# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_L _database_code_depnum_ccdc_archive 'CCDC 913108' #TrackingRef 'ACPs-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H54 N10 O12 S4' _chemical_formula_weight 1067.23 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' S S 0.1246 0.1234 '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 9.189(3) _cell_length_b 16.271(6) _cell_length_c 19.010(7) _cell_angle_alpha 114.021(5) _cell_angle_beta 98.024(5) _cell_angle_gamma 94.551(6) _cell_volume 2541.3(16) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.258 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9266 _exptl_absorpt_correction_T_max 0.9747 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16089 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.1415 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8495 _reflns_number_gt 4991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0000P)^2^+6.0551P] 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 8495 _refine_ls_number_parameters 657 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1457 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.1987 _refine_ls_wR_factor_gt 0.1754 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 S1 S 0.05344(16) 0.85595(10) 0.13627(8) 0.0270(4) Uani 1 1 d . . . S2 S 0.53528(16) 0.36415(9) 0.12729(8) 0.0251(3) Uani 1 1 d . . . S3 S 0.1191(2) 0.59912(12) 0.34730(10) 0.0438(5) Uani 1 1 d . . . S4 S 0.5837(2) 0.10669(13) 0.34761(11) 0.0568(6) Uani 1 1 d . . . O1 O 1.5006(5) 1.2702(3) 0.5701(3) 0.0524(13) Uani 1 1 d . . . O2 O 1.5632(5) 1.1580(3) 0.5957(3) 0.0548(14) Uani 1 1 d . . . O3 O 0.9696(5) 0.8343(3) 0.3564(2) 0.0395(11) Uani 1 1 d . . . O4 O 0.7136(4) 0.8433(3) 0.1376(2) 0.0272(9) Uani 1 1 d . . . O5 O 0.5288(6) 0.5371(4) 0.6799(3) 0.0581(14) Uani 1 1 d . . . O6 O 0.5972(5) 0.6711(3) 0.6872(3) 0.0503(13) Uani 1 1 d . . . O7 O 0.8746(5) 0.2960(3) 0.3897(2) 0.0335(10) Uani 1 1 d . . . O8 O 0.8896(4) 0.3467(3) 0.1458(2) 0.0307(10) Uani 1 1 d . . . O9 O -0.0348(5) 0.5465(3) 0.3228(3) 0.0565(15) Uani 1 1 d . . . O10 O 0.2193(4) 0.8665(3) 0.1376(2) 0.0335(10) Uani 1 1 d . . . O11 O 0.3692(4) 0.3645(3) 0.1168(2) 0.0317(10) Uani 1 1 d . . . O12 O 0.6950(5) 0.0433(3) 0.3201(3) 0.0581(15) Uani 1 1 d . . . N1 N 1.4754(6) 1.1925(4) 0.5647(3) 0.0390(13) Uani 1 1 d . . . N2 N 0.9377(5) 0.9799(3) 0.3727(2) 0.0266(11) Uani 1 1 d . . . H2A H 0.8770 1.0108 0.3569 0.032 Uiso 1 1 calc R . . N3 N 0.7496(5) 0.8617(3) 0.3028(2) 0.0256(11) Uani 1 1 d . . . H3A H 0.7034 0.9050 0.2981 0.031 Uiso 1 1 calc R . . N4 N 0.5011(5) 0.8244(3) 0.1846(2) 0.0226(11) Uani 1 1 d . . . H4A H 0.4190 0.8467 0.1964 0.027 Uiso 1 1 calc R . . N5 N 0.5115(5) 0.9111(3) 0.1153(2) 0.0212(10) Uani 1 1 d . . . H5A H 0.4190 0.9152 0.1218 0.025 Uiso 1 1 calc R . . N6 N 0.5897(6) 0.5882(4) 0.6560(3) 0.0370(13) Uani 1 1 d . . . N7 N 0.8424(5) 0.4333(3) 0.3871(3) 0.0303(12) Uani 1 1 d . . . H7A H 0.8553 0.4673 0.3617 0.036 Uiso 1 1 calc R . . N8 N 0.9424(5) 0.3283(3) 0.2911(3) 0.0285(12) Uani 1 1 d . . . H8A H 0.9366 0.3676 0.2703 0.034 Uiso 1 1 calc R . . N9 N 1.1298(5) 0.3324(3) 0.1848(3) 0.0266(11) Uani 1 1 d . . . H9A H 1.2219 0.3609 0.1992 0.032 Uiso 1 1 calc R . . N10 N 1.0834(5) 0.4262(3) 0.1239(2) 0.0226(11) Uani 1 1 d . . . H10A H 1.1808 0.4375 0.1309 0.027 Uiso 1 1 calc R . . C1 C 1.3334(6) 1.1366(4) 0.5173(3) 0.0302(14) Uani 1 1 d . . . C2 C 1.3086(6) 1.0465(4) 0.5027(3) 0.0305(14) Uani 1 1 d . . . H2 H 1.3807 1.0218 0.5259 0.037 Uiso 1 1 calc R . . C3 C 1.1798(6) 0.9914(4) 0.4545(3) 0.0298(14) Uani 1 1 d . . . H3 H 1.1652 0.9284 0.4430 0.036 Uiso 1 1 calc R . . C4 C 1.0704(6) 1.0286(4) 0.4226(3) 0.0271(13) Uani 1 1 d . . . C5 C 1.0977(7) 1.1220(4) 0.4400(3) 0.0302(14) Uani 1 1 d . . . H5 H 1.0255 1.1478 0.4179 0.036 Uiso 1 1 calc R . . C6 C 1.2269(7) 1.1767(4) 0.4883(3) 0.0313(14) Uani 1 1 d . . . H6 H 1.2425 1.2400 0.5013 0.038 Uiso 1 1 calc R . . C7 C 0.8919(6) 0.8876(4) 0.3456(3) 0.0265(13) Uani 1 1 d . . . C8 C 0.6698(6) 0.7724(4) 0.2657(3) 0.0217(12) Uani 1 1 d . . . C9 C 0.7043(7) 0.7023(4) 0.2861(3) 0.0309(14) Uani 1 1 d . . . H9 H 0.7914 0.7121 0.3236 0.037 Uiso 1 1 calc R . . C10 C 0.6142(7) 0.6184(4) 0.2528(3) 0.0320(15) Uani 1 1 d . . . H10 H 0.6393 0.5717 0.2680 0.038 Uiso 1 1 calc R . . C11 C 0.4886(7) 0.6028(4) 0.1978(3) 0.0311(14) Uani 1 1 d . . . H11 H 0.4256 0.5457 0.1760 0.037 Uiso 1 1 calc R . . C12 C 0.4533(6) 0.6704(4) 0.1740(3) 0.0276(14) Uani 1 1 d . . . H12 H 0.3677 0.6590 0.1351 0.033 Uiso 1 1 calc R . . C13 C 0.5441(6) 0.7545(4) 0.2073(3) 0.0228(13) Uani 1 1 d . . . C14 C 0.5868(6) 0.8577(3) 0.1443(3) 0.0176(12) Uani 1 1 d . . . C15 C 0.5712(6) 0.9595(4) 0.0762(3) 0.0216(12) Uani 1 1 d . . . C16 C 0.7179(6) 0.9941(4) 0.0936(3) 0.0271(14) Uani 1 1 d . . . H16 H 0.7835 0.9830 0.1310 0.033 Uiso 1 1 calc R . . C17 C 0.4709(6) 0.9735(3) 0.0189(3) 0.0202(12) Uani 1 1 d . . . C18 C 0.3174(6) 0.9372(4) -0.0025(3) 0.0252(13) Uani 1 1 d . . . H18 H 0.2778 0.9013 0.0211 0.030 Uiso 1 1 calc R . . C19 C 0.2265(6) 0.9539(4) -0.0571(3) 0.0332(15) Uani 1 1 d . . . H19 H 0.1237 0.9299 -0.0704 0.040 Uiso 1 1 calc R . . C20 C 0.6546(7) 0.5475(4) 0.5861(3) 0.0309(14) Uani 1 1 d . . . C21 C 0.6287(7) 0.4535(4) 0.5427(3) 0.0317(15) Uani 1 1 d . . . H21 H 0.5694 0.4161 0.5586 0.038 Uiso 1 1 calc R . . C22 C 0.6896(6) 0.4152(4) 0.4766(3) 0.0268(14) Uani 1 1 d . . . H22 H 0.6703 0.3511 0.4465 0.032 Uiso 1 1 calc R . . C23 C 0.7790(6) 0.4688(4) 0.4532(3) 0.0280(14) Uani 1 1 d . . . C24 C 0.8018(7) 0.5640(4) 0.4964(4) 0.0366(16) Uani 1 1 d . . . H24 H 0.8593 0.6018 0.4801 0.044 Uiso 1 1 calc R . . C25 C 0.7396(7) 0.6027(4) 0.5633(4) 0.0344(15) Uani 1 1 d . . . H25 H 0.7557 0.6669 0.5930 0.041 Uiso 1 1 calc R . . C26 C 0.8869(6) 0.3486(4) 0.3582(3) 0.0273(14) Uani 1 1 d . . . C27 C 1.0080(6) 0.2509(4) 0.2516(3) 0.0259(13) Uani 1 1 d . . . C28 C 0.9897(7) 0.1711(4) 0.2631(3) 0.0299(14) Uani 1 1 d . . . H28 H 0.9251 0.1665 0.2967 0.036 Uiso 1 1 calc R . . C29 C 1.0621(7) 0.1001(4) 0.2273(3) 0.0308(15) Uani 1 1 d . . . H29 H 1.0512 0.0483 0.2385 0.037 Uiso 1 1 calc R . . C30 C 1.1515(6) 0.1021(4) 0.1750(3) 0.0321(15) Uani 1 1 d . . . H30 H 1.2009 0.0520 0.1498 0.039 Uiso 1 1 calc R . . C31 C 1.1677(6) 0.1789(4) 0.1600(3) 0.0270(13) Uani 1 1 d . . . H31 H 1.2272 0.1806 0.1234 0.032 Uiso 1 1 calc R . . C32 C 1.0977(6) 0.2530(4) 0.1979(3) 0.0205(12) Uani 1 1 d . . . C33 C 1.0217(7) 0.3665(3) 0.1503(3) 0.0235(13) Uani 1 1 d . . . C34 C 0.9959(6) 0.4704(3) 0.0858(3) 0.0196(12) Uani 1 1 d . . . C35 C 0.8721(6) 0.5037(4) 0.1108(3) 0.0262(13) Uani 1 1 d . . . H35 H 0.8430 0.4983 0.1550 0.031 Uiso 1 1 calc R . . C36 C 1.0439(6) 0.4776(3) 0.0194(3) 0.0209(12) Uani 1 1 d . . . C37 C 1.1726(6) 0.4455(4) -0.0080(3) 0.0240(13) Uani 1 1 d . . . H37 H 1.2323 0.4177 0.0182 0.029 Uiso 1 1 calc R . . C38 C 1.2132(6) 0.4538(4) -0.0716(3) 0.0257(13) Uani 1 1 d . . . H38 H 1.2994 0.4307 -0.0895 0.031 Uiso 1 1 calc R . . C39 C 0.1386(7) 0.6494(4) 0.2825(3) 0.0380(16) Uani 1 1 d . . . H39A H 0.1385 0.6019 0.2301 0.057 Uiso 1 1 calc R . . H39B H 0.2325 0.6913 0.3011 0.057 Uiso 1 1 calc R . . H39C H 0.0556 0.6830 0.2799 0.057 Uiso 1 1 calc R . . C40 C 0.1153(7) 0.7010(4) 0.4313(3) 0.0391(16) Uani 1 1 d . . . H40A H 0.0318 0.7304 0.4199 0.059 Uiso 1 1 calc R . . H40B H 0.2087 0.7424 0.4446 0.059 Uiso 1 1 calc R . . H40C H 0.1035 0.6865 0.4755 0.059 Uiso 1 1 calc R . . C41 C -0.0289(7) 0.7994(5) 0.0350(3) 0.0443(18) Uani 1 1 d . . . H41A H -0.0101 0.8396 0.0094 0.066 Uiso 1 1 calc R . . H41B H -0.1363 0.7835 0.0295 0.066 Uiso 1 1 calc R . . H41C H 0.0145 0.7438 0.0104 0.066 Uiso 1 1 calc R . . C42 C 0.0169(7) 0.7669(4) 0.1645(4) 0.0381(16) Uani 1 1 d . . . H42A H 0.0554 0.7131 0.1306 0.057 Uiso 1 1 calc R . . H42B H -0.0906 0.7520 0.1595 0.057 Uiso 1 1 calc R . . H42C H 0.0656 0.7860 0.2191 0.057 Uiso 1 1 calc R . . C43 C 0.5721(7) 0.3217(5) 0.0298(3) 0.0443(18) Uani 1 1 d . . . H43A H 0.5039 0.2653 -0.0036 0.066 Uiso 1 1 calc R . . H43B H 0.6749 0.3095 0.0305 0.066 Uiso 1 1 calc R . . H43C H 0.5576 0.3671 0.0089 0.066 Uiso 1 1 calc R . . C44 C 0.5628(7) 0.2666(4) 0.1451(4) 0.0413(17) Uani 1 1 d . . . H44A H 0.5361 0.2753 0.1955 0.062 Uiso 1 1 calc R . . H44B H 0.6674 0.2582 0.1464 0.062 Uiso 1 1 calc R . . H44C H 0.5000 0.2127 0.1031 0.062 Uiso 1 1 calc R . . C45 C 0.4083(8) 0.0363(6) 0.3217(4) 0.060(2) Uani 1 1 d . . . H45A H 0.3877 -0.0029 0.2653 0.090 Uiso 1 1 calc R . . H45B H 0.3301 0.0746 0.3349 0.090 Uiso 1 1 calc R . . H45C H 0.4106 -0.0016 0.3508 0.090 Uiso 1 1 calc R . . C46 C 0.5529(9) 0.1500(5) 0.2753(5) 0.071(3) Uani 1 1 d . . . H46A H 0.6433 0.1887 0.2788 0.106 Uiso 1 1 calc R . . H46B H 0.4709 0.1858 0.2843 0.106 Uiso 1 1 calc R . . H46C H 0.5274 0.0992 0.2230 0.106 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 S1 0.0236(8) 0.0295(8) 0.0308(8) 0.0170(7) 0.0016(6) 0.0036(6) S2 0.0212(8) 0.0274(8) 0.0284(8) 0.0130(7) 0.0052(6) 0.0052(6) S3 0.0504(12) 0.0438(10) 0.0446(10) 0.0280(9) 0.0008(8) 0.0109(8) S4 0.0503(13) 0.0500(12) 0.0532(11) 0.0108(10) -0.0115(9) 0.0138(9) O1 0.045(3) 0.038(3) 0.065(3) 0.018(3) 0.002(2) -0.009(2) O2 0.030(3) 0.053(3) 0.068(3) 0.020(3) -0.012(2) 0.002(2) O3 0.033(3) 0.029(2) 0.054(3) 0.020(2) -0.008(2) 0.0090(19) O4 0.025(2) 0.038(2) 0.030(2) 0.025(2) 0.0050(18) 0.0109(18) O5 0.067(4) 0.069(4) 0.051(3) 0.034(3) 0.026(3) 0.011(3) O6 0.053(3) 0.041(3) 0.046(3) 0.004(2) 0.013(2) 0.015(2) O7 0.049(3) 0.032(2) 0.030(2) 0.022(2) 0.0134(19) 0.009(2) O8 0.019(2) 0.037(2) 0.044(2) 0.026(2) 0.0017(19) 0.0019(18) O9 0.059(3) 0.066(3) 0.056(3) 0.046(3) -0.004(2) -0.018(3) O10 0.021(2) 0.049(3) 0.042(2) 0.031(2) 0.0018(18) 0.0050(18) O11 0.020(2) 0.042(2) 0.047(2) 0.029(2) 0.0111(18) 0.0114(18) O12 0.038(3) 0.038(3) 0.100(4) 0.038(3) -0.010(3) 0.012(2) N1 0.031(3) 0.037(3) 0.042(3) 0.009(3) 0.008(3) 0.006(3) N2 0.030(3) 0.022(3) 0.028(3) 0.014(2) -0.007(2) 0.005(2) N3 0.024(3) 0.026(3) 0.032(3) 0.020(2) -0.005(2) 0.007(2) N4 0.019(3) 0.029(3) 0.031(3) 0.022(2) 0.007(2) 0.012(2) N5 0.014(2) 0.028(3) 0.030(2) 0.021(2) 0.0020(19) 0.0039(19) N6 0.031(3) 0.047(4) 0.029(3) 0.013(3) -0.001(2) 0.012(3) N7 0.038(3) 0.033(3) 0.038(3) 0.027(3) 0.018(2) 0.015(2) N8 0.041(3) 0.028(3) 0.030(3) 0.021(2) 0.016(2) 0.016(2) N9 0.019(3) 0.038(3) 0.031(3) 0.025(2) -0.003(2) 0.008(2) N10 0.020(3) 0.031(3) 0.023(2) 0.019(2) 0.0014(19) 0.002(2) C1 0.027(4) 0.038(4) 0.022(3) 0.012(3) 0.002(3) 0.000(3) C2 0.024(3) 0.039(4) 0.032(3) 0.021(3) -0.003(3) 0.005(3) C3 0.032(4) 0.031(3) 0.032(3) 0.019(3) 0.001(3) 0.008(3) C4 0.022(3) 0.034(3) 0.030(3) 0.019(3) 0.004(3) 0.003(3) C5 0.032(4) 0.034(3) 0.029(3) 0.018(3) 0.001(3) 0.010(3) C6 0.041(4) 0.023(3) 0.030(3) 0.010(3) 0.006(3) 0.008(3) C7 0.031(4) 0.027(3) 0.024(3) 0.013(3) 0.004(3) 0.008(3) C8 0.021(3) 0.025(3) 0.023(3) 0.014(3) 0.005(2) 0.006(2) C9 0.035(4) 0.036(4) 0.030(3) 0.022(3) 0.000(3) 0.010(3) C10 0.039(4) 0.030(3) 0.041(4) 0.025(3) 0.014(3) 0.013(3) C11 0.034(4) 0.023(3) 0.041(4) 0.017(3) 0.010(3) 0.002(3) C12 0.021(3) 0.028(3) 0.035(3) 0.016(3) 0.004(3) 0.001(2) C13 0.021(3) 0.030(3) 0.028(3) 0.022(3) 0.007(2) 0.006(2) C14 0.031(3) 0.014(3) 0.008(2) 0.007(2) -0.002(2) 0.000(2) C15 0.018(3) 0.031(3) 0.019(3) 0.016(3) -0.001(2) 0.002(2) C16 0.013(3) 0.042(4) 0.035(3) 0.029(3) -0.004(2) 0.000(2) C17 0.020(3) 0.023(3) 0.022(3) 0.015(2) 0.001(2) 0.004(2) C18 0.019(3) 0.031(3) 0.030(3) 0.020(3) 0.000(2) -0.003(2) C19 0.019(3) 0.047(4) 0.036(3) 0.026(3) -0.008(3) -0.007(3) C20 0.029(4) 0.035(4) 0.027(3) 0.012(3) 0.002(3) 0.008(3) C21 0.029(4) 0.039(4) 0.039(4) 0.028(3) 0.003(3) 0.006(3) C22 0.026(3) 0.027(3) 0.033(3) 0.019(3) 0.005(3) 0.009(3) C23 0.025(3) 0.037(4) 0.030(3) 0.023(3) 0.003(3) 0.008(3) C24 0.039(4) 0.032(4) 0.043(4) 0.020(3) 0.009(3) 0.004(3) C25 0.034(4) 0.023(3) 0.040(4) 0.010(3) -0.001(3) 0.002(3) C26 0.025(3) 0.035(3) 0.030(3) 0.021(3) 0.002(3) 0.007(3) C27 0.023(3) 0.032(3) 0.028(3) 0.019(3) 0.001(3) 0.004(2) C28 0.038(4) 0.029(3) 0.025(3) 0.015(3) 0.004(3) 0.003(3) C29 0.035(4) 0.025(3) 0.035(3) 0.019(3) -0.002(3) 0.000(3) C30 0.027(4) 0.028(3) 0.041(4) 0.017(3) -0.001(3) 0.005(3) C31 0.016(3) 0.037(3) 0.032(3) 0.019(3) 0.005(2) 0.004(2) C32 0.015(3) 0.027(3) 0.025(3) 0.021(3) -0.003(2) 0.001(2) C33 0.031(4) 0.017(3) 0.025(3) 0.011(3) 0.005(3) 0.006(2) C34 0.020(3) 0.026(3) 0.019(3) 0.016(2) 0.002(2) 0.004(2) C35 0.026(3) 0.035(3) 0.027(3) 0.021(3) 0.009(3) 0.005(3) C36 0.017(3) 0.022(3) 0.024(3) 0.013(2) -0.003(2) -0.001(2) C37 0.028(3) 0.023(3) 0.024(3) 0.014(3) 0.001(2) 0.005(2) C38 0.023(3) 0.031(3) 0.029(3) 0.019(3) 0.006(2) 0.008(2) C39 0.032(4) 0.047(4) 0.038(3) 0.020(3) 0.009(3) 0.001(3) C40 0.047(4) 0.046(4) 0.029(3) 0.020(3) 0.006(3) 0.007(3) C41 0.025(4) 0.071(5) 0.038(4) 0.025(4) 0.006(3) 0.005(3) C42 0.030(4) 0.050(4) 0.052(4) 0.037(4) 0.011(3) 0.010(3) C43 0.029(4) 0.067(5) 0.034(3) 0.020(4) 0.006(3) -0.002(3) C44 0.034(4) 0.038(4) 0.071(5) 0.036(4) 0.020(3) 0.017(3) C45 0.043(5) 0.087(6) 0.050(4) 0.028(4) 0.008(4) 0.017(4) C46 0.062(6) 0.045(5) 0.095(6) 0.032(5) -0.023(5) -0.001(4) _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 S1 O10 1.516(4) . ? S1 C42 1.763(6) . ? S1 C41 1.779(6) . ? S2 O11 1.512(4) . ? S2 C44 1.782(6) . ? S2 C43 1.788(6) . ? S3 O9 1.500(5) . ? S3 C39 1.755(6) . ? S3 C40 1.780(6) . ? S4 O12 1.504(5) . ? S4 C46 1.782(8) . ? S4 C45 1.783(7) . ? O1 N1 1.226(6) . ? O2 N1 1.235(6) . ? O3 C7 1.227(6) . ? O4 C14 1.221(6) . ? O5 N6 1.231(7) . ? O6 N6 1.223(6) . ? O7 C26 1.234(6) . ? O8 C33 1.213(6) . ? N1 C1 1.469(7) . ? N2 C7 1.381(7) . ? N2 C4 1.388(7) . ? N2 H2A 0.8800 . ? N3 C7 1.373(7) . ? N3 C8 1.413(6) . ? N3 H3A 0.8800 . ? N4 C14 1.392(7) . ? N4 C13 1.435(6) . ? N4 H4A 0.8800 . ? N5 C14 1.383(6) . ? N5 C15 1.413(6) . ? N5 H5A 0.8800 . ? N6 C20 1.459(8) . ? N7 C26 1.381(7) . ? N7 C23 1.385(7) . ? N7 H7A 0.8800 . ? N8 C26 1.364(7) . ? N8 C27 1.411(7) . ? N8 H8A 0.8800 . ? N9 C33 1.388(6) . ? N9 C32 1.427(6) . ? N9 H9A 0.8800 . ? N10 C33 1.381(7) . ? N10 C34 1.430(6) . ? N10 H10A 0.8800 . ? C1 C2 1.370(8) . ? C1 C6 1.389(8) . ? C2 C3 1.380(8) . ? C2 H2 0.9500 . ? C3 C4 1.404(8) . ? C3 H3 0.9500 . ? C4 C5 1.410(8) . ? C5 C6 1.381(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.392(7) . ? C8 C13 1.406(7) . ? C9 C10 1.385(8) . ? C9 H9 0.9500 . ? C10 C11 1.375(8) . ? C10 H10 0.9500 . ? C11 C12 1.394(7) . ? C11 H11 0.9500 . ? C12 C13 1.392(7) . ? C12 H12 0.9500 . ? C15 C16 1.359(7) . ? C15 C17 1.429(7) . ? C16 C19 1.404(8) 2_675 ? C16 H16 0.9500 . ? C17 C18 1.419(7) . ? C17 C17 1.445(10) 2_675 ? C18 C19 1.368(7) . ? C18 H18 0.9500 . ? C19 C16 1.404(8) 2_675 ? C19 H19 0.9500 . ? C20 C25 1.380(9) . ? C20 C21 1.392(8) . ? C21 C22 1.377(8) . ? C21 H21 0.9500 . ? C22 C23 1.392(8) . ? C22 H22 0.9500 . ? C23 C24 1.409(8) . ? C24 C25 1.395(9) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C27 C28 1.404(7) . ? C27 C32 1.407(8) . ? C28 C29 1.359(8) . ? C28 H28 0.9500 . ? C29 C30 1.383(8) . ? C29 H29 0.9500 . ? C30 C31 1.392(8) . ? C30 H30 0.9500 . ? C31 C32 1.390(8) . ? C31 H31 0.9500 . ? C34 C35 1.361(8) . ? C34 C36 1.439(7) . ? C35 C38 1.412(7) 2_765 ? C35 H35 0.9500 . ? C36 C37 1.411(8) . ? C36 C36 1.444(10) 2_765 ? C37 C38 1.366(7) . ? C37 H37 0.9500 . ? C38 C35 1.412(7) 2_765 ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 S1 C42 105.2(3) . . ? O10 S1 C41 104.7(3) . . ? C42 S1 C41 99.6(3) . . ? O11 S2 C44 105.2(3) . . ? O11 S2 C43 104.4(3) . . ? C44 S2 C43 98.0(3) . . ? O9 S3 C39 107.3(3) . . ? O9 S3 C40 106.3(3) . . ? C39 S3 C40 97.1(3) . . ? O12 S4 C46 103.5(4) . . ? O12 S4 C45 106.2(3) . . ? C46 S4 C45 97.9(3) . . ? O1 N1 O2 123.9(5) . . ? O1 N1 C1 118.1(5) . . ? O2 N1 C1 118.0(5) . . ? C7 N2 C4 126.1(5) . . ? C7 N2 H2A 116.9 . . ? C4 N2 H2A 116.9 . . ? C7 N3 C8 126.6(4) . . ? C7 N3 H3A 116.7 . . ? C8 N3 H3A 116.7 . . ? C14 N4 C13 121.3(5) . . ? C14 N4 H4A 119.4 . . ? C13 N4 H4A 119.4 . . ? C14 N5 C15 125.3(5) . . ? C14 N5 H5A 117.3 . . ? C15 N5 H5A 117.3 . . ? O6 N6 O5 123.5(6) . . ? O6 N6 C20 118.4(6) . . ? O5 N6 C20 118.1(6) . . ? C26 N7 C23 124.7(5) . . ? C26 N7 H7A 117.6 . . ? C23 N7 H7A 117.6 . . ? C26 N8 C27 126.9(5) . . ? C26 N8 H8A 116.6 . . ? C27 N8 H8A 116.6 . . ? C33 N9 C32 122.6(4) . . ? C33 N9 H9A 118.7 . . ? C32 N9 H9A 118.7 . . ? C33 N10 C34 122.9(5) . . ? C33 N10 H10A 118.6 . . ? C34 N10 H10A 118.6 . . ? C2 C1 C6 121.5(5) . . ? C2 C1 N1 119.5(5) . . ? C6 C1 N1 119.0(5) . . ? C1 C2 C3 120.6(5) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C2 C3 C4 119.8(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? N2 C4 C3 125.0(5) . . ? N2 C4 C5 116.6(5) . . ? C3 C4 C5 118.3(5) . . ? C6 C5 C4 121.5(5) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C1 118.2(5) . . ? C5 C6 H6 120.9 . . ? C1 C6 H6 120.9 . . ? O3 C7 N3 123.7(5) . . ? O3 C7 N2 124.5(5) . . ? N3 C7 N2 111.8(5) . . ? C9 C8 C13 118.0(5) . . ? C9 C8 N3 123.8(5) . . ? C13 C8 N3 118.1(5) . . ? C10 C9 C8 121.4(5) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C9 120.1(5) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.1(5) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 119.7(5) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C8 120.6(5) . . ? C12 C13 N4 118.6(5) . . ? C8 C13 N4 120.7(5) . . ? O4 C14 N5 124.7(5) . . ? O4 C14 N4 123.8(5) . . ? N5 C14 N4 111.4(5) . . ? C16 C15 N5 121.6(4) . . ? C16 C15 C17 120.7(5) . . ? N5 C15 C17 117.7(5) . . ? C15 C16 C19 120.7(5) . 2_675 ? C15 C16 H16 119.6 . . ? C19 C16 H16 119.6 2_675 . ? C18 C17 C15 122.9(5) . . ? C18 C17 C17 118.9(5) . 2_675 ? C15 C17 C17 118.2(6) . 2_675 ? C19 C18 C17 120.2(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C16 121.2(5) . 2_675 ? C18 C19 H19 119.4 . . ? C16 C19 H19 119.4 2_675 . ? C25 C20 C21 120.8(6) . . ? C25 C20 N6 119.7(6) . . ? C21 C20 N6 119.5(6) . . ? C22 C21 C20 119.5(6) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 121.1(6) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? N7 C23 C22 123.2(5) . . ? N7 C23 C24 117.8(5) . . ? C22 C23 C24 118.9(6) . . ? C25 C24 C23 119.8(6) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C20 C25 C24 119.8(6) . . ? C20 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? O7 C26 N8 123.7(5) . . ? O7 C26 N7 122.7(5) . . ? N8 C26 N7 113.6(5) . . ? C28 C27 C32 117.5(5) . . ? C28 C27 N8 123.5(5) . . ? C32 C27 N8 119.0(5) . . ? C29 C28 C27 121.6(6) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C28 C29 C30 121.0(5) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C29 C30 C31 118.8(6) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? C32 C31 C30 120.7(6) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C27 120.2(5) . . ? C31 C32 N9 117.6(5) . . ? C27 C32 N9 122.0(5) . . ? O8 C33 N10 124.9(5) . . ? O8 C33 N9 123.2(5) . . ? N10 C33 N9 111.8(5) . . ? C35 C34 N10 121.5(5) . . ? C35 C34 C36 121.4(5) . . ? N10 C34 C36 117.0(5) . . ? C34 C35 C38 120.4(5) . 2_765 ? C34 C35 H35 119.8 . . ? C38 C35 H35 119.8 2_765 . ? C37 C36 C34 123.5(5) . . ? C37 C36 C36 119.1(6) . 2_765 ? C34 C36 C36 117.3(6) . 2_765 ? C38 C37 C36 121.3(5) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C35 120.5(6) . 2_765 ? C37 C38 H38 119.8 . . ? C35 C38 H38 119.8 2_765 . ? S3 C39 H39A 109.5 . . ? S3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? S3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? S3 C40 H40A 109.5 . . ? S3 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? S3 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? S1 C41 H41A 109.5 . . ? S1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? S1 C42 H42A 109.5 . . ? S1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? S2 C43 H43A 109.5 . . ? S2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? S2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? S2 C44 H44A 109.5 . . ? S2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? S2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? S4 C45 H45A 109.5 . . ? S4 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? S4 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? S4 C46 H46A 109.5 . . ? S4 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? S4 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.869 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.095 data_1 _database_code_depnum_ccdc_archive 'CCDC 913109' #TrackingRef 'ACPs-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H102 N12 O12 S' _chemical_formula_weight 1335.70 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/c ' 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 12.501(6) _cell_length_b 19.167(9) _cell_length_c 16.971(6) _cell_angle_alpha 90.00 _cell_angle_beta 120.12(2) _cell_angle_gamma 90.00 _cell_volume 3517(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 0.115 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9663 _exptl_absorpt_correction_T_max 0.9773 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22029 _diffrn_reflns_av_R_equivalents 0.0971 _diffrn_reflns_av_sigmaI/netI 0.1043 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.13 _reflns_number_total 6108 _reflns_number_gt 3594 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0000P)^2^+16.8235P] 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 6108 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1885 _refine_ls_R_factor_gt 0.1266 _refine_ls_wR_factor_ref 0.2759 _refine_ls_wR_factor_gt 0.2498 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.196 _refine_ls_shift/su_max 0.010 _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 -0.1588(7) 0.4735(3) -0.0043(5) 0.090(2) Uani 1 1 d . . . O2 O -0.2000(7) 0.5797(4) -0.0546(4) 0.085(2) Uani 1 1 d . . . O3 O 0.2848(4) 0.7416(2) 0.3116(3) 0.0458(12) Uani 1 1 d . . . O4 O 0.8482(6) 0.7103(3) 0.5141(4) 0.0650(16) Uani 1 1 d . . . N1 N -0.1377(8) 0.5365(4) 0.0045(5) 0.068(2) Uani 1 1 d . . . N2 N 0.2679(5) 0.6252(3) 0.3340(4) 0.0453(15) Uani 1 1 d . . . H2A H 0.2981 0.5930 0.3748 0.054 Uiso 1 1 d R . . N3 N 0.4315(5) 0.6883(3) 0.4420(4) 0.0398(14) Uani 1 1 d . . . H3A H 0.4541 0.6489 0.4698 0.048 Uiso 1 1 d R . . N4 N 0.6829(5) 0.6712(3) 0.5258(5) 0.063(2) Uani 1 1 d . . . H4A H 0.6469 0.6352 0.5321 0.076 Uiso 1 1 d R . . N5 N 0.7987(5) 0.5940(3) 0.4996(4) 0.0514(17) Uani 1 1 d . . . H5A H 0.7545 0.5625 0.5057 0.062 Uiso 1 1 d R . . C1 C -0.0319(7) 0.5610(4) 0.0888(5) 0.0488(19) Uani 1 1 d . . . C2 C 0.0496(8) 0.5125(4) 0.1517(6) 0.053(2) Uani 1 1 d . . . H2 H 0.0363 0.4639 0.1398 0.064 Uiso 1 1 calc R . . C3 C 0.1483(7) 0.5358(4) 0.2304(6) 0.051(2) Uani 1 1 d . . . H3 H 0.2061 0.5031 0.2720 0.061 Uiso 1 1 calc R . . C4 C 0.1668(6) 0.6073(3) 0.2515(5) 0.0399(17) Uani 1 1 d . . . C5 C 0.0838(6) 0.6547(4) 0.1872(5) 0.0437(17) Uani 1 1 d . . . H5 H 0.0945 0.7033 0.1996 0.052 Uiso 1 1 calc R . . C6 C -0.0129(7) 0.6312(4) 0.1065(5) 0.0488(19) Uani 1 1 d . . . H6 H -0.0673 0.6638 0.0623 0.059 Uiso 1 1 calc R . . C7 C 0.3245(6) 0.6897(3) 0.3595(4) 0.0342(15) Uani 1 1 d . . . C8 C 0.5078(6) 0.7458(3) 0.4842(4) 0.0344(15) Uani 1 1 d . . . C9 C 0.4596(7) 0.8111(3) 0.4855(5) 0.0440(18) Uani 1 1 d . . . H9 H 0.3725 0.8170 0.4562 0.053 Uiso 1 1 calc R . . C10 C 0.5354(8) 0.8673(4) 0.5282(5) 0.054(2) Uani 1 1 d . . . H10 H 0.5007 0.9119 0.5260 0.064 Uiso 1 1 calc R . . C11 C 0.6611(8) 0.8587(4) 0.5740(6) 0.060(2) Uani 1 1 d . . . H11 H 0.7138 0.8971 0.6045 0.072 Uiso 1 1 calc R . . C12 C 0.7113(8) 0.7943(5) 0.5759(6) 0.070(3) Uani 1 1 d . . . H12 H 0.7985 0.7882 0.6100 0.084 Uiso 1 1 calc R . . C13 C 0.6350(7) 0.7381(4) 0.5281(5) 0.052(2) Uani 1 1 d . . . C14 C 0.7833(7) 0.6609(5) 0.5143(5) 0.052(2) Uani 1 1 d . . . C15 C 0.8887(6) 0.5735(4) 0.4742(4) 0.0400(16) Uani 1 1 d . . . N6 N 0.5948(5) 0.4024(3) 0.2787(4) 0.0420(15) Uani 1 1 d . . . C20 C 0.6646(6) 0.4029(4) 0.2264(4) 0.0382(16) Uani 1 1 d . . . H20A H 0.6979 0.3555 0.2291 0.046 Uiso 1 1 calc R . . H20B H 0.6052 0.4133 0.1617 0.046 Uiso 1 1 calc R . . C21 C 0.7701(7) 0.4545(4) 0.2605(5) 0.0450(18) Uani 1 1 d . . . H21A H 0.8254 0.4483 0.3269 0.054 Uiso 1 1 calc R . . H21B H 0.7367 0.5026 0.2499 0.054 Uiso 1 1 calc R . . C22 C 0.8437(7) 0.4445(4) 0.2121(6) 0.052(2) Uani 1 1 d . . . H22A H 0.8971 0.4858 0.2231 0.063 Uiso 1 1 calc R . . H22B H 0.7859 0.4410 0.1456 0.063 Uiso 1 1 calc R . . C23 C 0.9241(8) 0.3789(4) 0.2450(6) 0.063(2) Uani 1 1 d . . . H23A H 0.8710 0.3375 0.2253 0.094 Uiso 1 1 calc R . . H23B H 0.9741 0.3796 0.3116 0.094 Uiso 1 1 calc R . . H23C H 0.9787 0.3777 0.2191 0.094 Uiso 1 1 calc R . . C24 C 0.6757(7) 0.3764(4) 0.3749(5) 0.047(2) Uani 1 1 d . . . H24A H 0.7425 0.4109 0.4079 0.057 Uiso 1 1 calc R . . H24B H 0.6252 0.3753 0.4049 0.057 Uiso 1 1 calc R . . C25 C 0.7331(9) 0.3074(6) 0.3863(6) 0.094(4) Uani 1 1 d . . . H25A H 0.6692 0.2744 0.3439 0.113 Uiso 1 1 calc R . . H25B H 0.7971 0.3108 0.3684 0.113 Uiso 1 1 calc R . . C26 C 0.7901(10) 0.2783(5) 0.4782(6) 0.076(3) Uani 1 1 d . . . H26A H 0.7245 0.2749 0.4945 0.092 Uiso 1 1 calc R . . H26B H 0.8506 0.3131 0.5199 0.092 Uiso 1 1 calc R . . C27 C 0.8538(10) 0.2105(7) 0.4997(7) 0.104(4) Uani 1 1 d . . . H27A H 0.9404 0.2175 0.5165 0.157 Uiso 1 1 calc R . . H27B H 0.8133 0.1801 0.4461 0.157 Uiso 1 1 calc R . . H27C H 0.8502 0.1888 0.5506 0.157 Uiso 1 1 calc R . . C28 C 0.4842(6) 0.3546(3) 0.2265(6) 0.050(2) Uani 1 1 d . . . H28A H 0.4421 0.3683 0.1615 0.060 Uiso 1 1 calc R . . H28B H 0.5155 0.3065 0.2307 0.060 Uiso 1 1 calc R . . C29 C 0.3916(8) 0.3532(5) 0.2555(8) 0.077(3) Uani 1 1 d . . . H29A H 0.3507 0.3993 0.2440 0.092 Uiso 1 1 calc R . . H29B H 0.4330 0.3439 0.3218 0.092 Uiso 1 1 calc R . . C30 C 0.2921(8) 0.2957(4) 0.2031(7) 0.077(3) Uani 1 1 d . . . H30A H 0.2675 0.2974 0.1379 0.092 Uiso 1 1 calc R . . H30B H 0.3292 0.2493 0.2269 0.092 Uiso 1 1 calc R . . C31 C 0.1827(9) 0.3036(6) 0.2113(9) 0.102(4) Uani 1 1 d . . . H31A H 0.1325 0.3423 0.1727 0.152 Uiso 1 1 calc R . . H31B H 0.2075 0.3134 0.2749 0.152 Uiso 1 1 calc R . . H31C H 0.1343 0.2604 0.1918 0.152 Uiso 1 1 calc R . . C32 C 0.5545(8) 0.4763(4) 0.2855(6) 0.060(2) Uani 1 1 d . . . H32A H 0.6293 0.5049 0.3225 0.072 Uiso 1 1 calc R . . H32B H 0.5075 0.4745 0.3181 0.072 Uiso 1 1 calc R . . C33 C 0.4748(9) 0.5127(4) 0.1939(8) 0.076(3) Uani 1 1 d . . . H33A H 0.4057 0.4814 0.1537 0.091 Uiso 1 1 calc R . . H33B H 0.5255 0.5204 0.1648 0.091 Uiso 1 1 calc R . . C34 C 0.4211(10) 0.5832(5) 0.2011(9) 0.091(4) Uani 1 1 d . . . H34A H 0.3674 0.6019 0.1389 0.109 Uiso 1 1 calc R . . H34B H 0.3687 0.5753 0.2287 0.109 Uiso 1 1 calc R . . C35 C 0.5097(10) 0.6324(5) 0.2519(8) 0.091(3) Uani 1 1 d . . . H35A H 0.5660 0.6380 0.2279 0.136 Uiso 1 1 calc R . . H35B H 0.5567 0.6170 0.3155 0.136 Uiso 1 1 calc R . . H35C H 0.4695 0.6770 0.2485 0.136 Uiso 1 1 calc R . . S1 S 0.5000 0.5000 0.5000 0.0330(5) Uani 1 2 d S . . O5 O 0.3778(8) 0.5250(5) 0.4809(6) 0.045(2) Uani 0.50 1 d P . . O6 O 0.5175(7) 0.5666(4) 0.5504(5) 0.0285(19) Uani 0.50 1 d P . . O7 O 0.5469(9) 0.5525(4) 0.4536(6) 0.044(2) Uani 0.50 1 d P . . O8 O 0.4116(8) 0.5045(5) 0.4072(5) 0.042(2) Uani 0.50 1 d P . . C19 C 0.9560(6) 0.5124(3) 0.5116(4) 0.0349(15) Uani 1 1 d . . . C17 C 0.9910(7) 0.5877(4) 0.3868(5) 0.0469(19) Uani 1 1 d . . . H17 H 1.0015 0.6150 0.3444 0.056 Uiso 1 1 calc R . . C16 C 0.9039(7) 0.6093(4) 0.4121(5) 0.0510(19) Uani 1 1 d . . . H16 H 0.8553 0.6498 0.3848 0.061 Uiso 1 1 calc R . . C18 C 1.0592(6) 0.5295(4) 0.4214(5) 0.0450(18) Uani 1 1 d . . . H18 H 1.1164 0.5155 0.4031 0.054 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 0.121(6) 0.065(4) 0.086(5) -0.025(4) 0.052(5) -0.031(4) O2 0.091(5) 0.075(5) 0.064(4) 0.002(4) 0.021(4) -0.017(4) O3 0.045(3) 0.028(2) 0.057(3) 0.018(2) 0.021(3) 0.008(2) O4 0.077(4) 0.057(4) 0.080(4) -0.007(3) 0.054(4) 0.003(3) N1 0.089(6) 0.064(5) 0.063(5) -0.012(4) 0.046(5) -0.028(5) N2 0.033(3) 0.039(3) 0.056(4) 0.025(3) 0.017(3) 0.010(3) N3 0.039(3) 0.029(3) 0.058(4) 0.018(3) 0.030(3) 0.009(3) N4 0.031(4) 0.061(4) 0.096(5) -0.032(4) 0.030(4) -0.007(3) N5 0.026(3) 0.067(4) 0.051(4) -0.022(3) 0.012(3) 0.008(3) C1 0.058(5) 0.052(5) 0.041(4) -0.002(4) 0.028(4) -0.003(4) C2 0.056(5) 0.034(4) 0.086(6) 0.000(4) 0.047(5) -0.006(4) C3 0.034(4) 0.035(4) 0.091(6) 0.011(4) 0.036(5) 0.007(3) C4 0.035(4) 0.029(4) 0.059(5) 0.012(3) 0.026(4) 0.004(3) C5 0.037(4) 0.040(4) 0.049(4) 0.010(3) 0.018(4) 0.005(3) C6 0.054(5) 0.048(5) 0.048(4) 0.017(4) 0.029(4) 0.005(4) C7 0.035(4) 0.029(4) 0.041(4) 0.014(3) 0.021(3) 0.004(3) C8 0.044(4) 0.039(4) 0.027(3) 0.006(3) 0.023(3) 0.001(3) C9 0.052(5) 0.036(4) 0.055(5) 0.019(3) 0.035(4) 0.012(3) C10 0.079(6) 0.041(4) 0.049(5) 0.005(4) 0.039(5) 0.011(4) C11 0.069(6) 0.044(5) 0.071(6) -0.021(4) 0.038(5) -0.005(4) C12 0.052(5) 0.074(6) 0.081(6) -0.047(5) 0.031(5) -0.013(5) C13 0.044(5) 0.058(5) 0.053(5) -0.017(4) 0.024(4) 0.004(4) C14 0.039(5) 0.070(6) 0.048(5) -0.017(4) 0.023(4) 0.000(4) C15 0.028(4) 0.046(4) 0.033(4) -0.012(3) 0.005(3) -0.002(3) N6 0.029(3) 0.039(3) 0.069(4) -0.027(3) 0.033(3) -0.012(3) C20 0.034(4) 0.052(4) 0.032(4) -0.021(3) 0.019(3) -0.006(3) C21 0.041(4) 0.054(5) 0.048(4) -0.014(3) 0.028(4) -0.009(3) C22 0.055(5) 0.054(5) 0.064(5) -0.011(4) 0.041(4) -0.009(4) C23 0.058(5) 0.059(5) 0.085(6) -0.005(5) 0.046(5) -0.013(4) C24 0.052(5) 0.055(5) 0.055(5) -0.033(4) 0.041(4) -0.027(4) C25 0.088(8) 0.131(9) 0.040(5) -0.015(5) 0.014(5) 0.062(7) C26 0.113(9) 0.064(6) 0.059(6) -0.015(5) 0.048(6) -0.037(6) C27 0.081(8) 0.180(13) 0.056(6) 0.033(7) 0.038(6) 0.060(8) C28 0.022(4) 0.027(4) 0.085(6) -0.008(4) 0.014(4) -0.009(3) C29 0.044(5) 0.063(6) 0.134(9) -0.026(6) 0.053(6) -0.019(4) C30 0.043(5) 0.053(5) 0.121(9) 0.003(5) 0.032(5) 0.002(4) C31 0.052(6) 0.101(9) 0.148(11) 0.005(7) 0.047(7) -0.024(6) C32 0.074(6) 0.032(4) 0.113(7) -0.030(4) 0.077(6) -0.021(4) C33 0.065(6) 0.032(4) 0.154(10) -0.006(5) 0.071(7) -0.002(4) C34 0.096(8) 0.056(6) 0.159(11) -0.021(6) 0.092(9) -0.006(6) C35 0.111(9) 0.080(7) 0.114(9) -0.043(6) 0.081(8) -0.025(6) S1 0.0330(13) 0.0259(11) 0.0335(12) 0.0035(9) 0.0118(10) 0.0107(10) O5 0.033(5) 0.060(6) 0.037(5) 0.009(4) 0.013(4) 0.029(5) O6 0.035(5) 0.023(4) 0.029(4) 0.004(3) 0.017(4) 0.008(4) O7 0.044(6) 0.022(4) 0.058(6) 0.007(4) 0.020(5) -0.006(4) O8 0.042(6) 0.041(5) 0.025(4) 0.002(4) 0.004(4) 0.019(4) C19 0.026(3) 0.034(4) 0.040(4) -0.012(3) 0.012(3) -0.007(3) C17 0.071(6) 0.036(4) 0.040(4) 0.001(3) 0.033(4) -0.002(4) C16 0.057(5) 0.054(5) 0.040(4) -0.003(4) 0.023(4) 0.001(4) C18 0.037(4) 0.042(4) 0.052(4) -0.018(3) 0.020(4) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 N1 1.229(9) . ? O2 N1 1.230(9) . ? O3 C7 1.221(7) . ? O4 C14 1.248(9) . ? N1 C1 1.456(10) . ? N2 C4 1.379(9) . ? N2 C7 1.383(8) . ? N2 H2A 0.8599 . ? N3 C7 1.368(8) . ? N3 C8 1.397(8) . ? N3 H3A 0.8598 . ? N4 C14 1.379(9) . ? N4 C13 1.423(9) . ? N4 H4A 0.8599 . ? N5 C14 1.338(9) . ? N5 C15 1.447(9) . ? N5 H5A 0.8601 . ? C1 C6 1.374(10) . ? C1 C2 1.396(10) . ? C2 C3 1.361(11) . ? C2 H2 0.9500 . ? C3 C4 1.404(9) . ? C3 H3 0.9500 . ? C4 C5 1.398(9) . ? C5 C6 1.371(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C13 1.384(10) . ? C8 C9 1.395(9) . ? C9 C10 1.376(10) . ? C9 H9 0.9500 . ? C10 C11 1.369(11) . ? C10 H10 0.9500 . ? C11 C12 1.376(11) . ? C11 H11 0.9500 . ? C12 C13 1.399(10) . ? C12 H12 0.9500 . ? C15 C16 1.348(10) . ? C15 C19 1.396(9) . ? N6 C24 1.509(10) . ? N6 C28 1.519(8) . ? N6 C20 1.526(8) . ? N6 C32 1.527(8) . ? C20 C21 1.512(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.523(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.529(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.470(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.462(12) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.471(13) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.469(11) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.563(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.450(12) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.530(13) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.540(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.378(13) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? S1 O8 1.401(8) 3_666 ? S1 O8 1.401(8) . ? S1 O5 1.474(8) 3_666 ? S1 O5 1.474(8) . ? S1 O6 1.491(8) 3_666 ? S1 O6 1.491(8) . ? S1 O7 1.561(9) 3_666 ? S1 O7 1.561(9) . ? O5 O8 1.557(12) . ? O5 O6 1.736(13) . ? O5 O7 1.810(12) 3_666 ? O6 O8 1.588(11) 3_666 ? O7 O8 1.730(13) . ? O7 O5 1.810(12) 3_666 ? O8 O6 1.588(11) 3_666 ? C19 C19 1.424(12) 3_766 ? C19 C18 1.479(10) 3_766 ? C17 C18 1.347(10) . ? C17 C16 1.418(10) . ? C17 H17 0.9500 . ? C16 H16 0.9500 . ? C18 C19 1.479(10) 3_766 ? C18 H18 0.9500 . ? 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 N1 O2 123.6(8) . . ? O1 N1 C1 118.0(8) . . ? O2 N1 C1 118.4(7) . . ? C4 N2 C7 127.2(5) . . ? C4 N2 H2A 116.6 . . ? C7 N2 H2A 116.2 . . ? C7 N3 C8 125.1(5) . . ? C7 N3 H3A 117.5 . . ? C8 N3 H3A 117.4 . . ? C14 N4 C13 124.0(7) . . ? C14 N4 H4A 118.2 . . ? C13 N4 H4A 117.8 . . ? C14 N5 C15 121.5(7) . . ? C14 N5 H5A 119.3 . . ? C15 N5 H5A 119.2 . . ? C6 C1 C2 120.4(7) . . ? C6 C1 N1 120.1(7) . . ? C2 C1 N1 119.5(7) . . ? C3 C2 C1 119.0(7) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 121.5(7) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? N2 C4 C5 125.0(6) . . ? N2 C4 C3 116.8(6) . . ? C5 C4 C3 118.2(7) . . ? C6 C5 C4 120.3(7) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 120.5(7) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? O3 C7 N3 124.0(6) . . ? O3 C7 N2 123.2(6) . . ? N3 C7 N2 112.7(5) . . ? C13 C8 C9 118.5(7) . . ? C13 C8 N3 119.7(6) . . ? C9 C8 N3 121.8(6) . . ? C10 C9 C8 121.5(7) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C9 119.6(7) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.2(8) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 120.5(8) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C8 C13 C12 119.6(7) . . ? C8 C13 N4 117.9(7) . . ? C12 C13 N4 122.4(7) . . ? O4 C14 N5 124.9(7) . . ? O4 C14 N4 122.1(7) . . ? N5 C14 N4 113.0(7) . . ? C16 C15 C19 119.6(7) . . ? C16 C15 N5 122.0(7) . . ? C19 C15 N5 118.3(6) . . ? C24 N6 C28 110.5(5) . . ? C24 N6 C20 111.3(5) . . ? C28 N6 C20 106.4(5) . . ? C24 N6 C32 107.1(6) . . ? C28 N6 C32 111.5(5) . . ? C20 N6 C32 110.2(5) . . ? C21 C20 N6 115.1(5) . . ? C21 C20 H20A 108.5 . . ? N6 C20 H20A 108.5 . . ? C21 C20 H20B 108.5 . . ? N6 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C20 C21 C22 111.0(6) . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 111.8(6) . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 N6 117.3(6) . . ? C25 C24 H24A 108.0 . . ? N6 C24 H24A 108.0 . . ? C25 C24 H24B 108.0 . . ? N6 C24 H24B 108.0 . . ? H24A C24 H24B 107.2 . . ? C26 C25 C24 115.3(7) . . ? C26 C25 H25A 108.4 . . ? C24 C25 H25A 108.4 . . ? C26 C25 H25B 108.4 . . ? C24 C25 H25B 108.4 . . ? H25A C25 H25B 107.5 . . ? C25 C26 C27 120.9(8) . . ? C25 C26 H26A 107.1 . . ? C27 C26 H26A 107.1 . . ? C25 C26 H26B 107.1 . . ? C27 C26 H26B 107.1 . . ? H26A C26 H26B 106.8 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 N6 117.1(7) . . ? C29 C28 H28A 108.0 . . ? N6 C28 H28A 108.0 . . ? C29 C28 H28B 108.0 . . ? N6 C28 H28B 108.0 . . ? H28A C28 H28B 107.3 . . ? C28 C29 C30 110.9(7) . . ? C28 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? C28 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C31 C30 C29 113.0(8) . . ? C31 C30 H30A 109.0 . . ? C29 C30 H30A 109.0 . . ? C31 C30 H30B 109.0 . . ? C29 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C32 C33 114.7(6) . . ? N6 C32 H32A 108.6 . . ? C33 C32 H32A 108.6 . . ? N6 C32 H32B 108.6 . . ? C33 C32 H32B 108.6 . . ? H32A C32 H32B 107.6 . . ? C32 C33 C34 114.0(9) . . ? C32 C33 H33A 108.8 . . ? C34 C33 H33A 108.8 . . ? C32 C33 H33B 108.8 . . ? C34 C33 H33B 108.8 . . ? H33A C33 H33B 107.6 . . ? C35 C34 C33 113.8(9) . . ? C35 C34 H34A 108.8 . . ? C33 C34 H34A 108.8 . . ? C35 C34 H34B 108.8 . . ? C33 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O8 S1 O8 179.998(2) 3_666 . ? O8 S1 O5 65.6(5) 3_666 3_666 ? O8 S1 O5 114.4(5) . 3_666 ? O8 S1 O5 114.4(5) 3_666 . ? O8 S1 O5 65.6(5) . . ? O5 S1 O5 179.998(2) 3_666 . ? O8 S1 O6 113.5(4) 3_666 3_666 ? O8 S1 O6 66.5(4) . 3_666 ? O5 S1 O6 71.6(5) 3_666 3_666 ? O5 S1 O6 108.4(5) . 3_666 ? O8 S1 O6 66.5(4) 3_666 . ? O8 S1 O6 113.5(4) . . ? O5 S1 O6 108.4(5) 3_666 . ? O5 S1 O6 71.6(5) . . ? O6 S1 O6 179.999(2) 3_666 . ? O8 S1 O7 71.2(5) 3_666 3_666 ? O8 S1 O7 108.8(5) . 3_666 ? O5 S1 O7 106.8(5) 3_666 3_666 ? O5 S1 O7 73.2(5) . 3_666 ? O6 S1 O7 75.7(4) 3_666 3_666 ? O6 S1 O7 104.3(4) . 3_666 ? O8 S1 O7 108.8(5) 3_666 . ? O8 S1 O7 71.2(5) . . ? O5 S1 O7 73.2(5) 3_666 . ? O5 S1 O7 106.8(5) . . ? O6 S1 O7 104.3(4) 3_666 . ? O6 S1 O7 75.7(4) . . ? O7 S1 O7 179.999(2) 3_666 . ? S1 O5 O8 55.0(4) . . ? S1 O5 O6 54.6(4) . . ? O8 O5 O6 94.4(6) . . ? S1 O5 O7 55.6(4) . 3_666 ? O8 O5 O7 91.0(6) . 3_666 ? O6 O5 O7 85.6(5) . 3_666 ? S1 O6 O8 54.0(4) . 3_666 ? S1 O6 O5 53.7(4) . . ? O8 O6 O5 93.2(6) 3_666 . ? S1 O7 O8 50.1(4) . . ? S1 O7 O5 51.2(4) . 3_666 ? O8 O7 O5 86.1(5) . 3_666 ? S1 O8 O5 59.5(4) . . ? S1 O8 O6 59.5(4) . 3_666 ? O5 O8 O6 99.7(6) . 3_666 ? S1 O8 O7 58.7(5) . . ? O5 O8 O7 95.6(7) . . ? O6 O8 O7 93.1(6) 3_666 . ? C15 C19 C19 121.7(8) . 3_766 ? C15 C19 C18 121.7(6) . 3_766 ? C19 C19 C18 116.6(7) 3_766 3_766 ? C18 C17 C16 121.6(7) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C15 C16 C17 121.2(7) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C17 C18 C19 119.2(6) . 3_766 ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 3_766 . ? 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 N1 C1 C6 -172.3(7) . . . . ? O2 N1 C1 C6 8.8(11) . . . . ? O1 N1 C1 C2 7.4(11) . . . . ? O2 N1 C1 C2 -171.5(8) . . . . ? C6 C1 C2 C3 -0.4(11) . . . . ? N1 C1 C2 C3 179.9(7) . . . . ? C1 C2 C3 C4 3.0(11) . . . . ? C7 N2 C4 C5 -17.5(11) . . . . ? C7 N2 C4 C3 161.0(6) . . . . ? C2 C3 C4 N2 178.3(7) . . . . ? C2 C3 C4 C5 -3.0(11) . . . . ? N2 C4 C5 C6 179.0(7) . . . . ? C3 C4 C5 C6 0.5(10) . . . . ? C4 C5 C6 C1 2.1(11) . . . . ? C2 C1 C6 C5 -2.1(11) . . . . ? N1 C1 C6 C5 177.5(7) . . . . ? C8 N3 C7 O3 2.1(10) . . . . ? C8 N3 C7 N2 179.7(6) . . . . ? C4 N2 C7 O3 5.0(11) . . . . ? C4 N2 C7 N3 -172.7(6) . . . . ? C7 N3 C8 C13 -139.1(7) . . . . ? C7 N3 C8 C9 42.5(9) . . . . ? C13 C8 C9 C10 0.8(10) . . . . ? N3 C8 C9 C10 179.1(6) . . . . ? C8 C9 C10 C11 -2.8(11) . . . . ? C9 C10 C11 C12 1.1(12) . . . . ? C10 C11 C12 C13 2.7(13) . . . . ? C9 C8 C13 C12 3.0(11) . . . . ? N3 C8 C13 C12 -175.4(7) . . . . ? C9 C8 C13 N4 -179.7(6) . . . . ? N3 C8 C13 N4 2.0(10) . . . . ? C11 C12 C13 C8 -4.8(13) . . . . ? C11 C12 C13 N4 178.0(8) . . . . ? C14 N4 C13 C8 139.7(7) . . . . ? C14 N4 C13 C12 -43.0(12) . . . . ? C15 N5 C14 O4 -5.2(12) . . . . ? C15 N5 C14 N4 171.9(6) . . . . ? C13 N4 C14 O4 7.4(12) . . . . ? C13 N4 C14 N5 -169.7(7) . . . . ? C14 N5 C15 C16 -43.1(10) . . . . ? C14 N5 C15 C19 140.8(7) . . . . ? C24 N6 C20 C21 -66.7(7) . . . . ? C28 N6 C20 C21 172.8(6) . . . . ? C32 N6 C20 C21 51.8(8) . . . . ? N6 C20 C21 C22 172.7(6) . . . . ? C20 C21 C22 C23 -73.7(8) . . . . ? C28 N6 C24 C25 62.4(9) . . . . ? C20 N6 C24 C25 -55.6(9) . . . . ? C32 N6 C24 C25 -176.0(7) . . . . ? N6 C24 C25 C26 -168.5(8) . . . . ? C24 C25 C26 C27 -178.3(10) . . . . ? C24 N6 C28 C29 67.9(8) . . . . ? C20 N6 C28 C29 -171.2(7) . . . . ? C32 N6 C28 C29 -51.1(9) . . . . ? N6 C28 C29 C30 -173.5(7) . . . . ? C28 C29 C30 C31 -165.1(9) . . . . ? C24 N6 C32 C33 177.9(6) . . . . ? C28 N6 C32 C33 -61.1(8) . . . . ? C20 N6 C32 C33 56.8(8) . . . . ? N6 C32 C33 C34 172.5(6) . . . . ? C32 C33 C34 C35 61.6(12) . . . . ? O8 S1 O5 O8 180.000(5) 3_666 . . . ? O5 S1 O5 O8 22(15) 3_666 . . . ? O6 S1 O5 O8 -52.2(6) 3_666 . . . ? O6 S1 O5 O8 127.8(6) . . . . ? O7 S1 O5 O8 -120.4(6) 3_666 . . . ? O7 S1 O5 O8 59.6(6) . . . . ? O8 S1 O5 O6 52.2(6) 3_666 . . . ? O8 S1 O5 O6 -127.8(6) . . . . ? O5 S1 O5 O6 -105(14) 3_666 . . . ? O6 S1 O5 O6 180.001(2) 3_666 . . . ? O7 S1 O5 O6 111.8(5) 3_666 . . . ? O7 S1 O5 O6 -68.2(5) . . . . ? O8 S1 O5 O7 -59.6(6) 3_666 . . 3_666 ? O8 S1 O5 O7 120.4(6) . . . 3_666 ? O5 S1 O5 O7 143(15) 3_666 . . 3_666 ? O6 S1 O5 O7 68.2(5) 3_666 . . 3_666 ? O6 S1 O5 O7 -111.8(5) . . . 3_666 ? O7 S1 O5 O7 179.999(3) . . . 3_666 ? O8 S1 O6 O8 180.002(5) . . . 3_666 ? O5 S1 O6 O8 -51.7(6) 3_666 . . 3_666 ? O5 S1 O6 O8 128.3(6) . . . 3_666 ? O6 S1 O6 O8 -169(2) 3_666 . . 3_666 ? O7 S1 O6 O8 61.8(6) 3_666 . . 3_666 ? O7 S1 O6 O8 -118.2(6) . . . 3_666 ? O8 S1 O6 O5 -128.3(6) 3_666 . . . ? O8 S1 O6 O5 51.7(6) . . . . ? O5 S1 O6 O5 179.998(2) 3_666 . . . ? O6 S1 O6 O5 63.2(19) 3_666 . . . ? O7 S1 O6 O5 -66.5(5) 3_666 . . . ? O7 S1 O6 O5 113.5(5) . . . . ? O8 O5 O6 S1 -40.5(4) . . . . ? O7 O5 O6 S1 50.2(4) 3_666 . . . ? S1 O5 O6 O8 -39.5(4) . . . 3_666 ? O8 O5 O6 O8 -80.0(7) . . . 3_666 ? O7 O5 O6 O8 10.7(6) 3_666 . . 3_666 ? O8 S1 O7 O8 180.0 3_666 . . . ? O5 S1 O7 O8 124.0(6) 3_666 . . . ? O5 S1 O7 O8 -56.0(6) . . . . ? O6 S1 O7 O8 58.6(5) 3_666 . . . ? O6 S1 O7 O8 -121.4(5) . . . . ? O7 S1 O7 O8 51(6) 3_666 . . . ? O8 S1 O7 O5 56.0(6) 3_666 . . 3_666 ? O8 S1 O7 O5 -124.0(6) . . . 3_666 ? O5 S1 O7 O5 180.001(3) . . . 3_666 ? O6 S1 O7 O5 -65.4(5) 3_666 . . 3_666 ? O6 S1 O7 O5 114.6(5) . . . 3_666 ? O7 S1 O7 O5 -73(8) 3_666 . . 3_666 ? O8 S1 O8 O5 -173(17) 3_666 . . . ? O5 S1 O8 O5 180.001(4) 3_666 . . . ? O6 S1 O8 O5 125.1(6) 3_666 . . . ? O6 S1 O8 O5 -54.9(6) . . . . ? O7 S1 O8 O5 60.7(6) 3_666 . . . ? O7 S1 O8 O5 -119.3(6) . . . . ? O8 S1 O8 O6 62(16) 3_666 . . 3_666 ? O5 S1 O8 O6 54.9(6) 3_666 . . 3_666 ? O5 S1 O8 O6 -125.1(6) . . . 3_666 ? O6 S1 O8 O6 180.000(4) . . . 3_666 ? O7 S1 O8 O6 -64.4(5) 3_666 . . 3_666 ? O7 S1 O8 O6 115.6(5) . . . 3_666 ? O8 S1 O8 O7 -54(17) 3_666 . . . ? O5 S1 O8 O7 -60.7(6) 3_666 . . . ? O5 S1 O8 O7 119.3(6) . . . . ? O6 S1 O8 O7 -115.6(5) 3_666 . . . ? O6 S1 O8 O7 64.4(5) . . . . ? O7 S1 O8 O7 180.0 3_666 . . . ? O6 O5 O8 S1 40.3(4) . . . . ? O7 O5 O8 S1 -45.4(4) 3_666 . . . ? S1 O5 O8 O6 45.7(5) . . . 3_666 ? O6 O5 O8 O6 86.0(7) . . . 3_666 ? O7 O5 O8 O6 0.3(7) 3_666 . . 3_666 ? S1 O5 O8 O7 -48.4(4) . . . . ? O6 O5 O8 O7 -8.1(6) . . . . ? O7 O5 O8 O7 -93.8(6) 3_666 . . . ? O5 O7 O8 S1 40.4(4) 3_666 . . . ? S1 O7 O8 O5 49.0(5) . . . . ? O5 O7 O8 O5 89.3(6) 3_666 . . . ? S1 O7 O8 O6 -51.1(4) . . . 3_666 ? O5 O7 O8 O6 -10.7(6) 3_666 . . 3_666 ? C16 C15 C19 C19 2.2(11) . . . 3_766 ? N5 C15 C19 C19 178.4(7) . . . 3_766 ? C16 C15 C19 C18 -178.8(6) . . . 3_766 ? N5 C15 C19 C18 -2.6(9) . . . 3_766 ? C19 C15 C16 C17 -2.8(11) . . . . ? N5 C15 C16 C17 -178.8(6) . . . . ? C18 C17 C16 C15 2.2(11) . . . . ? C16 C17 C18 C19 -0.8(10) . . . 3_766 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.889 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.088 data_2 _database_code_depnum_ccdc_archive 'CCDC 913110' #TrackingRef 'ACPs-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H174 N14 O16 S2' _chemical_formula_weight 1916.67 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' S S 0.1246 0.1234 '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 9.538(12) _cell_length_b 13.957(17) _cell_length_c 22.00(3) _cell_angle_alpha 94.690(15) _cell_angle_beta 100.617(17) _cell_angle_gamma 99.018(16) _cell_volume 2824(6) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9727 _exptl_absorpt_correction_T_max 0.9890 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17219 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.1165 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9520 _reflns_number_gt 5313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0000P)^2^+5.0000P] 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 9520 _refine_ls_number_parameters 621 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1487 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.1768 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.132 _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 S1 S 0.54319(12) 0.87063(7) 0.22414(5) 0.0248(3) Uani 1 1 d . . . O1 O 1.0849(5) 0.6328(3) 0.54827(18) 0.0753(14) Uani 1 1 d . . . O2 O 1.0973(5) 0.7902(3) 0.5491(2) 0.0938(15) Uani 1 1 d U . . O3 O 0.5363(3) 0.48901(19) 0.27751(14) 0.0373(8) Uani 1 1 d . . . O4 O 0.2402(3) 0.6710(2) -0.00813(13) 0.0391(8) Uani 1 1 d . . . O5 O 0.5792(3) 0.78856(18) 0.18296(12) 0.0280(7) Uani 1 1 d . . . O6 O 0.4104(3) 0.9024(2) 0.18989(14) 0.0391(8) Uani 1 1 d . . . O7 O 0.5130(4) 0.8290(2) 0.28261(13) 0.0410(8) Uani 1 1 d . . . O8 O 0.6688(3) 0.95186(19) 0.23940(15) 0.0402(8) Uani 1 1 d . . . N1 N 1.0552(9) 0.7069(5) 0.5217(4) 0.0290(19) Uani 0.60 1 d PU . . N1' N 1.021(2) 0.6966(13) 0.5350(8) 0.074(6) Uani 0.40 1 d PU . . N2 N 0.6119(4) 0.6572(2) 0.30334(15) 0.0273(8) Uani 1 1 d . . . H2A H 0.5954 0.7137 0.2913 0.033 Uiso 1 1 calc R . . N3 N 0.4482(4) 0.5995(2) 0.21252(15) 0.0255(8) Uani 1 1 d . . . H3A H 0.4676 0.6611 0.2061 0.031 Uiso 1 1 calc R . . N4 N 0.3455(4) 0.6673(2) 0.09691(15) 0.0268(8) Uani 1 1 d . . . H4A H 0.4106 0.7019 0.1276 0.032 Uiso 1 1 calc R . . N5 N 0.3804(4) 0.8105(2) 0.05221(16) 0.0348(10) Uani 1 1 d . . . H5A H 0.4257 0.8331 0.0905 0.042 Uiso 1 1 calc R . . N6 N 0.0077(4) 0.7493(2) 0.20977(18) 0.0340(9) Uani 1 1 d . . . N7 N 0.5680(4) 0.2060(2) 0.29034(16) 0.0321(9) Uani 1 1 d . . . C1 C 0.9319(6) 0.6906(3) 0.4681(2) 0.0439(13) Uani 1 1 d . . . C2 C 0.8777(5) 0.5960(3) 0.4377(2) 0.0410(12) Uani 1 1 d . . . H2 H 0.9130 0.5415 0.4542 0.049 Uiso 1 1 calc R . . C3 C 0.7703(5) 0.5817(3) 0.3824(2) 0.0351(11) Uani 1 1 d . . . H3 H 0.7350 0.5178 0.3615 0.042 Uiso 1 1 calc R . . C4 C 0.7153(5) 0.6618(3) 0.35818(19) 0.0276(10) Uani 1 1 d . . . C5 C 0.7723(5) 0.7571(3) 0.3906(2) 0.0433(13) Uani 1 1 d . . . H5 H 0.7359 0.8118 0.3751 0.052 Uiso 1 1 calc R . . C6 C 0.8797(6) 0.7716(3) 0.4445(2) 0.0539(15) Uani 1 1 d . . . H6 H 0.9172 0.8355 0.4650 0.065 Uiso 1 1 calc R . . C7 C 0.5307(5) 0.5734(3) 0.26489(19) 0.0246(10) Uani 1 1 d . . . C8 C 0.3331(4) 0.5380(3) 0.16648(19) 0.0239(10) Uani 1 1 d . . . C9 C 0.2675(5) 0.4461(3) 0.1799(2) 0.0306(11) Uani 1 1 d . . . H9 H 0.2993 0.4239 0.2190 0.037 Uiso 1 1 calc R . . C10 C 0.1546(5) 0.3871(3) 0.1352(2) 0.0353(12) Uani 1 1 d . . . H10 H 0.1111 0.3254 0.1444 0.042 Uiso 1 1 calc R . . C11 