# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_coden_Cambridge 440 _publ_contact_author_name 'Prof. Kari Rissanen' _publ_contact_author_address ; P O Box 35 FIN-40014 JYU ; _publ_contact_author_email kari.rissanen@cc.jyu.fi _publ_contact_author_phone '+358 14 260 2672' _publ_contact_author_fax '+358 14 260 2501' loop_ _publ_author_name _publ_author_address 'Rissanen, Kari' ; P. O. Box 35 FIN-40014 JYU ; 'Mansikkamaki, Heidi' ; P O Box 35 FIN-40014 JYU ; 'Nissinen, Maija' ; P O Box 35 FIN-40014 JYU ; 'Schalley , Christoph A.' ; Kekule-Institut fur Organische Chemie und Biochemie der Universit\"at Gerhard-Domagk-Str. 1 D-53121 Bonn Germany ; _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Weak Interactions between Resorcinarenes and Diquaternary Alkyl Ammonium Cations ; data_Complex1 _database_code_depnum_ccdc_archive 'CCDC 254958' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C60H56O8*0.5C4H12NBr*2.5CH4O*0.5H2O _chemical_formula_sum 'C64.5 H73 Br0.5 N0.5 O11' _chemical_formula_weight 2142.38 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 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 29.4551(5) _cell_length_b 15.4086(2) _cell_length_c 25.4790(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.503(3) _cell_angle_gamma 90.00 _cell_volume 11405.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4552 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; dx = 35 mm, 70 sec./deg., 1 deg. ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 17408 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0974 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10066 _reflns_number_gt 5632 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction 'SHELX97 (Sheldrick, 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics DIAMOND _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1494P)^2^+66.6174P] 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 10066 _refine_ls_number_parameters 680 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1861 _refine_ls_R_factor_gt 0.1075 _refine_ls_wR_factor_ref 0.3237 _refine_ls_wR_factor_gt 0.2758 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1191(2) 0.1530(4) 0.1685(2) 0.0413(15) Uani 1 1 d . . . C2 C 0.1380(2) 0.1388(3) 0.2213(2) 0.0376(14) Uani 1 1 d . . . H2 H 0.1634 0.1740 0.2363 0.045 Uiso 1 1 calc R . . C3 C 0.12262(19) 0.0766(4) 0.2540(2) 0.0389(14) Uani 1 1 d . . . C4 C 0.0851(2) 0.0253(4) 0.2301(3) 0.0498(16) Uani 1 1 d . . . O4 O 0.06788(19) -0.0392(3) 0.2589(2) 0.0704(15) Uani 1 1 d D . . H4 H 0.066(3) -0.021(6) 0.2892(18) 0.106 Uiso 1 1 d D . . C5 C 0.0647(2) 0.0391(5) 0.1781(3) 0.0534(18) Uani 1 1 d . . . H5 H 0.0390 0.0049 0.1632 0.064 Uiso 1 1 calc R . . C6 C 0.0810(2) 0.1012(4) 0.1476(2) 0.0476(16) Uani 1 1 d . . . O6 O 0.05832(16) 0.1096(3) 0.09623(17) 0.0605(13) Uani 1 1 d D . . H6 H 0.0656 0.1570 0.0836 0.091 Uiso 1 1 calc RD . . C7 C 0.14447(19) 0.0637(4) 0.3120(2) 0.0394(14) Uani 1 1 d . . . H7 H 0.1372 0.0030 0.3217 0.047 Uiso 1 1 calc R . . C8 C 0.12218(19) 0.1241(3) 0.3484(2) 0.0353(13) Uani 1 1 d . . . C9 C 0.13916(18) 0.2071(3) 0.3615(2) 0.0340(13) Uani 1 1 d . . . H9 H 0.1651 0.2261 0.3469 0.041 Uiso 1 1 calc R . . C10 C 0.12039(17) 0.2638(3) 0.3947(2) 0.0310(12) Uani 1 1 d . . . C11 C 0.08109(19) 0.2367(4) 0.4138(2) 0.0419(15) Uani 1 1 d . . . O11 O 0.05871(15) 0.2880(3) 0.44493(19) 0.0536(12) Uani 1 1 d D . . H11 H 0.056(3) 0.340(2) 0.435(3) 0.080 Uiso 1 1 d D . . C12 C 0.0630(2) 0.1544(4) 0.4018(3) 0.0518(17) Uani 1 1 d . . . H12 H 0.0365 0.1362 0.4157 0.062 Uiso 1 1 calc R . . C13 C 0.0833(2) 0.0983(4) 0.3694(3) 0.0452(15) Uani 1 1 d . . . O13 O 0.06530(19) 0.0175(3) 0.3588(2) 0.0713(15) Uani 1 1 d . . . H13 H 0.0530 0.0005 0.3845 0.107 Uiso 1 1 calc R . . C14 C 0.14100(18) 0.3529(3) 0.4090(2) 0.0343(13) Uani 1 1 d . . . H14 H 0.1325 0.3690 0.4442 0.041 Uiso 1 1 calc R . . C15 C 0.11997(17) 0.4218(3) 0.3692(2) 0.0341(13) Uani 1 1 d . . . C16 C 0.13439(17) 0.4330(3) 0.3207(2) 0.0319(13) Uani 1 1 d . . . H16 H 0.1577 0.3952 0.3124 0.038 Uiso 1 1 calc R . . C17 C 0.11721(18) 0.4959(3) 0.2830(2) 0.0374(14) Uani 1 1 d . . . C18 C 0.0818(2) 0.5483(4) 0.2965(3) 0.0488(16) Uani 1 1 d . . . O18 O 0.06186(19) 0.6099(3) 0.2608(2) 0.0677(15) Uani 1 1 d D . . H18 H 0.059(3) 0.594(6) 0.2286(14) 0.101 Uiso 1 1 d D . . C19 C 0.0662(2) 0.5389(4) 0.3439(3) 0.0527(17) Uani 1 1 d . . . H19 H 0.0421 0.5752 0.3518 0.063 Uiso 1 1 calc R . . C20 C 0.0851(2) 0.4770(4) 0.3807(3) 0.0479(16) Uani 1 1 d . . . O20 O 0.06920(17) 0.4676(3) 0.42799(19) 0.0616(13) Uani 1 1 d D . . H20 H 0.070(3) 0.498(5) 0.455(2) 0.092 Uiso 1 1 d D . . C21 C 0.13702(18) 0.5092(4) 0.2324(2) 0.0373(13) Uani 1 1 d . . . H21 H 0.1273 0.5687 0.2194 0.045 Uiso 1 1 calc R . . C22 C 0.11629(18) 0.4470(4) 0.1889(2) 0.0396(14) Uani 1 1 d . . . C23 C 0.13478(19) 0.3661(4) 0.1813(2) 0.0394(14) Uani 1 1 d . . . H23 H 0.1611 0.3483 0.2056 0.047 Uiso 1 1 calc R . . C24 C 0.1175(2) 0.3091(4) 0.1403(2) 0.0450(15) Uani 1 1 d . . . C25 C 0.0796(3) 0.3375(4) 0.1049(3) 0.062(2) Uani 1 1 d . . . O25 O 0.0609(2) 0.2838(3) 0.0636(2) 0.091(2) Uani 1 1 d D . . H25 H 0.0410 0.3111 0.0426 0.137 Uiso 1 1 calc RD . . C26 C 0.0589(3) 0.4167(5) 0.1112(3) 0.071(2) Uani 1 1 d . . . H26 H 0.0323 0.4340 0.0870 0.085 Uiso 1 1 calc R . . C27 C 0.0772(2) 0.4709(4) 0.1531(3) 0.0549(18) Uani 1 1 d . . . O27 O 0.05642(17) 0.5489(3) 0.1580(2) 0.0688(15) Uani 1 1 d D . . H27 H 0.050(3) 0.573(6) 0.1286(19) 0.103 Uiso 1 1 d D . . C28 C 0.1380(2) 0.2193(4) 0.1341(2) 0.0460(15) Uani 1 1 d . . . H28 H 0.1273 0.2013 0.0964 0.055 Uiso 1 1 calc R . . C29 C 0.19710(19) 0.0713(4) 0.3212(2) 0.0415(14) Uani 1 1 d . . . H29A H 0.2093 0.0374 0.2936 0.050 Uiso 1 1 calc R . . H29B H 0.2058 0.1328 0.3175 0.050 Uiso 1 1 calc R . . C30 C 0.2190(2) 0.0384(4) 0.3763(3) 0.0536(17) Uani 1 1 d . . . H30A H 0.1978 0.0515 0.4016 0.064 Uiso 1 1 calc R . . H30B H 0.2219 -0.0255 0.3746 0.064 Uiso 1 1 calc R . . C31 C 0.2656(2) 0.0757(4) 0.3980(2) 0.0429(15) Uani 1 1 d . . . C32 C 0.3059(3) 0.0278(6) 0.4059(3) 0.073(2) Uani 1 1 d . . . H32 H 0.3049 -0.0322 0.3972 0.088 Uiso 1 1 calc R . . C33 C 0.3481(3) 0.0664(10) 0.4266(4) 0.106(4) Uani 1 1 d . . . H33 H 0.3756 0.0331 0.4316 0.127 Uiso 1 1 calc R . . C34 C 0.3493(3) 0.1520(11) 0.4395(4) 0.104(4) Uani 1 1 d . . . H34 H 0.3777 0.1780 0.4545 0.125 Uiso 1 1 calc R . . C35 C 0.3116(3) 0.1992(7) 0.4314(4) 0.092(3) Uani 1 1 d . . . H35 H 0.3133 0.2594 0.4397 0.110 Uiso 1 1 calc R . . C36 C 0.2698(2) 0.1626(5) 0.4111(3) 0.0613(19) Uani 1 1 d . . . H36 H 0.2431 0.1982 0.4059 0.074 Uiso 1 1 calc R . . C37 C 0.19344(17) 0.3536(4) 0.4164(2) 0.0361(13) Uani 1 1 d . . . H37A H 0.2031 0.3401 0.3819 0.043 Uiso 1 1 calc R . . H37B H 0.2055 0.3073 0.4418 0.043 Uiso 1 1 calc R . . C38 C 0.21493(19) 0.4406(4) 0.4369(3) 0.0491(16) Uani 1 1 d . . . H38A H 0.2012 0.4878 0.4130 0.059 Uiso 1 1 calc R . . H38B H 0.2077 0.4520 0.4728 0.059 Uiso 1 1 calc R . . C39 C 0.2663(2) 0.4409(4) 0.4394(3) 0.0457(15) Uani 1 1 d . . . C40 C 0.2959(3) 0.4186(7) 0.4850(3) 0.084(3) Uani 1 1 d . . . H40 H 0.2835 0.4022 0.5157 0.101 Uiso 1 1 calc R . . C41 C 0.3428(3) 0.4192(8) 0.4874(4) 0.104(3) Uani 1 1 d . . . H41 H 0.3623 0.4047 0.5197 0.124 Uiso 1 1 calc R . . C42 C 0.3616(3) 0.4406(7) 0.4438(5) 0.091(3) Uani 1 1 d . . . H42 H 0.3941 0.4402 0.4455 0.109 Uiso 1 1 calc R . . C43 C 0.3329(3) 0.4632(5) 0.3964(4) 0.068(2) Uani 1 1 d . . . H43 H 0.3454 0.4788 0.3657 0.081 Uiso 1 1 calc R . . C44 C 0.2860(2) 0.4623(4) 0.3955(3) 0.0507(16) Uani 1 1 d . . . H44 H 0.2664 0.4769 0.3633 0.061 Uiso 1 1 calc R . . C45 C 0.18967(18) 0.5091(4) 0.2417(2) 0.0389(14) Uani 1 1 d . . . H45A H 0.2008 0.4511 0.2545 0.047 Uiso 1 1 calc R . . H45B H 0.2003 0.5197 0.2073 0.047 Uiso 1 1 calc R . . C46 C 0.21088(19) 0.5774(4) 0.2818(2) 0.0406(14) Uani 1 1 d . . . H46A H 0.2010 0.5650 0.3163 0.049 Uiso 1 1 calc R . . H46B H 0.2448 0.5711 0.2870 0.049 Uiso 1 1 calc R . . C47 C 0.19884(19) 0.6711(4) 0.2668(3) 0.0441(15) Uani 1 1 d . . . C48 C 0.1822(3) 0.7250(5) 0.3019(3) 0.073(2) Uani 1 1 d . . . H48 H 0.1764 0.7029 0.3350 0.087 Uiso 1 1 calc R . . C49 C 0.1738(4) 0.8127(5) 0.2893(4) 0.096(3) Uani 1 1 d . . . H49 H 0.1617 0.8495 0.3135 0.115 Uiso 1 1 calc R . . C50 C 0.1829(4) 0.8453(5) 0.2427(4) 0.090(3) Uani 1 1 d . . . H50 H 0.1783 0.9053 0.2349 0.108 Uiso 1 1 calc R . . C51 C 0.1987(4) 0.7912(5) 0.2069(4) 0.090(3) Uani 1 1 d . . . H51 H 0.2047 0.8136 0.1740 0.108 Uiso 1 1 calc R . . C52 C 0.2057(3) 0.7048(5) 0.2186(3) 0.075(2) Uani 1 1 d . . . H52 H 0.2155 0.6676 0.1930 0.090 Uiso 1 1 calc R . . C53 C 0.1910(2) 0.2191(4) 0.1425(3) 0.0564(18) Uani 1 1 d . . . H53A H 0.2018 0.1587 0.1396 0.068 Uiso 1 1 calc R . . H53B H 0.2029 0.2399 0.1789 0.068 Uiso 1 1 calc R . . C54 C 0.2110(3) 0.2761(5) 0.1021(4) 0.080(2) Uani 1 1 d . . . H54A H 0.2029 0.3375 0.1075 0.096 Uiso 1 1 calc R . . H54B H 0.2449 0.2714 0.1090 0.096 Uiso 1 1 calc R . . C55 C 0.1937(5) 0.2516(7) 0.0454(5) 0.1280(19) Uani 1 1 d . . . C56 C 0.1661(5) 0.3076(7) 0.0116(4) 0.1280(19) Uani 1 1 d . . . H56 H 0.1576 0.3619 0.0248 0.154 Uiso 1 1 calc R . . C57 C 0.1506(5) 0.2857(7) -0.0413(4) 0.1280(19) Uani 1 1 d . . . H57 H 0.1322 0.3251 -0.0644 0.154 Uiso 1 1 calc R . . C58 C 0.1617(5) 0.2089(7) -0.0591(5) 0.1280(19) Uani 1 1 d . . . H58 H 0.1497 0.1923 -0.0946 0.154 Uiso 1 1 calc R . . C59 C 0.1904(5) 0.1530(7) -0.0271(4) 0.1280(19) Uani 1 1 d . . . H59 H 0.1990 0.0991 -0.0408 0.154 Uiso 1 1 calc R . . C60 C 0.2067(5) 0.1756(7) 0.0250(4) 0.1280(19) Uani 1 1 d . . . H60 H 0.2272 0.1378 0.0468 0.154 Uiso 1 1 calc R . . Br1 Br -0.00175(6) 0.38849(9) 0.53812(5) 0.0495(4) Uani 0.50 1 d P A 1 O1W O -0.0356(5) 0.3747(7) 0.5370(6) 0.094(4) Uani 0.50 1 d P B 2 N1 N 0.0000 0.2874(5) 0.2500 0.0451(18) Uani 1 2 d SD . . C1C C -0.0502(7) 0.265(2) 0.2412(16) 0.198(7) Uiso 0.50 1 d PD . . C2C C 0.0147(13) 0.279(3) 0.1956(10) 0.198(7) Uiso 0.50 1 d PD . . C3C C 0.0000 0.1887(13) 0.2500 0.198(7) Uiso 1 2 d SD . . C4C C -0.0211(13) 0.351(2) 0.2080(13) 0.198(7) Uiso 0.50 1 d PD . . O1M O 0.0424(5) -0.1709(9) 0.1926(6) 0.106(4) Uiso 0.50 1 d PD . . C2M C 0.0747(7) -0.2136(15) 0.1653(9) 0.116(7) Uiso 0.50 1 d PD . . O3M O 0.0215(3) 0.7296(5) 0.3115(3) 0.119(2) Uiso 1 1 d D . . C4M C 0.0563(6) 0.7775(11) 0.3442(7) 0.122(8) Uiso 0.67(3) 1 d PD C 1 C4MB C 0.0467(14) 0.787(2) 0.2826(16) 0.15(2) Uiso 0.33(3) 1 d PD C 2 O7M O 0.0135(4) -0.0418(7) 0.4299(5) 0.083(3) Uiso 0.50 1 d PD D 1 C8M C 0.0297(9) -0.1085(16) 0.4660(10) 0.129(8) Uiso 0.50 1 d PD D 1 O7MB O -0.0099(6) -0.0397(14) 0.4581(9) 0.075(6) Uiso 0.25 1 d PD E 2 C8MB C 0.0382(7) -0.0505(19) 0.4641(11) 0.053(7) Uiso 0.25 1 d PD E 2 O7MC O -0.0452(8) -0.1886(17) 0.4338(9) 0.097(7) Uiso 0.25 1 d PD F 3 C8MC C -0.0184(9) -0.1815(18) 0.4851(9) 0.057(7) Uiso 0.25 1 d PD F 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.043(3) 0.046(3) 0.034(3) -0.012(3) 0.004(3) 0.020(3) C2 0.045(3) 0.029(3) 0.036(3) -0.008(3) -0.002(3) 0.010(2) C3 0.040(3) 0.033(3) 0.040(3) -0.009(3) -0.004(3) 0.012(3) C4 0.053(4) 0.041(4) 0.052(4) -0.007(3) -0.001(3) -0.003(3) O4 0.091(4) 0.060(3) 0.055(3) -0.012(3) -0.005(3) -0.024(3) C5 0.041(3) 0.068(5) 0.046(4) -0.021(4) -0.011(3) 0.004(3) C6 0.044(3) 0.062(4) 0.033(4) -0.006(3) -0.004(3) 0.019(3) O6 0.055(3) 0.083(4) 0.039(3) -0.008(2) -0.008(2) 0.007(3) C7 0.044(3) 0.030(3) 0.041(4) -0.007(3) 0.000(3) 0.004(3) C8 0.040(3) 0.031(3) 0.033(3) -0.006(2) 0.000(2) -0.001(2) C9 0.032(3) 0.038(3) 0.032(3) -0.001(3) 0.003(2) 0.005(2) C10 0.030(3) 0.030(3) 0.031(3) -0.001(2) 0.000(2) 0.006(2) C11 0.039(3) 0.044(4) 0.043(4) -0.006(3) 0.005(3) 0.003(3) O11 0.054(3) 0.051(3) 0.062(3) -0.016(2) 0.027(2) -0.001(2) C12 0.042(3) 0.056(4) 0.061(4) -0.006(3) 0.019(3) -0.011(3) C13 0.049(4) 0.038(3) 0.049(4) -0.006(3) 0.010(3) -0.005(3) O13 0.087(4) 0.050(3) 0.085(4) -0.023(3) 0.037(3) -0.035(3) C14 0.036(3) 0.036(3) 0.031(3) -0.004(2) 0.004(2) 0.004(2) C15 0.031(3) 0.031(3) 0.041(4) -0.009(2) 0.008(3) 0.000(2) C16 0.029(3) 0.024(3) 0.043(4) -0.008(2) 0.005(2) 0.004(2) C17 0.033(3) 0.025(3) 0.055(4) -0.006(3) 0.012(3) 0.000(2) C18 0.043(3) 0.035(3) 0.072(5) 0.010(3) 0.021(3) 0.015(3) O18 0.086(3) 0.055(3) 0.071(3) 0.023(3) 0.040(3) 0.037(3) C19 0.050(4) 0.045(4) 0.072(5) 0.004(3) 0.034(4) 0.021(3) C20 0.054(4) 0.041(4) 0.052(4) -0.008(3) 0.019(3) 0.008(3) O20 0.082(3) 0.058(3) 0.054(3) -0.007(2) 0.036(3) 0.023(2) C21 0.037(3) 0.032(3) 0.045(4) 0.007(3) 0.013(3) 0.003(2) C22 0.032(3) 0.041(3) 0.045(4) 0.007(3) 0.007(3) 0.006(3) C23 0.034(3) 0.045(3) 0.039(3) 0.011(3) 0.005(3) 0.010(3) C24 0.048(4) 0.046(4) 0.039(4) 0.000(3) 0.002(3) 0.017(3) C25 0.080(5) 0.047(4) 0.051(4) -0.007(3) -0.018(4) 0.022(4) O25 0.128(5) 0.055(3) 0.070(4) -0.010(3) -0.043(3) 0.037(3) C26 0.065(5) 0.048(4) 0.085(6) 0.004(4) -0.030(4) 0.021(4) C27 0.041(3) 0.039(4) 0.080(5) 0.000(3) -0.005(3) 0.014(3) O27 0.066(3) 0.039(3) 0.087(4) -0.005(2) -0.030(3) 0.026(2) C28 0.061(4) 0.043(3) 0.033(3) 0.000(3) 0.005(3) 0.022(3) C29 0.047(3) 0.036(3) 0.039(4) -0.006(3) 0.000(3) 0.003(3) C30 0.053(4) 0.045(4) 0.055(4) 0.009(3) -0.013(3) -0.002(3) C31 0.043(3) 0.049(4) 0.035(3) -0.005(3) 0.000(3) 0.013(3) C32 0.083(6) 0.083(6) 0.048(4) -0.016(4) -0.008(4) 0.040(5) C33 0.044(5) 0.197(13) 0.072(7) 0.008(8) 0.000(4) 0.054(7) C34 0.050(6) 0.191(13) 0.066(6) 0.019(8) -0.003(4) -0.025(7) C35 0.087(7) 0.093(7) 0.088(7) -0.001(5) -0.011(5) -0.040(6) C36 0.049(4) 0.053(4) 0.080(5) -0.005(4) 0.004(4) 0.001(3) C37 0.031(3) 0.038(3) 0.038(3) -0.009(3) 0.004(2) 0.006(2) C38 0.041(3) 0.047(4) 0.058(4) -0.022(3) 0.005(3) -0.005(3) C39 0.041(3) 0.053(4) 0.041(4) -0.016(3) 0.002(3) -0.008(3) C40 0.056(5) 0.151(9) 0.042(5) -0.007(5) -0.004(4) -0.013(5) C41 0.061(6) 0.161(10) 0.077(7) -0.013(7) -0.023(5) 0.002(6) C42 0.041(4) 0.116(8) 0.115(8) -0.029(6) 0.008(5) -0.014(5) C43 0.056(5) 0.061(5) 0.090(6) -0.007(4) 0.026(4) -0.009(4) C44 0.052(4) 0.044(4) 0.054(4) -0.004(3) 0.003(3) -0.004(3) C45 0.034(3) 0.038(3) 0.046(4) 0.004(3) 0.009(3) -0.003(2) C46 0.033(3) 0.043(3) 0.046(4) 0.008(3) 0.008(3) -0.007(3) C47 0.040(3) 0.045(4) 0.051(4) 0.000(3) 0.016(3) -0.004(3) C48 0.108(6) 0.059(5) 0.058(5) 0.003(4) 0.031(5) 0.010(4) C49 0.154(9) 0.054(5) 0.084(7) -0.010(5) 0.031(6) 0.035(5) C50 0.143(8) 0.043(4) 0.087(7) 0.012(5) 0.026(6) 0.006(5) C51 0.141(8) 0.044(4) 0.098(7) 0.018(5) 0.060(6) 0.007(5) C52 0.104(6) 0.050(4) 0.081(6) 0.010(4) 0.047(5) 0.009(4) C53 0.058(4) 0.052(4) 0.059(4) 0.004(3) 0.011(3) 0.023(3) C54 0.089(6) 0.060(5) 0.098(7) 0.013(5) 0.041(5) 0.025(4) C55 0.226(6) 0.089(3) 0.087(3) 0.002(2) 0.078(4) 0.021(3) C56 0.226(6) 0.089(3) 0.087(3) 0.002(2) 0.078(4) 0.021(3) C57 0.226(6) 0.089(3) 0.087(3) 0.002(2) 0.078(4) 0.021(3) C58 0.226(6) 0.089(3) 0.087(3) 0.002(2) 0.078(4) 0.021(3) C59 0.226(6) 0.089(3) 0.087(3) 0.002(2) 0.078(4) 0.021(3) C60 0.226(6) 0.089(3) 0.087(3) 0.002(2) 0.078(4) 0.021(3) Br1 0.0576(9) 0.0485(8) 0.0423(8) -0.0201(6) 0.0075(6) 0.0016(7) O1W 0.106(10) 0.065(8) 0.119(11) -0.029(7) 0.045(9) -0.028(7) N1 0.030(3) 0.040(4) 0.062(5) 0.000 -0.001(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.386(8) . ? C1 C6 1.408(9) . ? C1 C28 1.510(9) . ? C2 C3 1.395(9) . ? C2 H2 0.9500 . ? C3 C4 1.412(8) . ? C3 C7 1.525(8) . ? C4 C5 1.377(9) . ? C4 O4 1.381(8) . ? O4 H4 0.84(2) . ? C5 C6 1.368(10) . ? C5 H5 0.9500 . ? C6 O6 1.374(7) . ? O6 H6 0.8400 . ? C7 C29 1.534(8) . ? C7 C8 1.534(8) . ? C7 H7 1.0000 . ? C8 C9 1.394(7) . ? C8 C13 1.400(8) . ? C9 C10 1.393(7) . ? C9 H9 0.9500 . ? C10 C11 1.391(8) . ? C10 C14 1.522(7) . ? C11 O11 1.365(7) . ? C11 C12 1.391(9) . ? O11 H11 0.84(2) . ? C12 C13 1.397(9) . ? C12 H12 0.9500 . ? C13 O13 1.363(7) . ? O13 H13 0.8400 . ? C14 C37 1.525(7) . ? C14 C15 1.527(8) . ? C14 H14 1.0000 . ? C15 C16 1.382(8) . ? C15 C20 1.400(8) . ? C16 C17 1.400(8) . ? C16 H16 0.9500 . ? C17 C18 1.405(8) . ? C17 C21 1.513(8) . ? C18 C19 1.370(9) . ? C18 O18 1.378(8) . ? O18 H18 0.85(2) . ? C19 C20 1.387(9) . ? C19 H19 0.9500 . ? C20 O20 1.372(8) . ? O20 H20 0.83(2) . ? C21 C22 1.516(8) . ? C21 C45 1.530(7) . ? C21 H21 1.0000 . ? C22 C23 1.386(8) . ? C22 C27 1.396(8) . ? C23 C24 1.396(8) . ? C23 H23 0.9500 . ? C24 C25 1.384(9) . ? C24 C28 1.528(8) . ? C25 O25 1.380(8) . ? C25 C26 1.386(9) . ? O25 H25 0.8400 . ? C26 C27 1.392(10) . ? C26 H26 0.9500 . ? C27 O27 1.364(7) . ? O27 H27 0.83(2) . ? C28 C53 1.539(9) . ? C28 H28 1.0000 . ? C29 C30 1.531(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.507(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C36 1.380(9) . ? C31 C32 1.383(9) . ? C32 C33 1.400(14) . ? C32 H32 0.9500 . ? C33 C34 1.357(15) . ? C33 H33 0.9500 . ? C34 C35 1.314(15) . ? C34 H34 0.9500 . ? C35 C36 1.375(11) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.536(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.504(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.377(10) . ? C39 C44 1.383(9) . ? C40 C41 1.375(11) . ? C40 H40 0.9500 . ? C41 C42 1.361(13) . ? C41 H41 0.9500 . ? C42 C43 1.398(12) . ? C42 H42 0.9500 . ? C43 C44 1.376(9) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.526(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.521(8) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.370(9) . ? C47 C52 1.377(10) . ? C48 C49 1.402(11) . ? C48 H48 0.9500 . ? C49 C50 1.356(12) . ? C49 H49 0.9500 . ? C50 C51 1.372(12) . ? C50 H50 0.9500 . ? C51 C52 1.372(10) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.542(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.499(15) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C60 1.361(14) . ? C55 C56 1.384(16) . ? C56 C57 1.391(16) . ? C56 H56 0.9500 . ? C57 C58 1.327(14) . ? C57 H57 0.9500 . ? C58 C59 1.377(16) . ? C58 H58 0.9500 . ? C59 C60 1.379(16) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? N1 C1C 1.50(2) 2 ? N1 C1C 1.50(2) . ? N1 C4C 1.51(2) 2 ? N1 C4C 1.51(2) . ? N1 C3C 1.521(19) . ? N1 C2C 1.52(2) . ? N1 C2C 1.52(2) 2 ? C1C C2C 1.78(5) 2 ? C1C C4C 1.85(5) . ? C1C C3C 1.87(4) . ? C2C C4C 1.59(5) . ? C2C C1C 1.78(5) 2 ? C3C C1C 1.87(4) 2 ? O1M C2M 1.429(16) . ? O3M C4M 1.417(14) . ? O3M C4MB 1.433(18) . ? O7M C8M 1.408(16) . ? O7MB C8MB 1.410(17) . ? O7MC C8MC 1.416(17) . ? 