 122.9(5) . . ? C70 C71 N73 119.0(5) . . ? C72 C71 N73 118.0(5) . . ? C71 C72 C67 119.0(5) . . ? C71 C72 H72 120.5 . . ? C67 C72 H72 120.5 . . ? O75 N73 O74 122.4(6) . . ? O75 N73 C71 119.0(6) . . ? O74 N73 C71 118.6(6) . . ? C62 C76 C6 120.3(4) . . ? C62 C76 C77 120.3(4) . . ? C6 C76 C77 119.4(4) . . ? N78 C77 C76 112.1(3) . . ? N78 C77 H77A 109.2 . . ? C76 C77 H77A 109.2 . . ? N78 C77 H77B 109.2 . . ? C76 C77 H77B 109.2 . . ? H77A C77 H77B 107.9 . . ? C79 N78 C77 120.0(4) . . ? C79 N78 H78 124(3) . . ? C77 N78 H78 115(3) . . ? O80 C79 N78 122.1(4) . . ? O80 C79 C81 120.4(4) . . ? N78 C79 C81 117.5(4) . . ? C82 C81 C86 118.2(4) . . ? C82 C81 C79 124.2(4) . . ? C86 C81 C79 117.6(4) . . ? C81 C82 C83 121.2(5) . . ? C81 C82 H82 119.4 . . ? C83 C82 H82 119.4 . . ? C84 C83 C82 121.2(5) . . ? C84 C83 H83 119.4 . . ? C82 C83 H83 119.4 . . ? C83 C84 C85 117.2(5) . . ? C83 C84 H84 121.4 . . ? C85 C84 H84 121.4 . . ? C84 C85 C86 123.0(5) . . ? C84 C85 N87 118.2(5) . . ? C86 C85 N87 118.7(5) . . ? C81 C86 C85 119.2(5) . . ? C81 C86 H86 120.4 . . ? C85 C86 H86 120.4 . . ? O89 N87 O88 124.0(6) . . ? O89 N87 C85 118.6(6) . . ? O88 N87 C85 117.3(6) . . ? C91 N90 C103 109.2(3) . . ? C91 N90 C99 108.3(3) . . ? C103 N90 C99 111.1(3) . . ? C91 N90 C95 112.0(3) . . ? C103 N90 C95 107.4(3) . . ? C99 N90 C95 109.0(3) . . ? N90 C91 C92 114.0(4) . . ? N90 C91 H91A 108.8 . . ? C92 C91 H91A 108.8 . . ? N90 C91 H91B 108.8 . . ? C92 C91 H91B 108.8 . . ? H91A C91 H91B 107.6 . . ? C93 C92 C91 113.5(4) . . ? C93 C92 H92A 108.9 . . ? C91 C92 H92A 108.9 . . ? C93 C92 H92B 108.9 . . ? C91 C92 H92B 108.9 . . ? H92A C92 H92B 107.7 . . ? C94 C93 C92 111.2(4) . . ? C94 C93 H93A 109.4 . . ? C92 C93 H93A 109.4 . . ? C94 C93 H93B 109.4 . . ? C92 C93 H93B 109.4 . . ? H93A C93 H93B 108.0 . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C96 C95 N90 115.3(4) . . ? C96 C95 H95A 108.5 . . ? N90 C95 H95A 108.5 . . ? C96 C95 H95B 108.5 . . ? N90 C95 H95B 108.5 . . ? H95A C95 H95B 107.5 . . ? C97 C96 C95 110.7(4) . . ? C97 C96 H96A 109.5 . . ? C95 C96 H96A 109.5 . . ? C97 C96 H96B 109.5 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 108.1 . . ? C96 C97 C98 112.2(4) . . ? C96 C97 H97A 109.2 . . ? C98 C97 H97A 109.2 . . ? C96 C97 H97B 109.2 . . ? C98 C97 H97B 109.2 . . ? H97A C97 H97B 107.9 . . ? C100 C99 N90 117.3(4) . . ? C100 C99 H99A 108.0 . . ? N90 C99 H99A 108.0 . . ? C100 C99 H99B 108.0 . . ? N90 C99 H99B 108.0 . . ? H99A C99 H99B 107.2 . . ? C97 C98 H98A 109.5 . . ? C97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C99 C100 C101 108.6(4) . . ? C99 C100 H10I 110.0 . . ? C101 C100 H10I 110.0 . . ? C99 C100 H10J 110.0 . . ? C101 C100 H10J 110.0 . . ? H10I C100 H10J 108.3 . . ? C100 C101 C102 114.1(5) . . ? C100 C101 H10P 108.7 . . ? C102 C101 H10P 108.7 . . ? C100 C101 H10Q 108.7 . . ? C102 C101 H10Q 108.7 . . ? H10P C101 H10Q 107.6 . . ? C101 C102 H10R 109.5 . . ? C101 C102 H10S 109.5 . . ? H10R C102 H10S 109.5 . . ? C101 C102 H10T 109.5 . . ? H10R C102 H10T 109.5 . . ? H10S C102 H10T 109.5 . . ? C104 C103 N90 117.7(4) . . ? C104 C103 H10A 107.9 . . ? N90 C103 H10A 107.9 . . ? C104 C103 H10B 107.9 . . ? N90 C103 H10B 107.9 . . ? H10A C103 H10B 107.2 . . ? C105 C104 C103 108.8(4) . . ? C105 C104 H10C 109.9 . . ? C103 C104 H10C 109.9 . . ? C105 C104 H10D 109.9 . . ? C103 C104 H10D 109.9 . . ? H10C C104 H10D 108.3 . . ? C106 C105 C104 114.6(4) . . ? C106 C105 H10K 108.6 . . ? C104 C105 H10K 108.6 . . ? C106 C105 H10L 108.6 . . ? C104 C105 H10L 108.6 . . ? H10K C105 H10L 107.6 . . ? C105 C106 H10M 109.5 . . ? C105 C106 H10N 109.5 . . ? H10M C106 H10N 109.5 . . ? C105 C106 H10O 109.5 . . ? H10M C106 H10O 109.5 . . ? H10N C106 H10O 109.5 . . ? C116 N107 C112 108.0(3) . . ? C116 N107 C120 