C 0.1065(5) 0.4191(3) 0.0774(2) 0.0314(11) Uani 1 1 d . . . H11 H 0.0313 0.3789 0.0475 0.038 Uiso 1 1 calc R . . C12 C 0.1694(5) 0.5101(3) 0.0641(2) 0.0303(11) Uani 1 1 d . . . H12 H 0.1360 0.5316 0.0250 0.036 Uiso 1 1 calc R . . C13 C 0.2837(4) 0.5716(3) 0.10846(19) 0.0248(10) Uani 1 1 d . . . C14 C 0.3143(5) 0.7122(3) 0.0423(2) 0.0296(11) Uani 1 1 d . . . C15 C 0.3825(5) 0.8786(3) 0.0066(2) 0.0298(11) Uani 1 1 d . . . C16 C 0.4999(5) 0.9631(3) 0.02136(18) 0.0258(10) Uani 1 1 d . . . C17 C 0.6126(5) 0.9759(3) 0.07669(19) 0.0286(10) Uani 1 1 d . . . H17 H 0.6149 0.9268 0.1042 0.034 Uiso 1 1 calc R . . C18 C 0.7173(5) 1.0599(3) 0.0896(2) 0.0325(11) Uani 1 1 d . . . H18 H 0.7886 1.0683 0.1269 0.039 Uiso 1 1 calc R . . C19 C 0.7213(5) 1.1336(3) 0.0490(2) 0.0323(11) Uani 1 1 d . . . H19 H 0.7935 1.1907 0.0593 0.039 Uiso 1 1 calc R . . C20 C 0.0520(5) 0.7789(3) 0.1489(2) 0.0407(12) Uani 1 1 d . . . H20A H 0.0822 0.7224 0.1279 0.049 Uiso 1 1 calc R . . H20B H 0.1375 0.8320 0.1599 0.049 Uiso 1 1 calc R . . C21 C -0.0668(6) 0.8137(4) 0.1019(3) 0.0537(15) Uani 1 1 d . . . H21A H -0.1448 0.7578 0.0837 0.064 Uiso 1 1 calc R . . H21B H -0.1098 0.8632 0.1237 0.064 Uiso 1 1 calc R . . C22 C 0.0010(6) 0.8584(3) 0.0497(3) 0.0541(15) Uani 1 1 d . . . H22A H -0.0775 0.8661 0.0151 0.065 Uiso 1 1 calc R . . H22B H 0.0586 0.8128 0.0334 0.065 Uiso 1 1 calc R . . C23 C 0.1005(6) 0.9595(3) 0.0724(3) 0.0573(15) Uani 1 1 d . . . H23A H 0.0449 1.0045 0.0897 0.086 Uiso 1 1 calc R . . H23B H 0.1366 0.9860 0.0372 0.086 Uiso 1 1 calc R . . H23C H 0.1825 0.9515 0.1045 0.086 Uiso 1 1 calc R . . C24 C -0.0358(5) 0.8356(3) 0.2463(2) 0.0416(13) Uani 1 1 d . . . H24A H -0.0619 0.8141 0.2852 0.050 Uiso 1 1 calc R . . H24B H -0.1229 0.8537 0.2211 0.050 Uiso 1 1 calc R . . C25 C 0.0870(6) 0.9281(3) 0.2632(3) 0.0631(17) Uani 1 1 d . . . H25A H 0.1700 0.9126 0.2926 0.076 Uiso 1 1 calc R . . H25B H 0.1211 0.9455 0.2250 0.076 Uiso 1 1 calc R . . C26 C 0.0347(7) 1.0157(4) 0.2926(3) 0.072(2) Uani 1 1 d . . . H26A H 0.1105 1.0744 0.2969 0.086 Uiso 1 1 calc R . . H26B H -0.0532 1.0278 0.2647 0.086 Uiso 1 1 calc R . . C27 C 0.0018(8) 1.0005(5) 0.3536(3) 0.085(2) Uani 1 1 d . . . H27A H -0.0943 0.9601 0.3485 0.128 Uiso 1 1 calc R . . H27B H 0.0028 1.0638 0.3768 0.128 Uiso 1 1 calc R . . H27C H 0.0746 0.9676 0.3767 0.128 Uiso 1 1 calc R . . C28 C 0.1389(5) 0.7152(3) 0.2480(2) 0.0361(12) Uani 1 1 d . . . H28A H 0.1579 0.6571 0.2240 0.043 Uiso 1 1 calc R . . H28B H 0.2244 0.7673 0.2519 0.043 Uiso 1 1 calc R . . C29 C 0.1272(5) 0.6892(3) 0.3136(2) 0.0427(12) Uani 1 1 d . . . H29A H 0.0405 0.6385 0.3111 0.051 Uiso 1 1 calc R . . H29B H 0.1158 0.7478 0.3396 0.051 Uiso 1 1 calc R . . C30 C 0.2647(6) 0.6508(3) 0.3446(2) 0.0472(13) Uani 1 1 d . . . H30A H 0.2705 0.5894 0.3200 0.057 Uiso 1 1 calc R . . H30B H 0.3513 0.6991 0.3428 0.057 Uiso 1 1 calc R . . C31 C 0.2690(7) 0.6317(5) 0.4122(3) 0.0773(19) Uani 1 1 d . . . H31A H 0.2599 0.6914 0.4368 0.116 Uiso 1 1 calc R . . H31B H 0.3611 0.6118 0.4291 0.116 Uiso 1 1 calc R . . H31C H 0.1886 0.5796 0.4142 0.116 Uiso 1 1 calc R . . C32 C -0.1280(5) 0.6676(3) 0.1951(2) 0.0331(11) Uani 1 1 d . . . H32A H -0.2091 0.6932 0.1706 0.040 Uiso 1 1 calc R . . H32B H -0.1557 0.6518 0.2348 0.040 Uiso 1 1 calc R . . C33 C -0.1091(5) 0.5716(3) 0.1586(2) 0.0418(13) Uani 1 1 d . . . H33A H -0.0411 0.5388 0.1856 0.050 Uiso 1 1 calc R . . H33B H -0.0671 0.5875 0.1219 0.050 Uiso 1 1 calc R . . C34 C -0.2575(6) 0.5013(3) 0.1366(2) 0.0470(14) Uani 1 1 d . . . H34A H -0.2394 0.4356 0.1233 0.056 Uiso 1 1 calc R . . H34B H -0.3070 0.4956 0.1723 0.056 Uiso 1 1 calc R . . C35 C -0.3582(6) 0.5348(4) 0.0828(2) 0.0551(15) Uani 1 1 d . . . H35A H -0.3809 0.5983 0.0963 0.083 Uiso 1 1 calc R . . H35B H -0.4480 0.4868 0.0706 0.083 Uiso 1 1 calc R . . H35C H -0.3100 0.5407 0.0473 0.083 Uiso 1 1 calc R . . C36 C 0.7093(5) 0.2769(3) 0.2901(2) 0.0408(12) Uani 1 1 d . . . H36A H 0.6853 0.3293 0.2644 0.049 Uiso 1 1 calc R . . H36B H 0.7500 0.3079 0.3332 0.049 Uiso 1 1 calc R . . C37 C 0.8254(6) 0.2305(4) 0.2659(3) 0.0542(15) Uani 1 1 d . . . H37A H 0.8677 0.1907 0.2973 0.065 Uiso 1 1 calc R . . H37B H 0.7794 0.1861 0.2276 0.065 Uiso 1 1 calc R . . C38 C 0.9441(8) 0.3028(5) 0.2517(4) 0.111(3) Uani 1 1 d . . . H38A H 0.9099 0.3214 0.2097 0.133 Uiso 1 1 calc R . . H38B H 1.0267 0.2687 0.2489 0.133 Uiso 1 1 calc R . . C39 C 1.0021(8) 0.3961(5) 0.2950(4) 0.095(2) Uani 1 1 d . . . H39A H 0.9238 0.4334 0.2969 0.143 Uiso 1 1 calc R . . H39B H 1.0797 0.4352 0.2795 0.143 Uiso 1 1 calc R . . H39C H 1.0403 0.3802 0.3367 0.143 Uiso 1 1 calc R . . C40 C 0.6087(5) 0.1272(3) 0.3331(2) 0.0405(12) Uani 1 1 d . . . H40A H 0.6668 0.0867 0.3125 0.049 Uiso 1 1 calc R . . H40B H 0.6715 0.1608 0.3723 0.049 Uiso 1 1 calc R . . C41 C 0.4830(6) 0.0590(3) 0.3495(2) 0.0458(13) Uani 1 1 d . . . H41A H 0.4278 0.0158 0.3120 0.055 Uiso 1 1 calc R . . H41B H 0.4165 0.0975 0.3659 0.055 Uiso 1 1 calc R . . C42 C 0.5479(6) -0.0030(3) 0.3998(2) 0.0483(14) Uani 1 1 d . . . H42A H 0.6185 -0.0377 0.3834 0.058 Uiso 1 1 calc R . . H42B H 0.6012 0.0415 0.4371 0.058 Uiso 1 1 calc R . . C43 C 0.4338(7) -0.0780(4) 0.4192(3) 0.0694(19) Uani 1 1 d . . . H43A H 0.3683 -0.0440 0.4388 0.104 Uiso 1 1 calc R . . H43B H 0.4821 -0.1170 0.4489 0.104 Uiso 1 1 calc R . . H43C H 0.3782 -0.1210 0.3824 0.104 Uiso 1 1 calc R . . C44 C 0.4955(5) 0.1585(3) 0.2233(2) 0.0374(12) Uani 1 1 d . . . H44A H 0.5499 0.1076 0.2112 0.045 Uiso 1 1 calc R . . H44B H 0.3959 0.1256 0.2236 0.045 Uiso 1 1 calc R . . C45 C 0.4877(6) 0.2295(3) 0.1736(2) 0.0428(13) Uani 1 1 d . . . H45A H 0.5864 0.2519 0.1664 0.051 Uiso 1 1 calc R . . H45B H 0.4509 0.2874 0.1891 0.051 Uiso 1 1 calc R . . C46 C 0.3878(5) 0.1822(3) 0.1110(2) 0.0425(13) Uani 1 1 d . . . H46A H 0.4185 0.1207 0.0973 0.051 Uiso 1 1 calc R . . H46B H 0.2868 0.1660 0.1169 0.051 Uiso 1 1 calc R . . C47 C 0.3947(6) 0.2526(4) 0.0601(2) 0.0540(15) Uani 1 1 d . . . H47A H 0.3568 0.3111 0.0721 0.081 Uiso 1 1 calc R . . H47B H 0.3363 0.2198 0.0203 0.081 Uiso 1 1 calc R . . H47C H 0.4955 0.2713 0.0558 0.081 Uiso 1 1 calc R . . C48 C 0.4648(6) 0.2648(3) 0.3160(2) 0.0451(13) Uani 1 1 d . . . H48A H 0.3696 0.2217 0.3110 0.054 Uiso 1 1 calc R . . H48B H 0.4507 0.3185 0.2901 0.054 Uiso 1 1 calc R . . C49 C 0.5113(7) 0.3093(4) 0.3844(3) 0.0615(17) Uani 1 1 d . . . H49A H 0.6004 0.3589 0.3898 0.074 Uiso 1 1 calc R . . H49B H 0.5318 0.2577 0.4114 0.074 Uiso 1 1 calc R . . C50 C 0.3838(8) 0.3582(5) 0.4028(3) 0.092(2) Uani 1 1 d DU . . H50A H 0.3646 0.4083 0.3745 0.110 Uiso 1 1 calc R . . H50B H 0.2954 0.3075 0.3950 0.110 Uiso 1 1 calc R . . C51 C 0.4060(18) 0.4045(10) 0.4673(5) 0.256(7) Uani 1 1 d DU . . H51A H 0.3626 0.3582 0.4926 0.384 Uiso 1 1 calc R . . H51B H 0.3602 0.4626 0.4677 0.384 Uiso 1 1 calc R . . H51C H 0.5101 0.4234 0.4844 0.384 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 S1 0.0235(6) 0.0196(5) 0.0288(6) 0.0009(4) 0.0003(5) 0.0036(4) O1 0.089(4) 0.066(3) 0.059(3) 0.005(2) -0.028(2) 0.030(2) O2 0.0943(17) 0.0907(16) 0.0932(17) 0.0079(10) 0.0101(10) 0.0179(10) O3 0.044(2) 0.0211(15) 0.0416(19) 0.0068(13) -0.0052(16) 0.0038(13) O4 0.044(2) 0.0340(16) 0.0296(18) 0.0015(14) -0.0052(15) -0.0070(14) O5 0.0263(18) 0.0250(14) 0.0301(16) -0.0045(12) 0.0045(14) 0.0017(12) O6 0.027(2) 0.0430(17) 0.046(2) 0.0105(15) -0.0027(16) 0.0129(14) O7 0.063(2) 0.0373(17) 0.0312(18) 0.0104(14) 0.0194(17) 0.0205(15) O8 0.0282(19) 0.0271(15) 0.058(2) -0.0067(14) 0.0030(16) -0.0045(13) N1 0.029(2) 0.028(2) 0.029(2) 0.0022(10) 0.0048(11) 0.0043(10) N1' 0.074(6) 0.074(6) 0.074(6) 0.0086(12) 0.0148(15) 0.0125(14) N2 0.030(2) 0.0224(17) 0.029(2) 0.0049(14) 0.0007(17) 0.0063(14) N3 0.028(2) 0.0163(16) 0.030(2) 0.0055(14) 0.0015(17) 0.0009(14) N4 0.027(2) 0.0206(16) 0.027(2) 0.0060(15) -0.0048(17) -0.0026(14) N5 0.041(3) 0.0284(18) 0.025(2) 0.0038(16) -0.0075(18) -0.0078(16) N6 0.021(2) 0.0310(19) 0.052(2) 0.0044(17) 0.0091(19) 0.0081(15) N7 0.039(3) 0.0206(17) 0.035(2) 0.0013(15) 0.0043(18) 0.0058(15) C1 0.049(4) 0.047(3) 0.029(3) -0.003(2) -0.011(2) 0.013(2) C2 0.044(3) 0.042(3) 0.038(3) 0.009(2) 0.003(2) 0.016(2) C3 0.034(3) 0.033(2) 0.035(3) 0.004(2) -0.004(2) 0.009(2) C4 0.027(3) 0.028(2) 0.029(2) 0.0050(18) 0.009(2) 0.0073(18) C5 0.051(4) 0.029(2) 0.043(3) 0.000(2) -0.011(3) 0.011(2) C6 0.059(4) 0.038(3) 0.052(3) -0.007(2) -0.016(3) 0.008(2) C7 0.025(3) 0.023(2) 0.026(2) 0.0036(17) 0.007(2) 0.0035(17) C8 0.019(2) 0.0209(19) 0.030(2) 0.0010(17) 0.0026(19) 0.0017(16) C9 0.033(3) 0.026(2) 0.032(3) 0.0083(19) 0.003(2) 0.0054(18) C10 0.032(3) 0.022(2) 0.051(3) 0.004(2) 0.012(2) -0.0014(18) C11 0.027(3) 0.024(2) 0.038(3) 0.0018(19) -0.002(2) -0.0007(18) C12 0.026(3) 0.027(2) 0.033(3) 0.0034(19) -0.003(2) 0.0030(18) C13 0.025(3) 0.024(2) 0.027(2) 0.0035(17) 0.005(2) 0.0069(17) C14 0.027(3) 0.024(2) 0.035(3) 0.0044(19) 0.001(2) 0.0000(18) C15 0.034(3) 0.024(2) 0.030(2) 0.0050(18) 0.004(2) 0.0013(18) C16 0.027(3) 0.023(2) 0.029(3) 0.0035(17) 0.008(2) 0.0038(17) C17 0.034(3) 0.024(2) 0.029(2) 0.0061(18) 0.006(2) 0.0060(18) C18 0.029(3) 0.036(2) 0.029(3) 0.006(2) -0.003(2) 0.0023(19) C19 0.031(3) 0.026(2) 0.036(3) 0.0022(19) -0.002(2) 0.0003(18) C20 0.027(3) 0.045(3) 0.054(3) 0.017(2) 0.012(2) 0.005(2) C21 0.029(3) 0.056(3) 0.074(4) 0.032(3) 0.001(3) 0.002(2) C22 0.040(4) 0.050(3) 0.069(4) 0.027(3) -0.001(3) 0.002(2) C23 0.060(4) 0.047(3) 0.070(4) 0.022(3) 0.015(3) 0.011(3) C24 0.026(3) 0.033(2) 0.063(3) -0.004(2) 0.004(2) 0.008(2) C25 0.039(4) 0.040(3) 0.101(5) -0.012(3) 0.003(3) 0.000(2) C26 0.057(4) 0.038(3) 0.111(6) -0.014(3) 0.004(4) 0.005(3) C27 0.090(6) 0.080(5) 0.093(5) 0.005(4) 0.036(5) 0.018(4) C28 0.030(3) 0.029(2) 0.052(3) 0.005(2) 0.011(2) 0.0098(19) C29 0.034(3) 0.045(3) 0.053(3) 0.010(2) 0.013(3) 0.012(2) C30 0.037(3) 0.047(3) 0.060(4) 0.013(3) 0.009(3) 0.011(2) C31 0.071(5) 0.111(5) 0.063(4) 0.042(4) 0.015(4) 0.038(4) C32 0.020(3) 0.031(2) 0.049(3) 0.002(2) 0.012(2) 0.0009(18) C33 0.033(3) 0.034(2) 0.058(3) -0.004(2) 0.011(2) 0.007(2) C34 0.047(3) 0.033(2) 0.057(3) -0.007(2) 0.007(3) 0.005(2) C35 0.042(4) 0.057(3) 0.062(4) -0.014(3) 0.011(3) 0.004(3) C36 0.044(3) 0.032(2) 0.041(3) 0.003(2) 0.000(2) 0.000(2) C37 0.045(4) 0.052(3) 0.068(4) 0.010(3) 0.013(3) 0.012(3) C38 0.089(6) 0.081(5) 0.174(8) -0.008(5) 0.087(6) -0.009(4) C39 0.066(5) 0.081(5) 0.129(7) 0.011(4) 0.027(5) -0.024(4) C40 0.046(3) 0.030(2) 0.044(3) -0.005(2) 0.008(2) 0.009(2) C41 0.052(4) 0.034(2) 0.050(3) -0.004(2) 0.012(3) 0.005(2) C42 0.073(4) 0.035(3) 0.036(3) 0.002(2) 0.012(3) 0.008(2) C43 0.100(6) 0.051(3) 0.054(4) 0.010(3) 0.017(4) 0.000(3) C44 0.040(3) 0.027(2) 0.040(3) -0.002(2) -0.001(2) 0.0028(19) C45 0.050(3) 0.031(2) 0.047(3) 0.004(2) 0.004(3) 0.010(2) C46 0.039(3) 0.047(3) 0.039(3) 0.002(2) 0.000(2) 0.012(2) C47 0.060(4) 0.062(3) 0.045(3) 0.015(3) 0.011(3) 0.021(3) C48 0.061(4) 0.031(2) 0.051(3) 0.007(2) 0.022(3) 0.017(2) C49 0.082(5) 0.051(3) 0.058(4) 0.001(3) 0.022(3) 0.024(3) C50 0.093(2) 0.092(2) 0.092(2) 0.0080(10) 0.0189(11) 0.0192(11) C51 0.256(7) 0.256(7) 0.256(7) 0.0289(13) 0.0512(17) 0.0453(16) _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 S1 O8 1.483(3) . ? S1 O6 1.500(3) . ? S1 O7 1.510(3) . ? S1 O5 1.523(3) . ? O1 N1' 1.185(19) . ? O1 N1 1.274(9) . ? O2 N1 1.235(8) . ? O2 N1' 1.373(17) . ? O3 C7 1.239(5) . ? O4 C14 1.242(5) . ? N1 C1 1.478(9) . ? N1' C1 1.545(18) . ? N2 C4 1.401(5) . ? N2 C7 1.413(5) . ? N2 H2A 0.8800 . ? N3 C7 1.380(5) . ? N3 C8 1.455(5) . ? N3 H3A 0.8800 . ? N4 C14 1.404(5) . ? N4 C13 1.434(5) . ? N4 H4A 0.8800 . ? N5 C14 1.400(5) . ? N5 C15 1.437(5) . ? N5 H5A 0.8800 . ? N6 C28 1.537(6) . ? N6 C20 1.545(6) . ? N6 C24 1.546(5) . ? N6 C32 1.550(5) . ? N7 C48 1.532(6) . ? N7 C36 1.543(6) . ? N7 C40 1.554(6) . ? N7 C44 1.554(5) . ? C1 C2 1.404(6) . ? C1 C6 1.404(7) . ? C2 C3 1.416(6) . ? C2 H2 0.9500 . ? C3 C4 1.409(6) . ? C3 H3 0.9500 . ? C4 C5 1.431(5) . ? C5 C6 1.394(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.416(6) . ? C8 C13 1.420(6) . ? C9 C10 1.416(6) . ? C9 H9 0.9500 . ? C10 C11 1.402(6) . ? C10 H10 0.9500 . ? C11 C12 1.395(6) . ? C11 H11 0.9500 . ? C12 C13 1.434(5) . ? C12 H12 0.9500 . ? C15 C19 1.404(6) 2_675 ? C15 C16 1.463(6) . ? C16 C17 1.446(6) . ? C16 C16 1.449(8) 2_675 ? C17 C18 1.389(6) . ? C17 H17 0.9500 . ? C18 C19 1.416(6) . ? C18 H18 0.9500 . ? C19 C15 1.404(6) 2_675 ? C19 H19 0.9500 . ? C20 C21 1.553(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.547(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.559(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.570(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.530(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.458(9) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.536(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.556(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.528(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.557(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.561(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.534(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.522(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.490(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.512(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.527(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.558(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.534(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.534(6) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.552(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.552(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.534(7) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.583(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.474(8) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 S1 O6 111.7(2) . . ? O8 S1 O7 110.43(19) . . ? O6 S1 O7 110.1(2) . . ? O8 S1 O5 109.21(19) . . ? O6 S1 O5 108.22(18) . . ? O7 S1 O5 106.96(18) . . ? N1' O1 N1 22.7(9) . . ? N1 O2 N1' 20.9(8) . . ? O2 N1 O1 120.6(7) . . ? O2 N1 C1 118.7(6) . . ? O1 N1 C1 117.5(5) . . ? O1 N1' O2 116.7(15) . . ? O1 N1' C1 118.6(13) . . ? O2 N1' C1 106.3(12) . . ? C4 N2 C7 128.2(3) . . ? C4 N2 H2A 115.9 . . ? C7 N2 H2A 115.9 . . ? C7 N3 C8 128.3(3) . . ? C7 N3 H3A 115.8 . . ? C8 N3 H3A 115.8 . . ? C14 N4 C13 127.7(3) . . ? C14 N4 H4A 116.2 . . ? C13 N4 H4A 116.2 . . ? C14 N5 C15 127.1(3) . . ? C14 N5 H5A 116.5 . . ? C15 N5 H5A 116.5 . . ? C28 N6 C20 106.7(3) . . ? C28 N6 C24 111.1(3) . . ? C20 N6 C24 111.2(3) . . ? C28 N6 C32 111.7(3) . . ? C20 N6 C32 110.4(3) . . ? C24 N6 C32 105.8(3) . . ? C48 N7 C36 107.9(3) . . ? C48 N7 C40 111.1(4) . . ? C36 N7 C40 107.2(4) . . ? C48 N7 C44 109.1(4) . . ? C36 N7 C44 110.8(3) . . ? C40 N7 C44 110.9(3) . . ? C2 C1 C6 120.7(4) . . ? C2 C1 N1 120.0(5) . . ? C6 C1 N1 119.1(5) . . ? C2 C1 N1' 115.7(8) . . ? C6 C1 N1' 121.9(8) . . ? N1 C1 N1' 18.6(7) . . ? C1 C2 C3 119.9(4) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? N2 C4 C3 125.7(3) . . ? N2 C4 C5 116.2(4) . . ? C3 C4 C5 118.1(4) . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C1 119.2(4) . . ? C5 C6 H6 120.4 . . ? C1 C6 H6 120.4 . . ? O3 C7 N3 126.1(3) . . ? O3 C7 N2 123.3(4) . . ? N3 C7 N2 110.6(3) . . ? C9 C8 C13 119.8(4) . . ? C9 C8 N3 120.3(4) . . ? C13 C8 N3 119.8(3) . . ? C10 C9 C8 120.1(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.5(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 119.8(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 121.1(4) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C8 C13 C12 118.7(4) . . ? C8 C13 N4 119.2(3) . . ? C12 C13 N4 122.0(4) . . ? O4 C14 N5 124.1(4) . . ? O4 C14 N4 125.3(4) . . ? N5 C14 N4 110.5(3) . . ? C19 C15 N5 122.9(4) 2_675 . ? C19 C15 C16 121.0(4) 2_675 . ? N5 C15 C16 116.1(4) . . ? C17 C16 C16 119.6(4) . 2_675 ? C17 C16 C15 122.6(4) . . ? C16 C16 C15 117.8(5) 2_675 . ? C18 C17 C16 119.9(4) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 122.2(4) . . ? C17 C18 H18 118.9 . . ? C19 C18 H18 118.9 . . ? C15 C19 C18 119.4(4) 2_675 . ? C15 C19 H19 120.3 2_675 . ? C18 C19 H19 120.3 . . ? N6 C20 C21 115.6(4) . . ? N6 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? N6 C20 H20B 108.4 . . ? C21 C20 H20B 108.4 . . ? H20A C20 H20B 107.4 . . ? C22 C21 C20 109.4(4) . . ? C22 C21 H21A 109.8 . . ? C20 C21 H21A 109.8 . . ? C22 C21 H21B 109.8 . . ? C20 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C21 C22 C23 112.8(4) . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C24 C25 113.4(4) . . ? N6 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N6 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 112.0(5) . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C25 112.4(5) . . ? C27 C26 H26A 109.1 . . ? C25 C26 H26A 109.1 . . ? C27 C26 H26B 109.1 . . ? C25 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 N6 117.1(4) . . ? C29 C28 H28A 108.0 . . ? N6 C28 H28A 108.0 . . ? C29 C28 H28B 108.0 . . ? N6 C28 H28B 108.0 . . ? H28A C28 H28B 107.3 . . ? C28 C29 C30 110.7(4) . . ? C28 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C31 C30 C29 114.4(5) . . ? C31 C30 H30A 108.7 . . ? C29 C30 H30A 108.7 . . ? C31 C30 H30B 108.7 . . ? C29 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C32 C33 115.0(4) . . ? N6 C32 H32A 108.5 . . ? C33 C32 H32A 108.5 . . ? N6 C32 H32B 108.5 . . ? C33 C32 H32B 108.5 . . ? H32A C32 H32B 107.5 . . ? C32 C33 C34 110.9(4) . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 113.6(4) . . ? C35 C34 H34A 108.9 . . ? C33 C34 H34A 108.9 . . ? C35 C34 H34B 108.9 . . ? C33 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 N7 115.1(4) . . ? C37 C36 H36A 108.5 . . ? N7 C36 H36A 108.5 . . ? C37 C36 H36B 108.5 . . ? N7 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? C38 C37 C36 113.7(5) . . ? C38 C37 H37A 108.8 . . ? C36 C37 H37A 108.8 . . ? C38 C37 H37B 108.8 . . ? C36 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? C37 C38 C39 119.5(6) . . ? C37 C38 H38A 107.4 . . ? C39 C38 H38A 107.4 . . ? C37 C38 H38B 107.4 . . ? C39 C38 H38B 107.4 . . ? H38A C38 H38B 107.0 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 N7 116.6(4) . . ? C41 C40 H40A 108.2 . . ? N7 C40 H40A 108.2 . . ? C41 C40 H40B 108.2 . . ? N7 C40 H40B 108.2 . . ? H40A C40 H40B 107.3 . . ? C40 C41 C42 107.7(4) . . ? C40 C41 H41A 110.2 . . ? C42 C41 H41A 110.2 . . ? C40 C41 H41B 110.2 . . ? C42 C41 H41B 110.2 . . ? H41A C41 H41B 108.5 . . ? C43 C42 C41 113.6(5) . . ? C43 C42 H42A 108.8 . . ? C41 C42 H42A 108.8 . . ? C43 C42 H42B 108.8 . . ? C41 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 N7 115.0(3) . . ? C45 C44 H44A 108.5 . . ? N7 C44 H44A 108.5 . . ? C45 C44 H44B 108.5 . . ? N7 C44 H44B 108.5 . . ? H44A C44 H44B 107.5 . . ? C44 C45 C46 112.3(4) . . ? C44 C45 H45A 109.1 . . ? C46 C45 H45A 109.1 . . ? C44 C45 H45B 109.1 . . ? C46 C45 H45B 109.1 . . ? H45A C45 H45B 107.9 . . ? C47 C46 C45 110.7(4) . . ? C47 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N7 C48 C49 116.7(4) . . ? N7 C48 H48A 108.1 . . ? C49 C48 H48A 108.1 . . ? N7 C48 H48B 108.1 . . ? C49 C48 H48B 108.1 . . ? H48A C48 H48B 107.3 . . ? C48 C49 C50 108.3(5) . . ? C48 C49 H49A 110.0 . . ? C50 C49 H49A 110.0 . . ? C48 C49 H49B 110.0 . . ? C50 C49 H49B 110.0 . . ? H49A C49 H49B 108.4 . . ? C51 C50 C49 117.0(8) . . ? C51 C50 H50A 108.0 . . ? C49 C50 H50A 108.0 . . ? C51 C50 H50B 108.0 . . ? C49 C50 H50B 108.0 . . ? H50A C50 H50B 107.3 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.871 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.075 data_3 _database_code_depnum_ccdc_archive 'CCDC 913111' #TrackingRef 'ACPs-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H174 N14 O16 S2' _chemical_formula_weight 1916.67 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.889(4) _cell_length_b 16.427(2) _cell_length_c 24.753(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.540(2) _cell_angle_gamma 90.00 _cell_volume 11215(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4176 _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9725 _exptl_absorpt_correction_T_max 0.9889 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.196 -0.013 0.920 26 2 ' ' 2 0.804 -0.013 0.580 26 2 ' ' 3 0.500 0.135 0.250 157 37 ' ' 4 0.196 0.013 0.420 26 2 ' ' 5 0.804 0.013 0.080 26 2 ' ' 6 0.000 0.365 0.750 157 37 ' ' 7 0.304 0.487 0.580 26 2 ' ' 8 0.696 0.487 0.920 26 2 ' ' 9 0.304 0.513 0.080 26 2 ' ' 10 0.696 0.513 0.420 26 2 ' ' 11 0.000 0.635 0.250 157 37 ' ' 12 0.500 0.865 0.750 157 37 ' ' _platon_squeeze_details ; ; _diffrn_ambient_temperature 153(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43384 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.49 _reflns_number_total 12576 _reflns_number_gt 5466 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0000P)^2^+39.9903P] 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 12576 _refine_ls_number_parameters 594 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1931 _refine_ls_R_factor_gt 0.1040 _refine_ls_wR_factor_ref 0.1990 _refine_ls_wR_factor_gt 0.1741 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.034 _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 S1 S 0.17387(5) 0.69537(7) 0.19020(4) 0.0647(3) Uani 1 1 d . . . O1 O 0.40456(17) 0.3377(7) -0.0292(2) 0.344(7) Uani 1 1 d . . . O2 O 0.44947(15) 0.3827(3) 0.03722(19) 0.1266(16) Uani 1 1 d . . . O3 O 0.21732(11) 0.2231(2) 0.10383(11) 0.0737(9) Uani 1 1 d . . . O4 O 0.13570(12) 0.2391(2) 0.34266(11) 0.0799(10) Uani 1 1 d . . . O6 O 0.19527(11) 0.76121(18) 0.16165(11) 0.0749(9) Uani 1 1 d . . . O5 O 0.21334(11) 0.63588(17) 0.20945(11) 0.0678(8) Uani 1 1 d . . . O7 O 0.15502(10) 0.7275(2) 0.23831(10) 0.0761(9) Uani 1 1 d . . . O8 O 0.13515(13) 0.6555(2) 0.15366(13) 0.0927(11) Uani 1 1 d . . . N1 N 0.41394(17) 0.3476(4) 0.0187(2) 0.125(2) Uani 1 1 d . . . N2 N 0.29195(13) 0.2194(2) 0.15728(12) 0.0617(9) Uani 1 1 d . . . H2A H 0.3069 0.2068 0.1901 0.074 Uiso 1 1 calc R . . N3 N 0.22484(13) 0.1775(2) 0.19209(12) 0.0589(9) Uani 1 1 d . . . H3A H 0.2458 0.1689 0.2218 0.071 Uiso 1 1 calc R . . N4 N 0.19075(13) 0.1853(2) 0.29257(12) 0.0616(9) Uani 1 1 d . . . H4A H 0.2218 0.1752 0.2929 0.074 Uiso 1 1 calc R . . N5 N 0.21634(13) 0.2366(2) 0.37646(12) 0.0608(9) Uani 1 1 d . . . H5A H 0.2453 0.2274 0.3676 0.073 Uiso 1 1 calc R . . N6 N 0.1505(2) 0.4237(3) 0.2145(2) 0.1138(18) Uani 1 1 d . . . N7 N 0.09177(14) 0.8544(2) 0.04015(13) 0.0708(10) Uani 1 1 d . . . C1 C 0.38180(17) 0.3109(3) 0.05294(19) 0.0828(15) Uani 1 1 d . . . C2 C 0.39751(17) 0.3072(3) 0.10813(18) 0.0791(14) Uani 1 1 d . . . H2 H 0.4289 0.3257 0.1233 0.095 Uiso 1 1 calc R . . C3 C 0.36629(17) 0.2758(3) 0.14060(17) 0.0729(13) Uani 1 1 d . . . H3 H 0.3768 0.2722 0.1788 0.087 Uiso 1 1 calc R . . C4 C 0.32045(15) 0.2493(3) 0.12023(15) 0.0566(10) Uani 1 1 d . . . C5 C 0.30657(16) 0.2508(3) 0.06356(16) 0.0707(13) Uani 1 1 d . . . H5 H 0.2758 0.2301 0.0479 0.085 Uiso 1 1 calc R . . C6 C 0.33721(17) 0.2820(4) 0.03077(18) 0.0870(17) Uani 1 1 d . . . H6 H 0.3275 0.2838 -0.0077 0.104 Uiso 1 1 calc R . . C7 C 