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 C2 C1 C6 116.4(6) . . ? C2 C1 C28 122.8(6) . . ? C6 C1 C28 120.8(6) . . ? C1 C2 C3 124.8(6) . . ? C1 C2 H2 117.6 . . ? C3 C2 H2 117.6 . . ? C2 C3 C4 115.8(5) . . ? C2 C3 C7 122.8(5) . . ? C4 C3 C7 121.4(6) . . ? C5 C4 O4 118.8(6) . . ? C5 C4 C3 121.0(6) . . ? O4 C4 C3 120.2(6) . . ? C4 O4 H4 109(7) . . ? C6 C5 C4 121.1(6) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 O6 116.5(6) . . ? C5 C6 C1 120.9(6) . . ? O6 C6 C1 122.5(6) . . ? C6 O6 H6 109.5 . . ? C3 C7 C29 113.1(5) . . ? C3 C7 C8 110.6(4) . . ? C29 C7 C8 112.6(4) . . ? C3 C7 H7 106.7 . . ? C29 C7 H7 106.7 . . ? C8 C7 H7 106.7 . . ? C9 C8 C13 116.9(5) . . ? C9 C8 C7 121.9(5) . . ? C13 C8 C7 121.1(5) . . ? C10 C9 C8 124.0(5) . . ? C10 C9 H9 118.0 . . ? C8 C9 H9 118.0 . . ? C11 C10 C9 117.4(5) . . ? C11 C10 C14 120.6(5) . . ? C9 C10 C14 121.9(5) . . ? O11 C11 C10 122.6(5) . . ? O11 C11 C12 116.8(5) . . ? C10 C11 C12 120.6(5) . . ? C11 O11 H11 115(6) . . ? C11 C12 C13 120.5(6) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? O13 C13 C12 119.5(5) . . ? O13 C13 C8 120.0(5) . . ? C12 C13 C8 120.5(5) . . ? C13 O13 H13 109.5 . . ? C10 C14 C37 113.1(4) . . ? C10 C14 C15 111.5(4) . . ? C37 C14 C15 111.6(5) . . ? C10 C14 H14 106.8 . . ? C37 C14 H14 106.8 . . ? C15 C14 H14 106.8 . . ? C16 C15 C20 117.0(5) . . ? C16 C15 C14 122.0(5) . . ? C20 C15 C14 121.0(5) . . ? C15 C16 C17 124.8(5) . . ? C15 C16 H16 117.6 . . ? C17 C16 H16 117.6 . . ? C16 C17 C18 115.3(5) . . ? C16 C17 C21 122.2(5) . . ? C18 C17 C21 122.5(5) . . ? C19 C18 O18 119.1(5) . . ? C19 C18 C17 121.8(6) . . ? O18 C18 C17 119.1(6) . . ? C18 O18 H18 114(7) . . ? C18 C19 C20 120.7(5) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? O20 C20 C19 120.4(5) . . ? O20 C20 C15 119.2(6) . . ? C19 C20 C15 120.3(6) . . ? C20 O20 H20 134(6) . . ? C17 C21 C22 111.8(4) . . ? C17 C21 C45 113.2(5) . . ? C22 C21 C45 112.8(5) . . ? C17 C21 H21 106.2 . . ? C22 C21 H21 106.2 . . ? C45 C21 H21 106.2 . . ? C23 C22 C27 116.5(6) . . ? C23 C22 C21 123.5(5) . . ? C27 C22 C21 120.1(5) . . ? C22 C23 C24 124.6(5) . . ? C22 C23 H23 117.7 . . ? C24 C23 H23 117.7 . . ? C25 C24 C23 116.3(5) . . ? C25 C24 C28 120.6(6) . . ? C23 C24 C28 123.0(5) . . ? O25 C25 C24 118.9(6) . . ? O25 C25 C26 119.3(6) . . ? C24 C25 C26 121.8(6) . . ? C25 O25 H25 109.5 . . ? C25 C26 C27 119.6(6) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? O27 C27 C26 118.4(5) . . ? O27 C27 C22 120.4(6) . . ? C26 C27 C22 121.2(6) . . ? C27 O27 H27 110(7) . . ? C1 C28 C24 111.3(5) . . ? C1 C28 C53 112.4(5) . . ? C24 C28 C53 113.4(5) . . ? C1 C28 H28 106.4 . . ? C24 C28 H28 106.4 . . ? C53 C28 H28 106.4 . . ? C30 C29 C7 112.1(5) . . ? C30 C29 H29A 109.2 . . ? C7 C29 H29A 109.2 . . ? C30 C29 H29B 109.2 . . ? C7 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C31 C30 C29 115.5(5) . . ? C31 C30 H30A 108.4 . . ? C29 C30 H30A 108.4 . . ? C31 C30 H30B 108.4 . . ? C29 C30 H30B 108.4 . . ? H30A C30 H30B 107.5 . . ? C36 C31 C32 116.2(6) . . ? C36 C31 C30 119.9(5) . . ? C32 C31 C30 123.8(6) . . ? C31 C32 C33 120.9(8) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C34 C33 C32 119.3(8) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 120.9(9) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 120.7(10) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C35 C36 C31 121.9(8) . . ? C35 C36 H36 119.1 . . ? C31 C36 H36 119.1 . . ? C14 C37 C38 113.6(4) . . ? C14 C37 H37A 108.8 . . ? C38 C37 H37A 108.8 . . ? C14 C37 H37B 108.8 . . ? C38 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? C39 C38 C37 111.9(5) . . ? C39 C38 H38A 109.2 . . ? C37 C38 H38A 109.2 . . ? C39 C38 H38B 109.2 . . ? C37 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C40 C39 C44 116.8(6) . . ? C40 C39 C38 121.8(6) . . ? C44 C39 C38 121.4(6) . . ? C41 C40 C39 121.8(8) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C42 C41 C40 120.5(8) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 119.6(7) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C44 C43 C42 118.4(8) . . ? C44 C43 H43 120.8 . . ? C42 C43 H43 120.8 . . ? C43 C44 C39 122.8(7) . . ? C43 C44 H44 118.6 . . ? C39 C44 H44 118.6 . . ? C46 C45 C21 113.2(5) . . ? C46 C45 H45A 108.9 . . ? C21 C45 H45A 108.9 . . ? C46 C45 H45B 108.9 . . ? C21 C45 H45B 108.9 . . ? H45A C45 H45B 107.7 . . ? C47 C46 C45 115.7(5) . . ? C47 C46 H46A 108.4 . . ? C45 C46 H46A 108.4 . . ? C47 C46 H46B 108.4 . . ? C45 C46 H46B 108.4 . . ? H46A C46 H46B 107.4 . . ? C48 C47 C52 118.3(6) . . ? C48 C47 C46 120.3(6) . . ? C52 C47 C46 121.3(6) . . ? C47 C48 C49 120.2(8) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C50 C49 C48 120.4(8) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 119.6(8) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C50 C51 C52 120.1(8) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C51 C52 C47 121.3(8) . . ? C51 C52 H52 119.3 . . ? C47 C52 H52 119.3 . . ? C28 C53 C54 113.4(6) . . ? C28 C53 H53A 108.9 . . ? C54 C53 H53A 108.9 . . ? C28 C53 H53B 108.9 . . ? C54 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? C55 C54 C53 113.1(8) . . ? C55 C54 H54A 109.0 . . ? C53 C54 H54A 109.0 . . ? C55 C54 H54B 109.0 . . ? C53 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? C60 C55 C56 118.2(12) . . ? C60 C55 C54 120.9(11) . . ? C56 C55 C54 120.8(9) . . ? C55 C56 C57 121.1(11) . . ? C55 C56 H56 119.5 . . ? C57 C56 H56 119.5 . . ? C58 C57 C56 119.1(12) . . ? C58 C57 H57 120.4 . . ? C56 C57 H57 120.4 . . ? C57 C58 C59 121.2(12) . . ? C57 C58 H58 119.4 . . ? C59 C58 H58 119.4 . . ? C58 C59 C60 119.5(11) . . ? C58 C59 H59 120.2 . . ? C60 C59 H59 120.2 . . ? C55 C60 C59 120.6(12) . . ? C55 C60 H60 119.7 . . ? C59 C60 H60 119.7 . . ? C1C N1 C1C 153(3) 2 . ? C1C N1 C4C 76(2) 2 2 ? C1C N1 C4C 122(2) . 2 ? C1C N1 C4C 122(2) 2 . ? C1C N1 C4C 76(2) . . ? C4C N1 C4C 99(3) 2 . ? C1C N1 C3C 76.7(15) 2 . ? C1C N1 C3C 76.7(15) . . ? C4C N1 C3C 130.5(15) 2 . ? C4C N1 C3C 130.5(15) . . ? C1C N1 C2C 72(2) 2 . ? C1C N1 C2C 105(2) . . ? C4C N1 C2C 124(2) 2 . ? C4C N1 C2C 63.4(19) . . ? C3C N1 C2C 85.3(15) . . ? C1C N1 C2C 105(2) 2 2 ? C1C N1 C2C 72(2) . 2 ? C4C N1 C2C 63.4(19) 2 2 ? C4C N1 C2C 124(2) . 2 ? C3C N1 C2C 85.3(15) . 2 ? C2C N1 C2C 171(3) . 2 ? N1 C1C C2C 54.5(11) . 2 ? N1 C1C C4C 52.1(11) . . ? C2C C1C C4C 94.4(18) 2 . ? N1 C1C C3C 52.2(9) . . ? C2C C1C C3C 68.7(16) 2 . ? C4C C1C C3C 95.0(14) . . ? N1 C2C C4C 57.8(11) . . ? N1 C2C C1C 53.2(11) . 2 ? C4C C2C C1C 102.5(18) . 2 ? N1 C3C C1C 51.1(9) . 2 ? N1 C3C C1C 51.1(9) . . ? C1C C3C C1C 102.2(17) 2 . ? N1 C4C C2C 58.8(11) . . ? N1 C4C C1C 51.7(11) . . ? C2C C4C C1C 88.1(19) . . ? C4M O3M C4MB 66.1(19) . . ? 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 C6 C1 C2 C3 1.4(8) . . . . ? C28 C1 C2 C3 -177.9(5) . . . . ? C1 C2 C3 C4 0.3(8) . . . . ? C1 C2 C3 C7 -179.7(5) . . . . ? C2 C3 C4 C5 -1.9(9) . . . . ? C7 C3 C4 C5 178.1(6) . . . . ? C2 C3 C4 O4 178.7(5) . . . . ? C7 C3 C4 O4 -1.3(9) . . . . ? O4 C4 C5 C6 -178.9(6) . . . . ? C3 C4 C5 C6 1.8(10) . . . . ? C4 C5 C6 O6 179.8(6) . . . . ? C4 C5 C6 C1 0.1(10) . . . . ? C2 C1 C6 C5 -1.6(8) . . . . ? C28 C1 C6 C5 177.7(5) . . . . ? C2 C1 C6 O6 178.8(5) . . . . ? C28 C1 C6 O6 -2.0(8) . . . . ? C2 C3 C7 C29 -39.8(7) . . . . ? C4 C3 C7 C29 140.2(6) . . . . ? C2 C3 C7 C8 87.6(6) . . . . ? C4 C3 C7 C8 -92.4(6) . . . . ? C3 C7 C8 C9 -90.4(6) . . . . ? C29 C7 C8 C9 37.3(7) . . . . ? C3 C7 C8 C13 88.9(7) . . . . ? C29 C7 C8 C13 -143.4(6) . . . . ? C13 C8 C9 C10 1.4(8) . . . . ? C7 C8 C9 C10 -179.3(5) . . . . ? C8 C9 C10 C11 -3.0(8) . . . . ? C8 C9 C10 C14 178.4(5) . . . . ? C9 C10 C11 O11 -177.5(5) . . . . ? C14 C10 C11 O11 1.1(8) . . . . ? C9 C10 C11 C12 3.0(8) . . . . ? C14 C10 C11 C12 -178.3(5) . . . . ? O11 C11 C12 C13 178.9(6) . . . . ? C10 C11 C12 C13 -1.5(10) . . . . ? C11 C12 C13 O13 179.1(6) . . . . ? C11 C12 C13 C8 -0.2(10) . . . . ? C9 C8 C13 O13 -179.0(5) . . . . ? C7 C8 C13 O13 1.6(9) . . . . ? C9 C8 C13 C12 0.3(9) . . . . ? C7 C8 C13 C12 -179.0(6) . . . . ? C11 C10 C14 C37 144.5(5) . . . . ? C9 C10 C14 C37 -37.0(7) . . . . ? C11 C10 C14 C15 -88.8(6) . . . . ? C9 C10 C14 C15 89.7(6) . . . . ? C10 C14 C15 C16 -80.8(6) . . . . ? C37 C14 C15 C16 46.7(7) . . . . ? C10 C14 C15 C20 99.6(6) . . . . ? C37 C14 C15 C20 -132.9(5) . . . . ? C20 C15 C16 C17 1.0(8) . . . . ? C14 C15 C16 C17 -178.6(5) . . . . ? C15 C16 C17 C18 -1.9(8) . . . . ? C15 C16 C17 C21 175.2(5) . . . . ? C16 C17 C18 C19 1.2(9) . . . . ? C21 C17 C18 C19 -175.9(6) . . . . ? C16 C17 C18 O18 -177.8(5) . . . . ? C21 C17 C18 O18 5.2(9) . . . . ? O18 C18 C19 C20 179.3(6) . . . . ? C17 C18 C19 C20 0.4(10) . . . . ? C18 C19 C20 O20 -179.7(6) . . . . ? C18 C19 C20 C15 -1.4(10) . . . . ? C16 C15 C20 O20 179.1(5) . . . . ? C14 C15 C20 O20 -1.3(8) . . . . ? C16 C15 C20 C19 0.7(9) . . . . ? C14 C15 C20 C19 -179.6(6) . . . . ? C16 C17 C21 C22 84.4(6) . . . . ? C18 C17 C21 C22 -98.7(6) . . . . ? C16 C17 C21 C45 -44.2(7) . . . . ? C18 C17 C21 C45 132.6(6) . . . . ? C17 C21 C22 C23 -90.7(6) . . . . ? C45 C21 C22 C23 38.1(7) . . . . ? C17 C21 C22 C27 91.1(7) . . . . ? C45 C21 C22 C27 -140.1(6) . . . . ? C27 C22 C23 C24 1.0(9) . . . . ? C21 C22 C23 C24 -177.3(6) . . . . ? C22 C23 C24 C25 1.0(10) . . . . ? C22 C23 C24 C28 -178.1(6) . . . . ? C23 C24 C25 O25 -179.9(7) . . . . ? C28 C24 C25 O25 -0.8(11) . . . . ? C23 C24 C25 C26 -2.5(11) . . . . ? C28 C24 C25 C26 176.6(7) . . . . ? O25 C25 C26 C27 179.4(8) . . . . ? C24 C25 C26 C27 2.0(13) . . . . ? C25 C26 C27 O27 179.4(7) . . . . ? C25 C26 C27 C22 0.2(12) . . . . ? C23 C22 C27 O27 179.2(6) . . . . ? C21 C22 C27 O27 -2.4(10) . . . . ? C23 C22 C27 C26 -1.6(10) . . . . ? C21 C22 C27 C26 176.7(7) . . . . ? C2 C1 C28 C24 -86.3(7) . . . . ? C6 C1 C28 C24 94.4(6) . . . . ? C2 C1 C28 C53 42.1(7) . . . . ? C6 C1 C28 C53 -137.2(6) . . . . ? C25 C24 C28 C1 -95.1(7) . . . . ? C23 C24 C28 C1 84.0(7) . . . . ? C25 C24 C28 C53 137.0(7) . . . . ? C23 C24 C28 C53 -43.9(8) . . . . ? C3 C7 C29 C30 -167.1(5) . . . . ? C8 C7 C29 C30 66.6(6) . . . . ? C7 C29 C30 C31 -155.3(5) . . . . ? C29 C30 C31 C36 66.8(8) . . . . ? C29 C30 C31 C32 -112.9(7) . . . . ? C36 C31 C32 C33 0.7(11) . . . . ? C30 C31 C32 C33 -179.6(7) . . . . ? C31 C32 C33 C34 0.5(14) . . . . ? C32 C33 C34 C35 -1.8(16) . . . . ? C33 C34 C35 C36 1.8(16) . . . . ? C34 C35 C36 C31 -0.5(14) . . . . ? C32 C31 C36 C35 -0.8(11) . . . . ? C30 C31 C36 C35 179.5(7) . . . . ? C10 C14 C37 C38 -173.5(5) . . . . ? C15 C14 C37 C38 59.8(7) . . . . ? C14 C37 C38 C39 -175.4(5) . . . . ? C37 C38 C39 C40 -92.9(8) . . . . ? C37 C38 C39 C44 85.9(8) . . . . ? C44 C39 C40 C41 1.5(13) . . . . ? C38 C39 C40 C41 -179.7(8) . . . . ? C39 C40 C41 C42 -1.4(16) . . . . ? C40 C41 C42 C43 0.9(16) . . . . ? C41 C42 C43 C44 -0.6(13) . . . . ? C42 C43 C44 C39 0.8(11) . . . . ? C40 C39 C44 C43 -1.2(10) . . . . ? C38 C39 C44 C43 -180.0(6) . . . . ? C17 C21 C45 C46 -57.1(6) . . . . ? C22 C21 C45 C46 174.8(5) . . . . ? C21 C45 C46 C47 -61.2(7) . . . . ? C45 C46 C47 C48 128.6(7) . . . . ? C45 C46 C47 C52 -53.5(8) . . . . ? C52 C47 C48 C49 -1.8(12) . . . . ? C46 C47 C48 C49 176.1(8) . . . . ? C47 C48 C49 C50 -1.3(15) . . . . ? C48 C49 C50 C51 2.6(16) . . . . ? C49 C50 C51 C52 -0.8(16) . . . . ? C50 C51 C52 C47 -2.4(15) . . . . ? C48 C47 C52 C51 3.6(12) . . . . ? C46 C47 C52 C51 -174.2(8) . . . . ? C1 C28 C53 C54 171.4(6) . . . . ? C24 C28 C53 C54 -61.3(8) . . . . ? C28 C53 C54 C55 -56.8(9) . . . . ? C53 C54 C55 C60 -69.6(14) . . . . ? C53 C54 C55 C56 113.8(12) . . . . ? C60 C55 C56 C57 2(2) . . . . ? C54 C55 C56 C57 179.0(11) . . . . ? C55 C56 C57 C58 1(2) . . . . ? C56 C57 C58 C59 -4(2) . . . . ? C57 C58 C59 C60 2(2) . . . . ? C56 C55 C60 C59 -4(2) . . . . ? C54 C55 C60 C59 179.5(11) . . . . ? C58 C59 C60 C55 2(2) . . . . ? C1C N1 C1C C2C 89.3(17) 2 . . 2 ? C4C N1 C1C C2C -41(3) 2 . . 2 ? C4C N1 C1C C2C -133(3) . . . 2 ? C3C N1 C1C C2C 89.3(17) . . . 2 ? C2C N1 C1C C2C 171(3) . . . 2 ? C1C N1 C1C C4C -138.1(17) 2 . . . ? C4C N1 C1C C4C 92(4) 2 . . . ? C3C N1 C1C C4C -138.1(17) . . . . ? C2C N1 C1C C4C -57(2) . . . . ? C2C N1 C1C C4C 133(3) 2 . . . ? C1C N1 C1C C3C 0.000(1) 2 . . . ? C4C N1 C1C C3C -130(2) 2 . . . ? C4C N1 C1C C3C 138.1(17) . . . . ? C2C N1 C1C C3C 81.2(17) . . . . ? C2C N1 C1C C3C -89.3(17) 2 . . . ? C1C N1 C2C C4C -142(3) 2 . . . ? C1C N1 C2C C4C 66(2) . . . . ? C4C N1 C2C C4C -83(4) 2 . . . ? C3C N1 C2C C4C 140.3(19) . . . . ? C2C N1 C2C C4C 140.3(19) 2 . . . ? C1C N1 C2C C1C -152(3) . . . 2 ? C4C N1 C2C C1C 59(3) 2 . . 2 ? C4C N1 C2C C1C 142(3) . . . 2 ? C3C N1 C2C C1C -77.5(17) . . . 2 ? C2C N1 C2C C1C -77.5(17) 2 . . 2 ? C1C N1 C3C C1C 180.0 . . . 2 ? C4C N1 C3C C1C -58(2) 2 . . 2 ? C4C N1 C3C C1C 122(2) . . . 2 ? C2C N1 C3C C1C 73(2) . . . 2 ? C2C N1 C3C C1C -107(2) 2 . . 2 ? C1C N1 C3C C1C 180.0 2 . . . ? C4C N1 C3C C1C 122(2) 2 . . . ? C4C N1 C3C C1C -58(2) . . . . ? C2C N1 C3C C1C -107(2) . . . . ? C2C N1 C3C C1C 73(2) 2 . . . ? C2C C1C C3C N1 -60.9(13) 2 . . . ? C4C C1C C3C N1 31.9(12) . . . . ? N1 C1C C3C C1C 0.0 . . . 2 ? C2C C1C C3C C1C -60.9(13) 2 . . 2 ? C4C C1C C3C C1C 31.9(12) . . . 2 ? C1C N1 C4C C2C 44(3) 2 . . . ? C1C N1 C4C C2C -115(2) . . . . ? C4C N1 C4C C2C 123(2) 2 . . . ? C3C N1 C4C C2C -57(2) . . . . ? C2C N1 C4C C2C -173(2) 2 . . . ? C1C N1 C4C C1C 159(3) 2 . . . ? C4C N1 C4C C1C -121(2) 2 . . . ? C3C N1 C4C C1C 59(2) . . . . ? C2C N1 C4C C1C 115(2) . . . . ? C2C N1 C4C C1C -57(3) 2 . . . ? C1C C2C C4C N1 -30.2(19) 2 . . . ? N1 C2C C4C C1C -45.2(13) . . . . ? C1C C2C C4C C1C -75(2) 2 . . . ? C2C C1C C4C N1 37.0(17) 2 . . . ? C3C C1C C4C N1 -32.0(12) . . . . ? N1 C1C C4C C2C 50.6(16) . . . . ? C2C C1C C4C C2C 88(2) 2 . . . ? C3C C1C C4C C2C 19(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O13 0.84(2) 1.87(2) 2.705(7) 176(10) . O11 H11 O20 0.84(2) 2.02(3) 2.826(7) 161(8) . O13 H13 O7M 0.84 1.89 2.713(13) 166.8 . O6 H6 O25 0.84 2.02 2.815(8) 158.0 . O18 H18 O27 0.85(2) 1.92(2) 2.763(8) 174(10) . O25 H25 O1W 0.84 2.23 2.908(14) 137.3 2 O25 H25 Br1 0.84 2.49 3.296(5) 161.2 2 O20 H20 O1W 0.83(2) 2.23(7) 2.823(13) 128(8) 5_566 O20 H20 Br1 0.83(2) 2.69(7) 3.190(4) 120(7) 5_566 O27 H27 Br1 0.83(2) 2.61(4) 3.387(5) 155(8) 6_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.912 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.088 #==END data_Complex2 _database_code_depnum_ccdc_archive 'CCDC 254959' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C36H40O8*2C8H18N2Br2*C3H8O*2H20 _chemical_formula_sum 'C55 H88 Br4 N4 O11' _chemical_formula_weight 1300.93 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' Br Br -0.2901 2.4595 '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 _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4513(2) _cell_length_b 13.6703(2) _cell_length_c 19.7836(4) _cell_angle_alpha 71.716(5) _cell_angle_beta 79.631(5) _cell_angle_gamma 72.3940(10) _cell_volume 3034.15(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 2.711 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; dx = 35 mm, 30 sec./deg., 1 deg. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 24114 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0868 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10106 _reflns_number_gt 6452 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELX97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1997)' _computing_molecular_graphics DIAMOND _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+5.0632P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10106 _refine_ls_number_parameters 716 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6302(3) 0.5225(3) 0.3717(2) 0.0192(10) Uani 1 1 d . . . C2 C 0.6017(3) 0.6000(3) 0.4078(2) 0.0195(11) Uani 1 1 d . . . H2 H 0.6576 0.6027 0.4337 0.023 Uiso 1 1 calc R . . C3 C 0.4966(3) 0.6743(3) 0.4088(2) 0.0205(11) Uani 1 1 d . . . C4 C 0.4169(3) 0.6704(4) 0.3682(2) 0.0243(11) Uani 1 1 d . . . O4 O 0.3101(3) 0.7390(3) 0.3638(2) 0.0352(10) Uani 1 1 d . . . H4 H 0.317(5) 0.788(5) 0.365(3) 0.053 Uiso 1 1 d . . . C5 C 0.4420(4) 0.5942(4) 0.3313(2) 0.0238(11) Uani 1 1 d . . . H5 H 0.3866 0.5911 0.3053 0.029 Uiso 1 1 calc R . . C6 C 0.5479(4) 0.5225(4) 0.3322(2) 0.0217(11) Uani 1 1 d . . . O6 O 0.5763(3) 0.4483(3) 0.29368(18) 0.0288(8) Uani 1 1 d . . . H6 H 0.530(4) 0.466(4) 0.265(3) 0.043 Uiso 1 1 d . . . C7 C 0.4705(4) 0.7552(4) 0.4520(2) 0.0228(11) Uani 1 1 d . . . H7 H 0.3863 0.7830 0.4576 0.027 Uiso 1 1 calc R . . C8 C 0.5178(3) 0.8508(3) 0.4106(2) 0.0202(11) Uani 1 1 d . . . C9 C 0.6241(3) 0.8569(4) 0.4180(2) 0.0207(11) Uani 1 1 d . . . H9 H 0.6688 0.7986 0.4507 0.025 Uiso 1 1 calc R . . C10 C 0.6697(3) 0.9414(3) 0.3812(2) 0.0194(10) Uani 1 1 d . . . C11 C 0.6018(4) 1.0258(3) 0.3332(2) 0.0235(11) Uani 1 1 d . . . O11 O 0.6492(3) 1.1081(3) 0.29399(19) 0.0328(9) Uani 1 1 d . . . H11 H 0.607(4) 1.146(4) 0.273(3) 0.049 Uiso 1 1 d . . . C12 C 0.4944(4) 1.0254(4) 0.3244(2) 0.0270(12) Uani 1 1 d . . . H12 H 0.4492 1.0843 0.2923 0.032 Uiso 1 1 calc R . . C13 C 0.4528(4) 0.9382(4) 0.3628(2) 0.0255(11) Uani 1 1 d . . . O13 O 0.3475(3) 0.9324(3) 0.35462(19) 0.0354(9) Uani 1 1 d . . . H13 H 0.312(4) 0.989(4) 0.326(3) 0.053 Uiso 1 1 d . . . C14 C 0.7848(3) 0.9466(4) 0.3928(2) 0.0214(11) Uani 1 1 d . A . H14 H 0.7814 1.0241 0.3809 0.026 Uiso 1 1 calc R . . C15 C 0.8797(3) 0.9001(4) 0.3420(2) 0.0220(11) Uani 1 1 d . . . C16 C 0.9261(3) 0.7905(4) 0.3544(2) 0.0228(11) Uani 1 1 d . . . H16 H 0.8945 0.7442 0.3943 0.027 Uiso 1 1 calc R . . C17 C 1.0167(3) 0.7449(3) 0.3111(2) 0.0201(11) Uani 1 1 d . . . C18 C 1.0607(3) 0.8142(4) 0.2530(2) 0.0239(11) Uani 1 1 d . . . O18 O 1.1502(3) 0.7696(3) 0.20953(18) 0.0319(9) Uani 1 1 d . . . H18 H 1.155(5) 0.808(5) 0.177(3) 0.048 Uiso 1 1 d . . . C19 C 1.0171(4) 0.9234(4) 0.2383(2) 0.0263(12) Uani 1 1 d . . . H19 H 1.0503 0.9693 0.1991 0.032 Uiso 1 1 calc R . . C20 C 0.9248(4) 0.9659(4) 0.2808(2) 0.0251(11) Uani 1 1 d . . . O20 O 0.8820(3) 1.0758(3) 0.26059(19) 0.0362(9) Uani 1 1 d . . . H20 H 0.817(4) 1.090(4) 0.273(3) 0.054 Uiso 1 1 d . . . C21 C 1.0644(3) 0.6240(4) 0.3260(2) 0.0224(11) Uani 1 1 d . . . H21 H 1.1382 0.6121 0.2959 0.027 Uiso 1 1 calc R . . C22 C 0.9894(3) 0.5740(3) 0.3015(2) 0.0189(10) Uani 1 1 d . . . C23 C 0.9056(3) 0.5317(3) 0.3462(2) 0.0185(10) Uani 1 1 d . . . H23 H 0.8939 0.5350 0.3944 0.022 Uiso 1 1 calc R . . C24 C 0.8370(3) 0.4843(3) 0.3250(2) 0.0197(11) Uani 1 1 d . . . C25 C 0.8552(4) 0.4820(4) 0.2538(2) 0.0240(11) Uani 1 1 d . . . O25 O 0.7929(3) 0.4393(3) 0.22530(18) 0.0374(10) Uani 1 1 d . . . H25 H 0.738(4) 0.447(5) 0.245(3) 0.056 Uiso 1 1 d . . . C26 C 0.9372(4) 0.5248(4) 0.2071(2) 0.0272(12) Uani 1 1 d . . . H26 H 0.9483 0.5223 0.1588 0.033 Uiso 1 1 calc R . . C27 C 1.0028(3) 0.5710(4) 0.2301(2) 0.0229(11) Uani 1 1 d . . . O27 O 1.0785(3) 0.6145(3) 0.17930(17) 0.0339(9) Uani 1 1 d . . . H27 H 1.108(4) 0.647(4) 0.193(3) 0.051 Uiso 1 1 d . . . C28 C 0.7445(3) 0.4392(3) 0.3757(2) 0.0181(10) Uani 1 1 d . . . H28 H 0.7359 0.3811 0.3581 0.022 Uiso 1 1 calc R . . C29 C 0.5088(4) 0.7034(4) 0.5273(2) 0.0269(12) Uani 1 1 d . . . H29A H 0.4816 0.6384 0.5491 0.032 Uiso 1 1 calc R . . H29B H 0.5926 0.6812 0.5238 0.032 Uiso 1 1 calc R . . C30 C 0.4661(5) 0.7768(4) 0.5759(3) 0.0462(15) Uani 1 1 d . . . H30A H 0.4929 0.7391 0.6233 0.069 Uiso 1 1 calc R . . H30B H 0.3831 0.7983 0.5803 0.069 Uiso 1 1 calc R . . H30C H 0.4946 0.8404 0.5554 0.069 Uiso 1 1 calc R . . C31 C 0.8128(4) 0.8971(4) 0.4714(3) 0.0375(13) Uani 1 1 d . . . H31A H 0.8105 0.8216 0.4858 0.045 Uiso 0.543(9) 1 calc PR A 1 H31B H 0.8916 0.8975 0.4735 0.045 Uiso 0.543(9) 1 calc PR A 1 H31C H 0.7428 0.9106 0.5038 0.045 Uiso 0.457(9) 1 calc PR A 2 H31D H 0.8445 0.8189 0.4808 0.045 Uiso 0.457(9) 1 calc PR A 2 C32 C 0.7426(8) 0.9462(7) 0.5229(5) 0.040(3) Uani 0.543(9) 1 d P A 1 H32A H 0.7693 0.9081 0.5702 0.061 Uiso 0.543(9) 1 calc PR A 1 H32B H 0.6646 0.9439 0.5235 0.061 Uiso 0.543(9) 1 calc PR A 1 H32C H 0.7454 1.0207 0.5106 0.061 Uiso 0.543(9) 1 calc PR A 1 C32B C 0.8980(9) 0.9461(9) 0.4859(6) 0.044(4) Uani 0.457(9) 1 d P A 2 H32D H 0.8813 0.9534 0.5346 0.066 Uiso 0.457(9) 1 calc PR A 2 H32E H 0.8931 1.0166 0.4517 0.066 Uiso 0.457(9) 1 calc PR A 2 H32F H 0.9745 0.8997 0.4805 0.066 Uiso 0.457(9) 1 calc PR A 2 C33 C 1.0917(4) 0.5707(4) 0.4043(2) 0.0253(11) Uani 1 1 d . . . H33A H 1.1367 0.6098 0.4171 0.030 Uiso 1 1 calc R . . H33B H 1.0201 0.5762 0.4359 0.030 Uiso 1 1 calc R . . C34 C 1.1575(4) 0.4532(4) 0.4177(3) 0.0368(13) Uani 1 1 d . . . H34A H 1.1722 0.4233 0.4682 0.055 Uiso 1 1 calc R . . H34B H 1.2296 0.4472 0.3877 0.055 Uiso 1 1 calc R . . H34C H 1.1130 0.4136 0.4060 0.055 Uiso 1 1 calc R . . C35 C 0.7747(3) 0.3875(3) 0.4531(2) 0.0230(11) Uani 1 1 d . . . H35A H 0.7920 0.4408 0.4707 0.028 Uiso 1 1 calc R . . H35B H 0.7081 0.3670 0.4833 0.028 Uiso 1 1 calc R . . C36 C 0.8754(4) 0.2891(4) 0.4614(3) 0.0383(14) Uani 1 1 d . . . H36A H 0.8905 0.2599 0.5118 0.058 Uiso 1 1 calc R . . H36B H 0.9421 0.3090 0.4325 0.058 Uiso 1 1 calc R . . H36C H 0.8582 0.2351 0.4453 0.058 Uiso 1 1 calc R . . Br1 Br 0.42396(4) 0.52139(4) 0.16473(3) 0.03231(14) Uani 1 1 d . . . Br2 Br 1.16691(4) 0.93366(4) 0.05426(3) 0.03150(14) Uani 1 1 d . . . Br3 Br 0.84656(4) 0.67817(4) 0.00338(3) 0.03636(15) Uani 1 1 d . . . Br4 Br 0.49550(4) 0.17560(4) 0.07329(3) 0.03733(15) Uani 1 1 d . . . N1C N 0.8568(3) 0.2609(3) 0.05551(18) 0.0172(8) Uani 1 1 d . . . N1CB N 0.7154(3) 0.8539(3) 0.1525(2) 0.0330(10) Uani 1 1 d . . . N2C N 0.7160(3) 0.4411(3) 0.01742(18) 0.0150(8) Uani 1 1 d . . . N2CB N 0.5267(3) 0.8195(3) 0.1543(2) 0.0338(10) Uani 1 1 d . . . C1C C 0.9418(3) 0.1550(3) 0.0779(2) 0.0254(11) Uani 1 1 d . . . H1C1 H 0.9367 0.1083 0.0504 0.038 Uiso 1 1 calc R . . H1C2 H 0.9261 0.1219 0.1290 0.038 Uiso 1 1 calc R . . H1C3 H 1.0181 0.1655 0.0688 0.038 Uiso 1 1 calc R . . C1CB C 0.8286(4) 0.8731(5) 0.1513(4) 0.079(2) Uani 1 1 d . . . H1C4 H 0.8537 0.8440 0.1995 0.118 Uiso 1 1 calc R . . H1C5 H 0.8218 0.9500 0.1350 0.118 Uiso 1 1 calc R . . H1C6 H 0.8839 0.8378 0.1186 0.118 Uiso 1 1 calc R . . C2C C 0.6335(3) 0.5488(3) -0.0060(2) 0.0219(11) Uani 1 1 d . . . H2C1 H 0.6720 0.6049 -0.0145 0.033 Uiso 1 1 calc R . . H2C2 H 0.5708 0.5567 0.0315 0.033 Uiso 1 1 calc R . . H2C3 H 0.6039 0.5548 -0.0502 0.033 Uiso 1 1 calc R . . C2CB C 0.4135(5) 0.7996(5) 0.1560(4) 0.085(3) Uani 1 1 d . . . H2C4 H 0.3547 0.8674 0.1491 0.127 Uiso 1 1 calc R . . H2C5 H 0.3965 0.7508 0.2023 0.127 Uiso 1 1 calc R . . H2C6 H 0.4158 0.7675 0.1177 0.127 Uiso 1 1 calc R . . C3C C 0.7394(3) 0.2466(3) 0.0679(2) 0.0211(11) Uani 1 1 d . . . H3C1 H 0.7160 0.2258 0.1199 0.025 Uiso 1 1 calc R . . H3C2 H 0.7373 0.1895 0.0478 0.025 Uiso 1 1 calc R . . C3CB C 0.6733(5) 0.8989(5) 0.0794(3) 0.0528(17) Uani 1 1 d . . . H3C3 H 0.7218 0.8576 0.0469 0.063 Uiso 1 1 calc R . . H3C4 H 0.6770 0.9741 0.0596 0.063 Uiso 1 1 calc R . . C4C C 0.6590(3) 0.3528(3) 0.0313(2) 0.0179(10) Uani 1 1 d . . . H4C1 H 0.6406 0.3492 -0.0143 0.022 Uiso 1 1 calc R . . H4C2 H 0.5876 0.3671 0.0625 0.022 Uiso 1 1 calc R . . C4CB C 0.5524(5) 0.8932(5) 0.0849(3) 0.0558(17) Uani 1 1 d . . . H4C3 H 0.4999 0.9651 0.0809 0.067 Uiso 1 1 calc R . . H4C4 H 0.5423 0.8676 0.0455 0.067 Uiso 1 1 calc R . . C5C C 0.8800(3) 0.3122(3) -0.0228(2) 0.0186(10) Uani 1 1 d . . . H5C1 H 0.8585 0.2744 -0.0514 0.022 Uiso 1 1 calc R . . H5C2 H 0.9617 0.3079 -0.0346 0.022 Uiso 1 1 calc R . . C5CB C 0.6294(4) 0.9062(5) 0.2027(3) 0.0458(15) Uani 1 1 d . . . H5C3 H 0.6130 0.9848 0.1835 0.055 Uiso 1 1 calc R . . H5C4 H 0.6591 0.8854 0.2498 0.055 Uiso 1 1 calc R . . C6C C 0.8115(3) 0.4286(3) -0.0405(2) 0.0187(10) Uani 1 1 d . . . H6C1 H 0.8603 0.4753 -0.0433 0.022 Uiso 1 1 calc R . . H6C2 H 0.7810 0.4493 -0.0874 0.022 Uiso 1 1 calc R . . C6CB C 0.5209(4) 0.8710(5) 0.2112(3) 0.0529(16) Uani 1 1 d . . . H6C3 H 0.5129 0.8200 0.2588 0.063 Uiso 1 1 calc R . . H6C4 H 0.4543 0.9337 0.2073 0.063 Uiso 1 1 calc R . . C7C C 0.8638(3) 0.3320(3) 0.0980(2) 0.0211(11) Uani 1 1 d . . . H7C1 H 0.9353 0.3539 0.0829 0.025 Uiso 1 1 calc R . . H7C2 H 0.8628 0.2932 0.1494 0.025 Uiso 1 1 calc R . . C7CB C 0.7236(4) 0.7364(4) 0.1765(3) 0.0467(15) Uani 1 1 d . . . H7C3 H 0.7365 0.7077 0.2278 0.056 Uiso 1 1 calc R . . H7C4 H 0.7884 0.6987 0.1490 0.056 Uiso 1 1 calc R . . C8C C 0.7621(3) 0.4311(3) 0.0852(2) 0.0199(10) Uani 1 1 d . . . H8C1 H 0.7032 0.4234 0.1259 0.024 Uiso 1 1 calc R . . H8C2 H 0.7862 0.4958 0.0807 0.024 Uiso 1 1 calc R . . C8CB C 0.6151(5) 0.7178(4) 0.1649(4) 0.067(2) Uani 1 1 d . . . H8C3 H 0.6272 0.6909 0.1224 0.080 Uiso 1 1 calc R . . H8C4 H 0.5916 0.6639 0.2070 0.080 Uiso 1 1 calc R . . O1W O 0.5222(4) 1.2608(3) 0.2021(2) 0.0488(11) Uani 1 1 d . . . H1WA H 1.231(5) 1.047(5) 0.098(3) 0.073 Uiso 1 1 d . . . H1WB H 1.277(5) 1.130(5) 0.112(4) 0.073 Uiso 1 1 d . . . O2W O 1.2674(4) 1.0711(4) 0.1287(3) 0.0711(14) Uani 1 1 d . . . H2WA H 0.487(6) 1.317(6) 0.204(4) 0.107 Uiso 1 1 d . . . H2WB H 0.506(6) 1.244(6) 0.169(4) 0.107 Uiso 1 1 d . . . O1P O 0.2284(4) 1.0877(3) 0.2637(2) 0.0648(13) Uani 1 1 d . . . H1P H 0.282(5) 1.092(5) 0.219(4) 0.097 Uiso 1 1 d . . . C2P C 0.1261(5) 1.1652(6) 0.2780(4) 0.077(2) Uani 1 1 d . . . H2P1 H 0.0872 1.1348 0.3247 0.093 Uiso 1 1 calc R . . H2P2 H 0.0747 1.1831 0.2406 0.093 Uiso 1 1 calc R . . C3P C 0.1523(7) 1.2643(6) 0.2794(5) 0.110(3) Uani 1 1 d . . . H3P1 H 0.0814 1.3138 0.2933 0.132 Uiso 1 1 calc R . . H3P2 H 0.2047 1.2452 0.3164 0.132 Uiso 1 1 calc R . . C4P C 0.2023(7) 1.3190(6) 0.2120(6) 0.140(4) Uani 1 1 d . . . H4P1 H 0.2195 1.3815 0.2172 0.210 Uiso 1 1 calc R . . H4P2 H 0.1492 1.3421 0.1755 0.210 Uiso 1 1 calc R . . H4P3 H 0.2723 1.2705 0.1975 0.210 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 C1 0.027(3) 0.017(3) 0.012(2) 0.003(2) -0.0037(19) -0.0084(19) C2 0.022(2) 0.023(3) 0.015(3) -0.002(2) -0.0045(19) -0.009(2) C3 0.027(3) 0.017(3) 0.012(3) 0.002(2) 0.0005(19) -0.007(2) C4 0.020(3) 0.026(3) 0.023(3) 0.000(2) -0.005(2) -0.007(2) O4 0.0255(19) 0.038(3) 0.046(2) -0.018(2) -0.0111(16) -0.0012(17) C5 0.024(3) 0.030(3) 0.021(3) -0.006(2) -0.007(2) -0.010(2) C6 0.036(3) 0.022(3) 0.012(3) -0.006(2) -0.005(2) -0.012(2) O6 0.030(2) 0.030(2) 0.032(2) -0.0113(18) -0.0161(15) -0.0066(15) C7 0.020(2) 0.025(3) 0.020(3) -0.004(2) 0.003(2) -0.006(2) C8 0.024(3) 0.022(3) 0.014(3) -0.008(2) -0.0008(19) -0.003(2) C9 0.027(3) 0.022(3) 0.012(2) -0.009(2) -0.0050(19) 0.002(2) C10 0.029(3) 0.014(3) 0.014(3) -0.009(2) 0.005(2) -0.003(2) C11 0.037(3) 0.014(3) 0.017(3) -0.005(2) 0.005(2) -0.007(2) O11 0.036(2) 0.019(2) 0.034(2) 0.0032(17) -0.0041(16) -0.0038(15) C12 0.029(3) 0.022(3) 0.022(3) 0.001(2) -0.009(2) 0.000(2) C13 0.024(3) 0.023(3) 0.028(3) -0.010(2) -0.004(2) -0.001(2) O13 0.028(2) 0.028(2) 0.043(2) 0.0018(18) -0.0173(16) -0.0027(15) C14 0.030(3) 0.019(3) 0.015(3) -0.001(2) -0.003(2) -0.008(2) C15 0.024(2) 0.022(3) 0.019(3) -0.003(2) -0.002(2) -0.008(2) C16 0.029(3) 0.024(3) 0.016(3) 0.000(2) -0.002(2) -0.012(2) C17 0.020(2) 0.024(3) 0.017(3) -0.004(2) -0.005(2) -0.005(2) C18 0.020(3) 0.031(3) 0.019(3) -0.007(2) -0.001(2) -0.005(2) O18 0.0284(18) 0.028(2) 0.028(2) 0.0006(17) 0.0060(17) -0.0043(16) C19 0.026(3) 0.028(3) 0.022(3) -0.001(2) 0.004(2) -0.012(2) C20 0.029(3) 0.017(3) 0.025(3) 0.003(2) -0.006(2) -0.007(2) O20 0.038(2) 0.025(2) 0.037(2) -0.0020(17) 0.0075(18) -0.0081(17) C21 0.019(2) 0.029(3) 0.018(3) -0.004(2) -0.0008(19) -0.006(2) C22 0.021(2) 0.016(3) 0.015(3) -0.001(2) -0.0047(19) 0.0017(19) C23 0.021(2) 0.022(3) 0.011(2) -0.007(2) -0.0027(19) -0.0015(19) C24 0.023(2) 0.015(3) 0.018(3) -0.004(2) -0.0060(19) 0.0028(19) C25 0.028(3) 0.025(3) 0.020(3) -0.010(2) -0.011(2) -0.001(2) O25 0.038(2) 0.061(3) 0.026(2) -0.0260(19) -0.0020(17) -0.017(2) C26 0.033(3) 0.032(3) 0.012(3) -0.008(2) -0.002(2) 0.000(2) C27 0.022(3) 0.026(3) 0.016(3) -0.006(2) 0.000(2) -0.001(2) O27 0.036(2) 0.054(3) 0.0143(19) -0.0088(17) 0.0067(15) -0.0207(17) C28 0.027(2) 0.016(3) 0.015(3) -0.006(2) -0.0069(19) -0.0055(19) C29 0.034(3) 0.024(3) 0.021(3) -0.003(2) 0.002(2) -0.009(2) C30 0.072(4) 0.040(4) 0.025(3) -0.009(3) -0.002(3) -0.015(3) C31 0.045(3) 0.052(4) 0.022(3) -0.011(3) -0.003(2) -0.022(3) C32 0.058(7) 0.032(6) 0.022(6) -0.013(5) -0.004(5) 0.008(5) C32B 0.056(8) 0.041(8) 0.042(8) 0.000(6) -0.029(6) -0.023(6) C33 0.027(3) 0.029(3) 0.022(3) -0.006(2) -0.009(2) -0.009(2) C34 0.037(3) 0.036(3) 0.032(3) 0.000(3) -0.016(2) -0.005(2) C35 0.027(3) 0.024(3) 0.021(3) -0.005(2) -0.004(2) -0.010(2) C36 0.056(3) 0.023(3) 0.031(3) 0.000(3) -0.019(3) -0.002(2) Br1 0.0427(3) 0.0299(3) 0.0271(3) -0.0088(2) -0.0151(2) -0.0058(2) Br2 0.0410(3) 0.0255(3) 0.0256(3) -0.0078(2) -0.0040(2) -0.0039(2) Br3 0.0274(3) 0.0403(3) 0.0462(4) -0.0115(3) -0.0034(2) -0.0161(2) Br4 0.0347(3) 0.0271(3) 0.0544(4) -0.0162(3) -0.0046(2) -0.0087(2) N1C 0.0163(19) 0.017(2) 0.015(2) -0.0021(17) -0.0011(15) -0.0027(15) N1CB 0.029(2) 0.029(3) 0.036(3) -0.007(2) 0.0022(19) -0.0038(18) N2C 0.0158(18) 0.016(2) 0.014(2) -0.0056(17) -0.0025(15) -0.0034(15) N2CB 0.043(3) 0.020(2) 0.039(3) 0.000(2) -0.014(2) -0.0114(19) C1C 0.027(3) 0.017(3) 0.026(3) -0.003(2) -0.010(2) 0.004(2) C1CB 0.031(3) 0.061(5) 0.129(7) -0.008(4) -0.005(4) -0.011(3) C2C 0.022(2) 0.016(3) 0.027(3) -0.010(2) -0.006(2) 0.0028(19) C2CB 0.067(5) 0.053(5) 0.147(7) -0.008(5) -0.053(5) -0.032(3) C3C 0.016(2) 0.022(3) 0.023(3) -0.003(2) -0.0020(19) -0.0048(19) C3CB 0.072(4) 0.036(4) 0.031(4) -0.002(3) 0.014(3) -0.004(3) C4C 0.016(2) 0.023(3) 0.017(3) -0.007(2) -0.0033(18) -0.0061(18) C4CB 0.066(4) 0.056(4) 0.039(4) 0.004(3) -0.027(3) -0.012(3) C5C 0.018(2) 0.024(3) 0.013(3) -0.008(2) 0.0003(18) -0.0043(19) C5CB 0.043(3) 0.052(4) 0.045(4) -0.027(3) -0.011(3) 0.001(3) C6C 0.017(2) 0.023(3) 0.014(3) -0.004(2) 0.0032(19) -0.0056(19) C6CB 0.034(3) 0.086(5) 0.044(4) -0.030(4) 0.006(3) -0.016(3) C7C 0.021(2) 0.027(3) 0.018(3) -0.009(2) -0.0081(19) -0.004(2) C7CB 0.044(3) 0.036(4) 0.045(4) -0.005(3) -0.001(3) 0.004(3) C8C 0.023(2) 0.027(3) 0.014(3) -0.011(2) -0.0044(19) -0.004(2) C8CB 0.061(4) 0.023(4) 0.108(6) -0.004(4) -0.028(4) -0.001(3) O1W 0.070(3) 0.028(2) 0.041(3) -0.007(2) -0.019(2) 0.0049(19) O2W 0.097(4) 0.055(3) 0.074(4) -0.015(3) -0.007(3) -0.041(3) O1P 0.071(3) 0.039(3) 0.073(3) -0.006(2) -0.037(2) 0.009(2) C2P 0.051(4) 0.070(5) 0.096(6) -0.004(5) -0.021(4) -0.006(4) C3P 0.110(7) 0.053(6) 0.122(8) -0.012(5) 0.024(6) 0.010(5) C4P 0.092(6) 0.063(6) 0.212(12) -0.009(7) 