111.0(3) . . ? C112 N107 C120 111.5(3) . . ? C116 N107 C108 110.6(3) . . ? C112 N107 C108 109.5(3) . . ? C120 N107 C108 106.2(3) . . ? C109 C108 N107 116.1(3) . . ? C109 C108 H10G 108.2 . . ? N107 C108 H10G 108.2 . . ? C109 C108 H10H 108.2 . . ? N107 C108 H10H 108.2 . . ? H10G C108 H10H 107.4 . . ? C108 C109 C110 110.9(4) . . ? C108 C109 H10E 109.5 . . ? C110 C109 H10E 109.5 . . ? C108 C109 H10F 109.5 . . ? C110 C109 H10F 109.5 . . ? H10E C109 H10F 108.0 . . ? C111 C110 C109 112.6(4) . . ? C111 C110 H11E 109.1 . . ? C109 C110 H11E 109.1 . . ? C111 C110 H11F 109.1 . . ? C109 C110 H11F 109.1 . . ? H11E C110 H11F 107.8 . . ? C110 C111 H11M 109.5 . . ? C110 C111 H11N 109.5 . . ? H11M C111 H11N 109.5 . . ? C110 C111 H11O 109.5 . . ? H11M C111 H11O 109.5 . . ? H11N C111 H11O 109.5 . . ? N107 C112 C113 116.6(4) . . ? N107 C112 H11C 108.2 . . ? C113 C112 H11C 108.2 . . ? N107 C112 H11D 108.2 . . ? C113 C112 H11D 108.2 . . ? H11C C112 H11D 107.3 . . ? C114 C113 C112 111.8(4) . . ? C114 C113 H11G 109.3 . . ? C112 C113 H11G 109.3 . . ? C114 C113 H11H 109.3 . . ? C112 C113 H11H 109.3 . . ? H11G C113 H11H 107.9 . . ? C113 C114 C115 112.7(5) . . ? C113 C114 H11I 109.1 . . ? C115 C114 H11I 109.1 . . ? C113 C114 H11J 109.1 . . ? C115 C114 H11J 109.1 . . ? H11I C114 H11J 107.8 . . ? C114 C115 H11U 109.5 . . ? C114 C115 H11V 109.5 . . ? H11U C115 H11V 109.5 . . ? C114 C115 H11W 109.5 . . ? H11U C115 H11W 109.5 . . ? H11V C115 H11W 109.5 . . ? N107 C116 C117 115.0(4) . . ? N107 C116 H11A 108.5 . . ? C117 C116 H11A 108.5 . . ? N107 C116 H11B 108.5 . . ? C117 C116 H11B 108.5 . . ? H11A C116 H11B 107.5 . . ? C118 C117 C116 112.5(4) . . ? C118 C117 H11K 109.1 . . ? C116 C117 H11K 109.1 . . ? C118 C117 H11L 109.1 . . ? C116 C117 H11L 109.1 . . ? H11K C117 H11L 107.8 . . ? C117 C118 C119 113.4(5) . . ? C117 C118 H11S 108.9 . . ? C119 C118 H11S 108.9 . . ? C117 C118 H11T 108.9 . . ? C119 C118 H11T 108.9 . . ? H11S C118 H11T 107.7 . . ? C118 C119 H11P 109.5 . . ? C118 C119 H11Q 109.5 . . ? H11P C119 H11Q 109.5 . . ? C118 C119 H11R 109.5 . . ? H11P C119 H11R 109.5 . . ? H11Q C119 H11R 109.5 . . ? C121 C120 N107 115.2(4) . . ? C121 C120 H12A 108.5 . . ? N107 C120 H12A 108.5 . . ? C121 C120 H12B 108.5 . . ? N107 C120 H12B 108.5 . . ? H12A C120 H12B 107.5 . . ? C120 C121 C122 109.4(4) . . ? C120 C121 H12E 109.8 . . ? C122 C121 H12E 109.8 . . ? C120 C121 H12F 109.8 . . ? C122 C121 H12F 109.8 . . ? H12E C121 H12F 108.2 . . ? C123 C122 C121 112.8(4) . . ? C123 C122 H12C 109.0 . . ? C121 C122 H12C 109.0 . . ? C123 C122 H12D 109.0 . . ? C121 C122 H12D 109.0 . . ? H12C C122 H12D 107.8 . . ? C122 C123 H12G 109.5 . . ? C122 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? C122 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A F2 0.958(18) 1.77(2) 2.719(5) 168(3) 1 O2 H2B F1 0.86(2) 1.87(2) 2.727(5) 179(8) 1 O3 H3A F1 0.86(2) 1.84(2) 2.686(4) 169(6) 1 N8 H8 F1 0.89(4) 1.92(4) 2.766(5) 160(4) 1 N22 H22 O2 0.78(4) 2.09(4) 2.868(5) 175(4) 1 N78 H78 F1 0.87(4) 1.99(4) 2.839(4) 166(4) 1 O1 H1B F1 0.89(2) 1.75(2) 2.628(4) 167(6) 1_554 O2 H2A F2 0.87(2) 1.80(2) 2.656(4) 168(7) 1_556 O5 H5A F2 0.91(2) 1.89(2) 2.784(4) 167(6) 1_556 N36 H36 F2 1.06(5) 1.77(5) 2.831(5) 174(4) 1_556 N50 H50 F2 0.79(4) 2.03(5) 2.790(5) 162(5) 1_556 N64 H64 O1 0.87(5) 2.05(5) 2.882(5) 161(4) 1_556 O3 H3B O5 0.86(2) 1.89(3) 2.737(6) 168(8) 2_677 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.770 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.057 # Attachment '- COMPLEX_2.cif' data_COMPLEX_2 _database_code_depnum_ccdc_archive 'CCDC 812290' #TrackingRef '- COMPLEX_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H136 N14 O26' _chemical_formula_weight 1926.21 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 ' 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 13.115(3) _cell_length_b 27.983(6) _cell_length_c 13.542(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.325(5) _cell_angle_gamma 90.00 _cell_volume 4961.8(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2259 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 20.07 _exptl_crystal_description Block _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9833 _exptl_absorpt_correction_T_max 0.9925 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25345 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0894 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8700 _reflns_number_gt 5194 _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^)+(0.1175P)^2^+0.0000P] 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 8700 _refine_ls_number_parameters 627 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.2208 _refine_ls_wR_factor_gt 0.1634 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.65576(17) 0.98256(8) 0.21773(16) 0.0307(6) Uani 1 1 d . . . C2 C 0.6847(3) 0.95441(12) 0.1506(2) 0.0283(8) Uani 1 1 d . . . O3 O 0.74116(17) 0.96523(8) 0.08373(17) 0.0300(6) Uani 1 1 d . . . C4 C 0.6457(3) 0.90318(13) 0.1553(3) 0.0420(10) Uani 1 1 d . . . H4A H 0.6538 0.8877 0.0931 0.063 Uiso 1 1 calc R . . H4B H 0.5747 0.9034 0.1693 0.063 Uiso 1 1 calc R . . H4C H 0.6840 0.8862 0.2067 0.063 Uiso 1 1 calc R . . C5 C 0.5075(2) 1.03748(12) 0.0688(2) 0.0253(8) Uani 1 1 d . . . C6 C 0.5179(3) 1.07823(12) 0.1425(2) 0.0310(8) Uani 1 1 d . . . H6A H 0.5053 1.1083 0.1084 0.037 Uiso 1 1 calc R . . H6B H 0.4673 1.0747 0.1915 0.037 Uiso 1 1 calc R . . N7 N 0.6190(2) 1.07879(10) 0.19124(19) 0.0273(7) Uani 1 1 d . . . H7 H 0.6456 1.0525 0.2130 0.033 Uiso 1 1 calc R . . C8 C 0.6719(3) 1.11938(12) 0.2032(2) 0.0284(8) Uani 1 1 d . . . O9 O 0.63645(17) 1.15933(8) 0.18223(17) 0.0366(6) Uani 1 1 d . . . C10 C 0.7805(3) 1.11394(12) 0.2426(2) 0.0279(8) Uani 1 1 d . . . C11 C 0.8142(3) 1.07573(12) 0.3023(2) 0.0311(8) Uani 1 1 d . . . H11 H 0.7680 1.0526 0.3207 0.037 Uiso 1 1 calc R . . C12 C 0.9164(3) 1.07204(13) 0.3343(3) 0.0343(9) Uani 1 1 d . . . H12 H 0.9383 1.0466 0.3744 0.041 Uiso 1 1 calc R . . C13 C 0.9865(3) 1.10635(13) 0.3067(3) 0.0349(9) Uani 1 1 d . . . H13 H 1.0551 1.1043 0.3281 0.042 Uiso 1 1 calc R . . C14 C 0.9515(3) 1.14322(12) 0.2469(3) 0.0310(8) Uani 1 1 d . . . C15 C 0.8498(3) 1.14839(12) 0.2151(2) 0.0298(8) Uani 1 1 d . . . H15 H 0.8284 1.1743 0.1761 0.036 Uiso 1 1 calc R . . N16 N 1.0263(2) 1.17727(11) 0.2099(2) 0.0377(8) Uani 1 1 d . . . O17 O 1.11712(19) 1.17113(9) 0.2356(2) 0.0492(7) Uani 1 1 d . . . O18 O 0.9958(2) 1.20919(10) 0.1538(2) 0.0523(8) Uani 1 1 d . . . C19 C 0.4406(2) 0.99940(12) 0.0827(2) 0.0257(8) Uani 1 1 d . . . C20 C 0.3802(3) 0.99682(13) 0.1746(2) 0.0296(8) Uani 1 1 d . . . H20A H 0.3552 1.0284 0.1905 0.036 Uiso 1 1 calc R . . H20B H 0.3218 0.9759 0.1628 0.036 Uiso 1 1 calc R . . N21 N 0.4458(2) 0.97857(10) 0.25734(19) 0.0281(7) Uani 1 1 d . . . H21 H 0.5109 0.9775 0.2533 0.034 Uiso 1 1 calc R . . C22 C 0.4029(3) 0.96346(12) 0.3399(2) 0.0278(8) Uani 1 1 d . . . O23 O 0.31073(19) 0.96322(9) 0.34831(17) 0.0375(6) Uani 1 1 d . . . C24 C 0.4751(3) 0.94782(11) 0.4248(2) 0.0288(8) Uani 1 1 d . . . C25 C 0.4322(3) 0.92456(12) 0.5039(2) 0.0374(9) Uani 1 1 d . . . H25 H 0.3624 0.9185 0.5013 0.045 Uiso 1 1 calc R . . C26 C 0.4928(3) 0.91039(13) 0.5862(3) 0.0397(10) Uani 1 1 d . . . H26 H 0.4634 0.8945 0.6378 0.048 Uiso 1 1 calc R . . C27 C 0.5969(3) 0.91985(12) 0.5920(3) 0.0371(9) Uani 1 1 d . . . H27 H 0.6378 0.9107 0.6471 0.045 Uiso 1 1 calc R . . C28 C 0.6381(3) 0.94313(12) 0.5136(2) 0.0324(8) Uani 1 1 d . . . C29 C 0.5791(3) 0.95709(12) 0.4298(2) 0.0270(8) Uani 1 1 d . . . H29 H 