0.24266(17) 0.2075(3) 0.14764(15) 0.0598(11) Uani 1 1 d . . . C8 C 0.17573(16) 0.1589(2) 0.19470(15) 0.0566(10) Uani 1 1 d . . . C9 C 0.14364(16) 0.1371(3) 0.14889(16) 0.0646(12) Uani 1 1 d . . . H9 H 0.1549 0.1348 0.1145 0.078 Uiso 1 1 calc R . . C10 C 0.09617(18) 0.1189(3) 0.15163(17) 0.0752(13) Uani 1 1 d . . . H10 H 0.0747 0.1051 0.1195 0.090 Uiso 1 1 calc R . . C11 C 0.07983(19) 0.1210(3) 0.2020(2) 0.0838(15) Uani 1 1 d . . . H11 H 0.0470 0.1084 0.2046 0.101 Uiso 1 1 calc R . . C12 C 0.11113(18) 0.1412(3) 0.24763(18) 0.0779(14) Uani 1 1 d . . . H12 H 0.0999 0.1409 0.2820 0.094 Uiso 1 1 calc R . . C13 C 0.15841(17) 0.1619(3) 0.24534(16) 0.0606(11) Uani 1 1 d . . . C14 C 0.17749(18) 0.2223(3) 0.33757(16) 0.0636(12) Uani 1 1 d . . . C15 C 0.21410(16) 0.2650(3) 0.43006(14) 0.0586(11) Uani 1 1 d . . . C16 C 0.17979(16) 0.3188(3) 0.44134(16) 0.0666(12) Uani 1 1 d . . . H16 H 0.1554 0.3369 0.4130 0.080 Uiso 1 1 calc R . . C17 C 0.25024(14) 0.2348(2) 0.47275(13) 0.0529(10) Uani 1 1 d . . . C18 C 0.28607(15) 0.1779(2) 0.46347(14) 0.0562(11) Uani 1 1 d . . . H18 H 0.2865 0.1576 0.4276 0.067 Uiso 1 1 calc R . . C19 C 0.31955(16) 0.1521(3) 0.50436(15) 0.0653(12) Uani 1 1 d . . . H19 H 0.3432 0.1138 0.4970 0.078 Uiso 1 1 calc R . . C20 C 0.1980(3) 0.3840(4) 0.2380(3) 0.135(3) Uani 1 1 d . . . H20A H 0.2074 0.3457 0.2106 0.162 Uiso 1 1 calc R . . H20B H 0.1928 0.3516 0.2704 0.162 Uiso 1 1 calc R . . C21 C 0.2416(3) 0.4445(7) 0.2555(4) 0.186(4) Uani 1 1 d . . . H21A H 0.2336 0.4965 0.2361 0.223 Uiso 1 1 calc R . . H21B H 0.2428 0.4557 0.2950 0.223 Uiso 1 1 calc R . . C22 C 0.2893(5) 0.4220(8) 0.2469(5) 0.277(5) Uani 1 1 d D . . H22A H 0.3127 0.4461 0.2766 0.332 Uiso 1 1 calc R . . H22B H 0.2922 0.3621 0.2503 0.332 Uiso 1 1 calc R . . C23 C 0.3024(5) 0.4443(8) 0.1983(5) 0.277(5) Uani 1 1 d D . . H23A H 0.2805 0.4188 0.1684 0.416 Uiso 1 1 calc R . . H23B H 0.3358 0.4266 0.1968 0.416 Uiso 1 1 calc R . . H23C H 0.3004 0.5036 0.1945 0.416 Uiso 1 1 calc R . . C24 C 0.1541(3) 0.4624(4) 0.1596(3) 0.130(3) Uani 1 1 d . . . H24A H 0.1833 0.4974 0.1634 0.156 Uiso 1 1 calc R . . H24B H 0.1255 0.4979 0.1493 0.156 Uiso 1 1 calc R . . C25 C 0.1568(3) 0.4015(4) 0.1137(3) 0.161(3) Uani 1 1 d . . . H25A H 0.1257 0.3715 0.1056 0.193 Uiso 1 1 calc R . . H25B H 0.1830 0.3617 0.1249 0.193 Uiso 1 1 calc R . . C26 C 0.1668(4) 0.4480(6) 0.0625(4) 0.216(5) Uani 1 1 d D . . H26A H 0.1492 0.4211 0.0296 0.259 Uiso 1 1 calc R . . H26B H 0.1542 0.5042 0.0638 0.259 Uiso 1 1 calc R . . C27 C 0.2182(6) 0.4512(9) 0.0580(5) 0.53(2) Uani 1 1 d D . . H27A H 0.2367 0.4658 0.0935 0.791 Uiso 1 1 calc R . . H27B H 0.2237 0.4921 0.0308 0.791 Uiso 1 1 calc R . . H27C H 0.2289 0.3978 0.0467 0.791 Uiso 1 1 calc R . . C28 C 0.1378(2) 0.4923(3) 0.2503(3) 0.106(2) Uani 1 1 d . . . H28A H 0.1068 0.5169 0.2330 0.127 Uiso 1 1 calc R . . H28B H 0.1631 0.5347 0.2517 0.127 Uiso 1 1 calc R . . C29 C 0.1326(2) 0.4684(4) 0.3084(3) 0.114(2) Uani 1 1 d . . . H29A H 0.1634 0.4446 0.3267 0.137 Uiso 1 1 calc R . . H29B H 0.1068 0.4271 0.3080 0.137 Uiso 1 1 calc R . . C30 C 0.1200(2) 0.5436(4) 0.3393(3) 0.111(2) Uani 1 1 d . . . H30A H 0.1463 0.5841 0.3394 0.133 Uiso 1 1 calc R . . H30B H 0.0899 0.5679 0.3195 0.133 Uiso 1 1 calc R . . C31 C 0.1128(3) 0.5271(5) 0.3971(3) 0.158(3) Uani 1 1 d . . . H31A H 0.0823 0.4978 0.3973 0.238 Uiso 1 1 calc R . . H31B H 0.1118 0.5788 0.4166 0.238 Uiso 1 1 calc R . . H31C H 0.1398 0.4940 0.4151 0.238 Uiso 1 1 calc R . . C32 C 0.1119(3) 0.3582(4) 0.2102(3) 0.131(3) Uani 1 1 d . . . H32A H 0.1209 0.3143 0.1862 0.157 Uiso 1 1 calc R . . H32B H 0.1116 0.3344 0.2469 0.157 Uiso 1 1 calc R . . C34 C 0.0261(4) 0.3160(5) 0.1777(4) 0.184(4) Uani 1 1 d . . . H34A H 0.0367 0.2794 0.1500 0.220 Uiso 1 1 calc R . . H34B H 0.0263 0.2843 0.2117 0.220 Uiso 1 1 calc R . . C35 C -0.0233(3) 0.3429(6) 0.1584(5) 0.240(7) Uani 1 1 d . . . H35A H -0.0347 0.3771 0.1864 0.361 Uiso 1 1 calc R . . H35B H -0.0445 0.2954 0.1513 0.361 Uiso 1 1 calc R . . H35C H -0.0239 0.3743 0.1247 0.361 Uiso 1 1 calc R . . C36 C 0.14596(19) 0.8673(3) 0.0519(2) 0.0900(16) Uani 1 1 d . . . H36A H 0.1585 0.8388 0.0863 0.108 Uiso 1 1 calc R . . H36B H 0.1609 0.8415 0.0223 0.108 Uiso 1 1 calc R . . C37 C 0.1621(3) 0.9541(5) 0.0569(4) 0.178(4) Uani 1 1 d . . . H37A H 0.1486 0.9816 0.0869 0.214 Uiso 1 1 calc R . . H37B H 0.1516 0.9840 0.0225 0.214 Uiso 1 1 calc R . . C38 C 0.2188(3) 0.9499(6) 0.0696(5) 0.220(4) Uani 1 1 d D . . H38A H 0.2279 0.9086 0.0984 0.264 Uiso 1 1 calc R . . H38B H 0.2313 0.9308 0.0363 0.264 Uiso 1 1 calc R . . C39 C 0.2429(3) 1.0255(6) 0.0870(4) 0.220(4) Uani 1 1 d D . . H39A H 0.2306 1.0691 0.0616 0.331 Uiso 1 1 calc R . . H39B H 0.2779 1.0195 0.0874 0.331 Uiso 1 1 calc R . . H39C H 0.2365 1.0392 0.1238 0.331 Uiso 1 1 calc R . . C40 C 0.0694(3) 0.8932(4) -0.01324(19) 0.156(2) Uani 1 1 d . . . H40A H 0.0804 0.9505 -0.0134 0.187 Uiso 1 1 calc R . . H40B H 0.0338 0.8938 -0.0146 0.187 Uiso 1 1 calc R . . C44 C 0.08376(19) 0.7634(3) 0.03813(19) 0.0831(14) Uani 1 1 d . . . H44A H 0.1003 0.7410 0.0087 0.100 Uiso 1 1 calc R . . H44B H 0.0999 0.7400 0.0730 0.100 Uiso 1 1 calc R . . C45 C 0.0319(2) 0.7338(4) 0.0289(3) 0.126(2) Uani 1 1 d . . . H45A H 0.0161 0.7480 0.0609 0.152 Uiso 1 1 calc R . . H45B H 0.0140 0.7613 -0.0036 0.152 Uiso 1 1 calc R . . C46 C 0.0299(3) 0.6441(5) 0.0204(4) 0.194(4) Uani 1 1 d . . . H46A H 0.0472 0.6166 0.0533 0.233 Uiso 1 1 calc R . . H46B H 0.0466 0.6299 -0.0109 0.233 Uiso 1 1 calc R . . C47 C -0.0219(4) 0.6139(9) 0.0096(7) 0.378(12) Uani 1 1 d . . . H47A H -0.0243 0.5689 -0.0167 0.566 Uiso 1 1 calc R . . H47B H -0.0433 0.6584 -0.0054 0.566 Uiso 1 1 calc R . . H47C H -0.0317 0.5948 0.0438 0.566 Uiso 1 1 calc R . . C48 C 0.06690(16) 0.8941(3) 0.08346(16) 0.0736(13) Uani 1 1 d . . . H48A H 0.0717 0.9536 0.0816 0.088 Uiso 1 1 calc R . . H48B H 0.0317 0.8835 0.0747 0.088 Uiso 1 1 calc R . . C49 C 0.08346(17) 0.8670(4) 0.14058(17) 0.104(2) Uani 1 1 d . . . H49A H 0.1168 0.8870 0.1529 0.125 Uiso 1 1 calc R . . H49B H 0.0840 0.8067 0.1421 0.125 Uiso 1 1 calc R . . C50 C 0.04931(17) 0.8997(4) 0.17820(18) 0.0866(16) Uani 1 1 d . . . H50A H 0.0457 0.9592 0.1726 0.104 Uiso 1 1 calc R . . H50B H 0.0169 0.8748 0.1677 0.104 Uiso 1 1 calc R . . C51 C 0.0656(2) 0.8840(6) 0.2367(2) 0.178(4) Uani 1 1 d . . . H51A H 0.0643 0.8254 0.2438 0.267 Uiso 1 1 calc R . . H51B H 0.0445 0.9128 0.2586 0.267 Uiso 1 1 calc R . . H51C H 0.0990 0.9033 0.2467 0.267 Uiso 1 1 calc R . . C33 C 0.0621(3) 0.3865(4) 0.1886(3) 0.144(3) Uani 1 1 d . . . H33A H 0.0629 0.4170 0.1542 0.173 Uiso 1 1 calc R . . H33B H 0.0508 0.4243 0.2153 0.173 Uiso 1 1 calc R . . C43 C 0.0523(3) 0.8909(7) -0.1174(3) 0.197(5) Uani 1 1 d D . . H43A H 0.0499 0.8547 -0.1496 0.237 Uiso 1 1 calc R . . H43B H 0.0197 0.9095 -0.1117 0.237 Uiso 1 1 calc R . . C42 C 0.0878(5) 0.9618(5) -0.1204(4) 0.227(6) Uani 1 1 d D . . H42A H 0.0803 1.0058 -0.0962 0.340 Uiso 1 1 calc R . . H42B H 0.0846 0.9819 -0.1580 0.340 Uiso 1 1 calc R . . H42C H 0.1210 0.9428 -0.1087 0.340 Uiso 1 1 calc R . . C41 C 0.0813(3) 0.8515(4) -0.06513(19) 0.156(2) Uani 1 1 d D . . H41A H 0.0731 0.7930 -0.0641 0.187 Uiso 1 1 calc R . . H41B H 0.1165 0.8562 -0.0665 0.187 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 S1 0.0897(8) 0.0616(7) 0.0442(5) -0.0012(5) 0.0144(5) -0.0161(7) O1 0.102(4) 0.82(2) 0.098(3) 0.198(7) -0.032(3) -0.160(7) O2 0.072(3) 0.174(5) 0.137(4) 0.040(3) 0.028(3) -0.004(3) O3 0.077(2) 0.099(3) 0.0451(15) 0.0079(15) 0.0080(14) 0.0018(18) O4 0.086(2) 0.104(3) 0.0529(17) -0.0037(16) 0.0182(15) 0.024(2) O6 0.115(2) 0.0568(19) 0.0633(17) 0.0038(14) 0.0474(17) -0.0025(17) O5 0.085(2) 0.0537(19) 0.0651(17) -0.0001(14) 0.0129(15) -0.0135(16) O7 0.078(2) 0.108(3) 0.0443(15) 0.0083(15) 0.0177(14) -0.0016(18) O8 0.117(3) 0.071(2) 0.079(2) -0.0056(18) -0.0223(19) -0.022(2) N1 0.060(3) 0.220(7) 0.092(4) 0.077(4) 0.000(3) 0.002(4) N2 0.071(2) 0.074(3) 0.0400(17) -0.0021(16) 0.0084(16) 0.0028(19) N3 0.077(2) 0.061(2) 0.0408(17) -0.0061(15) 0.0133(16) 0.0054(19) N4 0.079(2) 0.064(2) 0.0439(17) 0.0036(16) 0.0157(16) 0.0119(19) N5 0.079(2) 0.066(2) 0.0403(17) 0.0029(16) 0.0190(17) 0.0165(19) N6 0.156(5) 0.050(3) 0.152(5) 0.020(3) 0.081(4) 0.009(3) N7 0.084(3) 0.080(3) 0.050(2) -0.0124(19) 0.0128(18) 0.004(2) C1 0.066(3) 0.114(4) 0.070(3) 0.037(3) 0.014(2) 0.013(3) C2 0.063(3) 0.108(4) 0.064(3) 0.006(3) 0.002(2) 0.001(3) C3 0.071(3) 0.096(4) 0.052(2) 0.000(2) 0.007(2) 0.005(3) C4 0.065(3) 0.057(3) 0.048(2) 0.0003(19) 0.0087(19) 0.009(2) C5 0.063(3) 0.096(4) 0.051(2) 0.015(2) 0.005(2) -0.002(3) C6 0.062(3) 0.141(5) 0.056(3) 0.036(3) 0.001(2) 0.004(3) C7 0.078(3) 0.058(3) 0.044(2) -0.0041(19) 0.013(2) 0.009(2) C8 0.075(3) 0.049(3) 0.047(2) 0.0029(19) 0.015(2) 0.009(2) C9 0.079(3) 0.070(3) 0.049(2) -0.007(2) 0.021(2) 0.001(3) C10 0.086(3) 0.087(4) 0.055(3) -0.005(2) 0.016(2) -0.005(3) C11 0.078(3) 0.102(4) 0.073(3) 0.002(3) 0.020(3) -0.010(3) C12 0.086(4) 0.096(4) 0.057(3) 0.002(3) 0.027(2) -0.005(3) C13 0.080(3) 0.052(3) 0.051(2) 0.0022(19) 0.013(2) 0.007(2) C14 0.084(3) 0.065(3) 0.044(2) 0.007(2) 0.020(2) 0.015(3) C15 0.082(3) 0.056(3) 0.041(2) 0.0066(18) 0.023(2) 0.013(2) C16 0.086(3) 0.069(3) 0.047(2) 0.007(2) 0.015(2) 0.021(3) C17 0.072(3) 0.049(2) 0.0425(19) 0.0058(18) 0.0254(19) 0.007(2) C18 0.080(3) 0.055(3) 0.0388(19) 0.0029(18) 0.0248(19) 0.011(2) C19 0.089(3) 0.060(3) 0.050(2) 0.004(2) 0.023(2) 0.026(2) C20 0.183(8) 0.089(5) 0.155(6) 0.044(4) 0.100(6) 0.069(5) C21 0.129(7) 0.211(11) 0.240(10) 0.086(8) 0.099(7) 0.035(7) C22 0.362(12) 0.240(10) 0.260(12) 0.097(8) 0.151(10) 0.185(9) C23 0.362(12) 0.240(10) 0.260(12) 0.097(8) 0.151(10) 0.185(9) C24 0.180(7) 0.074(4) 0.151(6) 0.025(4) 0.078(5) 0.022(4) C25 0.279(10) 0.085(5) 0.135(6) 0.024(4) 0.090(6) 0.043(6) C26 0.353(15) 0.153(8) 0.169(8) 0.086(7) 0.131(9) 0.063(9) C27 0.81(4) 0.44(2) 0.48(2) 0.37(2) 0.56(3) 0.47(3) C28 0.120(5) 0.050(3) 0.160(6) -0.003(3) 0.058(4) 0.001(3) C29 0.127(5) 0.069(4) 0.163(6) 0.003(4) 0.073(5) -0.001(4) C30 0.110(5) 0.078(4) 0.149(6) -0.015(4) 0.033(4) 0.009(3) C31 0.180(8) 0.139(7) 0.166(8) -0.047(6) 0.058(6) 0.024(6) C32 0.177(7) 0.064(4) 0.170(7) -0.013(4) 0.084(6) 0.002(5) C34 0.210(10) 0.099(6) 0.266(11) -0.051(6) 0.116(9) -0.056(7) C35 0.147(8) 0.181(10) 0.421(18) -0.144(11) 0.137(10) -0.066(8) C36 0.101(4) 0.094(4) 0.085(3) -0.033(3) 0.048(3) -0.008(3) C37 0.133(6) 0.168(8) 0.268(10) -0.139(7) 0.141(7) -0.071(5) C38 0.162(6) 0.196(8) 0.332(9) -0.140(7) 0.131(6) -0.049(5) C39 0.162(6) 0.196(8) 0.332(9) -0.140(7) 0.131(6) -0.049(5) C40 0.277(6) 0.151(5) 0.044(2) 0.021(2) 0.042(3) 0.095(4) C44 0.100(4) 0.079(4) 0.070(3) -0.012(3) 0.012(3) 0.008(3) C45 0.115(5) 0.116(6) 0.154(6) -0.043(5) 0.037(4) -0.031(4) C46 0.193(9) 0.131(8) 0.282(12) -0.079(7) 0.111(8) -0.071(7) C47 0.266(15) 0.35(2) 0.57(3) -0.203(19) 0.219(17) -0.208(15) C48 0.066(3) 0.098(4) 0.060(3) -0.016(2) 0.015(2) -0.002(3) C49 0.068(3) 0.193(7) 0.050(3) -0.021(3) 0.008(2) 0.027(4) C50 0.071(3) 0.127(5) 0.065(3) -0.015(3) 0.020(2) 0.005(3) C51 0.117(5) 0.362(13) 0.057(3) -0.013(5) 0.019(3) 0.068(7) C33 0.186(8) 0.072(5) 0.190(8) -0.042(5) 0.077(7) -0.030(5) C43 0.146(7) 0.349(16) 0.108(6) -0.052(8) 0.054(5) -0.027(8) C42 0.410(18) 0.145(8) 0.167(8) -0.027(6) 0.181(11) -0.008(9) C41 0.277(6) 0.151(5) 0.044(2) 0.021(2) 0.042(3) 0.095(4) _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 S1 O8 1.457(3) . ? S1 O6 1.466(3) . ? S1 O7 1.469(3) . ? S1 O5 1.496(3) . ? O1 N1 1.186(7) . ? O2 N1 1.179(6) . ? O3 C7 1.230(4) . ? O4 C14 1.222(5) . ? N1 C1 1.453(6) . ? N2 C7 1.374(5) . ? N2 C4 1.390(5) . ? N2 H2A 0.8800 . ? N3 C7 1.365(5) . ? N3 C8 1.414(5) . ? N3 H3A 0.8800 . ? N4 C14 1.367(5) . ? N4 C13 1.420(5) . ? N4 H4A 0.8800 . ? N5 C14 1.359(5) . ? N5 C15 1.417(4) . ? N5 H5A 0.8800 . ? N6 C28 1.510(7) . ? N6 C20 1.513(8) . ? N6 C32 1.514(8) . ? N6 C24 1.518(7) . ? N7 C48 1.509(5) . ? N7 C36 1.511(6) . ? N7 C44 1.512(6) . ? N7 C40 1.515(6) . ? C1 C6 1.367(6) . ? C1 C2 1.373(6) . ? C2 C3 1.370(6) . ? C2 H2 0.9500 . ? C3 C4 1.374(6) . ? C3 H3 0.9500 . ? C4 C5 1.399(5) . ? C5 C6 1.363(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.383(5) . ? C8 C13 1.410(5) . ? C9 C10 1.369(6) . ? C9 H9 0.9500 . ? C10 C11 1.390(6) . ? C10 H10 0.9500 . ? C11 C12 1.362(6) . ? C11 H11 0.9500 . ? C12 C13 1.371(6) . ? C12 H12 0.9500 . ? C15 C16 1.361(5) . ? C15 C17 1.437(5) . ? C16 C19 1.424(5) 7_556 ? C16 H16 0.9500 . ? C17 C18 1.411(5) . ? C17 C17 1.441(7) 7_556 ? C18 C19 1.340(5) . ? C18 H18 0.9500 . ? C19 C16 1.424(5) 7_556 ? C19 H19 0.9500 . ? C20 C21 1.581(11) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.425(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.361(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.524(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.540(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.455(12) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.517(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.521(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.499(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.488(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C34 C35 1.457(12) . ? C34 C33 1.531(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.494(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.569(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.447(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.534(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C44 C45 1.510(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.490(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.514(11) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.489(6) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.526(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.476(7) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C43 C42 1.536(8) . ? C43 C41 1.560(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? 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 O8 S1 O6 110.47(19) . . ? O8 S1 O7 110.1(2) . . ? O6 S1 O7 110.26(18) . . ? O8 S1 O5 110.26(19) . . ? O6 S1 O5 107.60(18) . . ? O7 S1 O5 108.13(17) . . ? O2 N1 O1 120.3(5) . . ? O2 N1 C1 122.1(5) . . ? O1 N1 C1 117.6(6) . . ? C7 N2 C4 126.2(3) . . ? C7 N2 H2A 116.9 . . ? C4 N2 H2A 116.9 . . ? C7 N3 C8 125.9(3) . . ? C7 N3 H3A 117.1 . . ? C8 N3 H3A 117.1 . . ? C14 N4 C13 125.1(4) . . ? C14 N4 H4A 117.4 . . ? C13 N4 H4A 117.4 . . ? C14 N5 C15 125.4(3) . . ? C14 N5 H5A 117.3 . . ? C15 N5 H5A 117.3 . . ? C28 N6 C20 111.4(5) . . ? C28 N6 C32 110.2(4) . . ? C20 N6 C32 107.1(5) . . ? C28 N6 C24 105.4(4) . . ? C20 N6 C24 110.8(5) . . ? C32 N6 C24 112.1(6) . . ? C48 N7 C36 110.8(3) . . ? C48 N7 C44 111.7(4) . . ? C36 N7 C44 106.5(4) . . ? C48 N7 C40 105.4(4) . . ? C36 N7 C40 112.3(5) . . ? C44 N7 C40 110.3(4) . . ? C6 C1 C2 121.4(4) . . ? C6 C1 N1 120.8(4) . . ? C2 C1 N1 117.8(5) . . ? C3 C2 C1 117.6(4) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C2 C3 C4 122.8(4) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C3 C4 N2 117.5(4) . . ? C3 C4 C5 117.8(4) . . ? N2 C4 C5 124.6(4) . . ? C6 C5 C4 119.9(4) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.3(4) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? O3 C7 N3 123.8(4) . . ? O3 C7 N2 123.5(4) . . ? N3 C7 N2 112.7(4) . . ? C9 C8 C13 118.2(4) . . ? C9 C8 N3 122.1(3) . . ? C13 C8 N3 119.7(4) . . ? C10 C9 C8 121.9(4) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 119.2(4) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 119.6(5) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 121.9(4) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C12 C13 C8 119.1(4) . . ? C12 C13 N4 122.1(4) . . ? C8 C13 N4 118.8(4) . . ? O4 C14 N5 124.1(4) . . ? O4 C14 N4 124.2(4) . . ? N5 C14 N4 111.7(4) . . ? C16 C15 N5 122.4(4) . . ? C16 C15 C17 120.8(3) . . ? N5 C15 C17 116.8(3) . . ? C15 C16 C19 120.0(4) . 7_556 ? C15 C16 H16 120.0 . . ? C19 C16 H16 120.0 7_556 . ? C18 C17 C15 123.1(3) . . ? C18 C17 C17 119.2(4) . 7_556 ? C15 C17 C17 117.7(4) . 7_556 ? C19 C18 C17 121.1(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C16 121.1(4) . 7_556 ? C18 C19 H19 119.4 . . ? C16 C19 H19 119.4 7_556 . ? N6 C20 C21 115.4(6) . . ? N6 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? N6 C20 H20B 108.4 . . ? C21 C20 H20B 108.4 . . ? H20A C20 H20B 107.5 . . ? C22 C21 C20 119.5(10) . . ? C22 C21 H21A 107.4 . . ? C20 C21 H21A 107.4 . . ? C22 C21 H21B 107.4 . . ? C20 C21 H21B 107.4 . . ? H21A C21 H21B 107.0 . . ? C23 C22 C21 116.2(11) . . ? C23 C22 H22A 108.2 . . ? C21 C22 H22A 108.2 . . ? C23 C22 H22B 108.2 . . ? C21 C22 H22B 108.2 . . ? H22A C22 H22B 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C24 C25 114.2(5) . . ? N6 C24 H24A 108.7 . . ? C25 C24 H24A 108.7 . . ? N6 C24 H24B 108.7 . . ? C25 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C24 C25 C26 108.8(7) . . ? C24 C25 H25A 109.9 . . ? C26 C25 H25A 109.9 . . ? C24 C25 H25B 109.9 . . ? C26 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? C27 C26 C25 112.6(8) . . ? C27 C26 H26A 109.1 . . ? C25 C26 H26A 109.1 . . ? C27 C26 H26B 109.1 . . ? C25 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N6 C28 C29 115.3(5) . . ? N6 C28 H28A 108.5 . . ? C29 C28 H28A 108.5 . . ? N6 C28 H28B 108.5 . . ? C29 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? C28 C29 C30 109.1(5) . . ? C28 C29 H29A 109.9 . . ? C30 C29 H29A 109.9 . . ? C28 C29 H29B 109.9 . . ? C30 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? C31 C30 C29 114.0(6) . . ? C31 C30 H30A 108.8 . . ? C29 C30 H30A 108.8 . . ? C31 C30 H30B 108.8 . . ? C29 C30 H30B 108.8 . . ? H30A C30 H30B 107.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 N6 114.7(6) . . ? C33 C32 H32A 108.6 . . ? N6 C32 H32A 108.6 . . ? C33 C32 H32B 108.6 . . ? N6 C32 H32B 108.6 . . ? H32A C32 H32B 107.6 . . ? C35 C34 C33 113.1(8) . . ? C35 C34 H34A 109.0 . . ? C33 C34 H34A 109.0 . . ? C35 C34 H34B 109.0 . . ? C33 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 N7 115.5(5) . . ? C37 C36 H36A 108.4 . . ? N7 C36 H36A 108.4 . . ? C37 C36 H36B 108.4 . . ? N7 C36 H36B 108.4 . . ? H36A C36 H36B 107.5 . . ? C36 C37 C38 104.8(7) . . ? C36 C37 H37A 110.8 . . ? C38 C37 H37A 110.8 . . ? C36 C37 H37B 110.8 . . ? C38 C37 H37B 110.8 . . ? H37A C37 H37B 108.9 . . ? C39 C38 C37 115.5(8) . . ? C39 C38 H38A 108.4 . . ? C37 C38 H38A 108.4 . . ? C39 C38 H38B 108.4 . . ? C37 C38 H38B 108.4 . . ? H38A C38 H38B 107.5 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N7 C40 C41 115.5(5) . . ? N7 C40 H40A 108.4 . . ? C41 C40 H40A 108.4 . . ? N7 C40 H40B 108.4 . . ? C41 C40 H40B 108.4 . . ? H40A C40 H40B 107.5 . . ? C45 C44 N7 117.1(5) . . ? C45 C44 H44A 108.0 . . ? N7 C44 H44A 108.0 . . ? C45 C44 H44B 108.0 . . ? N7 C44 H44B 108.0 . . ? H44A C44 H44B 107.3 . . ? C46 C45 C44 110.7(6) . . ? C46 C45 H45A 109.5 . . ? C44 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? C45 C46 C47 111.3(9) . . ? C45 C46 H46A 109.4 . . ? C47 C46 H46A 109.4 . . ? C45 C46 H46B 109.4 . . ? C47 C46 H46B 109.4 . . ? H46A C46 H46B 108.0 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 N7 115.8(4) . . ? C49 C48 H48A 108.3 . . ? N7 C48 H48A 108.3 . . ? C49 C48 H48B 108.3 . . ? N7 C48 H48B 108.3 . . ? H48A C48 H48B 107.4 . . ? C48 C49 C50 109.9(4) . . ? C48 C49 H49A 109.7 . . ? C50 C49 H49A 109.7 . . ? C48 C49 H49B 109.7 . . ? C50 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? C51 C50 C49 114.0(4) . . ? C51 C50 H50A 108.7 . . ? C49 C50 H50A 108.7 . . ? C51 C50 H50B 108.7 . . ? C49 C50 H50B 108.7 . . ? H50A C50 H50B 107.6 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C32 C33 C34 112.3(7) . . ? C32 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? C32 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.9 . . ? C42 C43 C41 95.5(6) . . ? C42 C43 H43A 112.6 . . ? C41 C43 H43A 112.6 . . ? C42 C43 H43B 112.6 . . ? C41 C43 H43B 112.6 . . ? H43A C43 H43B 110.1 . . ? C43 C42 H42A 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C43 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C41 C43 111.1(5) . . ? C40 C41 H41A 109.4 . . ? C43 C41 H41A 109.4 . . ? C40 C41 H41B 109.4 . . ? C43 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.706 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.054 data_4 _database_code_depnum_ccdc_archive 'CCDC 913112' #TrackingRef 'ACPs-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H108 N12 O12' _chemical_formula_weight 1357.72 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 12.430(5) _cell_length_b 14.615(6) _cell_length_c 21.187(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.784(6) _cell_angle_gamma 90.00 _cell_volume 3813(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9800 _exptl_absorpt_correction_T_max 0.9840 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24472 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6688 _reflns_number_gt 3494 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0100P)^2^+9.9960P] 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 6688 _refine_ls_number_parameters 455 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.1952 _refine_ls_wR_factor_gt 0.1650 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.7784(5) 0.4910(4) -0.0552(3) 0.135(2) Uani 1 1 d . . . O2 O 0.7451(4) 0.4113(4) -0.1410(3) 0.1157(18) Uani 1 1 d . . . O3 O 0.5867(3) 0.1885(2) 0.14642(16) 0.0629(10) Uani 1 1 d . . . O4 O 0.2104(2) 0.0067(2) 0.19981(15) 0.0523(9) Uani 1 1 d . . . O5 O 0.3903(3) 0.1189(2) 0.93076(17) 0.0750(12) Uani 1 1 d . . . O6 O 0.3755(2) 0.0435(2) 1.01983(14) 0.0477(8) Uani 1 1 d . . . N1 N 0.7486(4) 0.4218(5) -0.0834(3) 0.0866(17) Uani 1 1 d . . . N2 N 0.6193(3) 0.1215(3) 0.05351(17) 0.0431(10) Uani 1 1 d . . . H2 H 0.6146 0.0696 0.0323 0.052 Uiso 1 1 calc R . . N3 N 0.5817(3) 0.0345(2) 0.13721(17) 0.0397(9) Uani 1 1 d . . . H3 H 0.5887 -0.0127 0.1123 0.048 Uiso 1 1 calc R . . N4 N 0.3689(3) 0.0230(3) 0.15656(17) 0.0434(10) Uani 1 1 d . . . H4 H 0.3936 0.0339 0.1203 0.052 Uiso 1 1 calc R . . N5 N 0.2075(3) 0.0275(3) 0.09300(17) 0.0436(10) Uani 1 1 d . . . H5 H 0.2496 0.0321 0.0629 0.052 Uiso 1 1 calc R . . N6 N 0.9734(3) 0.8012(3) 0.19788(19) 0.0501(10) Uani 1 1 d . . . C1 C 0.7132(4) 0.3440(4) -0.0479(3) 0.0656(16) Uani 1 1 d . . . C2 C 0.7230(5) 0.3499(4) 0.0175(3) 0.0739(17) Uani 1 1 d . . . H2A H 0.7515 0.4039 0.0385 0.089 Uiso 1 1 calc R . . C3 C 0.6913(4) 0.2775(4) 0.0525(3) 0.0638(15) Uani 1 1 d . . . H3A H 0.6980 0.2815 0.0976 0.077 Uiso 1 1 calc R . . C4 C 0.6498(3) 0.1986(3) 0.0217(2) 0.0457(12) Uani 1 1 d . . . C5 C 0.6407(4) 0.1944(4) -0.0450(2) 0.0537(13) Uani 1 1 d . . . H5A H 0.6122 0.1410 -0.0667 0.064 Uiso 1 1 calc R . . C6 C 0.6726(4) 0.2665(4) -0.0790(3) 0.0629(15) Uani 1 1 d . . . H6 H 0.6667 0.2630 -0.1242 0.075 Uiso 1 1 calc R . . C7 C 0.5959(4) 0.1189(3) 0.1154(2) 0.0435(11) Uani 1 1 d . . . C8 C 0.5556(3) 0.0193(3) 0.2000(2) 0.0380(11) Uani 1 1 d . . . C9 C 0.6373(4) 0.0101(3) 0.2501(2) 0.0506(13) Uani 1 1 d . . . H9 H 0.7108 0.0156 0.2430 0.061 Uiso 1 1 calc R . . C10 