0.035(7) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.383(6) . ? C1 C6 1.395(6) . ? C1 C28 1.528(6) . ? C2 C3 1.395(6) . ? C2 H2 0.9500 . ? C3 C4 1.406(6) . ? C3 C7 1.529(6) . ? C4 O4 1.376(5) . ? C4 C5 1.382(6) . ? O4 H4 0.71(5) . ? C5 C6 1.383(6) . ? C5 H5 0.9500 . ? C6 O6 1.381(5) . ? O6 H6 0.80(5) . ? C7 C29 1.529(6) . ? C7 C8 1.533(6) . ? C7 H7 1.0000 . ? C8 C9 1.386(6) . ? C8 C13 1.399(6) . ? C9 C10 1.381(6) . ? C9 H9 0.9500 . ? C10 C11 1.400(6) . ? C10 C14 1.517(6) . ? C11 O11 1.380(5) . ? C11 C12 1.381(6) . ? O11 H11 0.71(5) . ? C12 C13 1.389(6) . ? C12 H12 0.9500 . ? C13 O13 1.378(5) . ? O13 H13 0.85(5) . ? C14 C15 1.527(6) . ? C14 C31 1.547(6) . ? C14 H14 1.0000 . ? C15 C16 1.391(6) . ? C15 C20 1.402(6) . ? C16 C17 1.399(6) . ? C16 H16 0.9500 . ? C17 C18 1.387(6) . ? C17 C21 1.527(6) . ? C18 C19 1.378(6) . ? C18 O18 1.389(5) . ? O18 H18 0.70(5) . ? C19 C20 1.386(6) . ? C19 H19 0.9500 . ? C20 O20 1.385(5) . ? O20 H20 0.79(5) . ? C21 C22 1.527(6) . ? C21 C33 1.541(6) . ? C21 H21 1.0000 . ? C22 C23 1.385(6) . ? C22 C27 1.404(6) . ? C23 C24 1.399(6) . ? C23 H23 0.9500 . ? C24 C25 1.396(6) . ? C24 C28 1.529(6) . ? C25 O25 1.377(5) . ? C25 C26 1.386(6) . ? O25 H25 0.72(5) . ? C26 C27 1.379(6) . ? C26 H26 0.9500 . ? C27 O27 1.370(5) . ? O27 H27 0.79(5) . ? C28 C35 1.534(6) . ? C28 H28 1.0000 . ? C29 C30 1.521(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.416(9) . ? C31 C32B 1.521(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 H31C 0.9900 . ? C31 H31D 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C33 C34 1.529(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.524(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N1C C7C 1.498(5) . ? N1C C3C 1.500(5) . ? N1C C5C 1.501(5) . ? N1C C1C 1.501(5) . ? N1CB C5CB 1.497(6) . ? N1CB C7CB 1.501(6) . ? N1CB C1CB 1.504(6) . ? N1CB C3CB 1.505(7) . ? N2C C8C 1.504(5) . ? N2C C6C 1.506(5) . ? N2C C2C 1.506(5) . ? N2C C4C 1.509(5) . ? N2CB C8CB 1.470(6) . ? N2CB C4CB 1.474(6) . ? N2CB C6CB 1.484(7) . ? N2CB C2CB 1.507(6) . ? C1C H1C1 0.9800 . ? C1C H1C2 0.9800 . ? C1C H1C3 0.9800 . ? C1CB H1C4 0.9800 . ? C1CB H1C5 0.9800 . ? C1CB H1C6 0.9800 . ? C2C H2C1 0.9800 . ? C2C H2C2 0.9800 . ? C2C H2C3 0.9800 . ? C2CB H2C4 0.9800 . ? C2CB H2C5 0.9800 . ? C2CB H2C6 0.9800 . ? C3C C4C 1.536(5) . ? C3C H3C1 0.9900 . ? C3C H3C2 0.9900 . ? C3CB C4CB 1.514(7) . ? C3CB H3C3 0.9900 . ? C3CB H3C4 0.9900 . ? C4C H4C1 0.9900 . ? C4C H4C2 0.9900 . ? C4CB H4C3 0.9900 . ? C4CB H4C4 0.9900 . ? C5C C6C 1.523(6) . ? C5C H5C1 0.9900 . ? C5C H5C2 0.9900 . ? C5CB C6CB 1.531(7) . ? C5CB H5C3 0.9900 . ? C5CB H5C4 0.9900 . ? C6C H6C1 0.9900 . ? C6C H6C2 0.9900 . ? C6CB H6C3 0.9900 . ? C6CB H6C4 0.9900 . ? C7C C8C 1.538(6) . ? C7C H7C1 0.9900 . ? C7C H7C2 0.9900 . ? C7CB C8CB 1.516(7) . ? C7CB H7C3 0.9900 . ? C7CB H7C4 0.9900 . ? C8C H8C1 0.9900 . ? C8C H8C2 0.9900 . ? C8CB H8C3 0.9900 . ? C8CB H8C4 0.9900 . ? O1W H2WA 0.77(7) . ? O1W H2WB 0.83(7) . ? O2W H1WA 1.00(6) . ? O2W H1WB 0.80(6) . ? O1P C2P 1.438(7) . ? O1P H1P 1.01(7) . ? C2P C3P 1.495(10) . ? C2P H2P1 0.9900 . ? C2P H2P2 0.9900 . ? C3P C4P 1.443(10) . ? C3P H3P1 0.9900 . ? C3P H3P2 0.9900 . ? C4P H4P1 0.9800 . ? C4P H4P2 0.9800 . ? C4P H4P3 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 C2 C1 C6 116.6(4) . . ? C2 C1 C28 122.2(4) . . ? C6 C1 C28 121.2(4) . . ? C1 C2 C3 124.4(4) . . ? C1 C2 H2 117.8 . . ? C3 C2 H2 117.8 . . ? C2 C3 C4 116.5(4) . . ? C2 C3 C7 121.2(4) . . ? C4 C3 C7 122.3(4) . . ? O4 C4 C5 116.2(4) . . ? O4 C4 C3 122.9(4) . . ? C5 C4 C3 120.9(4) . . ? C4 O4 H4 105(5) . . ? C4 C5 C6 120.0(4) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? O6 C6 C5 121.1(4) . . ? O6 C6 C1 117.4(4) . . ? C5 C6 C1 121.6(4) . . ? C6 O6 H6 108(4) . . ? C3 C7 C29 112.1(4) . . ? C3 C7 C8 110.7(3) . . ? C29 C7 C8 113.1(4) . . ? C3 C7 H7 106.8 . . ? C29 C7 H7 106.8 . . ? C8 C7 H7 106.8 . . ? C9 C8 C13 116.6(4) . . ? C9 C8 C7 123.3(4) . . ? C13 C8 C7 120.1(4) . . ? C10 C9 C8 124.8(4) . . ? C10 C9 H9 117.6 . . ? C8 C9 H9 117.6 . . ? C9 C10 C11 116.2(4) . . ? C9 C10 C14 123.1(4) . . ? C11 C10 C14 120.7(4) . . ? O11 C11 C12 122.0(4) . . ? O11 C11 C10 116.2(4) . . ? C12 C11 C10 121.7(4) . . ? C11 O11 H11 106(5) . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? O13 C13 C12 121.9(4) . . ? O13 C13 C8 117.0(4) . . ? C12 C13 C8 121.0(4) . . ? C13 O13 H13 112(4) . . ? C10 C14 C15 112.6(4) . . ? C10 C14 C31 113.2(4) . . ? C15 C14 C31 111.4(4) . . ? C10 C14 H14 106.4 . . ? C15 C14 H14 106.4 . . ? C31 C14 H14 106.4 . . ? C16 C15 C20 116.9(4) . . ? C16 C15 C14 121.6(4) . . ? C20 C15 C14 121.5(4) . . ? C15 C16 C17 123.3(4) . . ? C15 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C18 C17 C16 117.1(4) . . ? C18 C17 C21 121.1(4) . . ? C16 C17 C21 121.8(4) . . ? C19 C18 C17 121.7(4) . . ? C19 C18 O18 120.8(4) . . ? C17 C18 O18 117.5(4) . . ? C18 O18 H18 108(5) . . ? C18 C19 C20 119.8(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? O20 C20 C19 116.6(4) . . ? O20 C20 C15 122.4(4) . . ? C19 C20 C15 121.0(4) . . ? C20 O20 H20 108(4) . . ? C22 C21 C17 111.7(3) . . ? C22 C21 C33 113.7(4) . . ? C17 C21 C33 111.8(4) . . ? C22 C21 H21 106.3 . . ? C17 C21 H21 106.3 . . ? C33 C21 H21 106.3 . . ? C23 C22 C27 116.9(4) . . ? C23 C22 C21 123.3(4) . . ? C27 C22 C21 119.8(4) . . ? C22 C23 C24 124.1(4) . . ? C22 C23 H23 117.9 . . ? C24 C23 H23 117.9 . . ? C25 C24 C23 116.6(4) . . ? C25 C24 C28 120.6(4) . . ? C23 C24 C28 122.8(4) . . ? O25 C25 C26 116.1(4) . . ? O25 C25 C24 122.9(4) . . ? C26 C25 C24 121.1(4) . . ? C25 O25 H25 106(5) . . ? C27 C26 C25 120.5(4) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? O27 C27 C26 116.0(4) . . ? O27 C27 C22 123.1(4) . . ? C26 C27 C22 120.8(4) . . ? C27 O27 H27 113(4) . . ? C1 C28 C24 111.6(3) . . ? C1 C28 C35 111.5(4) . . ? C24 C28 C35 113.8(3) . . ? C1 C28 H28 106.5 . . ? C24 C28 H28 106.5 . . ? C35 C28 H28 106.5 . . ? C30 C29 C7 113.4(4) . . ? C30 C29 H29A 108.9 . . ? C7 C29 H29A 108.9 . . ? C30 C29 H29B 108.9 . . ? C7 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? 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 C32B 82.7(7) . . ? C32 C31 C14 117.3(5) . . ? C32B C31 C14 109.8(6) . . ? C32 C31 H31A 108.0 . . ? C32B C31 H31A 129.5 . . ? C14 C31 H31A 108.0 . . ? C32 C31 H31B 108.0 . . ? C32B C31 H31B 28.6 . . ? C14 C31 H31B 108.0 . . ? H31A C31 H31B 107.2 . . ? C32 C31 H31C 27.3 . . ? C32B C31 H31C 109.7 . . ? C14 C31 H31C 109.7 . . ? H31A C31 H31C 87.2 . . ? H31B C31 H31C 132.7 . . ? C32 C31 H31D 123.3 . . ? C32B C31 H31D 109.7 . . ? C14 C31 H31D 109.7 . . ? H31A C31 H31D 23.9 . . ? H31B C31 H31D 84.4 . . ? H31C C31 H31D 108.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C32B H32D 109.5 . . ? C31 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C34 C33 C21 113.0(4) . . ? C34 C33 H33A 109.0 . . ? C21 C33 H33A 109.0 . . ? C34 C33 H33B 109.0 . . ? C21 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? 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 C28 113.3(4) . . ? C36 C35 H35A 108.9 . . ? C28 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C28 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C7C N1C C3C 109.2(3) . . ? C7C N1C C5C 109.7(3) . . ? C3C N1C C5C 108.1(3) . . ? C7C N1C C1C 109.5(3) . . ? C3C N1C C1C 110.4(3) . . ? C5C N1C C1C 109.9(3) . . ? C5CB N1CB C7CB 108.4(4) . . ? C5CB N1CB C1CB 110.6(4) . . ? C7CB N1CB C1CB 110.6(4) . . ? C5CB N1CB C3CB 107.9(4) . . ? C7CB N1CB C3CB 108.2(4) . . ? C1CB N1CB C3CB 110.9(4) . . ? C8C N2C C6C 109.7(3) . . ? C8C N2C C2C 109.9(3) . . ? C6C N2C C2C 109.4(3) . . ? C8C N2C C4C 108.4(3) . . ? C6C N2C C4C 108.7(3) . . ? C2C N2C C4C 110.7(3) . . ? C8CB N2CB C4CB 109.7(5) . . ? C8CB N2CB C6CB 111.0(4) . . ? C4CB N2CB C6CB 108.0(4) . . ? C8CB N2CB C2CB 109.6(4) . . ? C4CB N2CB C2CB 109.6(4) . . ? C6CB N2CB C2CB 108.8(5) . . ? N1C C1C H1C1 109.5 . . ? N1C C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? N1C C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? N1CB C1CB H1C4 109.5 . . ? N1CB C1CB H1C5 109.5 . . ? H1C4 C1CB H1C5 109.5 . . ? N1CB C1CB H1C6 109.5 . . ? H1C4 C1CB H1C6 109.5 . . ? H1C5 C1CB H1C6 109.5 . . ? N2C C2C H2C1 109.5 . . ? N2C C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? N2C C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? N2CB C2CB H2C4 109.5 . . ? N2CB C2CB H2C5 109.5 . . ? H2C4 C2CB H2C5 109.5 . . ? N2CB C2CB H2C6 109.5 . . ? H2C4 C2CB H2C6 109.5 . . ? H2C5 C2CB H2C6 109.5 . . ? N1C C3C C4C 108.2(3) . . ? N1C C3C H3C1 110.0 . . ? C4C C3C H3C1 110.0 . . ? N1C C3C H3C2 110.0 . . ? C4C C3C H3C2 110.0 . . ? H3C1 C3C H3C2 108.4 . . ? N1CB C3CB C4CB 109.3(4) . . ? N1CB C3CB H3C3 109.8 . . ? C4CB C3CB H3C3 109.8 . . ? N1CB C3CB H3C4 109.8 . . ? C4CB C3CB H3C4 109.8 . . ? H3C3 C3CB H3C4 108.3 . . ? N2C C4C C3C 108.7(3) . . ? N2C C4C H4C1 109.9 . . ? C3C C4C H4C1 109.9 . . ? N2C C4C H4C2 109.9 . . ? C3C C4C H4C2 109.9 . . ? H4C1 C4C H4C2 108.3 . . ? N2CB C4CB C3CB 109.1(4) . . ? N2CB C4CB H4C3 109.9 . . ? C3CB C4CB H4C3 109.9 . . ? N2CB C4CB H4C4 109.9 . . ? C3CB C4CB H4C4 109.9 . . ? H4C3 C4CB H4C4 108.3 . . ? N1C C5C C6C 108.9(3) . . ? N1C C5C H5C1 109.9 . . ? C6C C5C H5C1 109.9 . . ? N1C C5C H5C2 109.9 . . ? C6C C5C H5C2 109.9 . . ? H5C1 C5C H5C2 108.3 . . ? N1CB C5CB C6CB 109.0(4) . . ? N1CB C5CB H5C3 109.9 . . ? C6CB C5CB H5C3 109.9 . . ? N1CB C5CB H5C4 109.9 . . ? C6CB C5CB H5C4 109.9 . . ? H5C3 C5CB H5C4 108.3 . . ? N2C C6C C5C 108.3(3) . . ? N2C C6C H6C1 110.0 . . ? C5C C6C H6C1 110.0 . . ? N2C C6C H6C2 110.0 . . ? C5C C6C H6C2 110.0 . . ? H6C1 C6C H6C2 108.4 . . ? N2CB C6CB C5CB 108.9(4) . . ? N2CB C6CB H6C3 109.9 . . ? C5CB C6CB H6C3 109.9 . . ? N2CB C6CB H6C4 109.9 . . ? C5CB C6CB H6C4 109.9 . . ? H6C3 C6CB H6C4 108.3 . . ? N1C C7C C8C 108.8(3) . . ? N1C C7C H7C1 109.9 . . ? C8C C7C H7C1 109.9 . . ? N1C C7C H7C2 109.9 . . ? C8C C7C H7C2 109.9 . . ? H7C1 C7C H7C2 108.3 . . ? N1CB C7CB C8CB 109.7(4) . . ? N1CB C7CB H7C3 109.7 . . ? C8CB C7CB H7C3 109.7 . . ? N1CB C7CB H7C4 109.7 . . ? C8CB C7CB H7C4 109.7 . . ? H7C3 C7CB H7C4 108.2 . . ? N2C C8C C7C 108.0(3) . . ? N2C C8C H8C1 110.1 . . ? C7C C8C H8C1 110.1 . . ? N2C C8C H8C2 110.1 . . ? C7C C8C H8C2 110.1 . . ? H8C1 C8C H8C2 108.4 . . ? N2CB C8CB C7CB 108.6(5) . . ? N2CB C8CB H8C3 110.0 . . ? C7CB C8CB H8C3 110.0 . . ? N2CB C8CB H8C4 110.0 . . ? C7CB C8CB H8C4 110.0 . . ? H8C3 C8CB H8C4 108.4 . . ? H2WA O1W H2WB 111(7) . . ? H1WA O2W H1WB 115(6) . . ? C2P O1P H1P 129(4) . . ? O1P C2P C3P 110.5(6) . . ? O1P C2P H2P1 109.6 . . ? C3P C2P H2P1 109.6 . . ? O1P C2P H2P2 109.6 . . ? C3P C2P H2P2 109.6 . . ? H2P1 C2P H2P2 108.1 . . ? C4P C3P C2P 113.9(8) . . ? C4P C3P H3P1 108.8 . . ? C2P C3P H3P1 108.8 . . ? C4P C3P H3P2 108.8 . . ? C2P C3P H3P2 108.8 . . ? H3P1 C3P H3P2 107.7 . . ? C3P C4P H4P1 109.5 . . ? C3P C4P H4P2 109.5 . . ? H4P1 C4P H4P2 109.5 . . ? C3P C4P H4P3 109.5 . . ? H4P1 C4P H4P3 109.5 . . ? H4P2 C4P H4P3 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 C6 C1 C2 C3 2.0(6) . . . . ? C28 C1 C2 C3 -176.7(4) . . . . ? C1 C2 C3 C4 -1.9(6) . . . . ? C1 C2 C3 C7 178.0(4) . . . . ? C2 C3 C4 O4 -179.7(4) . . . . ? C7 C3 C4 O4 0.4(6) . . . . ? C2 C3 C4 C5 1.8(6) . . . . ? C7 C3 C4 C5 -178.1(4) . . . . ? O4 C4 C5 C6 179.4(4) . . . . ? C3 C4 C5 C6 -1.9(7) . . . . ? C4 C5 C6 O6 -177.6(4) . . . . ? C4 C5 C6 C1 2.1(7) . . . . ? C2 C1 C6 O6 177.6(4) . . . . ? C28 C1 C6 O6 -3.7(6) . . . . ? C2 C1 C6 C5 -2.0(6) . . . . ? C28 C1 C6 C5 176.6(4) . . . . ? C2 C3 C7 C29 -45.6(5) . . . . ? C4 C3 C7 C29 134.3(4) . . . . ? C2 C3 C7 C8 81.8(5) . . . . ? C4 C3 C7 C8 -98.4(5) . . . . ? C3 C7 C8 C9 -92.6(5) . . . . ? C29 C7 C8 C9 34.1(6) . . . . ? C3 C7 C8 C13 87.7(5) . . . . ? C29 C7 C8 C13 -145.5(4) . . . . ? C13 C8 C9 C10 -0.8(7) . . . . ? C7 C8 C9 C10 179.6(4) . . . . ? C8 C9 C10 C11 -0.3(6) . . . . ? C8 C9 C10 C14 177.8(4) . . . . ? C9 C10 C11 O11 -177.1(4) . . . . ? C14 C10 C11 O11 4.8(6) . . . . ? C9 C10 C11 C12 1.4(6) . . . . ? C14 C10 C11 C12 -176.7(4) . . . . ? O11 C11 C12 C13 177.0(4) . . . . ? C10 C11 C12 C13 -1.5(7) . . . . ? C11 C12 C13 O13 -178.2(4) . . . . ? C11 C12 C13 C8 0.3(7) . . . . ? C9 C8 C13 O13 179.4(4) . . . . ? C7 C8 C13 O13 -1.0(6) . . . . ? C9 C8 C13 C12 0.8(6) . . . . ? C7 C8 C13 C12 -179.5(4) . . . . ? C9 C10 C14 C15 91.8(5) . . . . ? C11 C10 C14 C15 -90.2(5) . . . . ? C9 C10 C14 C31 -35.6(6) . . . . ? C11 C10 C14 C31 142.3(4) . . . . ? C10 C14 C15 C16 -79.6(5) . . . . ? C31 C14 C15 C16 48.8(6) . . . . ? C10 C14 C15 C20 100.8(5) . . . . ? C31 C14 C15 C20 -130.7(4) . . . . ? C20 C15 C16 C17 2.8(6) . . . . ? C14 C15 C16 C17 -176.7(4) . . . . ? C15 C16 C17 C18 -0.4(6) . . . . ? C15 C16 C17 C21 -179.3(4) . . . . ? C16 C17 C18 C19 0.0(6) . . . . ? C21 C17 C18 C19 178.9(4) . . . . ? C16 C17 C18 O18 -179.5(4) . . . . ? C21 C17 C18 O18 -0.6(6) . . . . ? C17 C18 C19 C20 -2.1(7) . . . . ? O18 C18 C19 C20 177.4(4) . . . . ? C18 C19 C20 O20 -176.7(4) . . . . ? C18 C19 C20 C15 4.7(7) . . . . ? C16 C15 C20 O20 176.5(4) . . . . ? C14 C15 C20 O20 -3.9(7) . . . . ? C16 C15 C20 C19 -4.9(7) . . . . ? C14 C15 C20 C19 174.6(4) . . . . ? C18 C17 C21 C22 -101.3(5) . . . . ? C16 C17 C21 C22 77.5(5) . . . . ? C18 C17 C21 C33 130.0(4) . . . . ? C16 C17 C21 C33 -51.2(5) . . . . ? C17 C21 C22 C23 -93.9(5) . . . . ? C33 C21 C22 C23 33.8(6) . . . . ? C17 C21 C22 C27 85.1(5) . . . . ? C33 C21 C22 C27 -147.2(4) . . . . ? C27 C22 C23 C24 1.8(6) . . . . ? C21 C22 C23 C24 -179.1(4) . . . . ? C22 C23 C24 C25 -0.9(6) . . . . ? C22 C23 C24 C28 -179.5(4) . . . . ? C23 C24 C25 O25 -179.1(4) . . . . ? C28 C24 C25 O25 -0.5(6) . . . . ? C23 C24 C25 C26 0.0(6) . . . . ? C28 C24 C25 C26 178.6(4) . . . . ? O25 C25 C26 C27 179.0(4) . . . . ? C24 C25 C26 C27 -0.1(7) . . . . ? C25 C26 C27 O27 -177.6(4) . . . . ? C25 C26 C27 C22 1.1(7) . . . . ? C23 C22 C27 O27 176.8(4) . . . . ? C21 C22 C27 O27 -2.3(6) . . . . ? C23 C22 C27 C26 -1.9(6) . . . . ? C21 C22 C27 C26 179.0(4) . . . . ? C2 C1 C28 C24 -80.8(5) . . . . ? C6 C1 C28 C24 100.6(5) . . . . ? C2 C1 C28 C35 47.6(5) . . . . ? C6 C1 C28 C35 -130.9(4) . . . . ? C25 C24 C28 C1 -86.6(5) . . . . ? C23 C24 C28 C1 91.9(5) . . . . ? C25 C24 C28 C35 146.1(4) . . . . ? C23 C24 C28 C35 -35.4(6) . . . . ? C3 C7 C29 C30 -169.9(4) . . . . ? C8 C7 C29 C30 64.1(5) . . . . ? C10 C14 C31 C32 -63.2(7) . . . . ? C15 C14 C31 C32 168.7(6) . . . . ? C10 C14 C31 C32B -155.1(6) . . . . ? C15 C14 C31 C32B 76.8(7) . . . . ? C22 C21 C33 C34 61.9(5) . . . . ? C17 C21 C33 C34 -170.4(4) . . . . ? C1 C28 C35 C36 168.4(4) . . . . ? C24 C28 C35 C36 -64.3(5) . . . . ? C7C N1C C3C C4C 70.3(4) . . . . ? C5C N1C C3C C4C -49.0(4) . . . . ? C1C N1C C3C C4C -169.2(3) . . . . ? C5CB N1CB C3CB C4CB -50.1(6) . . . . ? C7CB N1CB C3CB C4CB 67.1(5) . . . . ? C1CB N1CB C3CB C4CB -171.4(5) . . . . ? C8C N2C C4C C3C -49.1(4) . . . . ? C6C N2C C4C C3C 70.2(4) . . . . ? C2C N2C C4C C3C -169.7(3) . . . . ? N1C C3C C4C N2C -18.3(5) . . . . ? C8CB N2CB C4CB C3CB -50.8(6) . . . . ? C6CB N2CB C4CB C3CB 70.4(6) . . . . ? C2CB N2CB C4CB C3CB -171.2(5) . . . . ? N1CB C3CB C4CB N2CB -15.9(6) . . . . ? C7C N1C C5C C6C -46.6(4) . . . . ? C3C N1C C5C C6C 72.4(4) . . . . ? C1C N1C C5C C6C -167.1(3) . . . . ? C7CB N1CB C5CB C6CB -50.0(5) . . . . ? C1CB N1CB C5CB C6CB -171.5(5) . . . . ? C3CB N1CB C5CB C6CB 67.0(5) . . . . ? C8C N2C C6C C5C 71.0(4) . . . . ? C2C N2C C6C C5C -168.4(3) . . . . ? C4C N2C C6C C5C -47.4(4) . . . . ? N1C C5C C6C N2C -20.2(4) . . . . ? C8CB N2CB C6CB C5CB 67.5(6) . . . . ? C4CB N2CB C6CB C5CB -52.8(6) . . . . ? C2CB N2CB C6CB C5CB -171.8(5) . . . . ? N1CB C5CB C6CB N2CB -13.8(6) . . . . ? C3C N1C C7C C8C -48.2(4) . . . . ? C5C N1C C7C C8C 70.0(4) . . . . ? C1C N1C C7C C8C -169.2(3) . . . . ? C5CB N1CB C7CB C8CB 68.5(6) . . . . ? C1CB N1CB C7CB C8CB -170.0(5) . . . . ? C3CB N1CB C7CB C8CB -48.3(6) . . . . ? C6C N2C C8C C7C -47.5(4) . . . . ? C2C N2C C8C C7C -167.7(3) . . . . ? C4C N2C C8C C7C 71.1(4) . . . . ? N1C C7C C8C N2C -19.5(5) . . . . ? C4CB N2CB C8CB C7CB 69.7(6) . . . . ? C6CB N2CB C8CB C7CB -49.6(6) . . . . ? C2CB N2CB C8CB C7CB -169.9(5) . . . . ? N1CB C7CB C8CB N2CB -16.4(7) . . . . ? O1P C2P C3P C4P 63.2(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O13 0.71(5) 2.06(6) 2.766(5) 171(7) . O6 H6 Br1 0.80(5) 2.39(5) 3.178(3) 169(5) . O11 H11 O1W 0.71(5) 1.92(5) 2.612(5) 167(7) . O13 H13 O1P 0.85(5) 1.73(5) 2.570(5) 169(5) . O18 H18 Br2 0.70(5) 2.51(5) 3.200(3) 173(7) . O20 H20 O11 0.79(5) 2.01(5) 2.784(5) 169(6) . O25 H25 O6 0.72(5) 2.07(5) 2.777(4) 170(7) . O27 H27 O18 0.79(5) 2.03(5) 2.790(5) 162(6) . O2W H1WA Br2 1.00(6) 2.37(6) 3.329(5) 160(5) . O2W H1WB Br4 0.80(6) 2.89(6) 3.415(5) 125(5) 1_665 O2W H1WB Br3 0.80(6) 3.08(6) 3.655(5) 131(6) 2_775 O1W H2WA Br1 0.77(7) 2.56(7) 3.281(4) 157(8) 1_565 O1W H2WB Br4 0.83(7) 2.40(8) 3.220(4) 169(7) 1_565 O1P H1P O2W 1.01(7) 1.94(7) 2.695(7) 130(5) 1_455 _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.835 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.092 _exptl_crystal_recrystallization_method 'n-propanol (aq)' #==END data_Complex3 _database_code_depnum_ccdc_archive 'CCDC 254960' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C36H40O8*C8H18N2Br2*C2H6O _chemical_formula_sum 'C46 H64 Br2 N2 O9' _chemical_formula_weight 948.81 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' Br Br -0.2901 2.4595 '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 _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.05440(10) _cell_length_b 12.8536(2) _cell_length_c 15.3163(2) _cell_angle_alpha 85.953(1) _cell_angle_beta 84.491(1) _cell_angle_gamma 69.520(1) _cell_volume 2211.14(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description prisms _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 1.890 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6972 _exptl_absorpt_correction_T_max 0.7309 _exptl_absorpt_process_details 'R. H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38.' _exptl_special_details ; dx = 30 mm, 20 sec./deg., 1 deg. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'rotation in phi and omega, 1 deg.' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 22107 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.67 _reflns_number_total 8301 _reflns_number_gt 7209 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELX97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+2.2889P] 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 SHELXL _refine_ls_extinction_coef 0.0013(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8301 _refine_ls_number_parameters 560 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.60152(17) 0.90210(16) 0.15227(13) 0.0164(4) Uani 1 1 d . . . C2 C 0.57228(17) 0.82770(17) 0.10474(13) 0.0169(4) Uani 1 1 d . . . H2 H 0.6279 0.7896 0.0593 0.020 Uiso 1 1 calc R . . C3 C 0.46658(17) 0.80602(17) 0.11993(13) 0.0167(4) Uani 1 1 d . . . C4 C 0.38504(17) 0.86500(17) 0.18596(13) 0.0182(4) Uani 1 1 d . . . O4 O 0.27911(12) 0.84641(13) 0.20133(10) 0.0240(3) Uani 1 1 d D . . H4 H 0.241(2) 0.879(2) 0.2458(14) 0.036 Uiso 1 1 d D . . C5 C 0.41122(18) 0.93845(17) 0.23575(13) 0.0193(4) Uani 1 1 d . . . H5 H 0.3552 0.9770 0.2808 0.023 Uiso 1 1 calc R . . C6 C 0.51896(18) 0.95576(17) 0.21987(13) 0.0178(4) Uani 1 1 d . . . O6 O 0.53766(14) 1.02690(13) 0.27497(10) 0.0256(3) Uani 1 1 d D . . H6 H 0.6061(17) 1.026(2) 0.2665(18) 0.038 Uiso 1 1 d D . . C7 C 0.44139(17) 0.71758(17) 0.07172(13) 0.0162(4) Uani 1 1 d . . . H7 H 0.3545 0.7460 0.0630 0.019 Uiso 1 1 calc R . . C8 C 0.46650(17) 0.61044(17) 0.12855(13) 0.0158(4) Uani 1 1 d . . . C9 C 0.58203(17) 0.53560(17) 0.13277(12) 0.0153(4) Uani 1 1 d . . . H9 H 0.6443 0.5547 0.1010 0.018 Uiso 1 1 calc R . . C10 C 0.61215(17) 0.43461(17) 0.18055(12) 0.0156(4) Uani 1 1 d . . . C11 C 0.52014(18) 0.41128(17) 0.23092(13) 0.0179(4) Uani 1 1 d . . . O11 O 0.54003(13) 0.31646(13) 0.28482(10) 0.0240(3) Uani 1 1 d D . . H11 H 0.6077(17) 0.297(2) 0.3018(17) 0.036 Uiso 1 1 d D . . C12 C 0.40349(18) 0.48284(18) 0.22777(13) 0.0200(4) Uani 1 1 d . . . H12 H 0.3416 0.4644 0.2607 0.024 Uiso 1 1 calc R . . C13 C 0.37639(17) 0.58110(18) 0.17702(13) 0.0183(4) Uani 1 1 d . . . O13 O 0.25857(12) 0.64593(13) 0.17654(10) 0.0247(3) Uani 1 1 d D . . H13 H 0.252(2) 0.7129(15) 0.1801(18) 0.037 Uiso 1 1 d D . . C14 C 0.73932(17) 0.35271(17) 0.17352(12) 0.0159(4) Uani 1 1 d . . . H14 H 0.7364 0.2792 0.1974 0.019 Uiso 1 1 calc R . . C15 C 0.81857(16) 0.38480(16) 0.23036(13) 0.0156(4) Uani 1 1 d . . . C16 C 0.88533(16) 0.44958(16) 0.19780(13) 0.0158(4) Uani 1 1 d . . . H16 H 0.8801 0.4750 0.1380 0.019 Uiso 1 1 calc R . . C17 C 0.95997(16) 0.47984(17) 0.24755(13) 0.0160(4) Uani 1 1 d . . . C18 C 0.96553(17) 0.44117(17) 0.33506(13) 0.0171(4) Uani 1 1 d . . . O18 O 1.03557(13) 0.46385(13) 0.39202(10) 0.0242(3) Uani 1 1 d D . . H18 H 1.050(2) 0.5213(17) 0.3791(17) 0.036 Uiso 1 1 d D . . C19 C 0.89943(17) 0.37670(17) 0.37076(13) 0.0185(4) Uani 1 1 d . . . H19 H 0.9047 0.3511 0.4305 0.022 Uiso 1 1 calc R . . C20 C 0.82560(17) 0.34977(17) 0.31878(13) 0.0176(4) Uani 1 1 d . . . O20 O 0.75864(14) 0.28659(13) 0.35217(10) 0.0247(3) Uani 1 1 d D . . H20 H 0.755(2) 0.286(2) 0.4061(11) 0.037 Uiso 1 1 d D . . C21 C 1.03161(17) 0.55153(17) 0.20806(13) 0.0170(4) Uani 1 1 d . . . H21 H 1.1052 0.5289 0.2403 0.020 Uiso 1 1 calc R . . C24 C 0.81491(17) 0.85440(17) 0.18741(13) 0.0177(4) Uani 1 1 d . . . C22 C 0.96584(17) 0.67430(17) 0.22475(13) 0.0174(4) Uani 1 1 d . . . C23 C 0.87682(17) 0.74234(17) 0.17284(13) 0.0175(4) Uani 1 1 d . . . H23 H 0.8575 0.7104 0.1250 0.021 Uiso 1 1 calc R . . C25 C 0.84417(18) 0.89956(17) 0.25875(14) 0.0200(4) Uani 1 1 d . . . O25 O 0.78121(14) 1.00978(13) 0.27494(11) 0.0277(4) Uani 1 1 d D . . H25 H 0.782(3) 1.015(2) 0.3286(12) 0.042 Uiso 1 1 d D . . C26 C 0.93251(18) 0.83525(18) 0.31190(14) 0.0222(5) Uani 1 1 d . . . H26 H 0.9523 0.8673 0.3595 0.027 Uiso 1 1 calc R . . C27 C 0.99138(17) 0.72412(18) 0.29492(14) 0.0198(4) Uani 1 1 d . . . O27 O 1.07153(13) 0.65581(13) 0.35163(10) 0.0263(4) Uani 1 1 d D . . H27 H 1.121(2) 0.681(2) 0.3664(18) 0.040 Uiso 1 1 d D . . C28 C 0.71680(17) 0.92592(17) 0.13029(13) 0.0185(4) Uani 1 1 d . . . H28 H 0.6993 1.0045 0.1462 0.022 Uiso 1 1 calc R . . C29 C 0.50784(18) 0.69407(17) -0.01943(13) 0.0182(4) Uani 1 1 d . . . H29A H 0.5941 0.6720 -0.0132 0.022 Uiso 1 1 calc R . . H29B H 0.4937 0.6305 -0.0431 0.022 Uiso 1 1 calc R . . C30 C 0.4713(2) 0.79243(19) -0.08506(14) 0.0266(5) Uani 1 1 d . . . H30A H 0.3872 0.8117 -0.0949 0.040 Uiso 1 1 calc R . . H30B H 0.5195 0.7726 -0.1407 0.040 Uiso 1 1 calc R . . H30C H 0.4838 0.8563 -0.0618 0.040 Uiso 1 1 calc R . . C31 C 0.78741(18) 0.33741(18) 0.07658(13) 0.0194(4) Uani 1 1 d . . . H31A H 0.7287 0.3217 0.0436 0.023 Uiso 1 1 calc R . . H31B H 0.7952 0.4081 0.0520 0.023 Uiso 1 1 calc R . . C32 C 0.9066(2) 0.2448(2) 0.06219(15) 0.0285(5) Uani 1 1 d . . . H32A H 0.9679 0.2643 0.0878 0.043 Uiso 1 1 calc R . . H32B H 0.9271 0.2349 -0.0009 0.043 Uiso 1 1 calc R . . H32C H 0.9018 0.1755 0.0904 0.043 Uiso 1 1 calc R . . C33 C 1.07286(18) 0.53151(18) 0.11050(13) 0.0210(4) Uani 1 1 d . . . H33A H 1.0024 0.5480 0.0766 0.025 Uiso 1 1 calc R . . H33B H 1.1145 0.5834 0.0886 0.025 Uiso 1 1 calc R . . C34 C 1.1552(2) 0.4130(2) 0.09467(16) 0.0321(5) Uani 1 1 d . . . H34A H 1.2264 0.3969 0.1267 0.048 Uiso 1 1 calc R . . H34B H 1.1783 0.4045 0.0317 0.048 Uiso 1 1 calc R . . H34C H 1.1141 0.3612 0.1154 0.048 Uiso 1 1 calc R . . C35 C 0.75685(19) 0.92091(18) 0.03163(14) 0.0219(4) Uani 1 1 d . . . H35A H 0.7944 0.8423 0.0156 0.026 Uiso 1 1 calc R . . H35B H 0.6866 0.9552 -0.0027 0.026 Uiso 1 1 calc R . . C36 C 0.8448(2) 0.9814(2) 0.00835(16) 0.0315(5) Uani 1 1 d . . . H36A H 0.8056 1.0607 0.0192 0.047 Uiso 1 1 calc R . . H36B H 0.8729 0.9722 -0.0538 0.047 Uiso 1 1 calc R . . H36C H 0.9124 0.9503 0.0446 0.047 Uiso 1 1 calc R . . Br1 Br 0.292358(18) 0.673365(18) 0.438462(14) 0.02329(7) Uani 1 1 d . . . Br2 Br 0.73056(2) 1.02107(2) 0.482138(16) 0.03063(8) Uani 1 1 d . . . N1 N 0.62104(14) 0.68891(14) 0.39874(11) 0.0171(4) Uani 1 1 d . . . N2 N 0.67700(15) 0.72743(14) 0.54629(11) 0.0192(4) Uani 1 1 d . . . C1C C 0.6199(2) 0.59666(18) 0.46475(14) 0.0228(5) Uani 1 1 d . . . H1CA H 0.6720 0.5243 0.4416 0.027 Uiso 1 1 calc R . . H1CB H 0.5383 0.5948 0.4754 0.027 Uiso 1 1 calc R . . C2C C 0.6633(2) 0.61542(18) 0.55030(14) 0.0236(5) Uani 1 1 d . . . H2CA H 0.6057 0.6111 0.5998 0.028 Uiso 1 1 calc R . . H2CB H 0.7406 0.5567 0.5604 0.028 Uiso 1 1 calc R . . C3C C 0.74246(18) 0.6969(2) 0.38947(14) 0.0261(5) Uani 1 1 d . . . H3CA H 0.7456 0.7540 0.3433 0.031 Uiso 1 1 calc R . . H3CB H 0.8016 0.6248 0.3714 0.031 Uiso 1 1 calc R . . C4C C 0.77292(18) 0.72766(19) 0.47595(14) 0.0226(5) Uani 1 1 d . . . H4CA H 0.8500 0.6735 0.4925 0.027 Uiso 1 1 calc R . . H4CB H 0.7801 0.8023 0.4695 0.027 Uiso 1 1 calc R . . C5C C 0.53344(19) 0.79691(18) 0.43145(14) 0.0219(4) Uani 1 1 d . . . H5CA H 0.4518 0.7952 0.4331 0.026 Uiso 1 1 calc R . . H5CB H 0.5384 0.8591 0.3911 0.026 Uiso 1 1 calc R . . C6C C 0.56075(18) 0.81479(19) 0.52300(14) 0.0248(5) Uani 1 1 d . . . H6CA H 0.5661 0.8897 0.5250 0.030 Uiso 1 1 calc R . . H6CB H 0.4959 0.8101 0.5662 0.030 Uiso 1 1 calc R . . C7C C 0.5894(2) 0.66386(19) 0.31213(14) 0.0249(5) Uani 1 1 d . . . H7CA H 0.5883 0.7245 0.2693 0.037 Uiso 1 1 calc R . . H7CB H 0.5108 0.6565 0.3192 0.037 Uiso 1 1 calc R . . H7CC H 0.6485 0.5942 0.2913 0.037 Uiso 1 1 calc R . . C8C C 0.7075(2) 0.7530(2) 0.63309(14) 0.0285(5) Uani 1 1 d . . . H8CA H 0.6420 0.7571 0.6775 0.043 Uiso 1 1 calc R . . H8CB H 0.7205 0.8244 0.6278 0.043 Uiso 1 1 calc R . . H8CC H 0.7800 0.6943 0.6507 0.043 Uiso 1 1 calc R . . O1E O 0.14643(15) 0.94138(15) 0.34274(12) 0.0345(4) Uani 1 1 d . . . H1E H 0.180(3) 0.929(3) 0.388(2) 0.052 Uiso 1 1 d . . . C2E C 0.0664(2) 1.0530(2) 0.34215(19) 0.0452(7) Uani 1 1 d . . . H2E1 H 0.0977 1.0996 0.3744 0.054 Uiso 1 1 calc R . . H2E2 H -0.0116 1.0562 0.3713 0.054 Uiso 1 1 calc R . . C3E C 0.0530(4) 1.0942(4) 0.2518(2) 0.1019(18) Uani 1 1 d . . . H3E1 H -0.0023 1.1710 0.2503 0.153 Uiso 1 1 calc R . . H3E2 H 0.0219 1.0478 0.2203 0.153 Uiso 1 1 calc R . . H3E3 H 0.1304 1.0915 0.2236 0.153 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 C1 0.0163(10) 0.0173(10) 0.0152(10) 0.0019(8) -0.0031(8) -0.0053(8) C2 0.0161(9) 0.0181(10) 0.0148(10) 0.0002(8) -0.0012(8) -0.0039(8) C3 0.0149(9) 0.0179(10) 0.0160(10) 0.0011(8) -0.0043(8) -0.0036(8) C4 0.0137(9) 0.0192(11) 0.0202(11) 0.0004(8) -0.0025(8) -0.0036(8) O4 0.0141(7) 0.0302(9) 0.0286(9) -0.0115(7) 0.0040(6) -0.0083(7) C5 0.0174(10) 0.0182(11) 0.0188(11) -0.0047(8) 0.0007(8) -0.0016(9) C6 0.0197(10) 0.0181(10) 0.0155(10) -0.0008(8) -0.0043(8) -0.0055(9) O6 0.0238(8) 0.0287(9) 0.0282(9) -0.0133(7) 0.0029(7) -0.0128(7) C7 0.0126(9) 0.0189(10) 0.0163(10) -0.0024(8) -0.0024(8) -0.0037(8) C8 0.0159(9) 0.0201(11) 0.0135(10) -0.0036(8) -0.0022(8) -0.0080(8) C9 0.0150(9) 0.0216(11) 0.0122(10) -0.0034(8) 0.0008(7) -0.0098(8) C10 0.0161(9) 0.0200(11) 0.0120(10) -0.0024(8) -0.0019(7) -0.0074(8) C11 0.0206(10) 0.0231(11) 0.0129(10) -0.0005(8) -0.0011(8) -0.0111(9) O11 0.0208(8) 0.0289(9) 0.0226(8) 0.0086(7) -0.0017(6) -0.0108(7) C12 0.0175(10) 0.0291(12) 0.0166(10) -0.0020(9) 0.0016(8) -0.0126(9) C13 0.0132(9) 0.0254(11) 0.0182(10) -0.0058(9) -0.0007(8) -0.0082(9) O13 0.0116(7) 0.0270(9) 0.0349(9) -0.0018(7) 0.0005(6) -0.0063(7) C14 0.0165(9) 0.0177(10) 0.0136(10) -0.0004(8) -0.0009(8) -0.0063(8) C15 0.0116(9) 0.0175(10) 0.0155(10) -0.0026(8) 0.0001(7) -0.0024(8) C16 0.0131(9) 0.0181(10) 0.0137(10) -0.0006(8) -0.0009(7) -0.0022(8) C17 0.0111(9) 0.0188(10) 0.0161(10) -0.0021(8) 0.0000(7) -0.0028(8) C18 0.0124(9) 0.0190(10) 0.0168(10) -0.0029(8) -0.0030(8) -0.0008(8) O18 0.0254(8) 0.0308(9) 0.0208(8) 0.0015(7) -0.0100(6) -0.0137(7) C19 0.0170(10) 0.0201(11) 0.0153(10) 0.0012(8) -0.0034(8) -0.0025(9) C20 0.0152(9) 0.0184(10) 0.0183(10) 0.0009(8) -0.0006(8) -0.0051(8) O20 0.0310(8) 0.0341(9) 0.0153(7) 0.0055(7) -0.0033(6) -0.0198(7) C21 0.0130(9) 0.0220(11) 0.0162(10) -0.0014(8) -0.0013(8) -0.0063(8) C24 0.0152(10) 0.0222(11) 0.0175(10) -0.0016(8) -0.0004(8) -0.0087(9) C22 0.0137(9) 0.0232(11) 0.0176(10) -0.0022(8) 0.0019(8) -0.0097(9) C23 0.0158(9) 0.0241(11) 0.0153(10) -0.0034(8) 0.0000(8) -0.0102(9) C25 0.0180(10) 0.0204(11) 0.0241(11) -0.0065(9) 0.0014(8) -0.0094(9) O25 0.0305(8) 0.0234(8) 0.0291(9) -0.0088(7) -0.0074(7) -0.0065(7) C26 0.0218(10) 0.0286(12) 0.0215(11) -0.0068(9) -0.0019(9) -0.0142(10) C27 0.0146(10) 0.0263(12) 0.0208(11) 0.0006(9) -0.0035(8) -0.0097(9) O27 0.0236(8) 0.0311(9) 0.0292(9) 0.0010(7) -0.0142(7) -0.0128(7) C28 0.0179(10) 0.0175(10) 0.0205(11) -0.0010(8) -0.0016(8) -0.0065(9) C29 0.0183(10) 0.0200(11) 0.0157(10) -0.0024(8) -0.0020(8) -0.0053(9) C30 0.0338(12) 0.0260(12) 0.0189(11) 0.0020(9) -0.0039(9) -0.0091(10) C31 0.0195(10) 0.0242(11) 0.0154(10) -0.0031(8) -0.0011(8) -0.0082(9) C32 0.0272(12) 0.0293(13) 0.0260(12) -0.0068(10) 0.0030(9) -0.0060(10) C33 0.0170(10) 0.0295(12) 0.0178(11) -0.0034(9) 0.0031(8) -0.0103(9) C34 0.0219(11) 0.0394(14) 0.0308(13) -0.0112(11) 0.0069(10) -0.0057(11) C35 0.0226(11) 0.0224(11) 0.0203(11) -0.0001(9) 0.0001(8) -0.0081(9) C36 0.0299(12) 0.0325(13) 0.0327(13) -0.0009(11) 0.0079(10) -0.0144(11) Br1 0.02208(12) 0.03023(13) 0.02127(12) 0.00167(9) -0.00472(8) -0.01342(9) Br2 0.02911(13) 0.02738(13) 0.03308(14) -0.01138(10) -0.00225(10) -0.00496(10) N1 0.0153(8) 0.0188(9) 0.0152(9) -0.0001(7) 0.0003(7) -0.0040(7) N2 0.0165(8) 0.0212(9) 0.0176(9) -0.0026(7) -0.0015(7) -0.0035(7) C1C 0.0297(11) 0.0188(11) 0.0196(11) 0.0032(9) -0.0029(9) -0.0087(9) C2C 0.0279(11) 0.0249(12) 0.0191(11) 0.0033(9) -0.0017(9) -0.0115(10) C3C 0.0172(10) 0.0375(13) 0.0232(12) -0.0040(10) 0.0047(9) -0.0101(10) C4C 0.0163(10) 0.0274(12) 0.0232(11) 0.0002(9) 0.0013(8) -0.0074(9) C5C 0.0210(10) 0.0180(11) 0.0204(11) -0.0031(9) -0.0031(8) 0.0019(9) C6C 0.0166(10) 0.0255(12) 0.0249(12) -0.0054(9) -0.0036(9) 0.0034(9) C7C 0.0307(12) 0.0283(12) 0.0139(11) -0.0045(9) -0.0033(9) -0.0068(10) C8C 0.0272(12) 0.0364(14) 0.0200(12) -0.0071(10) -0.0063(9) -0.0064(10) O1E 0.0261(9) 0.0420(11) 0.0305(10) -0.0079(8) -0.0011(7) -0.0048(8) C2E 0.0342(14) 0.0445(17) 0.0475(17) -0.0145(13) 0.0007(12) -0.0002(13) C3E 0.112(3) 0.076(3) 0.047(2) 0.0010(19) -0.006(2) 0.055(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 C1 C2 1.397(3) . ? C1 C6 1.400(3) . ? C1 C28 1.527(3) . ? C2 C3 1.392(3) . ? C3 C4 1.400(3) . ? C3 C7 1.527(3) . ? C4 O4 1.375(2) . ? C4 C5 1.389(3) . ? C5 C6 1.389(3) . ? C6 O6 1.374(2) . ? C7 C8 1.528(3) . ? C7 C29 1.535(3) . ? C8 C9 1.393(3) . ? C8 C13 1.402(3) . ? C9 C10 1.393(3) . ? C10 C11 1.397(3) . ? C10 C14 1.525(3) . ? C11 O11 1.384(2) . ? C11 C12 1.388(3) . ? C12 C13 1.388(3) . ? C13 O13 1.373(2) . ? C14 C15 1.526(3) . ? C14 C31 1.541(3) . ? C15 C16 1.387(3) . ? C15 C20 1.398(3) . ? C16 C17 1.400(3) . ? C17 C18 1.396(3) . ? C17 C21 1.529(3) . ? C18 O18 1.381(2) . ? C18 C19 1.391(3) . ? C19 C20 1.392(3) . ? C20 O20 1.376(2) . ? C21 C22 1.525(3) . ? C21 C33 1.539(3) . ? C24 C23 1.394(3) . ? C24 C25 1.401(3) . ? C24 C28 1.528(3) . ? C22 C23 1.399(3) . ? C22 C27 1.400(3) . ? C25 O25 1.380(3) . ? C25 C26 1.391(3) . ? C26 C27 1.385(3) . ? C27 O27 1.385(3) . ? C28 C35 1.540(3) . ? C29 C30 1.523(3) . ? C31 C32 1.520(3) . ? C33 C34 1.521(3) . ? C35 C36 1.523(3) . ? N1 C3C 1.496(3) . ? N1 C7C 1.501(3) . ? N1 C5C 1.505(3) . ? N1 C1C 1.506(3) . ? N2 C8C 1.501(3) . ? N2 C2C 1.502(3) . ? N2 C4C 1.503(3) . ? N2 C6C 1.513(3) . ? C1C C2C 1.521(3) . ? C3C C4C 1.521(3) . ? C5C C6C 1.521(3) . ? O1E C2E 1.422(3) . ? C2E C3E 1.450(4) . ? 