0.6091 0.9724 0.3779 0.032 Uiso 1 1 calc R . . N30 N 0.7472(2) 0.95457(12) 0.5197(2) 0.0423(8) Uani 1 1 d . . . O31 O 0.8015(2) 0.93472(12) 0.5847(2) 0.0679(10) Uani 1 1 d . . . O32 O 0.7795(2) 0.98350(10) 0.46037(18) 0.0462(7) Uani 1 1 d . . . C33 C 0.4330(2) 0.96213(11) 0.0139(2) 0.0249(7) Uani 1 1 d . . . C34 C 0.3565(2) 0.92232(12) 0.0284(2) 0.0280(8) Uani 1 1 d . . . H34A H 0.3744 0.8944 -0.0094 0.034 Uiso 1 1 calc R . . H34B H 0.3575 0.9134 0.0976 0.034 Uiso 1 1 calc R . . N35 N 0.2544(2) 0.93902(9) -0.00489(19) 0.0271(7) Uani 1 1 d . . . H35 H 0.2464 0.9672 -0.0293 0.032 Uiso 1 1 calc R . . C36 C 0.1734(3) 0.91047(12) 0.0027(2) 0.0270(8) Uani 1 1 d . . . O37 O 0.18079(18) 0.87037(8) 0.04128(18) 0.0375(6) Uani 1 1 d . . . C38 C 0.0711(3) 0.92815(11) -0.0392(2) 0.0257(8) Uani 1 1 d . . . C39 C 0.0587(3) 0.96940(12) -0.0957(2) 0.0288(8) Uani 1 1 d . . . H39 H 0.1147 0.9888 -0.1057 0.035 Uiso 1 1 calc R . . C40 C -0.0361(3) 0.98165(13) -0.1369(3) 0.0362(9) Uani 1 1 d . . . H40 H -0.0433 1.0094 -0.1744 0.043 Uiso 1 1 calc R . . C41 C -0.1209(3) 0.95347(13) -0.1236(3) 0.0361(9) Uani 1 1 d . . . H41 H -0.1846 0.9615 -0.1525 0.043 Uiso 1 1 calc R . . C42 C -0.1077(3) 0.91319(12) -0.0662(3) 0.0328(8) Uani 1 1 d . . . C43 C -0.0143(3) 0.89969(12) -0.0235(2) 0.0293(8) Uani 1 1 d . . . H43 H -0.0081 0.8722 0.0150 0.035 Uiso 1 1 calc R . . N44 N -0.1956(2) 0.88223(11) -0.0518(3) 0.0416(8) Uani 1 1 d . . . O45 O -0.2746(2) 0.88982(9) -0.1041(2) 0.0496(7) Uani 1 1 d . . . O46 O -0.1863(2) 0.84993(10) 0.0092(2) 0.0519(8) Uani 1 1 d . . . O47 O -0.0194(2) 0.95862(9) 0.3343(2) 0.0525(8) Uani 1 1 d . . . C48 C 0.0388(4) 0.93518(16) 0.4078(3) 0.0629(14) Uani 1 1 d . . . H48A H -0.0052 0.9250 0.4590 0.076 Uiso 1 1 calc R . . H48B H 0.0888 0.9572 0.4376 0.076 Uiso 1 1 calc R . . C49 C 0.0911(4) 0.8940(2) 0.3705(4) 0.0862(17) Uani 1 1 d . . . H49A H 0.1296 0.8784 0.4246 0.103 Uiso 1 1 calc R . . H49B H 0.1388 0.9043 0.3228 0.103 Uiso 1 1 calc R . . O50 O 0.0186(2) 0.86017(11) 0.3237(3) 0.0686(9) Uani 1 1 d . . . C51 C -0.0371(4) 0.88469(17) 0.2479(3) 0.0661(14) Uani 1 1 d . . . H51A H -0.0862 0.8631 0.2153 0.079 Uiso 1 1 calc R . . H51B H 0.0090 0.8956 0.1991 0.079 Uiso 1 1 calc R . . C52 C -0.0906(3) 0.92570(15) 0.2871(4) 0.0555(12) Uani 1 1 d . . . H52A H -0.1294 0.9417 0.2336 0.067 Uiso 1 1 calc R . . H52B H -0.1382 0.9148 0.3345 0.067 Uiso 1 1 calc R . . N53 N 0.3685(2) 0.24492(9) 0.31064(19) 0.0283(7) Uani 1 1 d . . . C54 C 0.3076(3) 0.29051(11) 0.2900(3) 0.0307(8) Uani 1 1 d . . . H54A H 0.3027 0.3075 0.3519 0.037 Uiso 1 1 calc R . . H54B H 0.3457 0.3106 0.2468 0.037 Uiso 1 1 calc R . . C55 C 0.2009(3) 0.28422(12) 0.2434(3) 0.0333(8) Uani 1 1 d . . . H55A H 0.1623 0.2633 0.2844 0.040 Uiso 1 1 calc R . . H55B H 0.2046 0.2693 0.1790 0.040 Uiso 1 1 calc R . . C56 C 0.1458(3) 0.33233(12) 0.2316(3) 0.0364(9) Uani 1 1 d . . . H56A H 0.1417 0.3469 0.2962 0.044 Uiso 1 1 calc R . . H56B H 0.1854 0.3534 0.1918 0.044 Uiso 1 1 calc R . . C57 C 0.0399(3) 0.32747(13) 0.1839(3) 0.0391(9) Uani 1 1 d . . . H57A H 0.0437 0.3143 0.1188 0.059 Uiso 1 1 calc R . . H57B H 0.0080 0.3584 0.1795 0.059 Uiso 1 1 calc R . . H57C H 0.0003 0.3067 0.2231 0.059 Uiso 1 1 calc R . . C58 C 0.3779(3) 0.21593(12) 0.2160(2) 0.0324(8) Uani 1 1 d . . . H58A H 0.4107 0.1858 0.2333 0.039 Uiso 1 1 calc R . . H58B H 0.3097 0.2088 0.1884 0.039 Uiso 1 1 calc R . . C59 C 0.4372(3) 0.23989(13) 0.1365(2) 0.0338(9) Uani 1 1 d . . . H59A H 0.5088 0.2419 0.1585 0.041 Uiso 1 1 calc R . . H59B H 0.4119 0.2721 0.1256 0.041 Uiso 1 1 calc R . . C60 C 0.4262(3) 0.21168(13) 0.0390(3) 0.0380(9) Uani 1 1 d . . . H60A H 0.4450 0.1786 0.0517 0.046 Uiso 1 1 calc R . . H60B H 0.3554 0.2123 0.0142 0.046 Uiso 1 1 calc R . . C61 C 0.4921(3) 