C 0.6135(4) -0.0070(4) 0.3106(2) 0.0573(14) Uani 1 1 d . . . H10 H 0.6702 -0.0141 0.3451 0.069 Uiso 1 1 calc R . . C11 C 0.5070(4) -0.0137(3) 0.3206(2) 0.0517(13) Uani 1 1 d . . . H11 H 0.4905 -0.0254 0.3623 0.062 Uiso 1 1 calc R . . C12 C 0.4237(4) -0.0039(3) 0.2714(2) 0.0447(11) Uani 1 1 d . . . H12 H 0.3504 -0.0083 0.2792 0.054 Uiso 1 1 calc R . . C13 C 0.4475(3) 0.0126(3) 0.2097(2) 0.0368(10) Uani 1 1 d . . . C14 C 0.2576(4) 0.0182(3) 0.1535(2) 0.0414(11) Uani 1 1 d . . . C15 C 0.0949(3) 0.0305(3) 0.0734(2) 0.0364(10) Uani 1 1 d . . . C16 C 0.0244(3) 0.0648(3) 0.1115(2) 0.0377(11) Uani 1 1 d . . . H16 H 0.0511 0.0864 0.1530 0.045 Uiso 1 1 calc R . . C17 C -0.0867(3) 0.0681(3) 0.0899(2) 0.0421(11) Uani 1 1 d . . . H17 H -0.1352 0.0916 0.1169 0.050 Uiso 1 1 calc R . . C18 C -0.1262(3) 0.0378(3) 0.0303(2) 0.0395(11) Uani 1 1 d . . . H18 H -0.2020 0.0412 0.0162 0.047 Uiso 1 1 calc R . . C19 C 0.0569(3) -0.0016(3) 0.0106(2) 0.0339(10) Uani 1 1 d . . . C20 C 0.3743(4) 0.1165(4) 0.9875(2) 0.0502(13) Uani 1 1 d . . . C21 C 0.3538(4) 0.2066(4) 1.0195(3) 0.0678(16) Uani 1 1 d . . . H21A H 0.3648 0.2573 0.9908 0.102 Uiso 1 1 calc R . . H21B H 0.4043 0.2127 1.0590 0.102 Uiso 1 1 calc R . . H21C H 0.2790 0.2079 1.0293 0.102 Uiso 1 1 calc R . . C22 C 0.9718(4) 0.8959(3) 0.2269(2) 0.0491(12) Uani 1 1 d . . . H22A H 1.0368 0.9294 0.2171 0.059 Uiso 1 1 calc R . . H22B H 0.9073 0.9287 0.2055 0.059 Uiso 1 1 calc R . . C23 C 0.9697(5) 0.9004(3) 0.2975(3) 0.0643(15) Uani 1 1 d . . . H23A H 1.0326 0.8664 0.3197 0.077 Uiso 1 1 calc R . . H23B H 0.9027 0.8709 0.3080 0.077 Uiso 1 1 calc R . . C24 C 0.9738(5) 0.9978(4) 0.3207(3) 0.0665(15) Uani 1 1 d . . . H24A H 0.9120 1.0318 0.2972 0.080 Uiso 1 1 calc R . . H24B H 1.0415 1.0265 0.3105 0.080 Uiso 1 1 calc R . . C25 C 0.9694(6) 1.0073(5) 0.3913(3) 0.096(2) Uani 1 1 d . . . H25A H 0.9017 0.9805 0.4017 0.144 Uiso 1 1 calc R . . H25B H 0.9723 1.0722 0.4029 0.144 Uiso 1 1 calc R . . H25C H 1.0314 0.9753 0.4150 0.144 Uiso 1 1 calc R . . C26 C 0.8736(4) 0.7480(3) 0.2094(3) 0.0619(15) Uani 1 1 d . . . H26A H 0.8761 0.6872 0.1891 0.074 Uiso 1 1 calc R . . H26B H 0.8763 0.7381 0.2558 0.074 Uiso 1 1 calc R . . C27 C 0.7668(5) 0.7925(5) 0.1849(3) 0.0861(19) Uani 1 1 d U . . H27A H 0.7643 0.8066 0.1390 0.103 Uiso 1 1 calc R . . H27B H 0.7594 0.8506 0.2079 0.103 Uiso 1 1 calc R . . C28 C 0.6715(7) 0.7269(5) 0.1949(4) 0.108(2) Uani 1 1 d U . . C29 C 0.6509(10) 0.7286(9) 0.2591(5) 0.064(3) Uani 0.50 1 d P . . C29' C 0.5827(12) 0.7542(11) 0.2105(13) 0.154(9) Uani 0.50 1 d P . . C30 C 0.9801(4) 0.8137(3) 0.1279(2) 0.0528(13) Uani 1 1 d . . . H30A H 1.0487 0.8460 0.1234 0.063 Uiso 1 1 calc R . . H30B H 0.9196 0.8539 0.1097 0.063 Uiso 1 1 calc R . . C31 C 0.9756(5) 0.7267(3) 0.0886(2) 0.0631(15) Uani 1 1 d . . . H31A H 1.0310 0.6832 0.1086 0.076 Uiso 1 1 calc R . . H31B H 0.9034 0.6978 0.0878 0.076 Uiso 1 1 calc R . . C32 C 0.9958(5) 0.7470(4) 0.0214(2) 0.0677(16) Uani 1 1 d . . . H32A H 1.0699 0.7723 0.0223 0.081 Uiso 1 1 calc R . . H32B H 0.9435 0.7940 0.0028 0.081 Uiso 1 1 calc R . . C33 C 0.9844(5) 0.6621(4) -0.0205(3) 0.086(2) Uani 1 1 d . . . H33A H 1.0336 0.6143 -0.0012 0.129 Uiso 1 1 calc R . . H33B H 1.0028 0.6773 -0.0628 0.129 Uiso 1 1 calc R . . H33C H 0.9093 0.6399 -0.0245 0.129 Uiso 1 1 calc R . . C34 C 1.0707(4) 0.7474(3) 0.2300(3) 0.0613(15) Uani 1 1 d . . . H34A H 1.0636 0.7405 0.2757 0.074 Uiso 1 1 calc R . . H34B H 1.0689 0.6853 0.2111 0.074 Uiso 1 1 calc R . . C35 C 1.1794(5) 0.7901(4) 0.2244(3) 0.089(2) Uani 1 1 d . . . H35A H 1.1779 0.8551 0.2373 0.106 Uiso 1 1 calc R . . H35B H 1.1919 0.7882 0.1793 0.106 Uiso 1 1 calc R . . C36 C 1.2741(7) 0.7423(5) 0.2652(4) 0.112(3) Uani 1 1 d . . . H36A H 1.2651 0.6753 0.2605 0.134 Uiso 1 1 calc R . . H36B H 1.3428 0.7594 0.2495 0.134 Uiso 1 1 calc R . . C37 C 1.2812(8) 0.7649(5) 0.3291(4) 0.138(3) Uani 1 1 d . . . H37A H 1.2688 0.8307 0.3334 0.207 Uiso 1 1 calc R . . H37B H 1.3536 0.7491 0.3507 0.207 Uiso 1 1 calc R . . H37C H 1.2262 0.7308 0.3485 0.207 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 0.178(6) 0.087(4) 0.146(5) 0.020(4) 0.043(4) -0.049(4) O2 0.131(4) 0.129(4) 0.094(4) 0.047(4) 0.040(3) -0.006(3) O3 0.100(3) 0.046(2) 0.047(2) -0.0047(18) 0.026(2) -0.001(2) O4 0.0450(18) 0.073(2) 0.041(2) 0.0074(18) 0.0148(15) -0.0047(17) O5 0.132(4) 0.056(2) 0.041(2) -0.0027(18) 0.030(2) -0.001(2) O6 0.0419(18) 0.065(2) 0.0379(19) -0.0057(17) 0.0101(15) -0.0062(17) N1 0.081(4) 0.093(5) 0.092(5) 0.029(4) 0.035(4) 0.002(3) N2 0.044(2) 0.050(2) 0.038(2) -0.0069(19) 0.0143(18) -0.0047(19) N3 0.041(2) 0.041(2) 0.038(2) -0.0034(18) 0.0093(17) -0.0021(18) N4 0.033(2) 0.068(3) 0.031(2) -0.0020(19) 0.0089(17) -0.0047(19) N5 0.0297(19) 0.069(3) 0.033(2) -0.0023(19) 0.0091(17) -0.0073(19) N6 0.061(3) 0.037(2) 0.053(3) 0.008(2) 0.010(2) -0.002(2) C1 0.059(3) 0.067(4) 0.076(4) 0.021(3) 0.027(3) 0.000(3) C2 0.095(5) 0.059(4) 0.073(4) -0.003(3) 0.031(4) -0.011(3) C3 0.085(4) 0.057(3) 0.053(4) -0.001(3) 0.025(3) -0.012(3) C4 0.036(3) 0.057(3) 0.046(3) 0.002(3) 0.015(2) 0.003(2) C5 0.043(3) 0.073(4) 0.047(3) 0.003(3) 0.012(2) 0.001(3) C6 0.051(3) 0.087(4) 0.055(4) 0.014(3) 0.020(3) 0.005(3) C7 0.041(3) 0.054(3) 0.036(3) -0.005(2) 0.009(2) -0.001(2) C8 0.039(3) 0.034(2) 0.040(3) -0.005(2) 0.004(2) -0.002(2) C9 0.044(3) 0.055(3) 0.051(3) -0.002(3) -0.001(2) -0.001(2) C10 0.065(4) 0.064(3) 0.040(3) 0.003(3) -0.004(3) 0.000(3) C11 0.072(4) 0.046(3) 0.036(3) 0.007(2) 0.005(3) -0.001(3) C12 0.050(3) 0.044(3) 0.040(3) 0.000(2) 0.009(2) -0.004(2) C13 0.046(3) 0.034(2) 0.031(3) -0.005(2) 0.006(2) 0.000(2) C14 0.042(3) 0.045(3) 0.039(3) -0.002(2) 0.011(2) -0.003(2) C15 0.032(2) 0.039(3) 0.039(3) 0.000(2) 0.009(2) -0.006(2) C16 0.039(3) 0.042(3) 0.034(3) -0.005(2) 0.010(2) -0.005(2) C17 0.039(3) 0.046(3) 0.045(3) -0.007(2) 0.018(2) 0.001(2) C18 0.032(2) 0.046(3) 0.042(3) -0.002(2) 0.009(2) -0.001(2) C19 0.035(2) 0.032(2) 0.036(3) 0.000(2) 0.0070(19) -0.003(2) C20 0.041(3) 0.064(4) 0.046(3) -0.008(3) 0.007(2) -0.005(3) C21 0.073(4) 0.072(4) 0.061(4) -0.021(3) 0.016(3) 0.010(3) C22 0.053(3) 0.040(3) 0.055(3) 0.004(2) 0.013(2) -0.001(2) C23 0.087(4) 0.051(3) 0.058(4) -0.003(3) 0.018(3) -0.009(3) C24 0.071(4) 0.061(4) 0.066(4) -0.011(3) 0.005(3) 0.001(3) C25 0.113(5) 0.091(5) 0.086(5) -0.029(4) 0.023(4) -0.024(4) C26 0.081(4) 0.051(3) 0.056(3) 0.003(3) 0.018(3) -0.022(3) C27 0.085(2) 0.086(2) 0.088(2) -0.0002(10) 0.0125(10) -0.0019(10) C28 0.107(2) 0.107(2) 0.108(2) -0.0002(7) 0.0152(8) -0.0016(7) C29 0.064(8) 0.081(9) 0.045(7) 0.009(6) 0.001(6) -0.036(7) C29' 0.075(11) 0.076(10) 0.32(3) -0.069(15) 0.067(15) -0.008(9) C30 0.069(3) 0.046(3) 0.045(3) 0.012(2) 0.014(3) -0.001(3) C31 0.085(4) 0.052(3) 0.054(4) 0.009(3) 0.015(3) -0.001(3) C32 0.090(4) 0.064(4) 0.051(4) 0.004(3) 0.015(3) -0.004(3) C33 0.115(5) 0.081(4) 0.063(4) -0.012(3) 0.015(4) -0.010(4) C34 0.082(4) 0.039(3) 0.061(4) 0.010(3) 0.002(3) 0.009(3) C35 0.071(4) 0.069(4) 0.123(6) 0.012(4) 0.004(4) 0.023(4) C36 0.140(7) 0.084(5) 0.103(6) -0.011(5) -0.010(5) 0.048(5) C37 0.194(9) 0.097(6) 0.116(7) 0.017(6) -0.001(7) 0.049(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 N1 1.207(7) . ? O2 N1 1.223(7) . ? O3 C7 1.225(5) . ? O4 C14 1.221(5) . ? O5 C20 1.245(6) . ? O6 C20 1.266(6) . ? N1 C1 1.464(7) . ? N2 C7 1.381(5) . ? N2 C4 1.390(6) . ? N3 C7 1.338(6) . ? N3 C8 1.430(5) . ? N4 C14 1.378(5) . ? N4 C13 1.396(5) . ? N5 C14 1.354(5) . ? N5 C15 1.406(5) . ? N6 C30 1.508(6) . ? N6 C26 1.512(6) . ? N6 C22 1.515(6) . ? N6 C34 1.524(6) . ? C1 C6 1.373(8) . ? C1 C2 1.376(8) . ? C2 C3 1.380(7) . ? C3 C4 1.389(7) . ? C4 C5 1.404(6) . ? C5 C6 1.365(7) . ? C8 C9 1.372(6) . ? C8 C13 1.390(6) . ? C9 C10 1.377(6) . ? C10 C11 1.372(7) . ? C11 C12 1.373(6) . ? C12 C13 1.399(6) . ? C15 C16 1.365(5) . ? C15 C19 1.429(6) . ? C16 C17 1.396(6) . ? C17 C18 1.365(6) . ? C18 C19 1.405(5) 3 ? C19 C18 1.405(5) 3 ? C19 C19 1.425(8) 3 ? C20 C21 1.519(7) . ? C22 C23 1.502(6) . ? C23 C24 1.503(7) . ? C24 C25 1.510(7) . ? C26 C27 1.505(7) . ? C27 C28 1.561(9) . ? C28 C29' 1.259(15) . ? C28 C29 1.419(13) . ? C30 C31 1.516(7) . ? C31 C32 1.509(7) . ? C32 C33 1.522(7) . ? C34 C35 1.508(7) . ? C35 C36 1.531(8) . ? C36 C37 1.385(9) . ? 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 N1 O2 124.5(7) . . ? O1 N1 C1 119.2(7) . . ? O2 N1 C1 116.3(7) . . ? C7 N2 C4 126.1(4) . . ? C7 N3 C8 121.5(4) . . ? C14 N4 C13 128.4(4) . . ? C14 N5 C15 126.5(4) . . ? C30 N6 C26 112.1(4) . . ? C30 N6 C22 107.1(3) . . ? C26 N6 C22 110.4(4) . . ? C30 N6 C34 110.9(4) . . ? C26 N6 C34 106.4(4) . . ? C22 N6 C34 110.1(4) . . ? C6 C1 C2 120.8(5) . . ? C6 C1 N1 120.6(6) . . ? C2 C1 N1 118.5(6) . . ? C1 C2 C3 120.0(6) . . ? C2 C3 C4 120.0(5) . . ? C3 C4 N2 123.5(5) . . ? C3 C4 C5 118.8(5) . . ? N2 C4 C5 117.6(5) . . ? C6 C5 C4 120.6(5) . . ? C5 C6 C1 119.8(5) . . ? O3 C7 N3 123.6(4) . . ? O3 C7 N2 122.2(5) . . ? N3 C7 N2 114.1(4) . . ? C9 C8 C13 120.5(4) . . ? C9 C8 N3 119.9(4) . . ? C13 C8 N3 119.6(4) . . ? C8 C9 C10 120.5(5) . . ? C11 C10 C9 119.3(5) . . ? C10 C11 C12 121.4(5) . . ? C11 C12 C13 119.5(4) . . ? C8 C13 N4 117.3(4) . . ? C8 C13 C12 118.8(4) . . ? N4 C13 C12 123.9(4) . . ? O4 C14 N5 124.4(4) . . ? O4 C14 N4 123.9(4) . . ? N5 C14 N4 111.7(4) . . ? C16 C15 N5 122.0(4) . . ? C16 C15 C19 120.9(4) . . ? N5 C15 C19 117.1(4) . . ? C15 C16 C17 120.3(4) . . ? C18 C17 C16 120.6(4) . . ? C17 C18 C19 121.2(4) . 3 ? C18 C19 C19 118.9(5) 3 3 ? C18 C19 C15 123.0(4) 3 . ? C19 C19 C15 118.1(5) 3 . ? O5 C20 O6 123.7(5) . . ? O5 C20 C21 117.7(5) . . ? O6 C20 C21 118.6(5) . . ? C23 C22 N6 116.6(4) . . ? C22 C23 C24 111.3(4) . . ? C23 C24 C25 114.0(5) . . ? C27 C26 N6 115.3(4) . . ? C26 C27 C28 109.7(5) . . ? C29' C28 C29 57.6(12) . . ? C29' C28 C27 123.3(10) . . ? C29 C28 C27 111.0(7) . . ? N6 C30 C31 115.8(4) . . ? C32 C31 C30 110.8(4) . . ? C31 C32 C33 112.1(5) . . ? C35 C34 N6 114.6(4) . . ? C34 C35 C36 113.3(6) . . ? C37 C36 C35 112.7(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.526 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.064 data_5 _database_code_depnum_ccdc_archive 'CCDC 913113' #TrackingRef 'ACPs-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H112 N12 O12' _chemical_formula_weight 1481.86 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 ' 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 8.627(3) _cell_length_b 35.844(11) _cell_length_c 13.660(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.017(4) _cell_angle_gamma 90.00 _cell_volume 4131(2) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9763 _exptl_absorpt_correction_T_max 0.9920 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16438 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0880 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7103 _reflns_number_gt 4566 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0750P)^2^+6.5098P] 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 7103 _refine_ls_number_parameters 491 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1293 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.2225 _refine_ls_wR_factor_gt 0.1944 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.064 _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 -0.0805(5) 0.35672(11) 0.2695(3) 0.0758(12) Uani 1 1 d . . . O2 O 0.0029(6) 0.35861(10) 0.1313(3) 0.0809(13) Uani 1 1 d . . . O3 O 0.2856(3) 0.19186(8) 0.4600(2) 0.0392(7) Uani 1 1 d . . . O4 O 0.2688(3) 0.01512(7) 0.3336(2) 0.0349(7) Uani 1 1 d . . . O5 O 0.4384(3) 0.16418(8) 1.1635(2) 0.0410(7) Uani 1 1 d . . . O6 O 0.2957(4) 0.11301(8) 1.1240(2) 0.0466(8) Uani 1 1 d . . . N1 N -0.0062(6) 0.34357(11) 0.2104(3) 0.0566(12) Uani 1 1 d . . . N2 N 0.2964(4) 0.20514(9) 0.2965(2) 0.0321(8) Uani 1 1 d . . . H2 H 0.3342 0.1964 0.2460 0.039 Uiso 1 1 calc R . . N3 N 0.3735(4) 0.14842(8) 0.3605(2) 0.0292(8) Uani 1 1 d . . . H3 H 0.3713 0.1429 0.2974 0.035 Uiso 1 1 calc R . . N4 N 0.3542(3) 0.07370(8) 0.3050(2) 0.0255(7) Uani 1 1 d . . . H4 H 0.3533 0.0907 0.2583 0.031 Uiso 1 1 calc R . . N5 N 0.2219(4) 0.03883(8) 0.1745(2) 0.0276(7) Uani 1 1 d . . . H5 H 0.2326 0.0589 0.1396 0.033 Uiso 1 1 calc R . . N6 N 0.8605(4) 0.39321(9) 0.7900(2) 0.0303(8) Uani 1 1 d . . . C1 C 0.0762(5) 0.30783(11) 0.2352(3) 0.0390(11) Uani 1 1 d . . . C2 C 0.1565(5) 0.29198(12) 0.1677(3) 0.0402(11) Uani 1 1 d . . . H2A H 0.1599 0.3041 0.1063 0.048 Uiso 1 1 calc R . . C3 C 0.2310(5) 0.25843(11) 0.1916(3) 0.0373(10) Uani 1 1 d . . . H3A H 0.2876 0.2473 0.1465 0.045 Uiso 1 1 calc R . . C4 C 0.2246(5) 0.24028(11) 0.2823(3) 0.0315(9) Uani 1 1 d . . . C5 C 0.1465(5) 0.25746(11) 0.3487(3) 0.0357(10) Uani 1 1 d . . . H5A H 0.1446 0.2460 0.4111 0.043 Uiso 1 1 calc R . . C6 C 0.0712(5) 0.29130(12) 0.3247(3) 0.0424(11) Uani 1 1 d . . . H6 H 0.0165 0.3030 0.3701 0.051 Uiso 1 1 calc R . . C7 C 0.3153(4) 0.18264(11) 0.3798(3) 0.0284(9) Uani 1 1 d . . . C8 C 0.4368(4) 0.12100(10) 0.4328(3) 0.0268(9) Uani 1 1 d . . . C9 C 0.5127(5) 0.13032(12) 0.5295(3) 0.0355(10) Uani 1 1 d . . . H9 H 0.5158 0.1557 0.5501 0.043 Uiso 1 1 calc R . . C10 C 0.5838(5) 0.10338(12) 0.5964(3) 0.0403(11) Uani 1 1 d . . . H10 H 0.6353 0.1102 0.6624 0.048 Uiso 1 1 calc R . . C11 C 0.5798(5) 0.06632(12) 0.5670(3) 0.0368(10) Uani 1 1 d . . . H11 H 0.6295 0.0477 0.6124 0.044 Uiso 1 1 calc R . . C12 C 0.5033(4) 0.05660(11) 0.4714(3) 0.0308(9) Uani 1 1 d . . . H12 H 0.5009 0.0312 0.4517 0.037 Uiso 1 1 calc R . . C13 C 0.4296(4) 0.08323(11) 0.4034(3) 0.0253(8) Uani 1 1 d . . . C14 C 0.2821(4) 0.04027(10) 0.2756(3) 0.0258(8) Uani 1 1 d . . . C15 C 0.1437(4) 0.00787(10) 0.1210(3) 0.0257(8) Uani 1 1 d . . . C16 C 0.0391(4) 0.01547(10) 0.0286(3) 0.0222(8) Uani 1 1 d . . . C17 C 0.0066(5) 0.05201(11) -0.0102(3) 0.0303(9) Uani 1 1 d . . . H17 H 0.0580 0.0727 0.0261 0.036 Uiso 1 1 calc R . . C18 C -0.0962(5) 0.05776(11) -0.0979(3) 0.0355(10) Uani 1 1 d . . . H18 H -0.1164 0.0826 -0.1217 0.043 Uiso 1 1 calc R . . C19 C 0.1736(5) -0.02819(11) 0.1548(3) 0.0345(10) Uani 1 1 d . . . H19 H 0.2461 -0.0329 0.2161 0.041 Uiso 1 1 calc R . . C20 C 0.3731(5) 0.14018(11) 1.1012(3) 0.0288(9) Uani 1 1 d . . . C21 C 0.3917(5) 0.14398(11) 0.9944(3) 0.0319(9) Uani 1 1 d . . . C22 C 0.3397(6) 0.11651(13) 0.9254(3) 0.0485(12) Uani 1 1 d . . . H22 H 0.2884 0.0951 0.9446 0.058 Uiso 1 1 calc R . . C23 C 0.3611(7) 0.11964(16) 0.8282(4) 0.0640(15) Uani 1 1 d . . . H23 H 0.3245 0.1005 0.7811 0.077 Uiso 1 1 calc R . . C24 C 0.4344(7) 0.15018(18) 0.8002(4) 0.0664(16) Uani 1 1 d . . . H24 H 0.4498 0.1521 0.7336 0.080 Uiso 1 1 calc R . . C25 C 0.4863(6) 0.17826(17) 0.8667(4) 0.0606(15) Uani 1 1 d . . . H25 H 0.5367 0.1996 0.8463 0.073 Uiso 1 1 calc R . . C26 C 0.4649(5) 0.17527(13) 0.9642(3) 0.0420(11) Uani 1 1 d . . . H26 H 0.5004 0.1947 1.0107 0.050 Uiso 1 1 calc R . . C27 C 0.9323(5) 0.38009(12) 0.7028(3) 0.0339(10) Uani 1 1 d . . . H27A H 0.9924 0.4011 0.6818 0.041 Uiso 1 1 calc R . . H27B H 1.0090 0.3599 0.7272 0.041 Uiso 1 1 calc R . . C28 C 0.8163(5) 0.36599(13) 0.6121(3) 0.0393(10) Uani 1 1 d . . . H28A H 0.7583 0.3874 0.5759 0.047 Uiso 1 1 calc R . . H28B H 0.7381 0.3494 0.6339 0.047 Uiso 1 1 calc R . . C29 C 0.9008(5) 0.34453(12) 0.5415(4) 0.0429(11) Uani 1 1 d U . . H29A H 0.8286 0.3422 0.4753 0.052 Uiso 1 1 calc R . . H29B H 0.9948 0.3589 0.5325 0.052 Uiso 1 1 calc R . . C30 C 0.9525(8) 0.30626(17) 0.5800(5) 0.0808(18) Uani 1 1 d U . . H30A H 1.0172 0.3082 0.6478 0.121 Uiso 1 1 calc R . . H30B H 1.0151 0.2947 0.5360 0.121 Uiso 1 1 calc R . . H30C H 0.8590 0.2909 0.5812 0.121 Uiso 1 1 calc R . . C31 C 0.7865(5) 0.36093(12) 0.8351(3) 0.0377(10) Uani 1 1 d . . . H31A H 0.7345 0.3709 0.8878 0.045 Uiso 1 1 calc R . . H31B H 0.7026 0.3500 0.7824 0.045 Uiso 1 1 calc R . . C32 C 0.8980(6) 0.33013(13) 0.8802(4) 0.0496(12) Uani 1 1 d . . . H32A H 0.9821 0.3405 0.9338 0.060 Uiso 1 1 calc R . . H32B H 0.9494 0.3194 0.8281 0.060 Uiso 1 1 calc R . . C33 C 0.8100(8) 0.29942(18) 0.9234(6) 0.093(2) Uani 1 1 d U . . H33A H 0.8874 0.2838 0.9694 0.111 Uiso 1 1 calc R . . H33B H 0.7379 0.3109 0.9626 0.111 Uiso 1 1 calc R . . C34 C 0.7184(11) 0.2759(3) 0.8451(7) 0.126(3) Uani 1 1 d U . . H34A H 0.6400 0.2912 0.8003 0.189 Uiso 1 1 calc R . . H34B H 0.6640 0.2565 0.8756 0.189 Uiso 1 1 calc R . . H34C H 0.7897 0.2643 0.8068 0.189 Uiso 1 1 calc R . . C35 C 0.9936(5) 0.41077(12) 0.8667(3) 0.0352(10) Uani 1 1 d . . . H35A H 1.0773 0.3918 0.8872 0.042 Uiso 1 1 calc R . . H35B H 1.0401 0.4313 0.8336 0.042 Uiso 1 1 calc R . . C36 C 0.9485(5) 0.42626(12) 0.9603(3) 0.0362(10) Uani 1 1 d . . . H36A H 0.8968 0.4066 0.9930 0.043 Uiso 1 1 calc R . . H36B H 0.8726 0.4471 0.9422 0.043 Uiso 1 1 calc R . . C37 C 1.0969(5) 0.44012(14) 1.0322(3) 0.0451(11) Uani 1 1 d . . . H37A H 1.1712 0.4190 1.0507 0.054 Uiso 1 1 calc R . . H37B H 1.1500 0.4591 0.9979 0.054 Uiso 1 1 calc R . . C38 C 1.0605(6) 0.45693(15) 1.1261(4) 0.0594(14) Uani 1 1 d . . . H38A H 0.9891 0.4783 1.1084 0.089 Uiso 1 1 calc R . . H38B H 1.1592 0.4653 1.1699 0.089 Uiso 1 1 calc R . . H38C H 1.0096 0.4382 1.1610 0.089 Uiso 1 1 calc R . . C39 C 0.7293(4) 0.42108(11) 0.7540(3) 0.0327(9) Uani 1 1 d . . . H39A H 0.6872 0.4292 0.8127 0.039 Uiso 1 1 calc R . . H39B H 0.6425 0.4080 0.7081 0.039 Uiso 1 1 calc R . . C40 C 0.7709(5) 0.45558(12) 0.7011(3) 0.0390(10) Uani 1 1 d . . . H40A H 0.8073 0.4483 0.6397 0.047 Uiso 1 1 calc R . . H40B H 0.8581 0.4692 0.7453 0.047 Uiso 1 1 calc R . . C41 C 0.6257(6) 0.48097(13) 0.6734(4) 0.0474(12) Uani 1 1 d . . . H41A H 0.5360 0.4662 0.6355 0.057 Uiso 1 1 calc R . . H41B H 0.5957 0.4897 0.7358 0.057 Uiso 1 1 calc R . . C42 C 0.6504(6) 0.51431(14) 0.6123(4) 0.0552(13) Uani 1 1 d . . . H42A H 0.7453 0.5278 0.6461 0.083 Uiso 1 1 calc R . . H42B H 0.5581 0.5308 0.6046 0.083 Uiso 1 1 calc R . . H42C H 0.6641 0.5061 0.5462 0.083 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 0.108(3) 0.069(3) 0.055(2) 0.003(2) 0.027(2) 0.048(2) O2 0.133(4) 0.061(2) 0.051(2) 0.022(2) 0.026(2) 0.044(2) O3 0.0483(18) 0.0412(17) 0.0309(17) 0.0017(13) 0.0147(14) 0.0090(14) O4 0.0479(17) 0.0289(15) 0.0264(15) 0.0023(12) 0.0044(13) -0.0041(13) O5 0.0391(17) 0.0508(18) 0.0356(17) -0.0128(15) 0.0134(14) -0.0079(14) O6 0.063(2) 0.0431(18) 0.0335(18) 0.0103(14) 0.0090(15) -0.0128(16) N1 0.081(3) 0.045(2) 0.041(3) 0.004(2) 0.006(2) 0.023(2) N2 0.0407(19) 0.0328(18) 0.0244(19) 0.0006(15) 0.0100(15) 0.0084(16) N3 0.0367(19) 0.0280(17) 0.0206(17) 0.0005(14) 0.0006(14) 0.0049(15) N4 0.0250(16) 0.0289(17) 0.0207(17) 0.0000(14) 0.0004(13) -0.0027(14) N5 0.0324(17) 0.0249(17) 0.0240(18) 0.0027(14) 0.0021(14) -0.0036(14) N6 0.0224(16) 0.0375(19) 0.0322(19) -0.0009(15) 0.0083(14) -0.0009(15) C1 0.054(3) 0.030(2) 0.033(3) 0.0021(19) 0.010(2) 0.011(2) C2 0.057(3) 0.039(2) 0.025(2) 0.0048(19) 0.008(2) 0.007(2) C3 0.047(3) 0.036(2) 0.031(2) 0.0014(19) 0.014(2) 0.002(2) C4 0.032(2) 0.031(2) 0.032(2) 0.0006(18) 0.0082(18) 0.0044(18) C5 0.046(3) 0.037(2) 0.027(2) 0.0028(18) 0.0128(19) 0.005(2) C6 0.051(3) 0.041(3) 0.038(3) 0.000(2) 0.015(2) 0.013(2) C7 0.030(2) 0.033(2) 0.021(2) -0.0013(17) 0.0038(17) 0.0001(17) C8 0.026(2) 0.030(2) 0.024(2) -0.0034(17) 0.0039(16) -0.0011(17) C9 0.038(2) 0.037(2) 0.030(2) -0.0038(19) 0.0033(19) 0.0025(19) C10 0.043(3) 0.048(3) 0.026(2) -0.002(2) -0.0032(19) 0.004(2) C11 0.036(2) 0.043(3) 0.028(2) 0.0068(19) -0.0002(18) 0.004(2) C12 0.029(2) 0.032(2) 0.031(2) 0.0027(18) 0.0057(17) 0.0016(17) C13 0.0172(18) 0.036(2) 0.024(2) 0.0001(17) 0.0063(15) -0.0036(16) C14 0.0238(19) 0.025(2) 0.029(2) 0.0002(17) 0.0065(16) 0.0029(16) C15 0.026(2) 0.031(2) 0.021(2) -0.0022(16) 0.0061(16) -0.0016(17) C16 0.0213(18) 0.0246(19) 0.022(2) 0.0013(16) 0.0070(15) -0.0004(15) C17 0.036(2) 0.028(2) 0.026(2) -0.0019(17) 0.0055(18) -0.0021(18) C18 0.047(3) 0.026(2) 0.029(2) 0.0033(17) -0.0023(19) 0.0001(19) C19 0.041(2) 0.033(2) 0.023(2) 0.0015(18) -0.0052(18) 0.0060(19) C20 0.028(2) 0.034(2) 0.023(2) 0.0026(18) 0.0019(17) 0.0026(18) C21 0.029(2) 0.038(2) 0.028(2) 0.0052(18) 0.0038(17) 0.0035(18) C22 0.065(3) 0.046(3) 0.033(3) -0.001(2) 0.008(2) -0.004(2) C23 0.096(4) 0.064(4) 0.033(3) -0.005(3) 0.017(3) 0.004(3) C24 0.078(4) 0.089(4) 0.039(3) 0.009(3) 0.026(3) 0.014(3) C25 0.060(3) 0.074(4) 0.053(3) 0.024(3) 0.024(3) 0.000(3) C26 0.041(3) 0.045(3) 0.040(3) 0.008(2) 0.011(2) 0.000(2) C27 0.026(2) 0.043(2) 0.033(2) -0.0056(19) 0.0078(17) 0.0015(18) C28 0.033(2) 0.045(3) 0.039(3) -0.005(2) 0.0065(19) -0.001(2) C29 0.0442(18) 0.0431(18) 0.0415(18) -0.0031(15) 0.0089(15) 0.0015(15) C30 0.083(2) 0.080(2) 0.079(2) -0.0011(10) 0.0162(10) 0.0030(10) C31 0.029(2) 0.044(2) 0.042(3) 0.005(2) 0.0110(19) -0.0030(19) C32 0.050(3) 0.048(3) 0.052(3) 0.015(2) 0.013(2) 0.011(2) C33 0.092(5) 0.072(4) 0.121(6) 0.033(4) 0.039(5) 0.022(4) C34 0.125(3) 0.124(3) 0.127(3) 0.0011(10) 0.0251(12) -0.0001(10) C35 0.025(2) 0.049(3) 0.032(2) -0.004(2) 0.0074(18) -0.0011(19) C36 0.032(2) 0.045(3) 0.031(2) 0.0007(19) 0.0061(18) 0.0088(19) C37 0.038(2) 0.059(3) 0.035(3) -0.010(2) 0.002(2) 0.006(2) C38 0.063(3) 0.069(4) 0.042(3) -0.015(3) 0.003(2) 0.009(3) C39 0.025(2) 0.041(2) 0.033(2) -0.0013(19) 0.0067(17) 0.0038(18) C40 0.040(2) 0.041(2) 0.039(3) 0.000(2) 0.015(2) -0.002(2) C41 0.044(3) 0.046(3) 0.052(3) 0.009(2) 0.010(2) 0.003(2) C42 0.051(3) 0.055(3) 0.058(3) 0.012(3) 0.008(3) -0.004(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 N1 1.224(5) . ? O2 N1 1.225(5) . ? O3 C7 1.223(5) . ? O4 C14 1.221(4) . ? O5 C20 1.258(5) . ? O6 C20 1.256(5) . ? N1 C1 1.470(5) . ? N2 C7 1.375(5) . ? N2 C4 1.400(5) . ? N2 H2 0.8800 . ? N3 C7 1.371(5) . ? N3 C8 1.420(5) . ? N3 H3 0.8800 . ? N4 C14 1.371(5) . ? N4 C13 1.409(5) . ? N4 H4 0.8800 . ? N5 C14 1.372(5) . ? N5 C15 1.419(5) . ? N5 H5 0.8800 . ? N6 C39 1.512(5) . ? N6 C31 1.513(5) . ? N6 C35 1.521(5) . ? N6 C27 1.526(5) . ? C1 C6 1.368(6) . ? C1 C2 1.385(6) . ? C2 C3 1.371(6) . ? C2 H2A 0.9500 . ? C3 C4 1.412(6) . ? C3 H3A 0.9500 . ? C4 C5 1.382(5) . ? C5 C6 1.383(6) . ? C5 H5A 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.387(6) . ? C8 C13 1.410(5) . ? C9 C10 1.383(6) . ? C9 H9 0.9500 . ? C10 C11 1.386(6) . ? C10 H10 0.9500 . ? C11 C12 1.379(6) . ? C11 H11 0.9500 . ? C12 C13 1.390(5) . ? C12 H12 0.9500 . ? C15 C19 1.378(5) . ? C15 C16 1.417(5) . ? C16 C17 1.419(5) . ? C16 C16 1.441(7) 3 ? C17 C18 1.350(6) . ? C17 H17 0.9500 . ? C18 C19 1.399(6) 3 ? C18 H18 0.9500 . ? C19 C18 1.399(6) 3 ? C19 H19 0.9500 . ? C20 C21 1.507(5) . ? C21 C22 1.372(6) . ? C21 C26 1.391(6) . ? C22 C23 1.382(7) . ? C22 H22 0.9500 . ? C23 C24 1.359(8) . ? C23 H23 0.9500 . ? C24 C25 1.367(8) . ? C24 H24 0.9500 . ? C25 C26 1.387(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.508(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.532(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.503(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.509(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.524(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.457(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.517(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.525(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.508(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.513(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.531(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.498(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 N1 O2 123.4(4) . . ? O1 N1 C1 118.6(4) . . ? O2 N1 C1 118.0(4) . . ? C7 N2 C4 128.0(3) . . ? C7 N2 H2 116.0 . . ? C4 N2 H2 116.0 . . ? C7 N3 C8 126.1(3) . . ? C7 N3 H3 117.0 . . ? C8 N3 H3 117.0 . . ? C14 N4 C13 125.6(3) . . ? C14 N4 H4 117.2 . . ? C13 N4 H4 117.2 . . ? C14 N5 C15 126.0(3) . . ? C14 N5 H5 117.0 . . ? C15 N5 H5 117.0 . . ? C39 N6 C31 106.7(3) . . ? C39 N6 C35 110.9(3) . . ? C31 N6 C35 111.0(3) . . ? C39 N6 C27 110.4(3) . . ? C31 N6 C27 110.9(3) . . ? C35 N6 C27 107.1(3) . . ? C6 C1 C2 122.0(4) . . ? C6 C1 N1 118.6(4) . . ? C2 C1 N1 119.3(4) . . ? C3 C2 C1 118.5(4) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 120.7(4) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C5 C4 N2 124.9(4) . . ? C5 C4 C3 119.0(4) . . ? N2 C4 C3 116.1(3) . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C1 C6 C5 119.4(4) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? O3 C7 N3 124.6(4) . . ? O3 C7 N2 124.9(4) . . ? N3 C7 N2 110.5(3) . . ? C9 C8 C13 119.1(4) . . ? C9 C8 N3 122.2(3) . . ? C13 C8 N3 118.6(3) . . ? C10 C9 C8 121.2(4) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 119.8(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 121.4(4) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 N4 121.8(3) . . ? C12 C13 C8 118.9(3) . . ? N4 C13 C8 119.3(3) . . ? O4 C14 N4 123.6(4) . . ? O4 C14 N5 123.9(3) . . ? N4 C14 N5 112.4(3) . . ? C19 C15 C16 121.2(3) . . ? C19 C15 N5 121.7(3) . . ? C16 C15 N5 117.0(3) . . ? C15 C16 C17 123.4(3) . . ? C15 C16 C16 118.4(4) . 3 ? C17 C16 C16 118.3(4) . 3 ? C18 C17 C16 121.0(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 121.8(4) . 3 ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 3 . ? C15 C19 C18 119.4(4) . 3 ? C15 C19 H19 120.3 . . ? C18 C19 H19 120.3 3 . ? O6 C20 O5 123.3(4) . . ? O6 C20 C21 118.7(4) . . ? O5 C20 C21 118.0(3) . . ? C22 C21 C26 118.6(4) . . ? C22 C21 C20 121.0(4) . . ? C26 C21 C20 120.4(4) . . ? C21 C22 C23 120.8(5) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 119.9(5) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.9(5) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C24 C25 C26 119.4(5) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C21 120.4(5) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C28 C27 N6 115.9(3) . . ? C28 C27 H27A 108.3 . . ? N6 C27 H27A 108.3 . . ? C28 C27 H27B 108.3 . . ? N6 C27 H27B 108.3 . . ? H27A C27 H27B 107.4 . . ? C27 C28 C29 111.4(4) . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C28 112.6(4) . . ? C30 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C30 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 N6 116.0(3) . . ? C32 C31 H31A 108.3 . . ? N6 C31 H31A 108.3 . . ? C32 C31 H31B 108.3 . . ? N6 C31 H31B 108.3 . . ? H31A C31 H31B 107.4 . . ? C31 C32 C33 111.1(4) . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 111.7(7) . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N6 116.3(3) . . ? C36 C35 H35A 108.2 . . ? N6 C35 H35A 108.2 . . ? C36 C35 H35B 108.2 . . ? N6 C35 H35B 108.2 . . ? H35A C35 H35B 107.4 . . ? C35 C36 C37 109.5(3) . . ? C35 C36 H36A 109.8 . . ? C37 C36 H36A 109.8 . . ? C35 C36 H36B 109.8 . . ? C37 C36 H36B 109.8 . . ? H36A C36 H36B 108.2 . . ? C38 C37 C36 112.5(4) . . ? C38 C37 H37A 109.1 . . ? C36 C37 H37A 109.1 . . ? C38 C37 H37B 109.1 . . ? C36 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? 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 . . ? N6 C39 C40 117.4(3) . . ? N6 C39 H39A 108.0 . . ? C40 C39 H39A 108.0 . . ? N6 C39 H39B 108.0 . . ? C40 C39 H39B 108.0 . . ? H39A C39 H39B 107.2 . . ? C39 C40 C41 109.9(3) . . ? C39 C40 H40A 109.7 . . ? C41 C40 H40A 109.7 . . ? C39 C40 H40B 109.7 . . ? C41 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C42 C41 C40 114.0(4) . . ? C42 C41 H41A 108.7 . . ? C40 C41 H41A 108.7 . . ? C42 C41 H41B 108.7 . . ? C40 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.656 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.063 data_6 _database_code_depnum_ccdc_archive 'CCDC 913114' #TrackingRef 'ACPs-R1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H106 N12 O12' _chemical_formula_weight 1403.75 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 ' 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 23.764(5) _cell_length_b 17.225(4) _cell_length_c 20.791(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.214(3) _cell_angle_gamma 90.00 _cell_volume 7822(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3016 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9760 _exptl_absorpt_correction_T_max 0.9800 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48002 _diffrn_reflns_av_R_equivalents 0.1318 _diffrn_reflns_av_sigmaI/netI 0.1765 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.15 _reflns_number_total 13578 _reflns_number_gt 6266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0000P)^2^+13.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13578 _refine_ls_number_parameters 927 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2458 _refine_ls_R_factor_gt 0.1378 _refine_ls_wR_factor_ref 0.1925 _refine_ls_wR_factor_gt 0.1693 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.003 _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 0.2976(2) 1.1518(3) 0.6016(2) 0.0699(14) Uani 1 1 d . . . O2 O 0.2440(2) 1.1479(3) 0.6651(3) 0.0794(16) Uani 1 1 d . . . O3 O 0.00903(17) 0.9280(2) 0.42368(19) 0.0442(10) Uani 1 1 d . . . O4 O -0.11626(18) 0.8940(2) 0.10637(19) 0.0530(12) Uani 1 1 d . . . N1 N 0.2547(3) 1.1253(3) 0.6140(3) 0.0628(16) Uani 1 1 d . . . N2 N 0.1065(2) 0.9014(2) 0.4315(2) 0.0400(12) Uani 1 1 d . . . H2 H 0.1265 0.8686 0.4175 0.048 Uiso 1 1 d R . . N3 N 0.0244(2) 0.8396(2) 0.3497(2) 0.0335(11) Uani 1 1 d . . . H3 H 0.0509 0.8198 0.3359 0.040 Uiso 1 1 d R . . N4 N -0.03697(18) 0.8504(2) 0.2036(2) 0.0322(11) Uani 1 1 d . . . H4 H 0.0023 0.8469 0.2225 0.039 Uiso 1 1 d R . . N5 N -0.01875(19) 0.8959(2) 0.1106(2) 0.0343(11) Uani 1 1 d . . . H5 H 0.0188 0.8854 0.1364 0.041 Uiso 1 1 d R . . C1 C 0.2156(3) 1.0659(3) 0.5690(3) 0.0458(17) Uani 1 1 d . . . C2 C 0.1575(3) 1.0545(3) 0.5664(3) 0.0414(16) Uani 1 1 d . . . H2A H 0.1435 1.0842 0.5957 0.050 Uiso 1 1 calc R . . C3 C 0.1195(3) 1.0005(3) 0.5217(3) 0.0390(15) Uani 1 1 d . . . H3A H 0.0792 0.9928 0.5195 0.047 Uiso 1 1 calc R . . C4 C 0.1413(3) 0.9567(3) 0.4790(3) 0.0362(15) Uani 1 1 d . . . C5 C 0.2003(3) 0.9683(3) 0.4844(3) 0.0517(18) Uani 1 1 d . . . H5A H 0.2153 0.9374 0.4568 0.062 Uiso 1 1 calc R . . C6 C 0.2383(3) 1.0233(4) 0.5286(3) 0.0562(18) Uani 1 1 d . . . H6 H 0.2787 1.0314 0.5311 0.067 Uiso 1 1 calc R . . C7 C 0.0435(3) 0.8926(3) 0.4033(3) 0.0341(14) Uani 1 1 d . . . C8 C -0.0377(2) 0.8168(3) 0.3165(3) 0.0314(13) Uani 1 1 d . . . C9 C -0.0679(3) 0.7868(3) 0.3563(3) 0.0427(16) Uani 1 1 d . . . H9A H -0.0459 0.7794 0.4052 0.051 Uiso 1 1 calc R . . C10 C -0.1286(3) 0.7678(3) 0.3265(3) 0.0475(16) Uani 1 1 d . . . H10A H -0.1487 0.7486 0.3547 0.057 Uiso 1 1 calc R . . C11 C -0.1611(3) 0.7768(3) 0.2548(3) 0.0477(17) Uani 1 1 d . . . H11 H -0.2035 0.7650 0.2338 0.057 Uiso 1 1 calc R . . C12 C -0.1305(3) 0.8032(3) 0.2142(3) 0.0404(15) Uani 1 1 d . . . H12A H -0.1520 0.8072 0.1649 0.048 Uiso 1 1 calc R . . C13 C -0.0693(2) 0.8239(3) 0.2442(3) 0.0311(14) Uani 1 1 d . . . C14 C -0.0622(3) 0.8807(3) 0.1373(3) 0.0339(14) Uani 1 1 d . . . C15 C -0.0323(2) 0.9273(3) 0.0430(3) 0.0362(15) Uani 1 1 d . . . C16 C 0.0068(2) 0.9839(3) 0.0340(2) 0.0267(13) Uani 1 1 d . . . C17 C 0.0581(3) 1.0106(4) 0.0897(3) 0.0577(19) Uani 1 1 d . . . H17A H 0.0682 0.9894 0.1351 0.069 Uiso 1 1 calc R . . C18 C -0.0817(3) 0.9016(4) -0.0122(3) 0.083(3) Uani 1 1 d . . . H18A H -0.1075 0.8630 -0.0057 0.099 Uiso 1 1 calc R . . C19 C 0.0946(3) 1.0674(5) 0.0797(3) 0.098(3) Uani 1 1 d . . . H19A H 0.1288 1.0862 0.1186 0.118 Uiso 1 1 calc R . . O5 O 0.2020(3) 0.2988(3) -0.0716(3) 0.115(3) Uani 1 1 d . . . O6 O 0.1612(3) 0.2750(3) 0.0028(4) 0.097(2) Uani 1 1 d . . . O7 O 0.42275(19) 0.0253(3) 0.0349(2) 0.0628(13) Uani 1 1 d . . . O8 O 0.59690(18) -0.0127(2) 0.33777(19) 0.0468(11) Uani 1 1 d . . . N6 N 0.1973(3) 0.2588(4) -0.0259(4) 0.085(2) Uani 1 1 d . . . N7 N 0.3442(2) -0.0058(3) 0.0690(3) 0.0587(15) Uani 1 1 d . . . H7 H 0.3300 -0.0431 0.0857 0.070 Uiso 1 1 d R . . N8 N 0.4364(2) -0.0654(3) 0.1191(2) 0.0518(14) Uani 1 1 d . . . H8 H 0.4183 -0.0902 0.1413 0.062 Uiso 1 1 d R . . N9 N 0.51484(19) -0.0773(3) 0.2591(2) 0.0418(12) Uani 1 1 d . . . H9 H 0.4783 -0.0929 0.2512 0.050 Uiso 1 1 d R . . N10 N 0.5141(2) -0.0427(3) 0.3644(2) 0.0436(13) Uani 1 1 d . . . H10 H 0.4773 -0.0603 0.3458 0.052 Uiso 1 1 d R . . C20 C 0.2362(3) 0.1892(4) -0.0031(4) 0.062(2) Uani 1 1 d . . . C21 C 0.2384(3) 0.1521(4) 0.0568(4) 0.068(2) Uani 1 1 d . . . H21 H 0.2160 0.1715 0.0824 0.082 Uiso 1 1 calc R . . C22 C 0.2737(3) 0.0866(4) 0.0784(3) 0.0607(19) Uani 1 1 d . . . H22 H 0.2752 0.0601 0.1191 0.073 Uiso 1 1 calc R . . C23 C 0.3076(3) 0.0583(4) 0.0419(3) 0.0535(18) Uani 1 1 d . . . C24 C 0.3023(3) 0.0948(4) -0.0194(3) 0.063(2) Uani 1 1 d . . . H24 H 0.3235 0.0747 -0.0461 0.076 Uiso 1 1 calc R . . C25 C 0.2669(3) 0.1596(4) -0.0419(4) 0.066(2) Uani 1 1 d . . . H25 H 0.2634 0.1843 -0.0842 0.079 Uiso 1 1 calc R . . C26 C 0.4031(3) -0.0127(4) 0.0712(3) 0.0476(17) Uani 1 1 d . . . C27 C 0.4991(2) -0.0837(3) 0.1358(3) 0.0437(16) Uani 1 1 d . . . C28 C 0.5215(3) -0.0965(3) 0.0846(3) 0.0493(17) Uani 1 1 d . . . H28 H 0.4950 -0.0920 0.0366 0.059 Uiso 1 1 calc R . . C29 C 0.5822(3) -0.1156(3) 0.1027(3) 0.0508(17) Uani 1 1 d . . . H29 H 0.5971 -0.1240 0.0672 0.061 Uiso 1 1 calc R . . C30 C 0.6213(3) -0.1225(3) 0.1722(3) 0.0458(16) Uani 1 1 d . . . H30 H 0.6632 -0.1354 0.1847 0.055 Uiso 1 1 calc R . . C31 C 0.5983(3) -0.1102(3) 0.2239(3) 0.0439(16) Uani 1 1 d . . . H31 H 0.6247 -0.1158 0.2718 0.053 Uiso 1 1 calc R . . C32 C 0.5376(2) -0.0900(3) 0.2062(3) 0.0360(14) Uani 1 1 d . . . C33 C 0.5476(3) -0.0422(3) 0.3219(3) 0.0367(15) Uani 1 1 d . . . C34 C 0.5349(3) -0.0175(3) 0.4345(3) 0.0403(15) Uani 1 1 d . . . C35 C 0.5945(3) -0.0033(4) 0.4737(3) 0.0592(19) Uani 1 1 d . . . H35 H 0.6237 -0.0076 0.4532 0.071 Uiso 1 1 calc R . . C36 C 0.6138(3) 0.0176(4) 0.5439(3) 0.062(2) Uani 1 1 d . . . H36 H 0.6559 0.0276 0.5708 0.075 Uiso 1 1 calc R . . C37 C 0.4900(3) -0.0105(3) 0.4640(3) 0.0380(15) Uani 1 1 d . . . C38 C 0.5723(3) 0.0238(3) 0.5741(3) 0.0488(17) Uani 1 1 d . . . H38 H 0.5862 0.0374 0.6222 0.059 Uiso 1 1 calc R . . N21 N 0.0338(2) 0.5957(2) 0.2384(2) 0.0412(13) Uani 1 1 d . . . C93 C -0.0219(3) 0.5465(3) 0.2287(3) 0.0434(16) Uani 1 1 d . . . H93A H -0.0322 0.5160 0.1852 0.052 Uiso 1 1 calc R . . H93B H -0.0102 0.5091 0.2679 0.052 Uiso 1 1 calc R . . C94 C -0.0789(3) 0.5877(3) 0.2246(3) 0.0459(16) Uani 1 1 d . . . H94A H -0.0903 0.6280 0.1877 0.055 Uiso 1 1 calc R . . H94B H -0.0715 0.6135 0.2698 0.055 Uiso 1 1 calc R . . C95 C -0.1304(3) 0.5294(3) 0.2080(3) 0.0528(18) Uani 1 1 d . . . H95A H -0.1369 0.5043 0.1628 0.063 Uiso 1 1 calc R . . H95B H -0.1174 0.4885 0.2445 0.063 Uiso 1 1 calc R . . C96 C -0.1900(3) 0.5624(4) 0.2037(4) 0.075(2) Uani 1 1 d . . . H96A H -0.2034 0.6031 0.1680 0.112 Uiso 1 1 calc R . . H96B H -0.1849 0.5844 0.2492 0.112 Uiso 1 1 calc R . . H96C H -0.2209 0.5211 0.1912 0.112 Uiso 1 1 calc R . . C97 C 0.0557(3) 0.6403(3) 0.3073(3) 0.0433(16) Uani 1 1 d . . . H97A H 0.0879 0.6771 0.3079 0.052 Uiso 1 1 calc R . . H97B H 0.0210 0.6715 0.3081 0.052 Uiso 1 1 calc R . . C98 C 0.0808(3) 0.5925(3) 0.3733(3) 0.061(2) Uani 1 1 d . . . H98A H 0.1162 0.5618 0.3738 0.074 Uiso 1 1 calc R . . H98B H 0.0489 0.5556 0.3738 0.074 Uiso 1 1 calc R . . C99 C 0.1006(4) 0.6425(4) 0.4381(3) 0.080(2) Uani 1 1 d . . . H99A H 0.1138 0.6935 0.4270 0.096 Uiso 1 1 calc R . . H99B H 0.0647 0.6516 0.4500 0.096 Uiso 1 1 calc R . . C100 C 0.1462(5) 0.6133(9) 0.4946(7) 0.322(13) Uani 1 1 d . . . H10B H 0.1386 0.5580 0.4991 0.482 Uiso 1 1 calc R . . H10C H 0.1479 0.6409 0.5366 0.482 Uiso 1 1 calc R . . H10D H 0.1852 0.6196 0.4895 0.482 Uiso 1 1 calc R . . C101 C 0.0181(3) 0.6563(3) 0.1816(3) 0.0441(16) Uani 1 1 d . . . H10E H 0.0553 0.6871 0.1892 0.053 Uiso 1 1 calc R . . H10F H -0.0126 0.6921 0.1865 0.053 Uiso 1 1 calc R . . C102 C -0.0067(3) 0.6258(3) 0.1075(3) 0.0544(18) Uani 1 1 d . . . H10G H -0.0474 0.6020 0.0966 0.065 Uiso 1 1 calc R . . H10H H 0.0210 0.5850 0.1033 0.065 Uiso 1 1 calc R . . C103 C -0.0125(3) 0.6904(3) 0.0553(3) 0.0569(19) Uani 1 1 d . . . H10I H -0.0363 0.6708 0.0075 0.068 Uiso 1 1 calc R . . H10J H -0.0358 0.7338 0.0641 0.068 Uiso 1 1 calc R . . C104 C 0.0483(3) 0.7211(4) 0.0586(3) 0.074(2) Uani 1 1 d . . . H10K H 0.0713 0.6788 0.0486 0.111 Uiso 1 1 calc R . . H10L H 0.0719 0.7419 0.1054 0.111 Uiso 1 1 calc R . . H10M H 0.0410 0.7624 0.0238 0.111 Uiso 1 1 calc R . . C105 C 0.0833(3) 0.5407(3) 0.2366(3) 0.0560(18) Uani 1 1 d . . . H10N H 0.0953 0.5061 0.2779 0.067 Uiso 1 1 calc R . . H10O H 0.0655 0.5077 0.1944 0.067 Uiso 1 1 calc R . . C106 C 0.1405(3) 0.5790(4) 0.2362(4) 0.070(2) Uani 1 1 d . . . H10P H 0.1553 0.6185 0.2738 0.084 Uiso 1 1 calc R . . H10Q H 0.1309 0.6054 0.1908 0.084 Uiso 1 1 calc R . . C107 C 0.1906(4) 0.5174(5) 0.2476(5) 0.108(3) Uani 1 1 d . . . H10R H 0.1725 0.4711 0.2186 0.130 Uiso 1 1 calc R . . H10S H 0.2081 0.5012 0.2973 0.130 Uiso 1 1 calc R . . C108 C 0.2419(5) 0.5515(8) 0.2274(6) 0.221(7) Uani 1 1 d . . . H10T H 0.2660 0.5889 0.2631 0.332 Uiso 1 1 calc R . . H10U H 0.2234 0.5776 0.1820 0.332 Uiso 1 1 calc R . . H10V H 0.2685 0.5094 0.2245 0.332 Uiso 1 1 calc R . . N22 N 0.4967(3) 0.1797(3) 0.2156(3) 0.0664(17) Uani 1 1 d . . . C109 C 0.4500(3) 0.1321(4) 0.2298(4) 0.074(2) Uani 1 1 d . . . H1 H 0.4717 0.0930 0.2660 0.089 Uiso 1 1 calc R . . H10W H 0.4250 0.1036 0.1865 0.089 Uiso 1 1 calc R . . C110 C 0.4074(3) 0.1781(4) 0.2538(4) 0.079(2) Uani 1 1 d . . . H11A H 0.4314 0.2157 0.2903 0.095 Uiso 1 1 calc R . . H11B H 0.3779 0.2077 0.2139 0.095 Uiso 1 1 calc R . . C111 C 0.3727(4) 0.1242(5) 0.2830(5) 0.100(3) Uani 1 1 d . . . H11C H 0.3500 0.0854 0.2469 0.119 Uiso 1 1 calc R . . H11D H 0.4023 0.0958 0.3237 0.119 Uiso 1 1 calc R . . C112 C 0.3280(4) 0.1676(5) 0.3055(5) 0.130(4) Uani 1 1 d . . . H11E H 0.3494 0.2102 0.3368 0.196 Uiso 1 1 calc R . . H11F H 0.3111 0.1320 0.3301 0.196 Uiso 1 1 calc R . . H11G H 0.2947 0.1886 0.2641 0.196 Uiso 1 1 calc R . . C113 C 0.5386(3) 0.2219(4) 0.2806(4) 0.076(2) Uani 1 1 d . . . H11H H 0.5709 0.2480 0.2697 0.091 Uiso 1 1 calc R . . H11I H 0.5146 0.2629 0.2915 0.091 Uiso 1 1 calc R . . C114 C 0.5693(4) 0.1735(4) 0.3454(4) 0.132(4) Uani 1 1 d . . . H11J H 0.5894 0.1279 0.3346 0.159 Uiso 1 1 calc R . . H11K H 0.5386 0.1548 0.3630 0.159 Uiso 1 1 calc R . . C115 C 0.6187(7) 0.2260(6) 0.4026(5) 0.229(8) Uani 1 1 d . . . H11L H 0.6415 0.2543 0.3791 0.274 Uiso 1 1 calc R . . H11M H 0.5962 0.2654 0.4179 0.274 Uiso 1 1 calc R . . C116 C 0.6608(9) 0.1929(8) 0.4614(8) 0.404(17) Uani 1 1 d . . . H11N H 0.6396 0.1637 0.4857 0.606 Uiso 1 1 calc R . . H11O H 0.6860 0.2335 0.4924 0.606 Uiso 1 1 calc R . . H11P H 0.6869 0.1576 0.4484 0.606 Uiso 1 1 calc R . . C117 C 0.4667(3) 0.2430(3) 0.1609(4) 0.066(2) Uani 1 1 d . . . H11Q H 0.4440 0.2785 0.1794 0.079 Uiso 1 1 calc R . . H11R H 0.4995 0.2736 0.1548 0.079 Uiso 1 1 calc R . . C118 C 0.4229(3) 0.2143(4) 0.0890(4) 0.078(2) Uani 1 1 d . . . H11S H 0.3848 0.1949 0.0920 0.093 Uiso 1 1 calc R . . H11T H 0.4421 0.1708 0.0738 0.093 Uiso 1 1 calc R . . C119 C 0.4077(3) 0.2808(4) 0.0353(4) 0.076(2) Uani 1 1 d . . . H11U H 0.3703 0.2674 -0.0060 0.092 Uiso 1 1 calc R . . H11V H 0.3992 0.3286 0.0563 0.092 Uiso 1 1 calc R . . C120 C 0.4602(3) 0.2960(4) 0.0120(4) 0.083(2) Uani 1 1 d . . . H12B H 0.4964 0.3133 0.0522 0.124 Uiso 1 1 calc R . . H12C H 0.4479 0.3363 -0.0242 0.124 Uiso 1 1 calc R . . H12D H 0.4698 0.2481 -0.0070 0.124 Uiso 1 1 calc R . . C121 C 0.5321(3) 0.1232(4) 0.1897(4) 0.076(2) Uani 1 1 d . . . H12E H 0.5022 0.0925 0.1510 0.092 Uiso 1 1 calc R . . H12F H 0.5541 0.0866 0.2282 0.092 Uiso 1 1 calc R . . C122 C 0.5785(4) 0.1587(4) 0.1639(4) 0.089(3) Uani 1 1 d . . . H12G H 0.5582 0.1993 0.1287 0.107 Uiso 1 1 calc R . . H12H H 0.6120 0.1835 0.2037 0.107 Uiso 1 1 calc R . . C123 C 0.6049(4) 0.0972(4) 0.1318(4) 0.086(3) Uani 1 1 d . . . H12I H 0.5708 0.0684 0.0961 0.103 Uiso 1 1 calc R . . H12J H 0.6286 0.0598 0.1687 0.103 Uiso 1 1 calc R . . C124 C 0.6464(4) 0.1296(5) 0.0978(4) 0.109(3) Uani 1 1 d . . . H12K H 0.6229 0.1651 0.0599 0.164 Uiso 1 1 calc R . . H12L H 0.6622 0.0867 0.0788 0.164 Uiso 1 1 calc R . . H12M H 0.6806 0.1576 0.1329 0.164 Uiso 1 1 calc R . . O17 O 0.08565(16) 0.8366(2) 0.2255(2) 0.0458(10) Uani 1 1 d . . . O18 O 0.13829(17) 0.8067(2) 0.3375(2) 0.0467(11) Uani 1 1 d . . . O19 O 0.3567(2) 0.9090(4) 0.1847(3) 0.118(2) Uani 1 1 d . . . O20 O 0.41063(19) 0.8642(3) 0.2891(2) 0.0687(14) Uani 1 1 d . . . C77 C 0.1350(2) 0.8264(3) 0.2777(3) 0.0348(14) Uani 1 1 d . . . C78 C 0.1938(2) 0.8397(3) 0.2681(3) 0.0314(14) Uani 1 1 d . . . C79 C 0.1924(3) 0.8649(3) 0.2042(3) 0.0453(16) Uani 1 1 d . . . H79 H 0.1544 0.8729 0.1658 0.054 Uiso 1 1 calc R . . C80 C 0.2469(3) 0.8781(3) 0.1970(3) 0.0510(17) Uani 1 1 d . . . H80 H 0.2458 0.8959 0.1533 0.061 Uiso 1 1 calc R . . C81 C 0.3026(2) 0.8662(3) 0.2507(3) 0.0397(15) Uani 1 1 d . . . C82 C 0.3028(2) 0.8404(3) 0.3133(3) 0.0482(17) Uani 1 1 d . . . H82 H 0.3407 0.8309 0.3514 0.058 Uiso 1 1 calc R . . C83 C 0.2495(2) 0.8282(3) 0.3213(3) 0.0421(15) Uani 1 1 d . . . H83 H 0.2511 0.8111 0.3654 0.050 Uiso 1 1 calc R . . C84 C 0.3612(3) 0.8811(4) 0.2418(4) 0.0595(19) 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 O1 0.055(3) 0.073(3) 0.070(3) -0.010(3) 0.012(3) -0.016(3) O2 0.058(3) 0.095(4) 0.073(4) -0.035(3) 0.014(3) -0.004(3) O3 0.053(3) 0.031(2) 0.050(3) -0.006(2) 0.021(2) 0.000(2) O4 0.043(3) 0.066(3) 0.041(2) 0.021(2) 0.007(2) -0.005(2) N1 0.051(4) 0.067(4) 0.060(4) -0.003(4) 0.012(3) 0.006(4) N2 0.044(3) 0.033(3) 0.044(3) -0.004(2) 0.018(2) 0.001(3) N3 0.050(3) 0.024(3) 0.030(3) -0.004(2) 0.019(2) -0.001(2) N4 0.030(3) 0.035(3) 0.030(3) -0.001(2) 0.010(2) -0.010(2) N5 0.035(3) 0.040(3) 0.027(3) 0.004(2) 0.012(2) -0.007(2) C1 0.038(4) 0.038(4) 0.043(4) -0.011(3) -0.003(3) -0.011(3) C2 0.046(4) 0.028(3) 0.041(4) 0.001(3) 0.008(3) 0.005(3) C3 0.047(4) 0.028(3) 0.036(3) 0.003(3) 0.009(3) 0.007(3) C4 0.037(4) 0.024(3) 0.038(4) 0.000(3) 0.004(3) 0.002(3) C5 0.045(4) 0.053(4) 0.047(4) -0.012(3) 0.009(3) 0.010(4) C6 0.043(4) 0.062(5) 0.061(5) -0.009(4) 0.018(4) 0.002(4) C7 0.054(4) 0.010(3) 0.040(4) 0.014(3) 0.020(3) 0.008(3) C8 0.040(3) 0.019(3) 0.036(4) 0.003(3) 0.017(3) -0.001(3) C9 0.056(4) 0.037(4) 0.038(4) 0.005(3) 0.021(3) -0.003(3) C10 0.065(5) 0.041(4) 0.053(4) 0.001(3) 0.041(4) -0.007(4) C11 0.049(4) 0.041(4) 0.056(4) -0.001(3) 0.023(4) -0.015(3) C12 0.048(4) 0.033(3) 0.040(4) -0.005(3) 0.017(3) -0.013(3) C13 0.040(3) 0.019(3) 0.035(3) 0.008(3) 0.015(3) -0.005(3) C14 0.037(4) 0.025(3) 0.030(3) 0.003(3) 0.002(3) -0.005(3) C15 0.050(4) 0.029(3) 0.024(3) 0.004(3) 0.009(3) -0.012(3) C16 0.036(3) 0.015(3) 0.025(3) 0.000(2) 0.008(3) -0.002(3) C17 0.058(4) 0.074(5) 0.034(4) 0.017(4) 0.011(3) -0.022(4) C18 0.088(5) 0.101(6) 0.043(4) 0.014(4) 0.009(4) -0.060(5) C19 0.083(5) 0.154(8) 0.032(4) 0.016(5) -0.005(4) -0.077(6) O5 0.155(6) 0.059(4) 0.083(4) 0.027(3) -0.003(4) 0.006(4) O6 0.076(4) 0.057(4) 0.139(6) -0.017(3) 0.021(4) 0.008(3) O7 0.064(3) 0.077(3) 0.056(3) 0.024(3) 0.032(3) 0.015(3) O8 0.051(3) 0.051(3) 0.042(2) -0.008(2) 0.022(2) -0.009(2) N6 0.078(5) 0.045(5) 0.092(6) -0.022(4) -0.009(5) -0.012(4) N7 0.034(3) 0.065(4) 0.071(4) 0.022(3) 0.014(3) 0.011(3) N8 0.049(3) 0.067(4) 0.045(3) 0.021(3) 0.024(3) 0.013(3) N9 0.031(3) 0.059(3) 0.038(3) 0.000(3) 0.016(2) -0.001(3) N10 0.034(3) 0.063(3) 0.037(3) -0.001(3) 0.019(2) 0.001(3) C20 0.055(5) 0.034(4) 0.069(5) 0.011(4) -0.007(4) 0.001(4) C21 0.050(4) 0.073(5) 0.067(5) 0.002(4) 0.008(4) 0.008(4) C22 0.051(4) 0.072(5) 0.055(4) 0.014(4) 0.017(4) 0.013(4) C23 0.036(4) 0.068(5) 0.051(4) 0.009(4) 0.012(3) 0.005(4) C24 0.037(4) 0.086(5) 0.054(4) 0.028(4) 0.005(3) 0.017(4) C25 0.048(4) 0.081(6) 0.060(5) 0.018(4) 0.012(4) 0.002(4) C26 0.043(4) 0.063(5) 0.030(4) 0.000(3) 0.007(3) 0.006(4) C27 0.030(3) 0.044(4) 0.054(4) 0.005(3) 0.013(3) 0.002(3) C28 0.058(4) 0.068(5) 0.026(3) 0.003(3) 0.021(3) 0.015(4) C29 0.054(4) 0.059(4) 0.044(4) -0.001(3) 0.024(3) 0.004(4) C30 0.042(4) 0.056(4) 0.043(4) -0.002(3) 0.021(3) 0.003(3) C31 0.042(4) 0.053(4) 0.035(4) 0.002(3) 0.013(3) 0.003(3) C32 0.038(4) 0.040(4) 0.030(3) -0.001(3) 0.014(3) 0.000(3) C33 0.041(4) 0.033(4) 0.034(4) 0.002(3) 0.013(3) 0.006(3) C34 0.035(4) 0.048(4) 0.040(4) 0.009(3) 0.016(3) 0.007(3) C35 0.048(4) 0.097(6) 0.042(4) -0.003(4) 0.027(3) 0.008(4) C36 0.033(4) 0.105(6) 0.049(4) -0.011(4) 0.017(3) 0.000(4) C37 0.033(3) 0.039(4) 0.038(3) 0.006(3) 0.011(3) 0.009(3) C38 0.045(4) 0.066(4) 0.037(4) 0.002(3) 0.018(3) 0.008(4) N21 0.074(4) 0.016(2) 0.032(3) -0.007(2) 0.019(2) 0.000(3) C93 0.068(4) 0.018(3) 0.037(4) -0.001(3) 0.013(3) -0.004(3) C94 0.063(4) 0.027(3) 0.045(4) 0.009(3) 0.018(3) 0.007(3) C95 0.062(4) 0.043(4) 0.042(4) 0.001(3) 0.009(3) -0.002(4) C96 0.079(5) 0.055(5) 0.079(5) 0.012(4) 0.020(4) -0.002(4) C97 0.068(4) 0.028(3) 0.037(4) -0.003(3) 0.025(3) 0.000(3) C98 0.097(5) 0.040(4) 0.036(4) -0.010(3) 0.014(4) -0.006(4) C99 0.115(6) 0.079(5) 0.033(4) -0.004(4) 0.014(4) 0.022(5) C100 0.229(14) 0.300(18) 0.224(15) -0.181(14) -0.138(12) 0.153(14) C101 0.073(4) 0.025(3) 0.033(3) -0.003(3) 0.021(3) -0.004(3) C102 0.083(5) 0.040(4) 0.039(4) -0.005(3) 0.022(3) -0.013(4) C103 0.086(5) 0.045(4) 0.036(4) 0.002(3) 0.020(4) -0.010(4) C104 0.101(6) 0.072(5) 0.053(5) -0.005(4) 0.035(4) -0.037(5) C105 0.076(5) 0.037(4) 0.057(4) -0.003(3) 0.028(4) 0.012(4) C106 0.070(5) 0.081(5) 0.059(5) -0.019(4) 0.026(4) 0.003(5) C107 0.066(6) 0.137(8) 0.126(8) -0.037(7) 0.043(6) 0.016(6) C108 0.158(12) 0.271(17) 0.184(13) -0.123(12) 0.014(10) 0.008(12) N22 0.091(4) 0.031(3) 0.075(4) -0.001(3) 0.029(4) 0.005(3) C109 0.107(6) 0.030(4) 0.085(6) 0.013(4) 0.036(5) -0.009(4) C110 0.103(6) 0.054(5) 0.091(6) 0.013(4) 0.048(5) 0.016(5) C111 0.103(7) 0.087(6) 0.115(7) 0.024(5) 0.051(6) -0.014(6) C112 0.111(7) 0.126(8) 0.191(11) 0.027(7) 0.098(8) 0.007(7) C113 0.082(5) 0.047(4) 0.082(6) 0.001(4) 0.015(4) 0.000(4) C114 0.202(10) 0.061(5) 0.072(6) 0.007(5) -0.012(6) 0.027(6) C115 0.384(19) 0.087(8) 0.071(7) -0.005(6) -0.065(10) 0.034(10) C116 0.59(3) 0.136(12) 0.201(17) -0.020(12) -0.15(2) 0.079(17) C117 0.076(5) 0.039(4) 0.080(5) 0.009(4) 0.027(4) 0.006(4) C118 0.079(5) 0.060(5) 0.080(6) 0.002(4) 0.015(4) -0.012(4) C119 0.082(6) 0.063(5) 0.074(5) 0.004(4) 0.020(4) -0.015(4) C120 0.106(6) 0.068(5) 0.079(6) -0.010(4) 0.043(5) -0.017(5) C121 0.086(6) 0.049(5) 0.085(6) 0.005(4) 0.024(5) 0.001(4) C122 0.111(7) 0.052(5) 0.110(7) 0.000(5) 0.051(6) 0.009(5) C123 0.085(6) 0.065(5) 0.098(7) -0.019(5) 0.025(5) 0.003(5) C124 0.118(7) 0.110(7) 0.103(7) -0.014(6) 0.048(6) 0.002(6) O17 0.034(2) 0.055(3) 0.049(3) 0.002(2) 0.017(2) -0.004(2) O18 0.054(3) 0.050(3) 0.045(3) 0.010(2) 0.028(2) 0.000(2) O19 0.069(4) 0.187(6) 0.129(5) 0.094(5) 0.075(4) 0.041(4) O20 0.038(3) 0.093(4) 0.078(3) -0.012(3) 0.026(3) -0.005(3) C77 0.034(4) 0.015(3) 0.052(4) -0.004(3) 0.013(3) 0.002(3) C78 0.036(3) 0.015(3) 0.043(4) -0.003(3) 0.016(3) 0.004(3) C79 0.033(4) 0.060(4) 0.041(4) 0.016(3) 0.013(3) 0.005(3) C80 0.054(4) 0.057(4) 0.052(4) 0.020(3) 0.032(4) 0.016(4) C81 0.034(4) 0.042(4) 0.043(4) 0.011(3) 0.016(3) 0.010(3) C82 0.026(3) 0.066(5) 0.045(4) 0.004(3) 0.006(3) 0.000(3) C83 0.037(4) 0.053(4) 0.034(3) 0.004(3) 0.011(3) 0.002(3) C84 0.052(5) 0.064(5) 0.067(5) -0.004(4) 0.029(4) 0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 N1 1.233(6) . ? O2 N1 1.248(7) . ? O3 C7 1.224(6) . ? O4 C14 1.211(6) . ? N1 C1 1.449(7) . ? N2 C7 1.383(6) . ? N2 C4 1.385(6) . ? N2 H2 0.8601 . ? N3 C7 1.371(6) . ? N3 C8 1.416(6) . ? N3 H3 0.8602 . ? N4 C14 1.372(6) . ? N4 C13 1.422(6) . ? N4 H4 0.8602 . ? N5 C14 1.375(7) . ? N5 C15 1.419(6) . ? N5 H5 0.8602 . ? C1 C2 1.375(7) . ? C1 C6 1.376(8) . ? C2 C3 1.372(7) . ? C2 H2A 0.9500 . ? C3 C4 1.410(7) . ? C3 H3A 0.9500 . ? C4 C5 1.376(7) . ? C5 C6 1.381(7) . ? C5 H5A 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.390(7) . ? C8 C13 1.396(7) . ? C9 C10 1.367(7) . ? C9 H9A 0.9500 . ? C10 C11 1.391(7) . ? C10 H10A 0.9500 . ? C11 C12 1.389(7) . ? C11 H11 0.9500 . ? C12 C13 1.384(7) . ? C12 H12A 0.9500 . ? C15 C18 1.353(7) . ? C15 C16 1.409(7) . ? C16 C17 1.388(7) . ? C16 C16 1.431(9) 3_575 ? C17 C19 1.376(8) . ? C17 H17A 0.9500 . ? C18 C19 1.419(8) 3_575 ? C18 H18A 0.9500 . ? C19 C18 1.419(8) 3_575 ? C19 H19A 0.9500 . ? O5 N6 1.213(9) . ? O6 N6 1.254(8) . ? O7 C26 1.221(7) . ? O8 C33 1.198(6) . ? N6 C20 1.474(9) . ? N7 C23 1.381(7) . ? N7 C26 1.388(7) . ? N7 H7 0.8601 . ? N8 C26 1.349(7) . ? N8 C27 1.424(6) . ? N8 H8 0.8603 . ? N9 C33 1.370(6) . ? N9 C32 1.420(6) . ? N9 H9 0.8600 . ? N10 C33 1.402(7) . ? N10 C34 1.411(7) . ? N10 H10 0.8601 . ? C20 C21 1.381(9) . ? C20 C25 1.383(9) . ? C21 C22 1.371(8) . ? C21 H21 0.9500 . ? C22 C23 1.396(8) . ? C22 H22 0.9500 . ? C23 C24 1.381(8) . ? C24 C25 1.364(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C27 C28 1.383(8) . ? C27 C32 1.392(7) . ? C28 C29 1.378(7) . ? C28 H28 0.9500 . ? C29 C30 1.381(7) . ? C29 H29 0.9500 . ? C30 C31 1.401(7) . ? C30 H30 0.9500 . ? C31 C32 1.385(7) . ? C31 H31 0.9500 . ? C34 C35 1.350(7) . ? C34 C37 1.429(7) . ? C35 C36 1.393(8) . ? C35 H35 0.9500 . ? C36 C38 1.365(8) . ? C36 H36 0.9500 . ? C37 C38 1.397(7) 3_656 ? C37 C37 1.428(10) 3_656 ? C38 C37 1.397(7) 3_656 ? C38 H38 0.9500 . ? N21 C101 1.509(6) . ? N21 C93 1.516(6) . ? N21 C105 1.522(7) . ? N21 C97 1.525(6) . ? C93 C94 1.503(7) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C95 1.513(7) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.497(8) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 C98 1.509(7) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C99 1.509(8) . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 C100 1.343(11) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C100 H10D 0.9800 . ? C101 C102 1.509(7) . ? C101 H10E 0.9900 . ? C101 H10F 0.9900 . ? C102 C103 1.522(7) . ? C102 H10G 0.9900 . ? C102 H10H 0.9900 . ? C103 C104 1.515(8) . ? C103 H10I 0.9900 . ? C103 H10J 0.9900 . ? C104 H10K 0.9800 . ? C104 H10L 0.9800 . ? C104 H10M 0.9800 . ? C105 C106 1.513(8) . ? C105 H10N 0.9900 . ? C105 H10O 0.9900 . ? C106 C107 1.541(9) . ? C106 H10P 0.9900 . ? C106 H10Q 0.9900 . ? C107 C108 1.552(14) . ? C107 H10R 0.9900 . ? C107 H10S 0.9900 . ? C108 H10T 0.9800 . ? C108 H10U 0.9800 . ? C108 H10V 0.9800 . ? N22 C109 1.499(8) . ? N22 C113 1.512(7) . ? N22 C121 1.516(8) . ? N22 C117 1.534(7) . ? C109 C110 1.518(9) . ? C109 H1 0.9900 . ? C109 H10W 0.9900 . ? C110 C111 1.518(9) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.515(10) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C113 C114 1.505(9) . ? C113 H11H 0.9900 . ? C113 H11I 0.9900 . ? C114 C115 1.584(11) . ? C114 H11J 0.9900 . ? C114 H11K 0.9900 . ? C115 C116 1.362(13) . ? C115 H11L 0.9900 . ? C115 H11M 0.9900 . ? C116 H11N 0.9800 . ? C116 H11O 0.9800 . ? C116 H11P 0.9800 . ? C117 C118 1.528(8) . ? C117 H11Q 0.9900 . ? C117 H11R 0.9900 . ? C118 C119 1.540(8) . ? C118 H11S 0.9900 . ? C118 H11T 0.9900 . ? C119 C120 1.529(9) . ? C119 H11U 0.9900 . ? C119 H11V 0.9900 . ? C120 H12B 0.9800 . ? C120 H12C 0.9800 . ? C120 H12D 0.9800 . ? C121 C122 1.532(9) . ? C121 H12E 0.9900 . ? C121 H12F 0.9900 . ? C122 C123 1.514(9) . ? C122 H12G 0.9900 . ? C122 H12H 0.9900 . ? C123 C124 1.527(10) . ? C123 H12I 0.9900 . ? C123 H12J 0.9900 . ? C124 H12K 0.9800 . ? C124 H12L 0.9800 . ? C124 H12M 0.9800 . ? O17 C77 1.256(6) . ? O18 C77 1.262(6) . ? O19 C84 1.247(8) . ? O20 C84 1.234(7) . ? C77 C78 1.506(7) . ? C78 C83 1.364(7) . ? C78 C79 1.385(7) . ? C79 C80 1.381(7) . ? C79 H79 0.9500 . ? C80 C81 1.368(7) . ? C80 H80 0.9500 . ? C81 C82 1.373(7) . ? C81 C84 1.498(8) . ? C82 C83 1.357(7) . ? C82 H82 0.9500 . ? C83 H83 0.9500 . ? 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 N1 O2 121.7(6) . . ? O1 N1 C1 119.9(6) . . ? O2 N1 C1 118.4(6) . . ? C7 N2 C4 128.3(5) . . ? C7 N2 H2 115.6 . . ? C4 N2 H2 116.0 . . ? C7 N3 C8 122.0(5) . . ? C7 N3 H3 118.8 . . ? C8 N3 H3 119.2 . . ? C14 N4 C13 126.5(4) . . ? C14 N4 H4 116.8 . . ? C13 N4 H4 116.7 . . ? C14 N5 C15 124.0(4) . . ? C14 N5 H5 117.9 . . ? C15 N5 H5 118.1 . . ? C2 C1 C6 122.0(5) . . ? C2 C1 N1 120.3(6) . . ? C6 C1 N1 117.7(6) . . ? C3 C2 C1 120.4(6) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 118.9(6) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 N2 117.4(5) . . ? C5 C4 C3 119.1(5) . . ? N2 C4 C3 123.5(5) . . ? C4 C5 C6 122.2(6) . . ? C4 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C1 C6 C5 117.5(6) . . ? C1 C6 H6 121.3 . . ? C5 C6 H6 121.3 . . ? O3 C7 N3 124.0(5) . . ? O3 C7 N2 123.9(5) . . ? N3 C7 N2 112.1(5) . . ? C9 C8 C13 119.3(5) . . ? C9 C8 N3 119.7(5) . . ? C13 C8 N3 121.0(5) . . ? C10 C9 C8 121.2(5) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C9 C10 C11 120.0(6) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 119.0(6) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C11 121.3(5) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? C12 C13 C8 119.1(5) . . ? C12 C13 N4 122.2(5) . . ? C8 C13 N4 118.7(5) . . ? O4 C14 N4 123.9(6) . . ? O4 C14 N5 123.9(5) . . ? N4 C14 N5 112.2(5) . . ? C18 C15 C16 120.7(5) . . ? C18 C15 N5 119.8(5) . . ? C16 C15 N5 119.5(4) . . ? C17 C16 C15 121.7(5) . . ? C17 C16 C16 118.5(6) . 3_575 ? C15 C16 C16 119.8(5) . 3_575 ? C19 C17 C16 120.6(5) . . ? C19 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C15 C18 C19 119.6(6) . 3_575 ? C15 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 3_575 . ? C17 C19 C18 120.9(6) . 3_575 ? C17 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 3_575 . ? O5 N6 O6 122.5(8) . . ? O5 N6 C20 118.4(9) . . ? O6 N6 C20 119.1(9) . . ? C23 N7 C26 123.1(6) . . ? C23 N7 H7 118.5 . . ? C26 N7 H7 118.4 . . ? C26 N8 C27 125.6(5) . . ? C26 N8 H8 117.3 . . ? C27 N8 H8 117.2 . . ? C33 N9 C32 124.1(5) . . ? C33 N9 H9 118.1 . . ? C32 N9 H9 117.9 . . ? C33 N10 C34 126.4(5) . . ? C33 N10 H10 116.7 . . ? C34 N10 H10 116.8 . . ? C21 C20 C25 121.0(7) . . ? C21 C20 N6 117.6(8) . . ? C25 C20 N6 121.3(8) . . ? C22 C21 C20 118.5(7) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C21 C22 C23 121.3(7) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? N7 C23 C24 123.8(7) . . ? N7 C23 C22 117.6(6) . . ? C24 C23 C22 118.7(6) . . ? C25 C24 C23 120.6(7) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C20 119.8(7) . . ? C24 C25 H25 120.1 . . ? C20 C25 H25 120.1 . . ? O7 C26 N8 124.1(6) . . ? O7 C26 N7 124.0(6) . . ? N8 C26 N7 111.9(6) . . ? C28 C27 C32 120.3(5) . . ? C28 C27 N8 122.0(5) . . ? C32 C27 N8 117.7(6) . . ? C29 C28 C27 120.4(5) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 120.5(6) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C31 118.9(6) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C32 C31 C30 121.0(5) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C27 118.9(5) . . ? C31 C32 N9 120.5(5) . . ? C27 C32 N9 120.6(5) . . ? O8 C33 N9 125.1(6) . . ? O8 C33 N10 124.5(5) . . ? N9 C33 N10 110.3(5) . . ? C35 C34 N10 122.5(5) . . ? C35 C34 C37 120.5(5) . . ? N10 C34 C37 116.9(5) . . ? C34 C35 C36 120.9(6) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C38 C36 C35 120.2(6) . . ? C38 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C37 118.4(7) 3_656 3_656 ? C38 C37 C34 123.2(5) 3_656 . ? C37 C37 C34 118.4(6) 3_656 . ? C36 C38 C37 121.5(6) . 3_656 ? C36 C38 H38 119.3 . . ? C37 C38 H38 119.3 3_656 . ? C101 N21 C93 110.4(4) . . ? C101 N21 C105 111.6(5) . . ? C93 N21 C105 106.9(4) . . ? C101 N21 C97 105.9(4) . . ? C93 N21 C97 111.3(5) . . ? C105 N21 C97 110.8(4) . . ? C94 C93 N21 117.7(4) . . ? C94 C93 H93A 107.9 . . ? N21 C93 H93A 107.9 . . ? C94 C93 H93B 107.9 . . ? N21 C93 H93B 107.9 . . ? H93A C93 H93B 107.2 . . ? C93 C94 C95 109.2(5) . . ? C93 C94 H94A 109.8 . . ? C95 C94 H94A 109.8 . . ? C93 C94 H94B 109.8 . . ? C95 C94 H94B 109.8 . . ? H94A C94 H94B 108.3 . . ? C96 C95 C94 115.0(5) . . ? C96 C95 H95A 108.5 . . ? C94 C95 H95A 108.5 . . ? C96 C95 H95B 108.5 . . ? C94 C95 H95B 108.5 . . ? H95A C95 H95B 107.5 . . ? C95 C96 H96A 109.5 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C95 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C98 C97 N21 116.5(4) . . ? C98 C97 H97A 108.2 . . ? N21 C97 H97A 108.2 . . ? C98 C97 H97B 108.2 . . ? N21 C97 H97B 108.2 . . ? H97A C97 H97B 107.3 . . ? C97 C98 C99 111.9(5) . . ? C97 C98 H98A 109.2 . . ? C99 C98 H98A 109.2 . . ? C97 C98 H98B 109.2 . . ? C99 C98 H98B 109.2 . . ? H98A C98 H98B 107.9 . . ? C100 C99 C98 115.3(7) . . ? C100 C99 H99A 108.5 . . ? C98 C99 H99A 108.5 . . ? C100 C99 H99B 108.5 . . ? C98 C99 H99B 108.5 . . ? H99A C99 H99B 107.5 . . ? C99 C100 H10B 109.5 . . ? C99 C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C99 C100 H10D 109.5 . . ? H10B C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? N21 C101 C102 115.7(4) . . ? N21 C101 H10E 108.4 . . ? C102 C101 H10E 108.4 . . ? N21 C101 H10F 108.4 . . ? C102 C101 H10F 108.4 . . ? H10E C101 H10F 107.4 . . ? C101 C102 C103 111.2(5) . . ? C101 C102 H10G 109.4 . . ? C103 C102 H10G 109.4 . . ? C101 C102 H10H 109.4 . . ? C103 C102 H10H 109.4 . . ? H10G C102 H10H 108.0 . . ? C104 C103 C102 114.0(5) . . ? C104 C103 H10I 108.7 . . ? C102 C103 H10I 108.7 . . ? C104 C103 H10J 108.7 . . ? C102 C103 H10J 108.7 . . ? H10I C103 H10J 107.6 . . ? C103 C104 H10K 109.5 . . ? C103 C104 H10L 109.5 . . ? H10K C104 H10L 109.5 . . ? C103 C104 H10M 109.5 . . ? H10K C104 H10M 109.5 . . ? H10L C104 H10M 109.5 . . ? C106 C105 N21 115.6(5) . . ? C106 C105 H10N 108.4 . . ? N21 C105 H10N 108.4 . . ? C106 C105 H10O 108.4 . . ? N21 C105 H10O 108.4 . . ? H10N C105 H10O 107.4 . . ? C105 C106 C107 109.9(6) . . ? C105 C106 H10P 109.7 . . ? C107 C106 H10P 109.7 . . ? C105 C106 H10Q 109.7 . . ? C107 C106 H10Q 109.7 . . ? H10P C106 H10Q 108.2 . . ? C106 C107 C108 109.8(9) . . ? C106 C107 H10R 109.7 . . ? C108 C107 H10R 109.7 . . ? C106 C107 H10S 109.7 . . ? C108 C107 H10S 109.7 . . ? H10R C107 H10S 108.2 . . ? C107 C108 H10T 109.5 . . ? C107 C108 H10U 109.5 . . ? H10T C108 H10U 109.5 . . ? C107 C108 H10V 109.5 . . ? H10T C108 H10V 109.5 . . ? H10U C108 H10V 109.5 . . ? C109 N22 C113 111.5(6) . . ? C109 N22 C121 106.0(5) . . ? C113 N22 C121 111.3(5) . . ? C109 N22 C117 111.8(5) . . ? C113 N22 C117 105.7(5) . . ? C121 N22 C117 110.7(6) . . ? N22 C109 C110 114.9(5) . . ? N22 C109 H1 108.5 . . ? C110 C109 H1 108.5 . . ? N22 C109 H10W 108.5 . . ? C110 C109 H10W 108.5 . . ? H1 C109 H10W 107.5 . . ? C111 C110 C109 110.5(6) . . ? C111 C110 H11A 109.6 . . ? C109 C110 H11A 109.6 . . ? C111 C110 H11B 109.6 . . ? C109 C110 H11B 109.6 . . ? H11A C110 H11B 108.1 . . ? C112 C111 C110 112.2(7) . . ? C112 C111 H11C 109.2 . . ? C110 C111 H11C 109.2 . . ? C112 C111 H11D 109.2 . . ? C110 C111 H11D 109.2 . . ? H11C C111 H11D 107.9 . . ? C111 C112 H11E 109.5 . . ? C111 C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C111 C112 H11G 109.5 . . ? H11E C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? C114 C113 N22 116.8(6) . . ? C114 C113 H11H 108.1 . . ? N22 C113 H11H 108.1 . . ? C114 C113 H11I 108.1 . . ? N22 C113 H11I 108.1 . . ? H11H C113 H11I 107.3 . . ? C113 C114 C115 108.1(7) . . ? C113 C114 H11J 110.1 . . ? C115 C114 H11J 110.1 . . ? C113 C114 H11K 110.1 . . ? C115 C114 H11K 110.1 . . ? H11J C114 H11K 108.4 . . ? C116 C115 C114 119.9(10) . . ? C116 C115 H11L 107.3 . . ? C114 C115 H11L 107.3 . . ? C116 C115 H11M 107.3 . . ? C114 C115 H11M 107.3 . . ? H11L C115 H11M 106.9 . . ? C115 C116 H11N 109.5 . . ? C115 C116 H11O 109.5 . . ? H11N C116 H11O 109.5 . . ? C115 C116 H11P 109.5 . . ? H11N C116 H11P 109.5 . . ? H11O C116 H11P 109.5 . . ? C118 C117 N22 115.6(5) . . ? C118 C117 H11Q 108.4 . . ? N22 C117 H11Q 108.4 . . ? C118 C117 H11R 108.4 . . ? N22 C117 H11R 108.4 . . ? H11Q C117 H11R 107.4 . . ? C117 C118 C119 110.0(5) . . ? C117 C118 H11S 109.7 . . ? C119 C118 H11S 109.7 . . ? C117 C118 H11T 109.7 . . ? C119 C118 H11T 109.7 . . ? H11S C118 H11T 108.2 . . ? C120 C119 C118 111.7(6) . . ? C120 C119 H11U 109.3 . . ? C118 C119 H11U 109.3 . . ? C120 C119 H11V 109.3 . . ? C118 C119 H11V 109.3 . . ? H11U C119 H11V 107.9 . . ? C119 C120 H12B 109.5 . . ? C119 C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C119 C120 H12D 109.5 . . ? H12B C120 H12D 109.5 . . ? H12C C120 H12D 109.5 . . ? N22 C121 C122 116.4(6) . . ? N22 C121 H12E 108.2 . . ? C122 C121 H12E 108.2 . . ? N22 C121 H12F 108.2 . . ? C122 C121 H12F 108.2 . . ? H12E C121 H12F 107.3 . . ? C123 C122 C121 110.9(6) . . ? C123 C122 H12G 109.5 . . ? C121 C122 H12G 109.5 . . ? C123 C122 H12H 109.5 . . ? C121 C122 H12H 109.5 . . ? H12G C122 H12H 108.1 . . ? C122 C123 C124 113.8(7) . . ? C122 C123 H12I 108.8 . . ? C124 C123 H12I 108.8 . . ? C122 C123 H12J 108.8 . . ? C124 C123 H12J 108.8 . . ? H12I C123 H12J 107.7 . . ? C123 C124 H12K 109.5 . . ? C123 C124 H12L 109.5 . . ? H12K C124 H12L 109.5 . . ? C123 C124 H12M 109.5 . . ? H12K C124 H12M 109.5 . . ? H12L C124 H12M 109.5 . . ? O17 C77 O18 124.3(5) . . ? O17 C77 C78 117.6(5) . . ? O18 C77 C78 118.1(5) . . ? C83 C78 C79 118.2(5) . . ? C83 C78 C77 121.7(5) . . ? C79 C78 C77 120.1(5) . . ? C80 C79 C78 119.1(5) . . ? C80 C79 H79 120.5 . . ? C78 C79 H79 120.5 . . ? C81 C80 C79 122.2(6) . . ? C81 C80 H80 118.9 . . ? C79 C80 H80 118.9 . . ? C80 C81 C82 117.6(5) . . ? C80 C81 C84 121.4(6) . . ? C82 C81 C84 121.0(5) . . ? C83 C82 C81 120.8(5) . . ? C83 C82 H82 119.6 . . ? C81 C82 H82 119.6 . . ? C82 C83 C78 122.1(6) . . ? C82 C83 H83 118.9 . . ? C78 C83 H83 118.9 . . ? O20 C84 O19 123.2(7) . . ? O20 C84 C81 120.1(7) . . ? O19 C84 C81 116.7(6) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.655 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.054 data_7 _database_code_depnum_ccdc_archive 'CCDC 913115' #TrackingRef 'ACPs-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H102 Cl2 N12 O8' _chemical_formula_weight 1310.54 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 Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.951(7) _cell_length_b 8.8842(15) _cell_length_c 19.048(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.546(2) _cell_angle_gamma 90.00 _cell_volume 7001(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816.0 _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.966 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21659 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6178 _reflns_number_gt 5200 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.1046P)^2^+3.0864P] 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 6139 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1600 _refine_ls_wR_factor_gt 0.1511 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 -0.03244(4) 0.8357(2) -0.20897(8) 0.0494(4) Uani 1 1 d . . . O2 O -0.04388(4) 0.9603(2) -0.11922(9) 0.0603(5) Uani 1 1 d . . . O3 O 0.05569(3) 0.58107(17) 0.14914(7) 0.0382(4) Uani 1 1 d . . . O4 O 0.20280(3) 0.22410(18) 0.20815(7) 0.0394(4) Uani 1 1 d . . . N1 N -0.02901(4) 0.8609(2) -0.14487(10) 0.0390(4) Uani 1 1 d . . . N2 N 0.06048(4) 0.50675(18) 0.03580(8) 0.0303(4) Uani 1 1 d . . . H2 H 0.0714 0.4478 0.0129 0.036 Uiso 1 1 calc R . . N3 N 0.09084(4) 0.39240(18) 0.13119(8) 0.0295(4) Uani 1 1 d . . . H3 H 0.0951 0.3272 0.1007 0.035 Uiso 1 1 calc R . . N4 N 0.15780(3) 0.35321(18) 0.15478(8) 0.0274(4) Uani 1 1 d . . . H4 H 0.1488 0.3940 0.1155 0.033 Uiso 1 1 calc R . . N5 N 0.19508(3) 0.27350(19) 0.08826(8) 0.0296(4) Uani 1 1 d . . . H5 H 0.1811 0.3061 0.0534 0.035 Uiso 1 1 calc R . . N6 N 0.14186(4) 0.87261(16) 0.26087(8) 0.0268(4) Uani 1 1 d . . . Cl1 Cl 0.126399(11) 0.62354(7) 0.48984(2) 0.03997(18) Uani 1 1 d . . . C1 C -0.00614(4) 0.7694(2) -0.09664(10) 0.0320(4) Uani 1 1 d . . . C2 C -0.00332(4) 0.7901(2) -0.02400(11) 0.0349(5) Uani 1 1 d . . . H2A H -0.0160 0.8613 -0.0059 0.042 Uiso 1 1 calc R . . C3 C 0.01857(4) 0.7039(2) 0.02178(10) 0.0331(4) Uani 1 1 d . . . H3A H 0.0206 0.7176 0.0707 0.040 Uiso 1 1 calc R . . C4 C 0.03747(4) 0.5970(2) -0.00563(10) 0.0274(4) Uani 1 1 d . . . C5 C 0.03391(4) 0.5777(2) -0.07966(10) 0.0332(4) Uani 1 1 d . . . H5A H 0.0463 0.5058 -0.0982 0.040 Uiso 1 1 calc R . . C6 C 0.01233(5) 0.6637(3) -0.12510(10) 0.0353(5) Uani 1 1 d . . . H6 H 0.0102 0.6511 -0.1741 0.042 Uiso 1 1 calc R . . C7 C 0.06790(4) 0.5006(2) 0.10901(9) 0.0273(4) Uani 1 1 d . . . C8 C 0.10775(4) 0.3834(2) 0.20192(9) 0.0254(4) Uani 1 1 d . . . C9 C 0.09148(5) 0.3919(2) 0.25985(10) 0.0309(4) Uani 1 1 d . . . H9 H 0.0690 0.3976 0.2522 0.037 Uiso 1 1 calc R . . C10 C 0.10842(5) 0.3919(2) 0.32884(10) 0.0339(5) Uani 1 1 d . . . H10 H 0.0974 0.3974 0.3673 0.041 Uiso 1 1 calc R . . C11 C 0.14192(5) 0.3836(2) 0.34038(10) 0.0311(4) Uani 1 1 d . . . H11 H 0.1534 0.3878 0.3865 0.037 Uiso 1 1 calc R . . C12 C 0.15830(5) 0.3692(2) 0.28359(10) 0.0278(4) Uani 1 1 d . . . H12 H 0.1807 0.3608 0.2920 0.033 Uiso 1 1 calc R . . C13 C 0.14169(4) 0.36721(19) 0.21387(9) 0.0233(4) Uani 1 1 d . . . C14 C 0.18671(4) 0.2795(2) 0.15481(9) 0.0265(4) Uani 1 1 d . . . C15 C 0.22456(4) 0.2187(2) 0.07171(9) 0.0247(4) Uani 1 1 d . . . C16 C 0.24236(4) 0.1097(2) 0.11189(10) 0.0286(4) Uani 1 1 d . . . H16 H 0.2354 0.0718 0.1523 0.034 Uiso 1 1 calc R . . C17 C 0.27104(4) 0.0554(2) 0.09218(10) 0.0288(4) Uani 1 1 d . . . H17 H 0.2827 -0.0187 0.1198 0.035 Uiso 1 1 calc R . . C18 C 0.23525(4) 0.2787(2) 0.00940(9) 0.0226(4) Uani 1 1 d . . . C19 C 0.21783(4) 0.3912(2) -0.03340(9) 0.0260(4) Uani 1 1 d . . . H19 H 0.1987 0.4290 -0.0215 0.031 Uiso 1 1 calc R . . C20 C 0.15535(4) 0.9868(2) 0.31699(10) 0.0284(4) Uani 1 1 d . . . H20A H 0.1387 1.0604 0.3208 0.034 Uiso 1 1 calc R . . H20B H 0.1731 1.0393 0.3009 0.034 Uiso 1 1 calc R . . C21 C 0.16745(5) 0.9230(2) 0.39091(10) 0.0353(5) Uani 1 1 d . . . H21A H 0.1840 0.8482 0.3881 0.042 Uiso 1 1 calc R . . H21B H 0.1498 0.8741 0.4089 0.042 Uiso 1 1 calc R . . C22 C 0.18128(5) 1.0485(3) 0.44187(11) 0.0384(5) Uani 1 1 d . . . H22A H 0.1653 1.1276 0.4403 0.046 Uiso 1 1 calc R . . H22B H 0.1852 1.0087 0.4899 0.046 Uiso 1 1 calc R . . C23 C 0.21229(5) 1.1162(3) 0.42561(13) 0.0480(6) Uani 1 1 d . . . H23A H 0.2282 1.0385 0.4263 0.072 Uiso 1 1 calc R . . H23B H 0.2200 1.1907 0.4608 0.072 Uiso 1 1 calc R . . H23C H 0.2083 1.1623 0.3794 0.072 Uiso 1 1 calc R . . C24 C 0.16737(4) 0.7566(2) 0.25065(11) 0.0322(4) Uani 1 1 d . . . H24A H 0.1586 0.6926 0.2108 0.039 Uiso 1 1 calc R . . H24B H 0.1713 0.6935 0.2928 0.039 Uiso 1 1 calc R . . C25 C 0.19974(5) 0.8185(2) 0.23716(12) 0.0390(5) Uani 1 1 d . . . H25A H 0.2129 0.8458 0.2821 0.047 Uiso 1 1 calc R . . H25B H 0.1961 0.9084 0.2080 0.047 Uiso 1 1 calc R . . C26 C 0.21751(5) 0.7008(3) 0.19937(12) 0.0435(5) Uani 1 1 d . . . H26A H 0.2403 0.7267 0.2058 0.052 Uiso 1 1 calc R . . H26B H 0.2157 0.6035 0.2214 0.052 Uiso 1 1 calc R . . C27 C 0.20459(6) 0.6886(3) 0.12055(13) 0.0519(6) Uani 1 1 d . . . H27A H 0.1823 0.6592 0.1138 0.078 Uiso 1 1 calc R . . H27B H 0.2168 0.6145 0.0996 0.078 Uiso 1 1 calc R . . H27C H 0.2065 0.7843 0.0982 0.078 Uiso 1 1 calc R . . C28 C 0.13119(4) 0.9621(2) 0.19266(9) 0.0286(4) Uani 1 1 d . . . H28A H 0.1160 1.0383 0.2024 0.034 Uiso 1 1 calc R . . H28B H 0.1499 1.0141 0.1809 0.034 Uiso 1 1 calc R . . C29 C 0.11568(5) 0.8736(2) 0.12750(10) 0.0333(4) Uani 1 1 d . . . H29A H 0.0944 0.8394 0.1337 0.040 Uiso 1 1 calc R . . H29B H 0.1287 0.7860 0.1212 0.040 Uiso 1 1 calc R . . C30 C 0.11309(6) 0.9756(3) 0.06240(11) 0.0484(6) Uani 1 1 d . . . H30A H 0.1004 1.0638 0.0698 0.058 Uiso 1 1 calc R . . H30B H 0.1345 1.0093 0.0569 0.058 Uiso 1 1 calc R . . C31 C 0.09743(7) 0.8961(4) -0.00547(13) 0.0727(9) Uani 1 1 d . . . H31A H 0.1096 0.8072 -0.0123 0.109 Uiso 1 1 calc R . . H31B H 0.0972 0.9624 -0.0454 0.109 Uiso 1 1 calc R . . H31C H 0.0757 0.8684 -0.0015 0.109 Uiso 1 1 calc R . . C32 C 0.11348(4) 0.7861(2) 0.28175(10) 0.0293(4) Uani 1 1 d . . . H32A H 0.1057 0.7153 0.2440 0.035 Uiso 1 1 calc R . . H32B H 0.1213 0.7281 0.3243 0.035 Uiso 1 1 calc R . . C33 C 0.08518(5) 0.8810(2) 0.29580(11) 0.0338(5) Uani 1 1 d . . . H33A H 0.0925 0.9537 0.3330 0.041 Uiso 1 1 calc R . . H33B H 0.0762 0.9357 0.2530 0.041 Uiso 1 1 calc R . . C34 C 0.05936(5) 0.7815(3) 0.31847(13) 0.0448(5) Uani 1 1 d . . . H34A H 0.0690 0.7207 0.3587 0.054 Uiso 1 1 calc R . . H34B H 0.0511 0.7138 0.2797 0.054 Uiso 1 1 calc R . . C35 C 0.03140(6) 0.8709(3) 0.33895(14) 0.0584(7) Uani 1 1 d . . . H35A H 0.0389 0.9278 0.3813 0.088 Uiso 1 1 calc R . . H35B H 0.0147 0.8030 0.3475 0.088 Uiso 1 1 calc R . . H35C H 0.0230 0.9382 0.3009 0.088 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 0.0484(9) 0.0609(11) 0.0327(9) 0.0095(8) -0.0114(7) 0.0042(8) O2 0.0592(10) 0.0665(12) 0.0516(10) 0.0080(9) -0.0012(8) 0.0313(9) O3 0.0402(7) 0.0501(9) 0.0222(7) -0.0037(6) -0.0011(6) 0.0136(7) O4 0.0363(7) 0.0617(10) 0.0176(7) 0.0081(6) -0.0028(6) 0.0155(7) N1 0.0332(8) 0.0434(10) 0.0368(11) 0.0092(8) -0.0052(8) 0.0027(8) N2 0.0303(8) 0.0394(9) 0.0197(8) -0.0031(7) -0.0002(6) 0.0078(7) N3 0.0304(8) 0.0385(9) 0.0168(8) -0.0056(7) -0.0042(6) 0.0042(7) N4 0.0293(8) 0.0370(9) 0.0139(7) 0.0046(6) -0.0022(6) 0.0049(6) N5 0.0268(7) 0.0440(10) 0.0158(7) 0.0071(7) -0.0026(6) 0.0078(7) N6 0.0300(8) 0.0241(8) 0.0247(8) 0.0027(6) 0.0002(6) -0.0012(6) Cl1 0.0374(3) 0.0655(4) 0.0157(3) -0.0064(2) 0.0004(2) -0.0181(2) C1 0.0277(9) 0.0369(11) 0.0289(10) 0.0064(8) -0.0027(8) -0.0016(8) C2 0.0313(9) 0.0404(11) 0.0321(11) 0.0000(9) 0.0029(8) 0.0044(8) C3 0.0317(9) 0.0431(12) 0.0233(10) -0.0026(8) 0.0012(8) 0.0036(8) C4 0.0243(8) 0.0339(10) 0.0218(9) 0.0009(8) -0.0031(7) -0.0030(7) C5 0.0344(10) 0.0419(11) 0.0215(10) -0.0032(8) -0.0005(8) 0.0046(8) C6 0.0362(10) 0.0469(12) 0.0203(9) 0.0009(9) -0.0031(8) 0.0029(9) C7 0.0243(8) 0.0348(10) 0.0212(9) -0.0024(8) -0.0014(7) -0.0023(7) C8 0.0306(9) 0.0259(9) 0.0173(9) -0.0013(7) -0.0030(7) -0.0003(7) C9 0.0339(9) 0.0344(10) 0.0240(10) 0.0006(8) 0.0038(8) 0.0010(8) C10 0.0492(11) 0.0342(11) 0.0191(9) 0.0024(8) 0.0080(8) 0.0051(9) C11 0.0476(11) 0.0266(10) 0.0157(9) 0.0003(7) -0.0045(8) 0.0025(8) C12 0.0349(9) 0.0261(9) 0.0195(9) 0.0005(7) -0.0041(8) 0.0001(7) C13 0.0306(9) 0.0212(9) 0.0164(9) 0.0010(7) -0.0013(7) -0.0018(7) C14 0.0243(8) 0.0330(10) 0.0197(9) 0.0013(8) -0.0036(7) -0.0009(7) C15 0.0250(8) 0.0299(10) 0.0168(8) -0.0018(7) -0.0036(7) -0.0010(7) C16 0.0319(9) 0.0336(10) 0.0186(9) 0.0038(8) -0.0004(8) -0.0002(8) C17 0.0300(9) 0.0310(10) 0.0217(9) 0.0045(8) -0.0062(7) 0.0046(8) C18 0.0237(8) 0.0254(9) 0.0154(8) -0.0024(7) -0.0062(7) -0.0023(7) C19 0.0241(8) 0.0320(10) 0.0191(9) -0.0002(7) -0.0048(7) 0.0034(7) C20 0.0337(9) 0.0230(9) 0.0256(10) 0.0026(8) -0.0034(8) -0.0016(7) C21 0.0437(10) 0.0327(10) 0.0262(10) 0.0079(9) -0.0037(9) -0.0014(9) C22 0.0444(11) 0.0424(12) 0.0240(10) 0.0059(9) -0.0072(8) 0.0016(9) C23 0.0457(12) 0.0486(14) 0.0424(13) 0.0080(10) -0.0145(10) -0.0054(10) C24 0.0349(9) 0.0267(10) 0.0340(11) 0.0006(8) 0.0031(8) 0.0019(8) C25 0.0352(10) 0.0381(11) 0.0431(12) -0.0026(10) 0.0041(9) -0.0015(9) C26 0.0343(10) 0.0502(13) 0.0448(13) -0.0021(11) 0.0029(9) 0.0044(9) C27 0.0487(12) 0.0626(16) 0.0448(14) -0.0055(12) 0.0096(11) -0.0035(12) C28 0.0340(9) 0.0277(9) 0.0229(9) 0.0047(8) 0.0015(8) -0.0021(7) C29 0.0337(9) 0.0371(11) 0.0268(10) -0.0026(8) -0.0013(8) -0.0022(8) C30 0.0469(12) 0.0690(16) 0.0266(11) 0.0071(11) -0.0012(9) -0.0201(11) C31 0.0634(16) 0.122(3) 0.0273(12) 0.0044(14) -0.0068(12) -0.0395(17) C32 0.0335(9) 0.0280(10) 0.0257(10) 0.0044(8) 0.0024(8) -0.0038(8) C33 0.0369(10) 0.0380(11) 0.0254(10) 0.0056(8) 0.0019(8) 0.0031(8) C34 0.0401(11) 0.0529(14) 0.0426(13) 0.0045(11) 0.0102(10) -0.0015(10) C35 0.0456(13) 0.086(2) 0.0468(15) 0.0135(13) 0.0161(12) 0.0077(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 N1 1.226(2) . ? O2 N1 1.228(2) . ? O3 C7 1.220(2) . ? O4 C14 1.226(2) . ? N1 C1 1.461(3) . ? N2 C7 1.379(2) . ? N2 C4 1.394(2) . ? N3 C7 1.376(2) . ? N3 C8 1.417(2) . ? N4 C14 1.379(2) . ? N4 C13 1.411(2) . ? N5 C14 1.371(2) . ? N5 C15 1.413(2) . ? N6 C20 1.513(2) . ? N6 C24 1.521(2) . ? N6 C32 1.524(2) . ? N6 C28 1.526(2) . ? C1 C2 1.381(3) . ? C1 C6 1.384(3) . ? C2 C3 1.387(3) . ? C3 C4 1.393(3) . ? C4 C5 1.404(3) . ? C5 C6 1.376(3) . ? C8 C9 1.393(3) . ? C8 C13 1.411(2) . ? C9 C10 1.387(3) . ? C10 C11 1.388(3) . ? C11 C12 1.380(3) . ? C12 C13 1.394(3) . ? C15 C16 1.375(3) . ? C15 C18 1.439(2) . ? C16 C17 1.404(3) . ? C17 C19 1.367(3) 7 ? C18 C19 1.415(3) . ? C18 C18 1.438(3) 7 ? C19 C17 1.368(3) 7 ? C20 C21 1.525(3) . ? C21 C22 1.528(3) . ? C22 C23 1.511(3) . ? C24 C25 1.526(3) . ? C25 C26 1.531(3) . ? C26 C27 1.513(3) . ? C28 C29 1.522(3) . ? C29 C30 1.525(3) . ? C30 C31 1.524(3) . ? C32 C33 1.516(3) . ? C33 C34 1.516(3) . ? C34 C35 1.520(3) . ? 