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 C2 C1 C6 116.91(18) . . ? C2 C1 C28 121.64(18) . . ? C6 C1 C28 121.44(17) . . ? C3 C2 C1 123.97(19) . . ? C2 C3 C4 116.89(18) . . ? C2 C3 C7 122.67(18) . . ? C4 C3 C7 120.34(17) . . ? O4 C4 C5 120.90(18) . . ? O4 C4 C3 118.04(17) . . ? C5 C4 C3 121.04(18) . . ? C4 C5 C6 120.24(19) . . ? O6 C6 C5 115.49(18) . . ? O6 C6 C1 123.63(18) . . ? C5 C6 C1 120.88(18) . . ? C3 C7 C8 110.35(15) . . ? C3 C7 C29 114.06(16) . . ? C8 C7 C29 110.74(16) . . ? C9 C8 C13 116.78(18) . . ? C9 C8 C7 120.57(17) . . ? C13 C8 C7 122.64(18) . . ? C10 C9 C8 124.24(18) . . ? C9 C10 C11 116.88(18) . . ? C9 C10 C14 120.38(17) . . ? C11 C10 C14 122.68(18) . . ? O11 C11 C12 117.12(17) . . ? O11 C11 C10 122.20(18) . . ? C12 C11 C10 120.68(19) . . ? C11 C12 C13 120.69(18) . . ? O13 C13 C12 116.80(18) . . ? O13 C13 C8 122.60(19) . . ? C12 C13 C8 120.60(18) . . ? C10 C14 C15 111.60(16) . . ? C10 C14 C31 110.53(16) . . ? C15 C14 C31 113.70(16) . . ? C16 C15 C20 117.29(17) . . ? C16 C15 C14 122.31(17) . . ? C20 C15 C14 120.40(17) . . ? C15 C16 C17 124.02(18) . . ? C18 C17 C16 116.50(18) . . ? C18 C17 C21 121.77(17) . . ? C16 C17 C21 121.73(17) . . ? O18 C18 C19 115.44(18) . . ? O18 C18 C17 123.08(18) . . ? C19 C18 C17 121.48(18) . . ? C18 C19 C20 119.82(19) . . ? O20 C20 C19 121.28(18) . . ? O20 C20 C15 117.85(17) . . ? C19 C20 C15 120.86(18) . . ? C22 C21 C17 111.43(16) . . ? C22 C21 C33 112.06(17) . . ? C17 C21 C33 113.53(16) . . ? C23 C24 C25 117.20(19) . . ? C23 C24 C28 122.32(18) . . ? C25 C24 C28 120.46(18) . . ? C23 C22 C27 116.54(19) . . ? C23 C22 C21 122.73(18) . . ? C27 C22 C21 120.72(18) . . ? C24 C23 C22 123.66(18) . . ? O25 C25 C26 121.27(18) . . ? O25 C25 C24 117.56(19) . . ? C26 C25 C24 121.16(19) . . ? C27 C26 C25 119.50(19) . . ? O27 C27 C26 120.59(18) . . ? O27 C27 C22 117.28(19) . . ? C26 C27 C22 121.93(19) . . ? C1 C28 C24 111.81(16) . . ? C1 C28 C35 113.34(16) . . ? C24 C28 C35 112.77(17) . . ? C30 C29 C7 113.92(17) . . ? C32 C31 C14 114.33(17) . . ? C34 C33 C21 112.74(18) . . ? C36 C35 C28 111.41(18) . . ? C3C N1 C7C 110.03(16) . . ? C3C N1 C5C 108.83(16) . . ? C7C N1 C5C 110.76(16) . . ? C3C N1 C1C 108.97(16) . . ? C7C N1 C1C 109.17(16) . . ? C5C N1 C1C 109.06(16) . . ? C8C N2 C2C 111.06(17) . . ? C8C N2 C4C 110.43(16) . . ? C2C N2 C4C 108.34(16) . . ? C8C N2 C6C 108.79(16) . . ? C2C N2 C6C 108.67(16) . . ? C4C N2 C6C 109.51(16) . . ? N1 C1C C2C 109.65(17) . . ? N2 C2C C1C 109.98(17) . . ? N1 C3C C4C 110.38(17) . . ? N2 C4C C3C 109.46(16) . . ? N1 C5C C6C 109.60(16) . . ? N2 C6C C5C 109.85(17) . . ? O1E C2E C3E 108.5(2) . . ? 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 C6 C1 C2 C3 1.1(3) . . . . ? C28 C1 C2 C3 -177.58(19) . . . . ? C1 C2 C3 C4 1.3(3) . . . . ? C1 C2 C3 C7 -175.07(18) . . . . ? C2 C3 C4 O4 178.99(18) . . . . ? C7 C3 C4 O4 -4.5(3) . . . . ? C2 C3 C4 C5 -2.3(3) . . . . ? C7 C3 C4 C5 174.19(18) . . . . ? O4 C4 C5 C6 179.53(19) . . . . ? C3 C4 C5 C6 0.9(3) . . . . ? C4 C5 C6 O6 -177.68(18) . . . . ? C4 C5 C6 C1 1.7(3) . . . . ? C2 C1 C6 O6 176.73(18) . . . . ? C28 C1 C6 O6 -4.6(3) . . . . ? C2 C1 C6 C5 -2.6(3) . . . . ? C28 C1 C6 C5 176.06(19) . . . . ? C2 C3 C7 C8 98.4(2) . . . . ? C4 C3 C7 C8 -77.9(2) . . . . ? C2 C3 C7 C29 -27.0(3) . . . . ? C4 C3 C7 C29 156.74(18) . . . . ? C3 C7 C8 C9 -81.3(2) . . . . ? C29 C7 C8 C9 46.0(2) . . . . ? C3 C7 C8 C13 100.1(2) . . . . ? C29 C7 C8 C13 -132.64(19) . . . . ? C13 C8 C9 C10 0.9(3) . . . . ? C7 C8 C9 C10 -177.82(18) . . . . ? C8 C9 C10 C11 -3.7(3) . . . . ? C8 C9 C10 C14 173.54(17) . . . . ? C9 C10 C11 O11 -176.44(17) . . . . ? C14 C10 C11 O11 6.4(3) . . . . ? C9 C10 C11 C12 4.4(3) . . . . ? C14 C10 C11 C12 -172.80(18) . . . . ? O11 C11 C12 C13 178.39(18) . . . . ? C10 C11 C12 C13 -2.4(3) . . . . ? C11 C12 C13 O13 178.90(18) . . . . ? C11 C12 C13 C8 -0.6(3) . . . . ? C9 C8 C13 O13 -178.12(18) . . . . ? C7 C8 C13 O13 0.6(3) . . . . ? C9 C8 C13 C12 1.3(3) . . . . ? C7 C8 C13 C12 -179.99(18) . . . . ? C9 C10 C14 C15 80.2(2) . . . . ? C11 C10 C14 C15 -102.7(2) . . . . ? C9 C10 C14 C31 -47.4(2) . . . . ? C11 C10 C14 C31 129.73(19) . . . . ? C10 C14 C15 C16 -93.2(2) . . . . ? C31 C14 C15 C16 32.6(3) . . . . ? C10 C14 C15 C20 86.3(2) . . . . ? C31 C14 C15 C20 -147.86(19) . . . . ? C20 C15 C16 C17 1.1(3) . . . . ? C14 C15 C16 C17 -179.33(18) . . . . ? C15 C16 C17 C18 0.0(3) . . . . ? C15 C16 C17 C21 179.98(18) . . . . ? C16 C17 C18 O18 179.72(18) . . . . ? C21 C17 C18 O18 -0.3(3) . . . . ? C16 C17 C18 C19 -0.5(3) . . . . ? C21 C17 C18 C19 179.50(18) . . . . ? O18 C18 C19 C20 179.68(18) . . . . ? C17 C18 C19 C20 -0.1(3) . . . . ? C18 C19 C20 O20 -179.70(18) . . . . ? C18 C19 C20 C15 1.3(3) . . . . ? C16 C15 C20 O20 179.21(18) . . . . ? C14 C15 C20 O20 -0.3(3) . . . . ? C16 C15 C20 C19 -1.7(3) . . . . ? C14 C15 C20 C19 178.70(18) . . . . ? C18 C17 C21 C22 -85.6(2) . . . . ? C16 C17 C21 C22 94.4(2) . . . . ? C18 C17 C21 C33 146.75(19) . . . . ? C16 C17 C21 C33 -33.3(3) . . . . ? C17 C21 C22 C23 -81.9(2) . . . . ? C33 C21 C22 C23 46.6(2) . . . . ? C17 C21 C22 C27 97.1(2) . . . . ? C33 C21 C22 C27 -134.41(19) . . . . ? C25 C24 C23 C22 -0.5(3) . . . . ? C28 C24 C23 C22 -179.02(18) . . . . ? C27 C22 C23 C24 0.4(3) . . . . ? C21 C22 C23 C24 179.41(18) . . . . ? C23 C24 C25 O25 -178.42(17) . . . . ? C28 C24 C25 O25 0.1(3) . . . . ? C23 C24 C25 C26 0.8(3) . . . . ? C28 C24 C25 C26 179.38(18) . . . . ? O25 C25 C26 C27 178.20(19) . . . . ? C24 C25 C26 C27 -1.0(3) . . . . ? C25 C26 C27 O27 -173.83(18) . . . . ? C25 C26 C27 C22 0.9(3) . . . . ? C23 C22 C27 O27 174.34(17) . . . . ? C21 C22 C27 O27 -4.7(3) . . . . ? C23 C22 C27 C26 -0.5(3) . . . . ? C21 C22 C27 C26 -179.60(18) . . . . ? C2 C1 C28 C24 -95.6(2) . . . . ? C6 C1 C28 C24 85.8(2) . . . . ? C2 C1 C28 C35 33.2(3) . . . . ? C6 C1 C28 C35 -145.39(19) . . . . ? C23 C24 C28 C1 76.3(2) . . . . ? C25 C24 C28 C1 -102.2(2) . . . . ? C23 C24 C28 C35 -52.8(2) . . . . ? C25 C24 C28 C35 128.7(2) . . . . ? C3 C7 C29 C30 -64.7(2) . . . . ? C8 C7 C29 C30 170.10(16) . . . . ? C10 C14 C31 C32 -171.44(17) . . . . ? C15 C14 C31 C32 62.1(2) . . . . ? C22 C21 C33 C34 170.79(17) . . . . ? C17 C21 C33 C34 -61.9(2) . . . . ? C1 C28 C35 C36 160.85(18) . . . . ? C24 C28 C35 C36 -70.8(2) . . . . ? C3C N1 C1C C2C 54.4(2) . . . . ? C7C N1 C1C C2C 174.58(17) . . . . ? C5C N1 C1C C2C -64.3(2) . . . . ? C8C N2 C2C C1C 174.12(18) . . . . ? C4C N2 C2C C1C -64.4(2) . . . . ? C6C N2 C2C C1C 54.5(2) . . . . ? N1 C1C C2C N2 8.0(2) . . . . ? C7C N1 C3C C4C 177.35(18) . . . . ? C5C N1 C3C C4C 55.8(2) . . . . ? C1C N1 C3C C4C -63.0(2) . . . . ? C8C N2 C4C C3C 177.72(18) . . . . ? C2C N2 C4C C3C 55.9(2) . . . . ? C6C N2 C4C C3C -62.5(2) . . . . ? N1 C3C C4C N2 6.5(2) . . . . ? C3C N1 C5C C6C -64.2(2) . . . . ? C7C N1 C5C C6C 174.71(18) . . . . ? C1C N1 C5C C6C 54.5(2) . . . . ? C8C N2 C6C C5C 174.82(18) . . . . ? C2C N2 C6C C5C -64.1(2) . . . . ? C4C N2 C6C C5C 54.0(2) . . . . ? N1 C5C C6C N2 8.2(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O1E 0.835(17) 1.830(17) 2.661(2) 173(3) . O18 H18 O27 0.825(17) 1.848(17) 2.672(2) 176(3) . O6 H6 O25 0.819(17) 2.063(18) 2.866(2) 167(3) . O13 H13 O4 0.841(17) 1.910(18) 2.729(2) 164(3) . O11 H11 O20 0.827(17) 2.002(18) 2.813(2) 167(3) . O25 H25 Br2 0.831(17) 2.373(18) 3.1774(17) 163(3) . O20 H20 Br1 0.822(17) 2.444(18) 3.2494(15) 167(3) 2_666 O27 H27 Br1 0.822(17) 2.41(2) 3.1698(14) 155(3) 1_655 O1E H1E Br2 0.82(3) 2.57(3) 3.3276(18) 155(3) 2_676 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.653 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.055 _exptl_crystal_recrystallization_method EtOH(aq) #==END data_Complex4 _database_code_depnum_ccdc_archive 'CCDC 254961' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C40H48O8*C8H18N2Cl2*2CH4O _chemical_formula_sum 'C50 H74 Cl2 N2 O10' _chemical_formula_weight 934.01 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' Cl Cl 0.1484 0.1585 '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 11.3877(2) _cell_length_b 12.5699(3) _cell_length_c 17.5983(4) _cell_angle_alpha 99.3590(10) _cell_angle_beta 91.1830(10) _cell_angle_gamma 98.7800(10) _cell_volume 2453.73(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13449 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; dx = 35 mm, 20 sec./deg., 1 deg. ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13447 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8606 _reflns_number_gt 5747 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELX97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+3.6908P] 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 SHELXL _refine_ls_extinction_coef 0.0034(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8606 _refine_ls_number_parameters 603 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6437(3) 0.9009(2) 0.24430(18) 0.0187(7) Uani 1 1 d . . . C2 C 0.5860(2) 0.7936(2) 0.22315(18) 0.0183(7) Uani 1 1 d . . . H2 H 0.5945 0.7570 0.1724 0.022 Uiso 1 1 calc R . . C3 C 0.5165(2) 0.7373(2) 0.27255(18) 0.0164(7) Uani 1 1 d . . . C4 C 0.5062(3) 0.7926(2) 0.34678(18) 0.0192(7) Uani 1 1 d . . . O4 O 0.44062(19) 0.73627(18) 0.39644(13) 0.0251(5) Uani 1 1 d D . . H4 H 0.450(3) 0.771(3) 0.4410(13) 0.038 Uiso 1 1 d D . . C5 C 0.5611(3) 0.9001(3) 0.37015(19) 0.0226(7) Uani 1 1 d . . . H5 H 0.5524 0.9368 0.4208 0.027 Uiso 1 1 calc R . . C6 C 0.6288(3) 0.9532(2) 0.31867(19) 0.0203(7) Uani 1 1 d . . . O6 O 0.6842(2) 1.05992(18) 0.34012(14) 0.0301(6) Uani 1 1 d D . . H6 H 0.638(3) 1.093(3) 0.369(2) 0.045 Uiso 1 1 d D . . C7 C 0.4554(3) 0.6189(2) 0.24932(18) 0.0180(7) Uani 1 1 d . . . H7 H 0.3808 0.6113 0.2783 0.022 Uiso 1 1 calc R . . C8 C 0.5323(3) 0.5408(2) 0.27587(18) 0.0180(7) Uani 1 1 d . . . C9 C 0.6269(3) 0.5123(2) 0.23195(18) 0.0180(7) Uani 1 1 d . . . H9 H 0.6443 0.5465 0.1883 0.022 Uiso 1 1 calc R . . C10 C 0.6971(2) 0.4367(2) 0.24841(18) 0.0177(7) Uani 1 1 d . . . C11 C 0.6729(3) 0.3909(2) 0.31434(19) 0.0198(7) Uani 1 1 d . . . O11 O 0.7429(2) 0.31729(18) 0.33265(14) 0.0261(5) Uani 1 1 d D . . H11 H 0.748(3) 0.320(3) 0.3798(11) 0.039 Uiso 1 1 d D . . C12 C 0.5816(3) 0.4188(2) 0.36097(19) 0.0213(7) Uani 1 1 d . . . H12 H 0.5670 0.3873 0.4061 0.026 Uiso 1 1 calc R . . C13 C 0.5114(3) 0.4930(2) 0.34163(18) 0.0189(7) Uani 1 1 d . . . O13 O 0.4219(2) 0.51389(18) 0.39030(14) 0.0283(6) Uani 1 1 d D . . H13 H 0.412(3) 0.5791(17) 0.394(2) 0.042 Uiso 1 1 d D . . C14 C 0.7931(3) 0.4035(2) 0.19378(18) 0.0193(7) Uani 1 1 d . . . H14 H 0.8153 0.3349 0.2075 0.023 Uiso 1 1 calc R . . C15 C 0.9053(3) 0.4891(2) 0.20641(18) 0.0189(7) Uani 1 1 d . . . C17 C 1.0309(3) 0.6490(2) 0.17074(18) 0.0191(7) Uani 1 1 d . . . C16 C 0.9306(3) 0.5684(2) 0.16024(18) 0.0185(7) Uani 1 1 d . . . H16 H 0.8759 0.5677 0.1186 0.022 Uiso 1 1 calc R . . C18 C 1.1106(3) 0.6479(3) 0.23221(19) 0.0220(7) Uani 1 1 d . . . O18 O 1.21304(19) 0.72133(19) 0.25013(14) 0.0294(6) Uani 1 1 d D . . H18 H 1.212(3) 0.776(2) 0.228(2) 0.044 Uiso 1 1 d D . . C19 C 1.0890(3) 0.5693(3) 0.27988(19) 0.0235(7) Uani 1 1 d . . . H19 H 1.1442 0.5690 0.3210 0.028 Uiso 1 1 calc R . . C20 C 0.9873(3) 0.4916(3) 0.26742(19) 0.0219(7) Uani 1 1 d . . . O20 O 0.9724(2) 0.42021(19) 0.31885(14) 0.0313(6) Uani 1 1 d D . . H20 H 0.903(2) 0.385(3) 0.314(2) 0.047 Uiso 1 1 d D . . C21 C 1.0519(3) 0.7389(2) 0.12194(18) 0.0196(7) Uani 1 1 d . . . H21 H 1.1397 0.7555 0.1165 0.023 Uiso 1 1 calc R . . C22 C 1.0133(3) 0.8433(2) 0.16429(18) 0.0188(7) Uani 1 1 d . . . C23 C 0.8941(3) 0.8562(2) 0.16568(18) 0.0186(7) Uani 1 1 d . . . H23 H 0.8371 0.7967 0.1410 0.022 Uiso 1 1 calc R . . C24 C 0.8524(3) 0.9499(2) 0.20070(18) 0.0190(7) Uani 1 1 d . . . C25 C 0.9368(3) 1.0326(2) 0.24121(18) 0.0227(7) Uani 1 1 d . . . O25 O 0.9091(2) 1.12862(19) 0.28124(16) 0.0386(7) Uani 1 1 d D . . H25 H 0.8374(19) 1.117(3) 0.291(3) 0.058 Uiso 1 1 d D . . C26 C 1.0566(3) 1.0236(3) 0.24177(19) 0.0238(7) Uani 1 1 d . . . H26 H 1.1131 1.0814 0.2689 0.029 Uiso 1 1 calc R . . C27 C 1.0946(3) 0.9308(3) 0.20311(18) 0.0210(7) Uani 1 1 d . . . O27 O 1.21334(18) 0.91921(18) 0.20243(14) 0.0264(5) Uani 1 1 d D . . H27 H 1.254(3) 0.974(2) 0.2288(19) 0.040 Uiso 1 1 d D . . C28 C 0.7214(3) 0.9606(3) 0.18975(18) 0.0213(7) Uani 1 1 d . . . H28 H 0.7161 1.0399 0.2046 0.026 Uiso 1 1 calc R . . C29 C 0.4181(3) 0.5881(2) 0.16386(19) 0.0223(7) Uani 1 1 d . . . H29A H 0.4903 0.5930 0.1334 0.027 Uiso 1 1 calc R . . H29B H 0.3699 0.6418 0.1498 0.027 Uiso 1 1 calc R . . C32 C 0.7444(3) 0.3763(3) 0.10978(19) 0.0227(7) Uani 1 1 d . . . H32A H 0.7177 0.4418 0.0951 0.027 Uiso 1 1 calc R . . H32B H 0.8094 0.3577 0.0760 0.027 Uiso 1 1 calc R . . C30 C 0.3464(3) 0.4737(3) 0.1418(2) 0.0326(9) Uani 1 1 d . . . H30A H 0.3928 0.4200 0.1578 0.039 Uiso 1 1 calc R . . H30B H 0.2719 0.4697 0.1699 0.039 Uiso 1 1 calc R . . C31 C 0.3159(4) 0.4438(4) 0.0558(2) 0.0598(13) Uani 1 1 d . . . H31A H 0.2775 0.3673 0.0437 0.090 Uiso 1 1 calc R . . H31B H 0.3888 0.4536 0.0274 0.090 Uiso 1 1 calc R . . H31C H 0.2615 0.4909 0.0408 0.090 Uiso 1 1 calc R . . C33 C 0.6412(3) 0.2818(3) 0.0960(2) 0.0313(8) Uani 1 1 d . . . H33A H 0.6661 0.2176 0.1138 0.038 Uiso 1 1 calc R . . H33B H 0.5740 0.3023 0.1270 0.038 Uiso 1 1 calc R . . C34 C 0.5993(2) 0.2510(2) 0.01182(14) 0.0471(11) Uani 1 1 d . . . H34A H 0.5359 0.1876 0.0055 0.071 Uiso 1 1 calc R . . H34B H 0.6660 0.2329 -0.0194 0.071 Uiso 1 1 calc R . . H34C H 0.5689 0.3126 -0.0051 0.071 Uiso 1 1 calc R . . C35 C 0.9944(2) 0.7066(2) 0.03999(14) 0.0221(7) Uani 1 1 d R . . H35A H 1.0173 0.6364 0.0159 0.026 Uiso 1 1 calc R . . H35B H 0.9068 0.6953 0.0433 0.026 Uiso 1 1 calc R . . C36 C 1.0302(3) 0.7918(3) -0.01128(19) 0.0284(8) Uani 1 1 d . . . H36A H 1.0094 0.8625 0.0137 0.034 Uiso 1 1 calc R . . H36B H 1.1176 0.8016 -0.0156 0.034 Uiso 1 1 calc R . . C37 C 0.9713(4) 0.7623(3) -0.0920(2) 0.0414(10) Uani 1 1 d . . . H37A H 1.0047 0.8161 -0.1234 0.062 Uiso 1 1 calc R . . H37B H 0.8854 0.7623 -0.0888 0.062 Uiso 1 1 calc R . . H37C H 0.9857 0.6896 -0.1156 0.062 Uiso 1 1 calc R . . C38 C 0.6767(3) 0.9277(3) 0.10512(18) 0.0224(7) Uani 1 1 d . . . H38A H 0.6783 0.8487 0.0888 0.027 Uiso 1 1 calc R . . H38B H 0.5930 0.9394 0.1008 0.027 Uiso 1 1 calc R . . C39 C 0.7493(3) 0.9908(3) 0.0506(2) 0.0317(8) Uani 1 1 d . . . H39A H 0.7504 1.0699 0.0679 0.038 Uiso 1 1 calc R . . H39B H 0.8323 0.9766 0.0531 0.038 Uiso 1 1 calc R . . C40 C 0.7003(4) 0.9599(4) -0.0321(2) 0.0473(11) Uani 1 1 d . . . H40A H 0.7500 1.0024 -0.0649 0.071 Uiso 1 1 calc R . . H40B H 0.6187 0.9755 -0.0351 0.071 Uiso 1 1 calc R . . H40C H 0.7003 0.8818 -0.0499 0.071 Uiso 1 1 calc R . . Cl1 Cl 0.51369(7) 0.84267(7) 0.56332(5) 0.0299(2) Uani 1 1 d . . . Cl2 Cl 0.79052(8) 0.36742(9) 0.50439(6) 0.0424(3) Uani 1 1 d . . . N2 N 0.8527(2) 0.7350(2) 0.42099(16) 0.0264(7) Uani 1 1 d . . . N1 N 0.8197(2) 0.7012(2) 0.55845(16) 0.0244(6) Uani 1 1 d . . . C50 C 0.8718(3) 0.7551(3) 0.3402(2) 0.0397(9) Uani 1 1 d . . . H50A H 0.9513 0.7968 0.3377 0.060 Uiso 1 1 calc R . . H50B H 0.8117 0.7965 0.3247 0.060 Uiso 1 1 calc R . . H50C H 0.8650 0.6850 0.3052 0.060 Uiso 1 1 calc R . . C51 C 0.7999(3) 0.6823(3) 0.6393(2) 0.0338(9) Uani 1 1 d . . . H51A H 0.7379 0.7228 0.6609 0.051 Uiso 1 1 calc R . . H51B H 0.8740 0.7075 0.6708 0.051 Uiso 1 1 calc R . . H51C H 0.7748 0.6041 0.6393 0.051 Uiso 1 1 calc R . . C52 C 0.8382(3) 0.8216(3) 0.5558(2) 0.0360(9) Uani 1 1 d . . . H52A H 0.8997 0.8603 0.5955 0.043 Uiso 1 1 calc R . . H52B H 0.7632 0.8507 0.5670 0.043 Uiso 1 1 calc R . . C54 C 0.9281(3) 0.6566(3) 0.5284(2) 0.0378(9) Uani 1 1 d . . . H54A H 0.9244 0.5804 0.5373 0.045 Uiso 1 1 calc R . . H54B H 1.0006 0.7008 0.5559 0.045 Uiso 1 1 calc R . . C55 C 0.9330(4) 0.6603(4) 0.4427(2) 0.0455(11) Uani 1 1 d . . . H55A H 1.0155 0.6864 0.4301 0.055 Uiso 1 1 calc R . . H55B H 0.9080 0.5860 0.4130 0.055 Uiso 1 1 calc R . . C53 C 0.8772(4) 0.8413(3) 0.4761(2) 0.0446(10) Uani 1 1 d . . . H53A H 0.8330 0.8953 0.4582 0.053 Uiso 1 1 calc R . . H53B H 0.9632 0.8708 0.4785 0.053 Uiso 1 1 calc R . . C56 C 0.7143(3) 0.6481(3) 0.5063(2) 0.0318(9) Uani 1 1 d . . . H56A H 0.6405 0.6679 0.5295 0.038 Uiso 1 1 calc R . . H56B H 0.7088 0.5677 0.4992 0.038 Uiso 1 1 calc R . . C57 C 0.7277(3) 0.6862(3) 0.4288(2) 0.0410(10) Uani 1 1 d . . . H57A H 0.7040 0.6234 0.3867 0.049 Uiso 1 1 calc R . . H57B H 0.6749 0.7409 0.4246 0.049 Uiso 1 1 calc R . . O1M O 0.8321(3) 0.1189(5) 0.5197(3) 0.1225(18) Uani 1 1 d D . . H1M H 0.7881 0.1448 0.4909 0.184 Uiso 1 1 calc RD . . C2M C 0.7714(4) 0.0963(4) 0.5844(3) 0.0631(13) Uani 1 1 d . . . H2MA H 0.7721 0.1642 0.6209 0.095 Uiso 1 1 calc R . . H2MB H 0.8104 0.0455 0.6090 0.095 Uiso 1 1 calc R . . H2MC H 0.6891 0.0632 0.5689 0.095 Uiso 1 1 calc R . . O3M O 1.3552(2) 1.0957(2) 0.27706(15) 0.0385(6) Uani 1 1 d D . . H3M H 1.390(4) 1.100(4) 0.3199(15) 0.058 Uiso 1 1 d D . . C4M C 1.4386(4) 1.1471(4) 0.2303(2) 0.0558(13) Uani 1 1 d . . . H4MA H 1.4838 1.0931 0.2035 0.084 Uiso 1 1 calc R . . H4MB H 1.4933 1.2053 0.2628 0.084 Uiso 1 1 calc R . . H4MC H 1.3964 1.1784 0.1924 0.084 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 C1 0.0170(15) 0.0191(17) 0.0223(19) 0.0066(14) 0.0044(13) 0.0066(13) C2 0.0187(15) 0.0194(17) 0.0179(18) 0.0019(13) 0.0022(13) 0.0073(13) C3 0.0127(14) 0.0189(16) 0.0208(18) 0.0084(14) 0.0006(12) 0.0069(12) C4 0.0195(16) 0.0214(17) 0.0196(18) 0.0082(14) 0.0055(13) 0.0066(13) O4 0.0321(12) 0.0247(13) 0.0175(13) 0.0035(10) 0.0081(10) 0.0002(10) C5 0.0260(17) 0.0220(18) 0.0206(19) 0.0031(14) 0.0053(14) 0.0069(14) C6 0.0200(16) 0.0161(16) 0.0249(19) 0.0046(14) 0.0029(13) 0.0022(13) O6 0.0359(14) 0.0202(13) 0.0313(15) -0.0009(11) 0.0146(11) -0.0008(10) C7 0.0156(15) 0.0188(16) 0.0205(18) 0.0061(14) 0.0014(13) 0.0026(12) C8 0.0166(15) 0.0152(16) 0.0211(18) 0.0026(13) -0.0014(13) -0.0005(12) C9 0.0196(16) 0.0183(16) 0.0160(17) 0.0040(13) 0.0013(13) 0.0013(13) C10 0.0167(15) 0.0178(16) 0.0181(18) 0.0033(14) 0.0005(12) 0.0008(13) C11 0.0201(16) 0.0148(16) 0.0260(19) 0.0065(14) 0.0000(13) 0.0037(13) O11 0.0297(12) 0.0274(13) 0.0269(14) 0.0143(11) 0.0039(11) 0.0122(10) C12 0.0232(16) 0.0187(17) 0.0230(19) 0.0096(14) 0.0030(14) 0.0001(13) C13 0.0161(15) 0.0196(17) 0.0207(18) 0.0055(14) 0.0050(13) -0.0008(13) O13 0.0301(13) 0.0282(13) 0.0318(15) 0.0139(12) 0.0144(10) 0.0096(11) C14 0.0224(16) 0.0167(16) 0.0211(18) 0.0076(14) 0.0018(13) 0.0053(13) C15 0.0182(15) 0.0184(16) 0.0211(18) 0.0012(14) 0.0047(13) 0.0079(13) C17 0.0172(15) 0.0204(17) 0.0207(18) 0.0039(14) 0.0050(13) 0.0053(13) C16 0.0194(16) 0.0199(17) 0.0177(18) 0.0032(14) 0.0013(13) 0.0073(13) C18 0.0171(16) 0.0233(18) 0.0258(19) 0.0021(15) 0.0028(13) 0.0053(13) O18 0.0199(11) 0.0297(14) 0.0392(16) 0.0138(11) -0.0075(10) -0.0013(10) C19 0.0179(16) 0.0278(18) 0.026(2) 0.0061(15) -0.0024(14) 0.0072(14) C20 0.0224(16) 0.0238(17) 0.0234(19) 0.0104(15) 0.0047(14) 0.0085(14) O20 0.0247(12) 0.0361(14) 0.0372(15) 0.0219(12) -0.0048(11) 0.0018(11) C21 0.0176(15) 0.0211(17) 0.0200(18) 0.0037(14) 0.0032(13) 0.0023(13) C22 0.0184(15) 0.0221(17) 0.0158(17) 0.0063(14) 0.0025(13) -0.0004(13) C23 0.0185(15) 0.0180(16) 0.0190(18) 0.0052(13) 0.0018(13) -0.0005(13) C24 0.0207(16) 0.0189(17) 0.0174(18) 0.0058(14) 0.0052(13) -0.0005(13) C25 0.0297(18) 0.0180(17) 0.0185(18) -0.0007(14) 0.0083(14) 0.0011(14) O25 0.0283(13) 0.0271(14) 0.0529(18) -0.0128(12) 0.0116(12) 0.0007(11) C26 0.0248(17) 0.0200(17) 0.0227(19) -0.0002(14) -0.0007(14) -0.0046(14) C27 0.0178(16) 0.0263(18) 0.0194(18) 0.0076(14) 0.0020(13) 0.0008(13) O27 0.0178(11) 0.0264(13) 0.0325(15) 0.0027(11) -0.0017(10) -0.0016(9) C28 0.0233(16) 0.0181(16) 0.0235(19) 0.0052(14) 0.0070(14) 0.0038(13) C29 0.0200(16) 0.0224(17) 0.0250(19) 0.0050(14) -0.0022(14) 0.0045(13) C32 0.0238(17) 0.0222(17) 0.0226(19) 0.0033(14) 0.0038(14) 0.0049(14) C30 0.0290(19) 0.033(2) 0.033(2) 0.0075(17) -0.0063(16) -0.0041(16) C31 0.071(3) 0.055(3) 0.040(3) 0.003(2) -0.022(2) -0.023(2) C33 0.0329(19) 0.0280(19) 0.030(2) 0.0014(16) 0.0006(16) -0.0004(15) C34 0.046(2) 0.047(2) 0.039(3) -0.004(2) -0.0078(19) -0.0086(19) C35 0.0237(16) 0.0218(17) 0.0199(19) 0.0016(14) 0.0050(13) 0.0025(13) C36 0.0368(19) 0.0273(19) 0.022(2) 0.0083(15) 0.0090(15) 0.0036(15) C37 0.050(2) 0.047(2) 0.029(2) 0.0135(19) 0.0052(18) 0.0080(19) C38 0.0225(16) 0.0251(18) 0.0210(18) 0.0079(14) 0.0019(13) 0.0040(14) C39 0.035(2) 0.033(2) 0.029(2) 0.0144(16) 0.0033(16) 0.0010(16) C40 0.057(3) 0.057(3) 0.030(2) 0.019(2) 0.0022(19) 0.002(2) Cl1 0.0359(5) 0.0291(5) 0.0238(5) 0.0011(4) 0.0034(4) 0.0055(4) Cl2 0.0304(5) 0.0684(7) 0.0336(6) 0.0195(5) 0.0021(4) 0.0123(5) N2 0.0237(14) 0.0317(16) 0.0231(16) 0.0021(13) 0.0005(12) 0.0052(12) N1 0.0211(14) 0.0269(15) 0.0259(17) 0.0030(13) 0.0015(12) 0.0076(12) C50 0.044(2) 0.053(2) 0.024(2) 0.0103(18) 0.0018(17) 0.0096(19) C51 0.035(2) 0.042(2) 0.026(2) 0.0083(17) 0.0073(16) 0.0095(17) C52 0.046(2) 0.028(2) 0.031(2) 0.0012(17) 0.0069(17) -0.0013(17) C54 0.0293(19) 0.057(3) 0.033(2) 0.0085(19) 0.0040(16) 0.0234(18) C55 0.048(2) 0.068(3) 0.031(2) 0.012(2) 0.0057(18) 0.037(2) C53 0.058(3) 0.032(2) 0.038(2) 0.0008(18) 0.007(2) -0.0064(19) C56 0.0205(17) 0.037(2) 0.038(2) 0.0134(17) -0.0041(15) -0.0024(15) C57 0.0264(19) 0.052(2) 0.046(3) 0.021(2) -0.0091(17) -0.0049(17) O1M 0.061(2) 0.180(5) 0.149(5) 0.094(4) 0.013(3) 0.014(3) C2M 0.068(3) 0.050(3) 0.075(4) 0.009(3) 0.011(3) 0.021(2) O3M 0.0318(14) 0.0465(16) 0.0317(16) 0.0045(13) -0.0072(11) -0.0079(12) C4M 0.053(3) 0.071(3) 0.035(3) 0.012(2) 0.000(2) -0.019(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.392(4) . ? C1 C2 1.395(4) . ? C1 C28 1.527(4) . ? C2 C3 1.393(4) . ? C2 H2 0.9500 . ? C3 C4 1.393(4) . ? C3 C7 1.529(4) . ? C4 O4 1.374(4) . ? C4 C5 1.391(4) . ? O4 H4 0.831(18) . ? C5 C6 1.389(4) . ? C5 H5 0.9500 . ? C6 O6 1.382(4) . ? O6 H6 0.843(18) . ? C7 C29 1.525(4) . ? C7 C8 1.530(4) . ? C7 H7 1.0000 . ? C8 C9 1.396(4) . ? C8 C13 1.397(4) . ? C9 C10 1.392(4) . ? C9 H9 0.9500 . ? C10 C11 1.392(4) . ? C10 C14 1.532(4) . ? C11 O11 1.380(4) . ? C11 C12 1.390(4) . ? O11 H11 0.826(18) . ? C12 C13 1.394(4) . ? C12 H12 0.9500 . ? C13 O13 1.374(4) . ? O13 H13 0.836(18) . ? C14 C15 1.526(4) . ? C14 C32 1.534(4) . ? C14 H14 1.0000 . ? C15 C16 1.386(4) . ? C15 C20 1.402(4) . ? C17 C16 1.393(4) . ? C17 C18 1.401(4) . ? C17 C21 1.521(4) . ? C16 H16 0.9500 . ? C18 O18 1.369(4) . ? C18 C19 1.394(5) . ? O18 H18 0.838(19) . ? C19 C20 1.384(4) . ? C19 H19 0.9500 . ? C20 O20 1.370(4) . ? O20 H20 0.838(18) . ? C21 C22 1.531(4) . ? C21 C35 1.537(4) . ? C21 H21 1.0000 . ? C22 C23 1.391(4) . ? C22 C27 1.397(4) . ? C23 C24 1.393(4) . ? C23 H23 0.9500 . ? C24 C25 1.393(4) . ? C24 C28 1.529(4) . ? C25 O25 1.378(4) . ? C25 C26 1.386(4) . ? O25 H25 0.837(19) . ? C26 C27 1.385(4) . ? C26 H26 0.9500 . ? C27 O27 1.382(4) . ? O27 H27 0.836(18) . ? C28 C38 1.534(4) . ? C28 H28 1.0000 . ? C29 C30 1.527(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C32 C33 1.523(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C30 C31 1.518(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C33 C34 1.517(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.524(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.523(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.520(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.517(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N2 C57 1.480(4) . ? N2 C55 1.493(5) . ? N2 C50 1.499(4) . ? N2 C53 1.502(4) . ? N1 C51 1.497(4) . ? N1 C56 1.497(4) . ? N1 C54 1.503(4) . ? N1 C52 1.505(4) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.527(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C54 C55 1.518(5) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C56 C57 1.520(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? O1M C2M 1.391(6) . ? O1M H1M 0.8400 . ? C2M H2MA 0.9800 . ? C2M H2MB 0.9800 . ? C2M H2MC 0.9800 . ? O3M C4M 1.419(5) . ? O3M H3M 0.837(19) . ? C4M H4MA 0.9800 . ? C4M H4MB 0.9800 . ? C4M H4MC 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 C6 C1 C2 117.2(3) . . ? C6 C1 C28 120.2(3) . . ? C2 C1 C28 122.6(3) . . ? C3 C2 C1 123.4(3) . . ? C3 C2 H2 118.3 . . ? C1 C2 H2 118.3 . . ? C4 C3 C2 117.1(3) . . ? C4 C3 C7 119.8(3) . . ? C2 C3 C7 123.1(3) . . ? O4 C4 C5 121.2(3) . . ? O4 C4 C3 117.3(3) . . ? C5 C4 C3 121.5(3) . . ? C4 O4 H4 110(3) . . ? C6 C5 C4 119.4(3) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? O6 C6 C5 120.7(3) . . ? O6 C6 C1 117.8(3) . . ? C5 C6 C1 121.4(3) . . ? C6 O6 H6 107(3) . . ? C29 C7 C3 113.6(2) . . ? C29 C7 C8 112.3(2) . . ? C3 C7 C8 110.4(2) . . ? C29 C7 H7 106.7 . . ? C3 C7 H7 106.7 . . ? C8 C7 H7 106.7 . . ? C9 C8 C13 117.0(3) . . ? C9 C8 C7 119.4(3) . . ? C13 C8 C7 123.5(3) . . ? C10 C9 C8 123.8(3) . . ? C10 C9 H9 118.1 . . ? C8 C9 H9 118.1 . . ? C11 C10 C9 117.2(3) . . ? C11 C10 C14 122.3(3) . . ? C9 C10 C14 120.5(3) . . ? O11 C11 C12 120.7(3) . . ? O11 C11 C10 118.2(3) . . ? C12 C11 C10 121.1(3) . . ? C11 O11 H11 111(3) . . ? C11 C12 C13 120.1(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? O13 C13 C12 115.9(3) . . ? O13 C13 C8 123.3(3) . . ? C12 C13 C8 120.7(3) . . ? C13 O13 H13 110(3) . . ? C15 C14 C10 111.1(2) . . ? C15 C14 C32 113.5(3) . . ? C10 C14 C32 111.1(2) . . ? C15 C14 H14 106.9 . . ? C10 C14 H14 106.9 . . ? C32 C14 H14 106.9 . . ? C16 C15 C20 116.8(3) . . ? C16 C15 C14 122.7(3) . . ? C20 C15 C14 120.4(3) . . ? C16 C17 C18 116.7(3) . . ? C16 C17 C21 123.0(3) . . ? C18 C17 C21 120.3(3) . . ? C15 C16 C17 124.5(3) . . ? C15 C16 H16 117.8 . . ? C17 C16 H16 117.8 . . ? O18 C18 C19 115.4(3) . . ? O18 C18 C17 123.8(3) . . ? C19 C18 C17 120.8(3) . . ? C18 O18 H18 111(3) . . ? C20 C19 C18 120.2(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? O20 C20 C19 115.7(3) . . ? O20 C20 C15 123.2(3) . . ? C19 C20 C15 121.0(3) . . ? C20 O20 H20 111(3) . . ? C17 C21 C22 110.1(2) . . ? C17 C21 C35 114.1(2) . . ? C22 C21 C35 111.5(2) . . ? C17 C21 H21 106.9 . . ? C22 C21 H21 106.9 . . ? C35 C21 H21 106.9 . . ? C23 C22 C27 116.3(3) . . ? C23 C22 C21 121.3(3) . . ? C27 C22 C21 122.4(3) . . ? C22 C23 C24 124.7(3) . . ? C22 C23 H23 117.7 . . ? C24 C23 H23 117.7 . . ? C23 C24 C25 116.4(3) . . ? C23 C24 C28 120.1(3) . . ? C25 C24 C28 123.4(3) . . ? O25 C25 C26 115.6(3) . . ? O25 C25 C24 123.5(3) . . ? C26 C25 C24 120.9(3) . . ? C25 O25 H25 108(3) . . ? C27 C26 C25 120.5(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? O27 C27 C26 122.0(3) . . ? O27 C27 C22 117.0(3) . . ? C26 C27 C22 121.0(3) . . ? C27 O27 H27 110(3) . . ? C1 C28 C24 111.7(3) . . ? C1 C28 C38 113.1(3) . . ? C24 C28 C38 112.0(3) . . ? C1 C28 H28 106.5 . . ? C24 C28 H28 106.5 . . ? C38 C28 H28 106.5 . . ? C7 C29 C30 113.9(3) . . ? C7 C29 H29A 108.8 . . ? C30 C29 H29A 108.8 . . ? C7 C29 H29B 108.8 . . ? C30 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C33 C32 C14 113.1(3) . . ? C33 C32 H32A 109.0 . . ? C14 C32 H32A 109.0 . . ? C33 C32 H32B 109.0 . . ? C14 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C31 C30 C29 112.4(3) . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30B 109.1 . . ? C29 C30 H30B 109.1 . . ? 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 . . ? C34 C33 C32 112.5(3) . . ? C34 C33 H33A 109.1 . . ? C32 C33 H33A 109.1 . . ? C34 C33 H33B 109.1 . . ? C32 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? 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 C21 113.2(2) . . ? C36 C35 H35A 108.9 . . ? C21 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C21 C35 H35B 108.9 . . ? H35A C35 H35B 107.8 . . ? C37 C36 C35 113.8(3) . . ? C37 C36 H36A 108.8 . . ? C35 C36 H36A 108.8 . . ? C37 C36 H36B 108.8 . . ? C35 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C28 113.7(3) . . ? C39 C38 H38A 108.8 . . ? C28 C38 H38A 108.8 . . ? C39 C38 H38B 108.8 . . ? C28 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? C40 C39 C38 112.6(3) . . ? C40 C39 H39A 109.1 . . ? C38 C39 H39A 109.1 . . ? C40 C39 H39B 109.1 . . ? C38 C39 H39B 109.1 . . ? H39A C39 H39B 107.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C57 N2 C55 109.1(3) . . ? C57 N2 C50 110.5(3) . . ? C55 N2 C50 110.8(3) . . ? C57 N2 C53 107.7(3) . . ? C55 N2 C53 109.0(3) . . ? C50 N2 C53 109.8(3) . . ? C51 N1 C56 110.8(3) . . ? C51 N1 C54 110.9(3) . . ? C56 N1 C54 108.9(3) . . ? C51 N1 C52 110.1(3) . . ? C56 N1 C52 108.0(3) . . ? C54 N1 C52 108.1(3) . . ? N2 C50 H50A 109.5 . . ? N2 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N2 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N1 C51 H51A 109.5 . . ? N1 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N1 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N1 C52 C53 109.8(3) . . ? N1 C52 H52A 109.7 . . ? C53 C52 H52A 109.7 . . ? N1 C52 H52B 109.7 . . ? C53 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? N1 C54 C55 109.0(3) . . ? N1 C54 H54A 109.9 . . ? C55 C54 H54A 109.9 . . ? N1 C54 H54B 109.9 . . ? C55 C54 H54B 109.9 . . ? H54A C54 H54B 108.3 . . ? N2 C55 C54 110.0(3) . . ? N2 C55 H55A 109.7 . . ? C54 C55 H55A 109.7 . . ? N2 C55 H55B 109.7 . . ? C54 C55 H55B 109.7 . . ? H55A C55 H55B 108.2 . . ? N2 C53 C52 108.8(3) . . ? N2 C53 H53A 109.9 . . ? C52 C53 H53A 109.9 . . ? N2 C53 H53B 109.9 . . ? C52 C53 H53B 109.9 . . ? H53A C53 H53B 108.3 . . ? N1 C56 C57 109.1(3) . . ? N1 C56 H56A 109.9 . . ? C57 C56 H56A 109.9 . . ? N1 C56 H56B 109.9 . . ? C57 C56 H56B 109.9 . . ? H56A C56 H56B 108.3 . . ? N2 C57 C56 110.0(3) . . ? N2 C57 H57A 109.7 . . ? C56 C57 H57A 109.7 . . ? N2 C57 H57B 109.7 . . ? C56 C57 H57B 109.7 . . ? H57A C57 H57B 108.2 . . ? C2M O1M H1M 109.5 . . ? O1M C2M H2MA 109.5 . . ? O1M C2M H2MB 109.5 . . ? H2MA C2M H2MB 109.5 . . ? O1M C2M H2MC 109.5 . . ? H2MA C2M H2MC 109.5 . . ? H2MB C2M H2MC 109.5 . . ? C4M O3M H3M 106(3) . . ? O3M C4M H4MA 109.5 . . ? O3M C4M H4MB 109.5 . . ? H4MA C4M H4MB 109.5 . . ? O3M C4M H4MC 109.5 . . ? H4MA C4M H4MC 109.5 . . ? H4MB C4M H4MC 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 C6 C1 C2 C3 -0.7(4) . . . . ? C28 C1 C2 C3 178.9(3) . . . . ? C1 C2 C3 C4 -0.4(4) . . . . ? C1 C2 C3 C7 -178.8(3) . . . . ? C2 C3 C4 O4 -178.1(3) . . . . ? C7 C3 C4 O4 0.3(4) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? C7 C3 C4 C5 179.6(3) . . . . ? O4 C4 C5 C6 178.5(3) . . . . ? C3 C4 C5 C6 -0.7(5) . . . . ? C4 C5 C6 O6 179.9(3) . . . . ? C4 C5 C6 C1 -0.5(5) . . . . ? C2 C1 C6 O6 -179.2(3) . . . . ? C28 C1 C6 O6 1.2(4) . . . . ? C2 C1 C6 C5 1.2(5) . . . . ? C28 C1 C6 C5 -178.4(3) . . . . ? C4 C3 C7 C29 150.0(3) . . . . ? C2 C3 C7 C29 -31.7(4) . . . . ? C4 C3 C7 C8 -82.8(3) . . . . ? C2 C3 C7 C8 95.6(3) . . . . ? C29 C7 C8 C9 46.9(4) . . . . ? C3 C7 C8 C9 -81.0(3) . . . . ? C29 C7 C8 C13 -131.3(3) . . . . ? C3 C7 C8 C13 100.8(3) . . . . ? C13 C8 C9 C10 2.6(4) . . . . ? C7 C8 C9 C10 -175.7(3) . . . . ? C8 C9 C10 C11 -2.5(4) . . . . ? C8 C9 C10 C14 175.3(3) . . . . ? C9 C10 C11 O11 -178.8(3) . . . . ? C14 C10 C11 O11 3.5(4) . . . . ? C9 C10 C11 C12 0.7(4) . . . . ? C14 C10 C11 C12 -177.0(3) . . . . ? O11 C11 C12 C13 -179.8(3) . . . . ? C10 C11 C12 C13 0.7(5) . . . . ? C11 C12 C13 O13 178.8(3) . . . . ? C11 C12 C13 C8 -0.6(4) . . . . ? C9 C8 C13 O13 179.7(3) . . . . ? C7 C8 C13 O13 -2.1(5) . . . . ? C9 C8 C13 C12 -1.0(4) . . . . ? C7 C8 C13 C12 177.2(3) . . . . ? C11 C10 C14 C15 -102.4(3) . . . . ? C9 C10 C14 C15 80.0(3) . . . . ? C11 C10 C14 C32 130.2(3) . . . . ? C9 C10 C14 C32 -47.4(4) . . . . ? C10 C14 C15 C16 -98.5(3) . . . . ? C32 C14 C15 C16 27.6(4) . . . . ? C10 C14 C15 C20 80.4(4) . . . . ? C32 C14 C15 C20 -153.5(3) . . . . ? C20 C15 C16 C17 -0.1(5) . . . . ? C14 C15 C16 C17 178.8(3) . . . . ? C18 C17 C16 C15 0.4(5) . . . . ? C21 C17 C16 C15 -176.1(3) . . . . ? C16 C17 C18 O18 180.0(3) . . . . ? C21 C17 C18 O18 -3.4(5) . . . . ? C16 C17 C18 C19 0.0(5) . . . . ? C21 C17 C18 C19 176.6(3) . . . . ? O18 C18 C19 C20 179.4(3) . . . . ? C17 C18 C19 C20 -0.6(5) . . . . ? C18 C19 C20 O20 -178.0(3) . . . . ? C18 C19 C20 C15 0.9(5) . . . . ? C16 C15 C20 O20 178.3(3) . . . . ? C14 C15 C20 O20 -0.7(5) . . . . ? C16 C15 C20 C19 -0.6(5) . . . . ? C14 C15 C20 C19 -179.5(3) . . . . ? C16 C17 C21 C22 97.8(3) . . . . ? C18 C17 C21 C22 -78.6(3) . . . . ? C16 C17 C21 C35 -28.4(4) . . . . ? C18 C17 C21 C35 155.2(3) . . . . ? C17 C21 C22 C23 -79.1(4) . . . . ? C35 C21 C22 C23 48.5(4) . . . . ? C17 C21 C22 C27 101.2(3) . . . . ? C35 C21 C22 C27 -131.1(3) . . . . ? C27 C22 C23 C24 1.9(5) . . . . ? C21 C22 C23 C24 -177.8(3) . . . . ? C22 C23 C24 C25 -4.5(5) . . . . ? C22 C23 C24 C28 172.0(3) . . . . ? C23 C24 C25 O25 -177.6(3) . . . . ? C28 C24 C25 O25 6.0(5) . . . . ? C23 C24 C25 C26 4.0(5) . . . . ? C28 C24 C25 C26 -172.4(3) . . . . ? O25 C25 C26 C27 -179.7(3) . . . . ? C24 C25 C26 C27 -1.2(5) . . . . ? C25 C26 C27 O27 179.9(3) . . . . ? C25 C26 C27 C22 -1.5(5) . . . . ? C23 C22 C27 O27 179.8(3) . . . . ? C21 C22 C27 O27 -0.5(4) . . . . ? C23 C22 C27 C26 1.2(5) . . . . ? C21 C22 C27 C26 -179.1(3) . . . . ? C6 C1 C28 C24 86.0(3) . . . . ? C2 C1 C28 C24 -93.6(3) . . . . ? C6 C1 C28 C38 -146.6(3) . . . . ? C2 C1 C28 C38 33.8(4) . . . . ? C23 C24 C28 C1 81.7(4) . . . . ? C25 C24 C28 C1 -102.1(3) . . . . ? C23 C24 C28 C38 -46.3(4) . . . . ? C25 C24 C28 C38 130.0(3) . . . . ? C3 C7 C29 C30 -174.3(3) . . . . ? C8 C7 C29 C30 59.4(3) . . . . ? C15 C14 C32 C33 173.4(3) . . . . ? C10 C14 C32 C33 -60.5(3) . . . . ? C7 C29 C30 C31 -177.2(3) . . . . ? C14 C32 C33 C34 -176.2(3) . . . . ? C17 C21 C35 C36 -172.2(3) . . . . ? C22 C21 C35 C36 62.3(3) . . . . ? C21 C35 C36 C37 -178.4(3) . . . . ? C1 C28 C38 C39 176.9(3) . . . . ? C24 C28 C38 C39 -55.8(4) . . . . ? C28 C38 C39 C40 -177.7(3) . . . . ? C51 N1 C52 C53 171.3(3) . . . . ? C56 N1 C52 C53 -67.7(4) . . . . ? C54 N1 C52 C53 50.1(4) . . . . ? C51 N1 C54 C55 170.6(3) . . . . ? C56 N1 C54 C55 48.4(4) . . . . ? C52 N1 C54 C55 -68.7(4) . . . . ? C57 N2 C55 C54 -68.1(4) . . . . ? C50 N2 C55 C54 170.2(3) . . . . ? C53 N2 C55 C54 49.2(4) . . . . ? N1 C54 C55 N2 16.7(4) . . . . ? C57 N2 C53 C52 50.7(4) . . . . ? C55 N2 C53 C52 -67.5(4) . . . . ? C50 N2 C53 C52 171.0(3) . . . . ? N1 C52 C53 N2 15.2(4) . . . . ? C51 N1 C56 C57 169.6(3) . . . . ? C54 N1 C56 C57 -68.1(4) . . . . ? C52 N1 C56 C57 49.0(4) . . . . ? C55 N2 C57 C56 48.2(4) . . . . ? C50 N2 C57 C56 170.2(3) . . . . ? C53 N2 C57 C56 -69.9(4) . . . . ? N1 C56 C57 N2 16.9(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 Cl1 0.831(18) 2.25(2) 3.064(2) 165(4) . O6 H6 Cl1 0.843(18) 2.30(2) 3.129(2) 169(4) 2_676 O11 H11 Cl2 0.826(18) 2.20(2) 3.006(3) 165(4) . O13 H13 O4 0.836(18) 1.95(2) 2.755(3) 163(4) . O25 H25 O6 0.837(19) 2.04(2) 2.847(3) 161(4) . O27 H27 O3M 0.836(18) 1.837(19) 2.670(3) 173(4) . O1M H1M Cl2 0.84 2.77 3.283(6) 121.5 . O18 H18 O27 0.838(19) 1.93(2) 2.751(3) 166(4) . O20 H20 O11 0.838(18) 1.95(2) 2.767(3) 165(4) . O3M H3M Cl1 0.837(19) 2.26(2) 3.080(3) 165(4) 2_776 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.957 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.065 #==END data_Complex5 _database_code_depnum_ccdc_archive 'CCDC 254962' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C52H72O8*1.5C8H18N3Br*C2H6O*H2O _chemical_formula_sum 'C66 H107 Br3 N3 O10' _chemical_formula_weight 1342.28 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 monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 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 53.2560(8) _cell_length_b 12.6490(3) _cell_length_c 20.5761(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.955(1) _cell_angle_gamma 90.00 _cell_volume 13727.