0.23169(17) -0.0388(3) 0.0569(12) Uani 1 1 d . . . H61A H 0.4748 0.2646 -0.0507 0.085 Uiso 1 1 calc R . . H61B H 0.4807 0.2139 -0.0990 0.085 Uiso 1 1 calc R . . H61C H 0.5627 0.2293 -0.0164 0.085 Uiso 1 1 calc R . . C62 C 0.4736(3) 0.26023(12) 0.3539(3) 0.0327(8) Uani 1 1 d . . . H62A H 0.5053 0.2804 0.3060 0.039 Uiso 1 1 calc R . . H62B H 0.4646 0.2794 0.4124 0.039 Uiso 1 1 calc R . . C63 C 0.5455(3) 0.21964(13) 0.3816(3) 0.0333(8) Uani 1 1 d . . . H63A H 0.5580 0.2011 0.3230 0.040 Uiso 1 1 calc R . . H63B H 0.5140 0.1988 0.4282 0.040 Uiso 1 1 calc R . . C64 C 0.6470(3) 0.23819(13) 0.4278(3) 0.0392(9) Uani 1 1 d . . . H64A H 0.6779 0.2595 0.3817 0.047 Uiso 1 1 calc R . . H64B H 0.6347 0.2562 0.4871 0.047 Uiso 1 1 calc R . . C65 C 0.7195(3) 0.19730(14) 0.4536(3) 0.0406(9) Uani 1 1 d . . . H65A H 0.6890 0.1762 0.4995 0.061 Uiso 1 1 calc R . . H65B H 0.7823 0.2098 0.4832 0.061 Uiso 1 1 calc R . . H65C H 0.7331 0.1800 0.3946 0.061 Uiso 1 1 calc R . . C66 C 0.3147(3) 0.21338(12) 0.3827(2) 0.0312(8) Uani 1 1 d . . . H66A H 0.2471 0.2060 0.3538 0.037 Uiso 1 1 calc R . . H66B H 0.3518 0.1835 0.3895 0.037 Uiso 1 1 calc R . . C67 C 0.3032(3) 0.23362(13) 0.4851(3) 0.0353(9) Uani 1 1 d . . . H67A H 0.2635 0.2629 0.4801 0.042 Uiso 1 1 calc R . . H67B H 0.3701 0.2413 0.5152 0.042 Uiso 1 1 calc R . . C68 C 0.2503(3) 0.19790(13) 0.5501(3) 0.0425(10) Uani 1 1 d . . . H68A H 0.1831 0.1907 0.5200 0.051 Uiso 1 1 calc R . . H68B H 0.2893 0.1684 0.5532 0.051 Uiso 1 1 calc R . . C69 C 0.2391(3) 0.21627(15) 0.6543(3) 0.0490(11) Uani 1 1 d . . . H69A H 0.3056 0.2211 0.6863 0.073 Uiso 1 1 calc R . . H69B H 0.2021 0.1933 0.6910 0.073 Uiso 1 1 calc R . . H69C H 0.2026 0.2460 0.6516 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0265(13) 0.0344(14) 0.0310(13) 0.0007(11) -0.0006(10) 0.0008(11) C2 0.0209(18) 0.032(2) 0.0316(19) 0.0031(16) -0.0033(16) 0.0005(15) O3 0.0235(13) 0.0303(13) 0.0367(13) 0.0035(11) 0.0051(11) -0.0031(10) C4 0.040(2) 0.031(2) 0.056(2) 0.0010(18) 0.0139(19) -0.0067(18) C5 0.0176(17) 0.0287(19) 0.0290(18) -0.0004(14) -0.0034(14) 0.0021(14) C6 0.0234(19) 0.034(2) 0.0349(19) -0.0032(16) -0.0037(15) 0.0006(16) N7 0.0206(15) 0.0282(16) 0.0327(16) -0.0017(12) -0.0027(12) -0.0021(12) C8 0.0246(19) 0.029(2) 0.0311(19) -0.0063(15) -0.0010(15) -0.0003(16) O9 0.0241(14) 0.0295(14) 0.0551(16) -0.0059(12) -0.0075(12) 0.0018(11) C10 0.0246(19) 0.0283(19) 0.0305(18) -0.0082(15) -0.0007(15) 0.0017(15) C11 0.033(2) 0.031(2) 0.0297(19) -0.0052(15) 0.0001(16) -0.0036(16) C12 0.034(2) 0.033(2) 0.034(2) -0.0001(16) -0.0091(16) 0.0019(17) C13 0.028(2) 0.034(2) 0.041(2) -0.0070(17) -0.0073(16) 0.0028(17) C14 0.026(2) 0.0288(19) 0.038(2) -0.0068(16) -0.0006(16) -0.0015(15) C15 0.026(2) 0.0241(18) 0.038(2) -0.0055(15) -0.0059(15) 0.0037(15) N16 0.0275(19) 0.0295(18) 0.056(2) -0.0090(15) -0.0026(15) -0.0047(14) O17 0.0216(15) 0.0420(16) 0.083(2) -0.0087(14) -0.0065(13) -0.0047(12) O18 0.0366(17) 0.0398(17) 0.080(2) 0.0137(15) -0.0038(15) -0.0056(13) C19 0.0197(18) 0.0303(19) 0.0265(17) 0.0035(15) -0.0050(14) 0.0005(15) C20 0.0201(18) 0.036(2) 0.0319(18) -0.0007(16) -0.0034(14) -0.0042(15) N21 0.0186(15) 0.0355(17) 0.0301(15) 0.0009(13) 0.0015(12) -0.0005(13) C22 0.027(2) 0.0264(19) 0.0296(19) -0.0073(14) 0.0026(15) -0.0044(15) O23 0.0272(15) 0.0510(16) 0.0348(14) -0.0042(12) 0.0058(11) -0.0041(12) C24 0.038(2) 0.0212(18) 0.0273(18) -0.0052(14) 0.0041(15) -0.0025(15) C25 0.050(2) 0.032(2) 0.032(2) -0.0056(16) 0.0107(18) -0.0076(18) C26 0.060(3) 0.029(2) 0.031(2) -0.0038(16) 0.0106(19) -0.0049(19) C27 0.056(3) 0.027(2) 0.0286(19) -0.0003(15) -0.0007(18) 0.0104(18) C28 0.040(2) 0.0276(19) 0.0302(19) 0.0001(15) 0.0032(16) 0.0086(16) C29 0.030(2) 0.0248(18) 0.0270(18) -0.0002(14) 0.0070(15) 