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 N1 O2 122.96(18) . . ? O1 N1 C1 118.75(17) . . ? O2 N1 C1 118.28(18) . . ? C7 N2 C4 127.89(15) . . ? C7 N3 C8 123.07(15) . . ? C14 N4 C13 125.40(15) . . ? C14 N5 C15 125.97(15) . . ? C20 N6 C24 110.85(14) . . ? C20 N6 C32 111.73(14) . . ? C24 N6 C32 106.75(14) . . ? C20 N6 C28 105.95(13) . . ? C24 N6 C28 110.94(14) . . ? C32 N6 C28 110.70(14) . . ? C2 C1 C6 121.45(18) . . ? C2 C1 N1 119.64(18) . . ? C6 C1 N1 118.91(18) . . ? C1 C2 C3 119.64(18) . . ? C2 C3 C4 119.94(18) . . ? N2 C4 C3 124.30(17) . . ? N2 C4 C5 116.51(16) . . ? C3 C4 C5 119.18(17) . . ? C6 C5 C4 120.88(18) . . ? C5 C6 C1 118.90(18) . . ? O3 C7 N3 124.20(16) . . ? O3 C7 N2 124.25(17) . . ? N3 C7 N2 111.55(15) . . ? C9 C8 C13 119.45(17) . . ? C9 C8 N3 121.09(16) . . ? C13 C8 N3 119.45(16) . . ? C10 C9 C8 120.61(18) . . ? C9 C10 C11 119.78(17) . . ? C12 C11 C10 120.23(18) . . ? C11 C12 C13 120.84(17) . . ? C12 C13 N4 122.10(16) . . ? C12 C13 C8 118.94(16) . . ? N4 C13 C8 118.94(16) . . ? O4 C14 N5 124.10(16) . . ? O4 C14 N4 123.67(16) . . ? N5 C14 N4 112.22(15) . . ? C16 C15 N5 122.23(16) . . ? C16 C15 C18 120.35(15) . . ? N5 C15 C18 117.41(15) . . ? C15 C16 C17 120.22(16) . . ? C19 C17 C16 121.60(17) 7 . ? C19 C18 C15 122.38(15) . . ? C19 C18 C18 119.38(19) . 7 ? C15 C18 C18 118.24(19) . 7 ? C17 C19 C18 120.20(16) 7 . ? N6 C20 C21 115.57(15) . . ? C20 C21 C22 110.41(16) . . ? C23 C22 C21 114.15(18) . . ? N6 C24 C25 116.23(16) . . ? C24 C25 C26 110.46(18) . . ? C27 C26 C25 113.16(19) . . ? C29 C28 N6 116.78(16) . . ? C28 C29 C30 108.60(17) . . ? C31 C30 C29 112.1(2) . . ? C33 C32 N6 115.74(16) . . ? C34 C33 C32 110.09(17) . . ? C33 C34 C35 112.7(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.326 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.067 data_8 _database_code_depnum_ccdc_archive 'CCDC 913116' #TrackingRef 'ACPs-R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H102 Br2 N12 O8' _chemical_formula_weight 1399.46 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9484(19) _cell_length_b 9.473(2) _cell_length_c 21.594(5) _cell_angle_alpha 83.826(3) _cell_angle_beta 84.847(2) _cell_angle_gamma 80.815(3) _cell_volume 1791.6(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4350 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.78 _exptl_crystal_description plate _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _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_000 740 _exptl_absorpt_coefficient_mu 1.192 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7162 _exptl_absorpt_correction_T_max 0.8901 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10718 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6119 _reflns_number_gt 5100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.1000P)^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 6119 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.001 _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 0.8590(5) 1.2530(5) -0.08385(17) 0.0895(14) Uani 1 1 d . . . O2 O 0.6720(5) 1.4152(5) -0.05746(18) 0.0797(12) Uani 1 1 d . . . O3 O 0.6588(3) 0.6763(3) 0.11468(12) 0.0418(7) Uani 1 1 d . . . O4 O 0.6155(3) 0.5559(3) 0.40536(11) 0.0368(6) Uani 1 1 d . . . N1 N 0.7412(5) 1.2915(5) -0.05255(17) 0.0593(11) Uani 1 1 d . . . N2 N 0.5055(3) 0.8927(3) 0.12697(13) 0.0314(7) Uani 1 1 d . . . H2A H 0.4232 0.9305 0.1484 0.038 Uiso 1 1 d R . . N3 N 0.4694(3) 0.6967(3) 0.19321(13) 0.0319(7) Uani 1 1 d . . . H3A H 0.3951 0.7577 0.2092 0.038 Uiso 1 1 d R . . N4 N 0.4865(3) 0.6569(3) 0.32062(12) 0.0275(6) Uani 1 1 d . . . H4A H 0.4426 0.7390 0.3027 0.033 Uiso 1 1 d R . . N5 N 0.5069(3) 0.7924(3) 0.39954(13) 0.0319(7) Uani 1 1 d . . . H5A H 0.4529 0.8585 0.3755 0.038 Uiso 1 1 d R . . C1 C 0.6826(5) 1.1861(5) -0.00526(17) 0.0433(10) Uani 1 1 d . . . C2 C 0.7588(5) 1.0492(5) 0.00166(17) 0.0455(11) Uani 1 1 d . . . H2 H 0.8475 1.0242 -0.0232 0.055 Uiso 1 1 calc R . . C3 C 0.7055(4) 0.9470(5) 0.04518(16) 0.0388(9) Uani 1 1 d . . . H3 H 0.7580 0.8541 0.0503 0.047 Uiso 1 1 calc R . . C4 C 0.5711(4) 0.9873(4) 0.08103(14) 0.0296(8) Uani 1 1 d . . . C5 C 0.4953(5) 1.1274(4) 0.07384(17) 0.0378(9) Uani 1 1 d . . . H5 H 0.4067 1.1538 0.0985 0.045 Uiso 1 1 calc R . . C6 C 0.5512(5) 1.2285(5) 0.02999(17) 0.0451(10) Uani 1 1 d . . . H6 H 0.5008 1.3223 0.0248 0.054 Uiso 1 1 calc R . . C7 C 0.5550(4) 0.7480(4) 0.14208(15) 0.0312(8) Uani 1 1 d . . . C8 C 0.4907(4) 0.5556(4) 0.22253(15) 0.0279(8) Uani 1 1 d . . . C9 C 0.5014(4) 0.4372(4) 0.18884(17) 0.0386(9) Uani 1 1 d . . . H9 H 0.5027 0.4503 0.1455 0.046 Uiso 1 1 calc R . . C10 C 0.5100(4) 0.3002(4) 0.21888(18) 0.0384(9) Uani 1 1 d . . . H10 H 0.5184 0.2217 0.1957 0.046 Uiso 1 1 calc R . . C11 C 0.5061(4) 0.2793(4) 0.28339(18) 0.0347(8) Uani 1 1 d . . . H11 H 0.5089 0.1872 0.3035 0.042 Uiso 1 1 calc R . . C12 C 0.4981(4) 0.3964(4) 0.31814(16) 0.0304(8) Uani 1 1 d . . . H12 H 0.4959 0.3823 0.3615 0.036 Uiso 1 1 calc R . . C13 C 0.4934(4) 0.5342(4) 0.28805(15) 0.0268(7) Uani 1 1 d . . . C14 C 0.5421(4) 0.6591(4) 0.37816(15) 0.0272(8) Uani 1 1 d . . . C15 C 0.5466(4) 0.8362(4) 0.45536(14) 0.0251(7) Uani 1 1 d . . . C16 C 0.6478(4) 0.7487(4) 0.49339(16) 0.0377(9) Uani 1 1 d . . . H16 H 0.6881 0.6564 0.4836 0.045 Uiso 1 1 calc R . . C17 C 0.6884(5) 0.8011(4) 0.54670(17) 0.0388(9) Uani 1 1 d . . . H17 H 0.7597 0.7436 0.5709 0.047 Uiso 1 1 calc R . . C18 C 0.6279(4) 0.9326(4) 0.56453(15) 0.0314(8) Uani 1 1 d . . . H18 H 0.6564 0.9627 0.6007 0.038 Uiso 1 1 calc R . . C19 C 0.4787(3) 0.9760(4) 0.47200(14) 0.0236(7) Uani 1 1 d . . . N11 N 0.9827(3) 0.5097(3) 0.27496(12) 0.0258(6) Uani 1 1 d . . . C39 C 1.0706(4) 0.4529(4) 0.21690(16) 0.0321(8) Uani 1 1 d . . . H39A H 1.1374 0.5208 0.1996 0.039 Uiso 1 1 calc R . . H39B H 1.1340 0.3633 0.2294 0.039 Uiso 1 1 calc R . . C40 C 0.9755(4) 0.4270(4) 0.16591(16) 0.0367(9) Uani 1 1 d . . . H40A H 0.9251 0.5182 0.1476 0.044 Uiso 1 1 calc R . . H40B H 0.8982 0.3702 0.1836 0.044 Uiso 1 1 calc R . . C41 C 1.0751(5) 0.3483(5) 0.11552(18) 0.0479(11) Uani 1 1 d . . . H41A H 1.1209 0.2550 0.1336 0.057 Uiso 1 1 calc R . . H41B H 1.1562 0.4024 0.0998 0.057 Uiso 1 1 calc R . . C42 C 0.9840(7) 0.3287(6) 0.0616(2) 0.0668(15) Uani 1 1 d . . . H42A H 0.9294 0.4198 0.0467 0.100 Uiso 1 1 calc R . . H42B H 0.9136 0.2634 0.0757 0.100 Uiso 1 1 calc R . . H42C H 1.0518 0.2904 0.0283 0.100 Uiso 1 1 calc R . . C43 C 0.8726(4) 0.6451(4) 0.25812(15) 0.0275(8) Uani 1 1 d . . . H43A H 0.8023 0.6224 0.2304 0.033 Uiso 1 1 calc R . . H43B H 0.8142 0.6740 0.2959 0.033 Uiso 1 1 calc R . . C44 C 0.9451(4) 0.7714(4) 0.22712(18) 0.0367(9) Uani 1 1 d . . . H44A H 0.9901 0.7499 0.1860 0.044 Uiso 1 1 calc R . . H44B H 1.0252 0.7878 0.2517 0.044 Uiso 1 1 calc R . . C45 C 0.8274(5) 0.9060(4) 0.2212(2) 0.0460(10) Uani 1 1 d . . . H45A H 0.7444 0.8865 0.1990 0.055 Uiso 1 1 calc R . . H45B H 0.7866 0.9293 0.2626 0.055 Uiso 1 1 calc R . . C46 C 0.8905(5) 1.0337(5) 0.1873(2) 0.0511(11) Uani 1 1 d . . . H46A H 0.9293 1.0120 0.1460 0.077 Uiso 1 1 calc R . . H46B H 0.9708 1.0552 0.2096 0.077 Uiso 1 1 calc R . . H46C H 0.8114 1.1151 0.1848 0.077 Uiso 1 1 calc R . . C47 C 1.0981(4) 0.5386(4) 0.31749(15) 0.0279(7) Uani 1 1 d . . . H47A H 1.1585 0.6063 0.2947 0.033 Uiso 1 1 calc R . . H47B H 1.1659 0.4496 0.3268 0.033 Uiso 1 1 calc R . . C48 C 1.0345(4) 0.5976(4) 0.37925(15) 0.0310(8) Uani 1 1 d . . . H48A H 0.9651 0.6861 0.3711 0.037 Uiso 1 1 calc R . . H48B H 0.9786 0.5288 0.4040 0.037 Uiso 1 1 calc R . . C49 C 1.1622(5) 0.6258(5) 0.41498(18) 0.0470(11) Uani 1 1 d . . . H49A H 1.2156 0.6961 0.3900 0.056 Uiso 1 1 calc R . . H49B H 1.2334 0.5376 0.4207 0.056 Uiso 1 1 calc R . . C50 C 1.1136(5) 0.6795(5) 0.47821(17) 0.0489(11) Uani 1 1 d . . . H50A H 1.0692 0.6070 0.5048 0.073 Uiso 1 1 calc R . . H50B H 1.0402 0.7650 0.4734 0.073 Uiso 1 1 calc R . . H50C H 1.2003 0.7007 0.4965 0.073 Uiso 1 1 calc R . . C51 C 0.8858(3) 0.4009(4) 0.30806(15) 0.0252(7) Uani 1 1 d . . . H51A H 0.8216 0.4466 0.3411 0.030 Uiso 1 1 calc R . . H51B H 0.8194 0.3795 0.2783 0.030 Uiso 1 1 calc R . . C52 C 0.9688(4) 0.2594(4) 0.33633(17) 0.0335(8) Uani 1 1 d . . . H52A H 1.0295 0.2770 0.3689 0.040 Uiso 1 1 calc R . . H52B H 1.0362 0.2125 0.3044 0.040 Uiso 1 1 calc R . . C53 C 0.8534(4) 0.1622(4) 0.36373(18) 0.0369(9) Uani 1 1 d . . . H53A H 0.7807 0.2134 0.3927 0.044 Uiso 1 1 calc R . . H53B H 0.7982 0.1395 0.3303 0.044 Uiso 1 1 calc R . . C54 C 0.9278(5) 0.0239(5) 0.3974(2) 0.0479(10) Uani 1 1 d . . . H54A H 0.9734 0.0453 0.4332 0.072 Uiso 1 1 calc R . . H54B H 1.0045 -0.0241 0.3697 0.072 Uiso 1 1 calc R . . H54C H 0.8527 -0.0371 0.4106 0.072 Uiso 1 1 calc R . . Br1 Br 0.29284(4) 0.97294(4) 0.267242(15) 0.03414(16) 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 O1 0.124(3) 0.094(3) 0.057(2) -0.012(2) 0.038(2) -0.058(3) O2 0.087(3) 0.075(3) 0.079(3) 0.036(2) -0.023(2) -0.038(2) O3 0.0417(15) 0.0396(17) 0.0407(14) -0.0078(12) 0.0082(12) 0.0008(13) O4 0.0452(15) 0.0314(16) 0.0329(13) -0.0114(11) -0.0115(11) 0.0071(12) N1 0.083(3) 0.068(3) 0.038(2) 0.004(2) -0.014(2) -0.046(3) N2 0.0313(15) 0.0335(19) 0.0284(14) -0.0016(13) -0.0024(12) -0.0028(13) N3 0.0391(16) 0.0258(17) 0.0289(14) -0.0036(12) -0.0010(12) 0.0003(13) N4 0.0358(15) 0.0224(16) 0.0253(13) -0.0033(12) -0.0070(12) -0.0040(13) N5 0.0397(17) 0.0251(17) 0.0308(15) -0.0080(13) -0.0092(13) 0.0022(13) C1 0.062(3) 0.044(3) 0.0310(19) 0.0016(18) -0.0107(18) -0.029(2) C2 0.046(2) 0.063(3) 0.032(2) -0.0092(19) -0.0010(17) -0.023(2) C3 0.040(2) 0.048(3) 0.0320(19) -0.0060(17) -0.0046(16) -0.0160(19) C4 0.0355(18) 0.036(2) 0.0214(15) -0.0051(15) -0.0056(14) -0.0135(16) C5 0.044(2) 0.034(2) 0.0350(19) 0.0020(17) -0.0060(16) -0.0086(18) C6 0.060(3) 0.040(3) 0.040(2) -0.0008(18) -0.0154(19) -0.018(2) C7 0.0339(19) 0.038(2) 0.0242(16) -0.0060(15) -0.0054(14) -0.0094(17) C8 0.0258(16) 0.029(2) 0.0329(17) -0.0096(15) -0.0084(14) -0.0071(15) C9 0.048(2) 0.034(2) 0.0347(19) -0.0107(17) -0.0097(16) 0.0003(18) C10 0.041(2) 0.031(2) 0.048(2) -0.0151(18) -0.0153(17) -0.0070(17) C11 0.0351(19) 0.024(2) 0.049(2) -0.0070(16) -0.0104(16) -0.0104(16) C12 0.0260(17) 0.029(2) 0.0370(18) -0.0010(15) -0.0060(14) -0.0072(15) C13 0.0215(16) 0.026(2) 0.0348(17) -0.0079(15) -0.0019(13) -0.0072(14) C14 0.0255(16) 0.031(2) 0.0252(16) -0.0067(15) -0.0002(13) -0.0017(15) C15 0.0276(16) 0.0263(19) 0.0231(15) -0.0064(14) -0.0006(13) -0.0076(14) C16 0.042(2) 0.035(2) 0.0357(19) -0.0094(17) -0.0113(16) 0.0040(18) C17 0.047(2) 0.036(2) 0.0348(19) -0.0071(17) -0.0189(16) 0.0008(18) C18 0.0349(19) 0.033(2) 0.0282(17) -0.0074(15) -0.0144(14) -0.0026(16) C19 0.0224(15) 0.0279(19) 0.0222(15) -0.0047(13) -0.0013(12) -0.0072(14) N11 0.0230(13) 0.0233(16) 0.0318(14) -0.0036(12) -0.0019(11) -0.0046(12) C39 0.0273(17) 0.032(2) 0.0351(18) -0.0056(16) 0.0064(14) -0.0036(16) C40 0.045(2) 0.033(2) 0.0344(19) -0.0095(16) -0.0033(16) -0.0099(18) C41 0.061(3) 0.043(3) 0.044(2) -0.0139(19) 0.0042(19) -0.016(2) C42 0.120(5) 0.047(3) 0.038(2) -0.012(2) 0.001(3) -0.026(3) C43 0.0241(16) 0.026(2) 0.0322(17) -0.0059(15) 0.0028(13) -0.0027(14) C44 0.043(2) 0.027(2) 0.040(2) 0.0001(16) -0.0020(16) -0.0068(17) C45 0.045(2) 0.028(2) 0.066(3) 0.0052(19) -0.020(2) -0.0075(19) C46 0.053(3) 0.034(3) 0.068(3) 0.003(2) -0.024(2) -0.007(2) C47 0.0256(16) 0.028(2) 0.0333(17) -0.0049(15) -0.0095(14) -0.0088(15) C48 0.0302(18) 0.035(2) 0.0310(17) -0.0081(15) -0.0029(14) -0.0114(16) C49 0.043(2) 0.057(3) 0.043(2) -0.017(2) -0.0136(18) 0.001(2) C50 0.062(3) 0.052(3) 0.036(2) -0.0021(19) -0.0150(19) -0.012(2) C51 0.0179(15) 0.0254(19) 0.0323(17) -0.0027(14) -0.0026(13) -0.0029(14) C52 0.0275(18) 0.029(2) 0.043(2) -0.0010(16) -0.0077(15) -0.0005(16) C53 0.042(2) 0.029(2) 0.041(2) -0.0012(17) -0.0075(16) -0.0074(17) C54 0.053(3) 0.030(2) 0.059(3) 0.0080(19) -0.009(2) -0.007(2) Br1 0.0379(2) 0.0283(2) 0.0362(2) -0.00832(15) -0.00664(15) 0.00068(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 N1 1.226(6) . ? O2 N1 1.233(6) . ? O3 C7 1.209(4) . ? O4 C14 1.214(4) . ? N1 C1 1.472(5) . ? N2 C7 1.385(5) . ? N2 C4 1.416(5) . ? N2 H2A 0.8799 . ? N3 C7 1.376(4) . ? N3 C8 1.407(5) . ? N3 H3A 0.8800 . ? N4 C14 1.383(4) . ? N4 C13 1.412(4) . ? N4 H4A 0.8798 . ? N5 C14 1.370(5) . ? N5 C15 1.408(4) . ? N5 H5A 0.8800 . ? C1 C2 1.365(6) . ? C1 C6 1.370(6) . ? C2 C3 1.385(6) . ? C2 H2 0.9300 . ? C3 C4 1.393(5) . ? C3 H3 0.9300 . ? C4 C5 1.390(6) . ? C5 C6 1.392(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.388(5) . ? C8 C13 1.409(5) . ? C9 C10 1.381(6) . ? C9 H9 0.9300 . ? C10 C11 1.384(5) . ? C10 H10 0.9300 . ? C11 C12 1.394(5) . ? C11 H11 0.9300 . ? C12 C13 1.391(5) . ? C12 H12 0.9300 . ? C15 C16 1.389(5) . ? C15 C19 1.434(5) . ? C16 C17 1.400(5) . ? C16 H16 0.9300 . ? C17 C18 1.358(5) . ? C17 H17 0.9300 . ? C18 C19 1.416(5) 2_676 ? C18 H18 0.9300 . ? C19 C18 1.416(5) 2_676 ? C19 C19 1.439(6) 2_676 ? N11 C47 1.517(4) . ? N11 C43 1.519(4) . ? N11 C39 1.521(4) . ? N11 C51 1.530(4) . ? C39 C40 1.513(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.524(5) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.524(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.516(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.520(6) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.507(6) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.529(4) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.508(5) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.512(5) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.520(5) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.530(5) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.513(6) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 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 O1 N1 O2 123.3(4) . . ? O1 N1 C1 118.3(5) . . ? O2 N1 C1 118.4(4) . . ? C7 N2 C4 127.8(3) . . ? C7 N2 H2A 116.3 . . ? C4 N2 H2A 115.9 . . ? C7 N3 C8 125.9(3) . . ? C7 N3 H3A 117.0 . . ? C8 N3 H3A 117.1 . . ? C14 N4 C13 125.8(3) . . ? C14 N4 H4A 117.2 . . ? C13 N4 H4A 117.0 . . ? C14 N5 C15 127.9(3) . . ? C14 N5 H5A 116.1 . . ? C15 N5 H5A 116.1 . . ? C2 C1 C6 122.0(4) . . ? C2 C1 N1 119.4(4) . . ? C6 C1 N1 118.6(4) . . ? C1 C2 C3 120.8(4) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C2 C3 C4 118.2(4) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C5 C4 C3 120.4(4) . . ? C5 C4 N2 116.2(3) . . ? C3 C4 N2 123.4(4) . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 118.1(4) . . ? C1 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? O3 C7 N3 124.4(4) . . ? O3 C7 N2 125.2(3) . . ? N3 C7 N2 110.3(3) . . ? C9 C8 N3 121.6(3) . . ? C9 C8 C13 119.1(3) . . ? N3 C8 C13 119.2(3) . . ? C10 C9 C8 120.8(3) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 120.0(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 119.8(3) . . ? C12 C13 N4 122.7(3) . . ? C8 C13 N4 117.5(3) . . ? O4 C14 N5 124.7(3) . . ? O4 C14 N4 123.6(3) . . ? N5 C14 N4 111.6(3) . . ? C16 C15 N5 121.9(3) . . ? C16 C15 C19 120.5(3) . . ? N5 C15 C19 117.6(3) . . ? C15 C16 C17 119.2(4) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 122.7(4) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C17 C18 C19 120.0(3) . 2_676 ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 2_676 . ? C18 C19 C15 122.5(3) 2_676 . ? C18 C19 C19 119.3(4) 2_676 2_676 ? C15 C19 C19 118.3(4) . 2_676 ? C47 N11 C43 111.1(3) . . ? C47 N11 C39 107.2(2) . . ? C43 N11 C39 111.0(3) . . ? C47 N11 C51 110.6(3) . . ? C43 N11 C51 106.0(2) . . ? C39 N11 C51 111.0(3) . . ? C40 C39 N11 115.8(3) . . ? C40 C39 H39A 108.3 . . ? N11 C39 H39A 108.3 . . ? C40 C39 H39B 108.3 . . ? N11 C39 H39B 108.3 . . ? H39A C39 H39B 107.4 . . ? C39 C40 C41 110.3(3) . . ? C39 C40 H40A 109.6 . . ? C41 C40 H40A 109.6 . . ? C39 C40 H40B 109.6 . . ? C41 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? C40 C41 C42 111.5(4) . . ? C40 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? C40 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 108.0 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N11 115.3(3) . . ? C44 C43 H43A 108.4 . . ? N11 C43 H43A 108.4 . . ? C44 C43 H43B 108.4 . . ? N11 C43 H43B 108.4 . . ? H43A C43 H43B 107.5 . . ? C43 C44 C45 110.5(3) . . ? C43 C44 H44A 109.6 . . ? C45 C44 H44A 109.6 . . ? C43 C44 H44B 109.6 . . ? C45 C44 H44B 109.6 . . ? H44A C44 H44B 108.1 . . ? C46 C45 C44 113.1(4) . . ? C46 C45 H45A 109.0 . . ? C44 C45 H45A 109.0 . . ? C46 C45 H45B 109.0 . . ? C44 C45 H45B 109.0 . . ? H45A C45 H45B 107.8 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N11 C47 C48 116.3(3) . . ? N11 C47 H47A 108.2 . . ? C48 C47 H47A 108.2 . . ? N11 C47 H47B 108.2 . . ? C48 C47 H47B 108.2 . . ? H47A C47 H47B 107.4 . . ? C49 C48 C47 110.0(3) . . ? C49 C48 H48A 109.7 . . ? C47 C48 H48A 109.7 . . ? C49 C48 H48B 109.7 . . ? C47 C48 H48B 109.7 . . ? H48A C48 H48B 108.2 . . ? C48 C49 C50 114.8(3) . . ? C48 C49 H49A 108.6 . . ? C50 C49 H49A 108.6 . . ? C48 C49 H49B 108.6 . . ? C50 C49 H49B 108.6 . . ? H49A C49 H49B 107.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 N11 117.3(3) . . ? C52 C51 H51A 108.0 . . ? N11 C51 H51A 108.0 . . ? C52 C51 H51B 108.0 . . ? N11 C51 H51B 108.0 . . ? H51A C51 H51B 107.2 . . ? C51 C52 C53 109.5(3) . . ? C51 C52 H52A 109.8 . . ? C53 C52 H52A 109.8 . . ? C51 C52 H52B 109.8 . . ? C53 C52 H52B 109.8 . . ? H52A C52 H52B 108.2 . . ? C54 C53 C52 112.3(3) . . ? C54 C53 H53A 109.1 . . ? C52 C53 H53A 109.1 . . ? C54 C53 H53B 109.1 . . ? C52 C53 H53B 109.1 . . ? H53A C53 H53B 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 N1 C1 C2 -1.1(6) . . . . ? O2 N1 C1 C2 -179.0(4) . . . . ? O1 N1 C1 C6 179.8(4) . . . . ? O2 N1 C1 C6 1.9(5) . . . . ? C6 C1 C2 C3 -0.1(6) . . . . ? N1 C1 C2 C3 -179.2(3) . . . . ? C1 C2 C3 C4 0.9(5) . . . . ? C2 C3 C4 C5 -1.4(5) . . . . ? C2 C3 C4 N2 -180.0(3) . . . . ? C7 N2 C4 C5 177.9(3) . . . . ? C7 N2 C4 C3 -3.5(5) . . . . ? C3 C4 C5 C6 1.2(5) . . . . ? N2 C4 C5 C6 179.8(3) . . . . ? C2 C1 C6 C5 -0.2(6) . . . . ? N1 C1 C6 C5 178.9(3) . . . . ? C4 C5 C6 C1 -0.4(6) . . . . ? C8 N3 C7 O3 1.7(6) . . . . ? C8 N3 C7 N2 -178.0(3) . . . . ? C4 N2 C7 O3 -5.4(5) . . . . ? C4 N2 C7 N3 174.3(3) . . . . ? C7 N3 C8 C9 -51.4(5) . . . . ? C7 N3 C8 C13 132.0(3) . . . . ? N3 C8 C9 C10 -174.7(3) . . . . ? C13 C8 C9 C10 1.9(5) . . . . ? C8 C9 C10 C11 0.8(6) . . . . ? C9 C10 C11 C12 -1.9(6) . . . . ? C10 C11 C12 C13 0.3(5) . . . . ? C11 C12 C13 C8 2.5(5) . . . . ? C11 C12 C13 N4 -179.4(3) . . . . ? C9 C8 C13 C12 -3.5(5) . . . . ? N3 C8 C13 C12 173.2(3) . . . . ? C9 C8 C13 N4 178.3(3) . . . . ? N3 C8 C13 N4 -5.0(4) . . . . ? C14 N4 C13 C12 27.4(5) . . . . ? C14 N4 C13 C8 -154.4(3) . . . . ? C15 N5 C14 O4 0.0(6) . . . . ? C15 N5 C14 N4 -178.7(3) . . . . ? C13 N4 C14 O4 6.4(5) . . . . ? C13 N4 C14 N5 -175.0(3) . . . . ? C14 N5 C15 C16 8.7(5) . . . . ? C14 N5 C15 C19 -171.4(3) . . . . ? N5 C15 C16 C17 176.9(3) . . . . ? C19 C15 C16 C17 -3.0(5) . . . . ? C15 C16 C17 C18 2.9(6) . . . . ? C16 C17 C18 C19 -1.3(6) . . . 2_676 ? C16 C15 C19 C18 -178.4(3) . . . 2_676 ? N5 C15 C19 C18 1.7(5) . . . 2_676 ? C16 C15 C19 C19 1.6(6) . . . 2_676 ? N5 C15 C19 C19 -178.3(3) . . . 2_676 ? C47 N11 C39 C40 -175.8(3) . . . . ? C43 N11 C39 C40 -54.2(4) . . . . ? C51 N11 C39 C40 63.4(4) . . . . ? N11 C39 C40 C41 -170.9(3) . . . . ? C39 C40 C41 C42 -176.6(4) . . . . ? C47 N11 C43 C44 57.1(4) . . . . ? C39 N11 C43 C44 -62.1(4) . . . . ? C51 N11 C43 C44 177.3(3) . . . . ? N11 C43 C44 C45 -171.7(3) . . . . ? C43 C44 C45 C46 -176.7(3) . . . . ? C43 N11 C47 C48 58.3(4) . . . . ? C39 N11 C47 C48 179.7(3) . . . . ? C51 N11 C47 C48 -59.1(4) . . . . ? N11 C47 C48 C49 -177.9(3) . . . . ? C47 C48 C49 C50 -177.9(4) . . . . ? C47 N11 C51 C52 -53.3(4) . . . . ? C43 N11 C51 C52 -173.8(3) . . . . ? C39 N11 C51 C52 65.6(4) . . . . ? N11 C51 C52 C53 -176.7(3) . . . . ? C51 C52 C53 C54 -175.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.957 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.082 ######END