0.0047(15) N30 0.036(2) 0.057(2) 0.0334(18) -0.0017(16) -0.0018(15) 0.0158(17) O31 0.049(2) 0.096(3) 0.0565(18) 0.0232(18) -0.0119(15) 0.0289(18) O32 0.0332(16) 0.069(2) 0.0366(15) 0.0050(14) 0.0000(12) 0.0025(14) C33 0.0179(17) 0.0255(18) 0.0306(18) 0.0021(14) -0.0044(14) -0.0006(14) C34 0.0240(19) 0.0283(19) 0.0315(18) 0.0058(15) -0.0009(15) -0.0034(15) N35 0.0214(16) 0.0251(15) 0.0341(16) 0.0054(12) -0.0036(12) -0.0024(12) C36 0.027(2) 0.029(2) 0.0250(17) 0.0003(15) 0.0010(14) -0.0060(15) O37 0.0323(15) 0.0323(15) 0.0472(15) 0.0121(12) -0.0024(12) -0.0070(11) C38 0.0248(19) 0.0258(18) 0.0265(17) -0.0051(14) 0.0011(14) -0.0041(15) C39 0.0237(19) 0.0259(19) 0.037(2) 0.0015(15) 0.0020(15) -0.0042(15) C40 0.029(2) 0.033(2) 0.046(2) 0.0045(17) 0.0002(17) 0.0009(16) C41 0.021(2) 0.034(2) 0.053(2) -0.0027(18) -0.0001(17) 0.0003(16) C42 0.0203(19) 0.030(2) 0.049(2) -0.0069(17) 0.0096(16) -0.0047(15) C43 0.027(2) 0.0268(19) 0.0350(19) -0.0042(15) 0.0065(15) -0.0027(15) N44 0.0212(18) 0.0357(19) 0.068(2) -0.0063(17) 0.0074(16) -0.0024(15) O45 0.0241(15) 0.0442(16) 0.080(2) -0.0067(15) -0.0008(14) -0.0078(13) O46 0.0353(17) 0.0340(16) 0.087(2) 0.0118(15) 0.0100(15) -0.0021(13) O47 0.0506(18) 0.0394(16) 0.0670(19) -0.0014(14) -0.0025(15) 0.0037(14) C48 0.083(4) 0.056(3) 0.046(3) 0.006(2) -0.023(2) -0.003(3) C49 0.064(4) 0.068(4) 0.123(5) 0.005(3) -0.026(3) 0.016(3) O50 0.061(2) 0.0413(18) 0.103(3) -0.0032(18) 0.0010(19) 0.0134(16) C51 0.085(4) 0.057(3) 0.057(3) -0.006(2) 0.008(3) -0.028(3) C52 0.039(3) 0.043(3) 0.083(3) 0.002(2) -0.014(2) -0.001(2) N53 0.0317(17) 0.0229(15) 0.0299(15) 0.0001(12) -0.0029(13) -0.0039(12) C54 0.036(2) 0.0218(18) 0.0340(19) -0.0008(15) -0.0025(16) -0.0010(15) C55 0.036(2) 0.030(2) 0.0338(19) -0.0024(15) 0.0014(16) -0.0008(16) C56 0.042(2) 0.0243(19) 0.043(2) -0.0020(16) -0.0006(18) 0.0017(16) C57 0.041(2) 0.036(2) 0.041(2) 0.0039(17) 0.0047(18) 0.0086(18) C58 0.035(2) 0.0261(19) 0.035(2) -0.0058(15) -0.0027(16) -0.0031(16) C59 0.032(2) 0.034(2) 0.036(2) -0.0027(16) -0.0025(16) -0.0035(16) C60 0.044(2) 0.033(2) 0.037(2) -0.0007(16) -0.0008(18) 0.0017(18) C61 0.047(3) 0.079(3) 0.046(2) -0.011(2) 0.009(2) -0.009(2) C62 0.031(2) 0.033(2) 0.0329(19) -0.0009(15) -0.0027(16) -0.0104(16) C63 0.032(2) 0.035(2) 0.0323(19) 0.0021(16) -0.0010(16) -0.0055(17) C64 0.036(2) 0.044(2) 0.037(2) 0.0019(17) -0.0022(17) -0.0135(18) C65 0.029(2) 0.050(2) 0.042(2) -0.0099(18) -0.0019(17) 0.0016(18) C66 0.032(2) 0.0253(19) 0.036(2) 0.0049(15) -0.0030(16) -0.0041(15) C67 0.031(2) 0.034(2) 0.042(2) 0.0010(17) 0.0013(17) -0.0016(16) C68 0.049(3) 0.035(2) 0.045(2) 0.0015(18) 0.0102(19) -0.0030(18) C69 0.052(3) 0.047(2) 0.049(2) 0.004(2) 0.016(2) 0.003(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 O1 C2 1.278(4) . ? C2 O3 1.240(4) . ? C2 O1 1.278(4) 1 ? C2 C4 1.525(5) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C19 1.400(5) . ? C5 C33 1.402(5) 3_675 ? C5 C6 1.516(4) . ? C6 N7 1.447(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? N7 C8 1.336(4) . ? N7 H7 0.8600 . ? C8 O9 1.238(4) . ? C8 C10 1.499(5) . ? C10 C15 1.391(5) . ? C10 C11 1.397(5) . ? C11 C12 1.388(5) . ? C11 H11 0.9300 . ? C12 C13 1.395(5) . ? C12 H12 0.9300 . ? C13 C14 1.374(5) . ? C13 H13 0.9300 . ? C14 C15 1.385(5) . ? C14 N16 1.476(5) . ? C15 H15 0.9300 . ? N16 O18 1.225(4) . ? N16 O17 1.233(4) . ? C19 C33 1.397(4) . ? C19 C20 1.516(5) . ? C20 N21 1.464(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? N21 C22 1.349(4) . ? N21 H21 0.8600 . ? C22 O23 1.221(4) . ? C22 C24 1.511(5) . ? C24 C29 1.386(5) . ? C24 C25 1.399(5) . ? C25 C26 1.389(5) . ? C25 H25 0.9300 . ? C26 C27 1.389(5) . ? C26 H26 0.9300 . ? C27 C28 1.382(5) . ? C27 H27 0.9300 . ? C28 C29 1.391(5) . ? C28 N30 1.465(5) . ? C29 H29 0.9300 . ? N30 O32 1.232(4) . ? N30 O31 1.233(4) . ? C33 C5 1.402(5) 3_675 ? C33 C34 1.520(4) . ? C34 N35 1.465(4) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? N35 C36 1.337(4) . ? N35 H35 0.8600 . ? C36 O37 1.239(4) . ? C36 C38 1.510(5) . ? C38 C39 1.389(4) . ? C38 C43 1.401(5) . ? C39 C40 1.376(5) . ? C39 H39 0.9300 . ? C40 C41 1.384(5) . ? C40 H40 0.9300 . ? C41 C42 1.374(5) . ? C41 H41 0.9300 . ? C42 C43 1.377(5) . ? C42 N44 1.463(4) . ? C43 H43 0.9300 . ? N44 O46 1.226(4) . ? N44 O45 1.239(4) . ? O47 C48 1.385(5) . ? O47 C52 1.436(5) . ? C48 C49 1.447(7) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 O50 1.460(6) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? O50 C51 1.404(6) . ? C51 C52 1.461(6) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? N53 C66 1.520(4) . ? N53 C54 1.523(4) . ? N53 C62 1.527(4) . ? N53 C58 1.527(4) . ? C54 C55 1.511(5) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.532(5) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.504(5) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 C59 1.521(5) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.538(5) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.509(5) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 C63 1.510(5) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.528(5) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C65 1.516(5) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 C67 1.514(5) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.525(5) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.517(5) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 C2 O1 125.7(3) . 1 ? O3 C2 O1 125.7(3) . . ? O3 C2 C4 118.5(3) . . ? O1 C2 C4 115.8(3) 1 . ? O1 C2 C4 115.8(3) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C19 C5 C33 119.7(3) . 3_675 ? C19 C5 C6 121.1(3) . . ? C33 C5 C6 119.2(3) 3_675 . ? N7 C6 C5 110.7(3) . . ? N7 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N7 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 N7 C6 121.3(3) . . ? C8 N7 H7 119.3 . . ? C6 N7 H7 119.3 . . ? O9 C8 N7 123.7(3) . . ? O9 C8 C10 120.7(3) . . ? N7 C8 C10 115.6(3) . . ? C15 C10 C11 119.7(3) . . ? C15 C10 C8 117.2(3) . . ? C11 C10 C8 123.1(3) . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 118.1(3) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? C13 C14 C15 123.0(3) . . ? C13 C14 N16 118.6(3) . . ? C15 C14 N16 118.3(3) . . ? C14 C15 C10 118.5(3) . . ? C14 C15 H15 120.8 . . ? C10 C15 H15 120.8 . . ? O18 N16 O17 123.5(3) . . ? O18 N16 C14 118.8(3) . . ? O17 N16 C14 117.7(3) . . ? C33 C19 C5 120.0(3) . . ? C33 C19 C20 119.4(3) . . ? C5 C19 C20 120.5(3) . . ? N21 C20 C19 109.4(3) . . ? N21 C20 H20A 109.8 . . ? C19 C20 H20A 109.8 . . ? N21 C20 H20B 109.8 . . ? C19 C20 H20B 109.8 . . ? H20A C20 H20B 108.2 . . ? C22 N21 C20 119.3(3) . . ? C22 N21 H21 120.4 . . ? C20 N21 H21 120.4 . . ? O23 C22 N21 122.8(3) . . ? O23 C22 C24 120.5(3) . . ? N21 C22 C24 116.6(3) . . ? C29 C24 C25 119.2(3) . . ? C29 C24 C22 123.7(3) . . ? C25 C24 C22 117.1(3) . . ? C26 C25 C24 120.8(4) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 120.3(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 118.3(3) . . ? C28 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? C27 C28 C29 122.4(4) . . ? C27 C28 N30 118.9(3) . . ? C29 C28 N30 118.7(3) . . ? C24 C29 C28 119.1(3) . . ? C24 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? O32 N30 O31 123.8(3) . . ? O32 N30 C28 118.5(3) . . ? O31 N30 C28 117.7(3) . . ? C19 C33 C5 120.4(3) . 3_675 ? C19 C33 C34 118.9(3) . . ? C5 C33 C34 120.7(3) 3_675 . ? N35 C34 C33 109.0(3) . . ? N35 C34 H34A 109.9 . . ? C33 C34 H34A 109.9 . . ? N35 C34 H34B 109.9 . . ? C33 C34 H34B 109.9 . . ? H34A C34 H34B 108.3 . . ? C36 N35 C34 120.1(3) . . ? C36 N35 H35 120.0 . . ? C34 N35 H35 120.0 . . ? O37 C36 N35 122.1(3) . . ? O37 C36 C38 120.1(3) . . ? N35 C36 C38 117.9(3) . . ? C39 C38 C43 119.1(3) . . ? C39 C38 C36 123.6(3) . . ? C43 C38 C36 117.3(3) . . ? C40 C39 C38 120.3(3) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C41 121.3(3) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C42 C41 C40 117.8(3) . . ? C42 C41 H41 121.1 . . ? C40 C41 H41 121.1 . . ? C41 C42 C43 122.8(3) . . ? C41 C42 N44 119.1(3) . . ? C43 C42 N44 118.0(3) . . ? C42 C43 C38 118.7(3) . . ? C42 C43 H43 120.6 . . ? C38 C43 H43 120.6 . . ? O46 N44 O45 123.9(3) . . ? O46 N44 C42 118.6(3) . . ? O45 N44 C42 117.5(3) . . ? C48 O47 C52 109.5(3) . . ? O47 C48 C49 112.2(4) . . ? O47 C48 H48A 109.2 . . ? C49 C48 H48A 109.2 . . ? O47 C48 H48B 109.2 . . ? C49 C48 H48B 109.2 . . ? H48A C48 H48B 107.9 . . ? C48 C49 O50 111.0(4) . . ? C48 C49 H49A 109.4 . . ? O50 C49 H49A 109.4 . . ? C48 C49 H49B 109.4 . . ? O50 C49 H49B 109.4 . . ? H49A C49 H49B 108.0 . . ? C51 O50 C49 107.4(4) . . ? O50 C51 C52 111.0(4) . . ? O50 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? O50 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? O47 C52 C51 110.6(4) . . ? O47 C52 H52A 109.5 . . ? C51 C52 H52A 109.5 . . ? O47 C52 H52B 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 108.1 . . ? C66 N53 C54 110.2(3) . . ? C66 N53 C62 111.1(2) . . ? C54 N53 C62 106.8(2) . . ? C66 N53 C58 107.0(2) . . ? C54 N53 C58 110.9(2) . . ? C62 N53 C58 110.9(3) . . ? C55 C54 N53 116.3(3) . . ? C55 C54 H54A 108.2 . . ? N53 C54 H54A 108.2 . . ? C55 C54 H54B 108.2 . . ? N53 C54 H54B 108.2 . . ? H54A C54 H54B 107.4 . . ? C54 C55 C56 111.1(3) . . ? C54 C55 H55A 109.4 . . ? C56 C55 H55A 109.4 . . ? C54 C55 H55B 109.4 . . ? C56 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? C57 C56 C55 112.6(3) . . ? C57 C56 H56A 109.1 . . ? C55 C56 H56A 109.1 . . ? C57 C56 H56B 109.1 . . ? C55 C56 H56B 109.1 . . ? H56A C56 H56B 107.8 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 N53 115.4(3) . . ? C59 C58 H58A 108.4 . . ? N53 C58 H58A 108.4 . . ? C59 C58 H58B 108.4 . . ? N53 C58 H58B 108.4 . . ? H58A C58 H58B 107.5 . . ? C58 C59 C60 110.8(3) . . ? C58 C59 H59A 109.5 . . ? C60 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 108.1 . . ? C61 C60 C59 112.4(3) . . ? C61 C60 H60A 109.1 . . ? C59 C60 H60A 109.1 . . ? C61 C60 H60B 109.1 . . ? C59 C60 H60B 109.1 . . ? H60A C60 H60B 107.9 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C63 C62 N53 114.9(3) . . ? C63 C62 H62A 108.5 . . ? N53 C62 H62A 108.5 . . ? C63 C62 H62B 108.5 . . ? N53 C62 H62B 108.5 . . ? H62A C62 H62B 107.5 . . ? C62 C63 C64 111.3(3) . . ? C62 C63 H63A 109.4 . . ? C64 C63 H63A 109.4 . . ? C62 C63 H63B 109.4 . . ? C64 C63 H63B 109.4 . . ? H63A C63 H63B 108.0 . . ? C65 C64 C63 111.0(3) . . ? C65 C64 H64A 109.4 . . ? C63 C64 H64A 109.4 . . ? C65 C64 H64B 109.4 . . ? C63 C64 H64B 109.4 . . ? H64A C64 H64B 108.0 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C67 C66 N53 116.5(3) . . ? C67 C66 H66A 108.2 . . ? N53 C66 H66A 108.2 . . ? C67 C66 H66B 108.2 . . ? N53 C66 H66B 108.2 . . ? H66A C66 H66B 107.3 . . ? C66 C67 C68 110.9(3) . . ? C66 C67 H67A 109.5 . . ? C68 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 108.1 . . ? C69 C68 C67 112.7(3) . . ? C69 C68 H68A 109.0 . . ? C67 C68 H68A 109.0 . . ? C69 C68 H68B 109.0 . . ? C67 C68 H68B 109.0 . . ? H68A C68 H68B 107.8 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7 O1 0.86 1.96 2.755(4) 153.0 1 N21 H21 O1 0.86 1.99 2.838(4) 168.0 1 N35 H35 O3 0.86 2.04 2.886(4) 168.5 3_675 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.456 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.095