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5672 _exptl_absorpt_coefficient_mu 1.819 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6147 _exptl_absorpt_correction_T_max 0.6473 _exptl_absorpt_process_details 'R. H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38.' _exptl_special_details ; dx = 30, 30 sec./deg., 1 deg. ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotaion in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 32427 _diffrn_reflns_av_R_equivalents 0.1370 _diffrn_reflns_av_sigmaI/netI 0.1194 _diffrn_reflns_limit_h_min -63 _diffrn_reflns_limit_h_max 61 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.05 _reflns_number_total 11413 _reflns_number_gt 6464 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+58.7597P] 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 11413 _refine_ls_number_parameters 789 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1450 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1656 _refine_ls_wR_factor_gt 0.1346 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.12658(9) 0.7599(5) 0.3201(3) 0.0229(13) Uani 1 1 d . . . C2 C 0.12452(9) 0.6729(5) 0.3598(3) 0.0225(13) Uani 1 1 d . . . H2 H 0.1362 0.6676 0.3990 0.027 Uiso 1 1 calc R . . C3 C 0.10648(9) 0.5917(5) 0.3469(3) 0.0223(13) Uani 1 1 d . . . C4 C 0.08883(9) 0.6064(5) 0.2906(3) 0.0237(13) Uani 1 1 d . . . O4 O 0.06997(7) 0.5309(3) 0.2769(2) 0.0293(10) Uani 1 1 d D . . H4 H 0.0586(9) 0.559(5) 0.251(3) 0.044 Uiso 1 1 d D . . C5 C 0.08968(9) 0.6925(5) 0.2490(3) 0.0254(14) Uani 1 1 d . . . H5 H 0.0773 0.6999 0.2113 0.030 Uiso 1 1 calc R . . C6 C 0.10858(9) 0.7672(5) 0.2623(3) 0.0233(13) Uani 1 1 d . . . O6 O 0.11008(7) 0.8507(4) 0.2204(2) 0.0328(11) Uani 1 1 d D . . H6 H 0.0985(9) 0.852(6) 0.188(2) 0.049 Uiso 1 1 d D . . C7 C 0.10743(9) 0.4943(5) 0.3887(3) 0.0245(13) Uani 1 1 d . . . H7 H 0.0951 0.4433 0.3649 0.029 Uiso 1 1 calc R . . C8 C 0.09873(9) 0.5132(5) 0.4558(3) 0.0230(13) Uani 1 1 d . . . C9 C 0.11503(9) 0.5270(5) 0.5142(3) 0.0248(14) Uani 1 1 d . . . H9 H 0.1327 0.5250 0.5121 0.030 Uiso 1 1 calc R . . C10 C 0.10741(9) 0.5435(5) 0.5751(3) 0.0213(13) Uani 1 1 d . . . C11 C 0.08138(10) 0.5470(5) 0.5775(3) 0.0264(14) Uani 1 1 d . . . O11 O 0.07062(7) 0.5620(4) 0.6339(2) 0.0393(12) Uani 1 1 d D . . H11 H 0.0815(10) 0.584(6) 0.664(3) 0.059 Uiso 1 1 d D . . C12 C 0.06427(9) 0.5338(5) 0.5202(3) 0.0263(14) Uani 1 1 d . . . H12 H 0.0466 0.5346 0.5225 0.032 Uiso 1 1 calc R . . C13 C 0.07265(9) 0.5198(5) 0.4609(3) 0.0268(14) Uani 1 1 d . . . O13 O 0.05471(7) 0.5100(4) 0.4061(2) 0.0343(11) Uani 1 1 d D . . H13 H 0.0612(12) 0.507(6) 0.372(2) 0.051 Uiso 1 1 d D . . C14 C 0.14756(9) 0.8419(5) 0.3362(3) 0.0252(14) Uani 1 1 d . . . H14 H 0.1454 0.8942 0.2993 0.030 Uiso 1 1 calc R . . C15 C 0.14448(9) 0.9033(5) 0.3980(3) 0.0248(14) Uani 1 1 d . . . C16 C 0.15658(9) 0.8792(5) 0.4607(3) 0.0249(14) Uani 1 1 d . . . H16 H 0.1673 0.8187 0.4654 0.030 Uiso 1 1 calc R . . C17 C 0.15415(9) 0.9369(5) 0.5167(3) 0.0205(13) Uani 1 1 d . . . C18 C 0.13823(10) 1.0270(5) 0.5087(3) 0.0276(14) Uani 1 1 d . . . O18 O 0.13439(9) 1.0921(4) 0.5590(2) 0.0490(13) Uani 1 1 d D . . H18 H 0.1374(14) 1.064(6) 0.596(2) 0.073 Uiso 1 1 d D . . C19 C 0.12565(10) 1.0526(5) 0.4479(3) 0.0321(15) Uani 1 1 d . . . H19 H 0.1146 1.1119 0.4432 0.038 Uiso 1 1 calc R . . C20 C 0.12887(9) 0.9929(5) 0.3935(3) 0.0275(14) Uani 1 1 d . . . O20 O 0.11605(8) 1.0150(4) 0.3324(2) 0.0403(12) Uani 1 1 d D . . H20 H 0.1079(12) 1.071(4) 0.338(4) 0.060 Uiso 1 1 d D . . C21 C 0.16799(9) 0.9083(5) 0.5840(3) 0.0254(14) Uani 1 1 d . . . H21 H 0.1715 0.9767 0.6079 0.030 Uiso 1 1 calc R . . C22 C 0.15093(9) 0.8446(5) 0.6241(3) 0.0256(14) Uani 1 1 d . . . C23 C 0.14648(9) 0.7365(5) 0.6151(3) 0.0246(14) Uani 1 1 d . . . H23 H 0.1547 0.7014 0.5831 0.030 Uiso 1 1 calc R . . C24 C 0.13088(9) 0.6768(5) 0.6494(3) 0.0250(14) Uani 1 1 d . . . O25 O 0.10263(9) 0.6726(4) 0.7287(2) 0.0491(13) Uani 1 1 d D . . H25 H 0.0972 0.7107 0.7572 0.074 Uiso 1 1 calc RD . . C25 C 0.11857(10) 0.7320(6) 0.6948(3) 0.0317(16) Uani 1 1 d . . . C26 C 0.12199(10) 0.8386(5) 0.7051(3) 0.0332(16) Uani 1 1 d . . . H26 H 0.1132 0.8739 0.7360 0.040 Uiso 1 1 calc R . . C27 C 0.13816(9) 0.8949(5) 0.6707(3) 0.0278(14) Uani 1 1 d . . . O27 O 0.14237(7) 1.0016(4) 0.6808(2) 0.0364(11) Uani 1 1 d D . . H27 H 0.1319(10) 1.029(5) 0.703(3) 0.055 Uiso 1 1 d D . . C28 C 0.12625(9) 0.5591(5) 0.6370(3) 0.0280(14) Uani 1 1 d . . . H28 H 0.1176 0.5330 0.6741 0.034 Uiso 1 1 calc R . . C29 C 0.13379(10) 0.4420(5) 0.3926(3) 0.0286(14) Uani 1 1 d . . . H29A H 0.1385 0.4384 0.3478 0.034 Uiso 1 1 calc R . . H29B H 0.1463 0.4881 0.4190 0.034 Uiso 1 1 calc R . . C30 C 0.13582(12) 0.3343(6) 0.4214(4) 0.054(2) Uani 1 1 d . . . H30A H 0.1225 0.2891 0.3973 0.065 Uiso 1 1 calc R . . H30B H 0.1326 0.3383 0.4676 0.065 Uiso 1 1 calc R . . C31 C 0.16208(14) 0.2812(6) 0.4193(4) 0.061(2) Uani 1 1 d . . . H31A H 0.1755 0.3294 0.4402 0.073 Uiso 1 1 calc R . . H31B H 0.1629 0.2156 0.4458 0.073 Uiso 1 1 calc R . . C32 C 0.16760(14) 0.2544(8) 0.3523(4) 0.070(3) Uani 1 1 d . . . H32A H 0.1657 0.3190 0.3248 0.084 Uiso 1 1 calc R . . H32B H 0.1549 0.2024 0.3324 0.084 Uiso 1 1 calc R . . C33 C 0.19429(18) 0.2087(9) 0.3514(5) 0.097(4) Uani 1 1 d . . . H33A H 0.2070 0.2607 0.3710 0.116 Uiso 1 1 calc R . . H33B H 0.1962 0.1439 0.3786 0.116 Uiso 1 1 calc R . . C35 C 0.17384(9) 0.7916(5) 0.3363(3) 0.0319(16) Uani 1 1 d . . . H35A H 0.1784 0.7512 0.3775 0.038 Uiso 1 1 calc R . . H35B H 0.1732 0.7415 0.2992 0.038 Uiso 1 1 calc R . . C36 C 0.19416(12) 0.8750(7) 0.3305(4) 0.056(2) Uani 1 1 d . . . H36A H 0.1884 0.9203 0.2922 0.068 Uiso 1 1 calc R . . H36B H 0.1957 0.9204 0.3701 0.068 Uiso 1 1 calc R . . C37 C 0.21937(14) 0.8335(8) 0.3234(5) 0.081(3) Uani 1 1 d . B . H37A H 0.2175 0.7804 0.2877 0.097 Uiso 1 1 calc R . . H37B H 0.2262 0.7965 0.3644 0.097 Uiso 1 1 calc R . . C38 C 0.23855(16) 0.9150(9) 0.3086(6) 0.103(4) Uani 1 1 d D . . H38A H 0.2301 0.9617 0.2735 0.124 Uiso 1 1 calc R A 1 H38B H 0.2428 0.9592 0.3483 0.124 Uiso 1 1 calc R A 1 C39 C 0.2614(3) 0.8802(14) 0.2892(10) 0.117(8) Uani 0.68(2) 1 d PD B 1 H39A H 0.2573 0.8248 0.2554 0.141 Uiso 0.68(2) 1 calc PR B 1 H39B H 0.2714 0.8460 0.3276 0.141 Uiso 0.68(2) 1 calc PR B 1 C40 C 0.2784(4) 0.9611(16) 0.2620(10) 0.122(9) Uani 0.68(2) 1 d PD B 1 H40A H 0.2941 0.9264 0.2529 0.183 Uiso 0.68(2) 1 calc PR B 1 H40B H 0.2827 1.0176 0.2942 0.183 Uiso 0.68(2) 1 calc PR B 1 H40C H 0.2696 0.9911 0.2212 0.183 Uiso 0.68(2) 1 calc PR B 1 C39B C 0.2435(4) 0.944(2) 0.2495(10) 0.073(12) Uani 0.32(2) 1 d PD B 2 H39C H 0.2285 0.9820 0.2268 0.087 Uiso 0.32(2) 1 calc PR B 2 H39D H 0.2458 0.8797 0.2237 0.087 Uiso 0.32(2) 1 calc PR B 2 C40B C 0.2667(5) 1.015(3) 0.2490(12) 0.095(15) Uani 0.32(2) 1 d PD B 2 H40D H 0.2694 1.0278 0.2036 0.142 Uiso 0.32(2) 1 calc PR B 2 H40E H 0.2816 0.9796 0.2727 0.142 Uiso 0.32(2) 1 calc PR B 2 H40F H 0.2639 1.0821 0.2704 0.142 Uiso 0.32(2) 1 calc PR B 2 C41 C 0.19386(9) 0.8559(5) 0.5831(3) 0.0329(16) Uani 1 1 d D . . H41A H 0.2012 0.8384 0.6288 0.039 Uiso 1 1 calc R . . H41B H 0.1914 0.7887 0.5584 0.039 Uiso 1 1 calc R . . C42 C 0.21260(10) 0.9234(6) 0.5529(4) 0.0420(18) Uani 1 1 d . . . H42A H 0.2130 0.9949 0.5726 0.050 Uiso 1 1 calc R . . H42B H 0.2067 0.9307 0.5053 0.050 Uiso 1 1 calc R . . C43 C 0.23921(11) 0.8782(7) 0.5624(4) 0.054(2) Uani 1 1 d . . . H43A H 0.2458 0.8800 0.6098 0.065 Uiso 1 1 calc R . . H43B H 0.2383 0.8032 0.5486 0.065 Uiso 1 1 calc R . . C44 C 0.25779(11) 0.9347(7) 0.5255(4) 0.062(2) Uani 1 1 d . . . H44A H 0.2581 1.0105 0.5375 0.074 Uiso 1 1 calc R . . H44B H 0.2518 0.9296 0.4779 0.074 Uiso 1 1 calc R . . C45 C 0.28483(13) 0.8903(8) 0.5392(5) 0.074(3) Uani 1 1 d . . . H45A H 0.2915 0.9034 0.5859 0.089 Uiso 1 1 calc R . . H45B H 0.2841 0.8128 0.5326 0.089 Uiso 1 1 calc R . . C46 C 0.30228(15) 0.9347(8) 0.4987(5) 0.081(3) Uani 1 1 d . . . H46A H 0.3190 0.9026 0.5104 0.122 Uiso 1 1 calc R . . H46B H 0.3035 1.0112 0.5057 0.122 Uiso 1 1 calc R . . H46C H 0.2961 0.9203 0.4524 0.122 Uiso 1 1 calc R . . C47 C 0.15077(10) 0.4955(5) 0.6399(3) 0.0309(15) Uani 1 1 d . . . H47A H 0.1590 0.5123 0.6008 0.037 Uiso 1 1 calc R . . H47B H 0.1625 0.5168 0.6793 0.037 Uiso 1 1 calc R . . C48 C 0.14619(11) 0.3768(6) 0.6423(3) 0.0392(17) Uani 1 1 d . . . H48A H 0.1367 0.3542 0.5997 0.047 Uiso 1 1 calc R . . H48B H 0.1354 0.3621 0.6766 0.047 Uiso 1 1 calc R . . C49 C 0.17050(12) 0.3100(6) 0.6564(3) 0.0467(18) Uani 1 1 d . . . H49A H 0.1807 0.3363 0.6971 0.056 Uiso 1 1 calc R . . H49B H 0.1657 0.2359 0.6643 0.056 Uiso 1 1 calc R . . C50 C 0.18638(13) 0.3115(7) 0.6032(4) 0.061(2) Uani 1 1 d . . . H50A H 0.1914 0.3854 0.5956 0.074 Uiso 1 1 calc R . . H50B H 0.1762 0.2857 0.5623 0.074 Uiso 1 1 calc R . . C51 C 0.21043(16) 0.2435(8) 0.6177(5) 0.081(3) Uani 1 1 d . . . H51A H 0.2202 0.2673 0.6597 0.097 Uiso 1 1 calc R . . H51B H 0.2054 0.1692 0.6235 0.097 Uiso 1 1 calc R . . C52 C 0.2274(2) 0.2474(10) 0.5656(6) 0.131(5) Uani 1 1 d . . . H52A H 0.2422 0.2026 0.5784 0.196 Uiso 1 1 calc R . . H52B H 0.2329 0.3205 0.5602 0.196 Uiso 1 1 calc R . . H52C H 0.2181 0.2218 0.5241 0.196 Uiso 1 1 calc R . . C34 C 0.1993(2) 0.1820(12) 0.2817(6) 0.142(6) Uani 1 1 d . . . H34A H 0.2164 0.1526 0.2834 0.213 Uiso 1 1 calc R . . H34B H 0.1979 0.2464 0.2549 0.213 Uiso 1 1 calc R . . H34C H 0.1869 0.1300 0.2622 0.213 Uiso 1 1 calc R . . Br1 Br 0.072915(11) 0.80747(6) 0.82483(4) 0.0431(2) Uani 1 1 d . . . Br2 Br 0.023558(12) 0.99544(6) 0.12129(4) 0.0518(2) Uani 1 1 d . . . Br3 Br 0.01643(3) 0.65015(12) 0.20186(7) 0.0343(3) Uani 0.50 1 d P C 1 O1A O 0.03000(19) 0.6210(9) 0.2087(5) 0.044(3) Uani 0.50 1 d P D 2 Br4 Br -0.00200(2) 0.57984(14) 0.44198(8) 0.0377(4) Uani 0.50 1 d P E 1 O2A O -0.00232(16) 0.6461(9) 0.4679(5) 0.043(3) Uani 0.50 1 d P F 2 N1 N 0.04754(8) 0.8770(4) 0.3798(2) 0.0299(12) Uani 1 1 d . . . N2 N 0.06684(8) 0.8527(4) 0.4993(3) 0.0321(13) Uani 1 1 d . . . C1C C 0.07826(12) 0.8391(6) 0.5695(3) 0.048(2) Uani 1 1 d . . . H1CA H 0.0950 0.8728 0.5766 0.072 Uiso 1 1 calc R . . H1CB H 0.0800 0.7636 0.5797 0.072 Uiso 1 1 calc R . . H1CC H 0.0672 0.8720 0.5981 0.072 Uiso 1 1 calc R . . C2C C 0.03657(12) 0.8926(6) 0.3101(3) 0.048(2) Uani 1 1 d . . . H2CA H 0.0370 0.8257 0.2863 0.073 Uiso 1 1 calc R . . H2CB H 0.0465 0.9458 0.2901 0.073 Uiso 1 1 calc R . . H2CC H 0.0190 0.9167 0.3078 0.073 Uiso 1 1 calc R . . C3C C 0.03252(10) 0.7966(5) 0.4121(3) 0.0348(16) Uani 1 1 d . . . H3CA H 0.0353 0.7252 0.3948 0.042 Uiso 1 1 calc R . . H3CB H 0.0142 0.8132 0.4029 0.042 Uiso 1 1 calc R . . C4C C 0.04127(10) 0.7998(5) 0.4861(3) 0.0358(16) Uani 1 1 d . . . H4CA H 0.0288 0.8394 0.5081 0.043 Uiso 1 1 calc R . . H4CB H 0.0424 0.7269 0.5038 0.043 Uiso 1 1 calc R . . C5C C 0.06333(10) 0.9672(5) 0.4833(3) 0.0300(15) Uani 1 1 d . . . H5CA H 0.0800 1.0011 0.4825 0.036 Uiso 1 1 calc R . . H5CB H 0.0549 1.0026 0.5173 0.036 Uiso 1 1 calc R . . C6C C 0.04725(10) 0.9787(5) 0.4167(3) 0.0291(14) Uani 1 1 d . . . H6CA H 0.0296 0.9970 0.4225 0.035 Uiso 1 1 calc R . . H6CB H 0.0541 1.0364 0.3917 0.035 Uiso 1 1 calc R . . C7C C 0.07457(10) 0.8368(6) 0.3851(4) 0.0427(19) Uani 1 1 d . . . H7CA H 0.0856 0.8928 0.3710 0.051 Uiso 1 1 calc R . . H7CB H 0.0753 0.7751 0.3558 0.051 Uiso 1 1 calc R . . C8C C 0.08410(10) 0.8048(5) 0.4558(3) 0.0377(17) Uani 1 1 d . . . H8CA H 0.0841 0.7269 0.4600 0.045 Uiso 1 1 calc R . . H8CB H 0.1016 0.8306 0.4686 0.045 Uiso 1 1 calc R . . N3 N -0.00150(9) 0.3145(5) 0.1887(3) 0.0418(15) Uani 1 1 d . . . C9C C -0.00359(13) 0.2047(6) 0.2146(4) 0.067(3) Uani 1 1 d . . . H9CA H -0.0212 0.1790 0.2036 0.080 Uiso 1 1 calc R . . H9CB H 0.0077 0.1566 0.1940 0.080 Uiso 1 1 calc R . . C10C C 0.02345(10) 0.3593(5) 0.2188(3) 0.0372(17) Uani 1 1 d . . . H10A H 0.0270 0.4254 0.1960 0.045 Uiso 1 1 calc R . . H10B H 0.0372 0.3083 0.2144 0.045 Uiso 1 1 calc R . . C11C C -0.00356(19) 0.3193(12) 0.1151(4) 0.129(6) Uani 1 1 d . . . H11A H 0.0100 0.2768 0.1004 0.193 Uiso 1 1 calc R . . H11B H -0.0019 0.3928 0.1013 0.193 Uiso 1 1 calc R . . H11C H -0.0201 0.2914 0.0956 0.193 Uiso 1 1 calc R . . C12C C -0.02231(10) 0.3814(5) 0.2099(3) 0.0309(15) Uani 1 1 d . . . H12A H -0.0188 0.4572 0.2035 0.037 Uiso 1 1 calc R . . H12B H -0.0387 0.3637 0.1834 0.037 Uiso 1 1 calc R . . O1E O 0.07409(8) 0.8454(4) 0.1166(2) 0.0436(11) Uiso 1 1 d . G . H1E H 0.0607 0.8627 0.1309 0.065 Uiso 1 1 calc R . . C2E C 0.06987(15) 0.7488(7) 0.0787(4) 0.065(2) Uiso 1 1 d D . . H2EA H 0.0566 0.7072 0.0965 0.078 Uiso 0.683(19) 1 calc PR G 1 H2EB H 0.0857 0.7066 0.0852 0.078 Uiso 0.683(19) 1 calc PR G 1 H2ED H 0.0758 0.6879 0.1069 0.078 Uiso 0.317(19) 1 calc PR G 2 H2EC H 0.0514 0.7399 0.0647 0.078 Uiso 0.317(19) 1 calc PR G 2 C3E C 0.0622(2) 0.7626(10) 0.0087(5) 0.054(4) Uiso 0.683(19) 1 d PD G 1 H3EA H 0.0518 0.7026 -0.0086 0.081 Uiso 0.683(19) 1 calc PR G 1 H3EB H 0.0774 0.7666 -0.0135 0.081 Uiso 0.683(19) 1 calc PR G 1 H3EC H 0.0525 0.8282 0.0010 0.081 Uiso 0.683(19) 1 calc PR G 1 C3EB C 0.0820(5) 0.748(2) 0.0251(11) 0.068(10) Uiso 0.317(19) 1 d PD G 2 H3ED H 0.0782 0.6824 0.0008 0.102 Uiso 0.317(19) 1 calc PR G 2 H3EE H 0.1003 0.7542 0.0388 0.102 Uiso 0.317(19) 1 calc PR G 2 H3EF H 0.0761 0.8085 -0.0031 0.102 Uiso 0.317(19) 1 calc PR G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(3) 0.027(4) 0.018(3) -0.003(3) 0.002(2) -0.006(2) C2 0.028(3) 0.022(4) 0.016(3) -0.001(3) -0.001(2) 0.000(2) C3 0.027(3) 0.019(4) 0.020(3) -0.003(3) 0.002(2) -0.001(2) C4 0.021(3) 0.022(4) 0.027(4) -0.007(3) 0.001(2) 0.001(2) O4 0.027(2) 0.026(3) 0.032(3) 0.000(2) -0.0051(16) -0.0083(17) C5 0.019(3) 0.038(4) 0.018(3) -0.001(3) 0.000(2) -0.006(2) C6 0.029(3) 0.022(4) 0.019(3) 0.004(3) 0.003(2) 0.003(2) O6 0.028(2) 0.039(3) 0.028(3) 0.015(2) -0.0075(16) -0.0098(18) C7 0.026(3) 0.025(4) 0.020(3) -0.002(3) -0.003(2) -0.003(2) C8 0.025(3) 0.021(4) 0.023(3) 0.002(3) 0.002(2) 0.000(2) C9 0.019(3) 0.026(4) 0.029(4) -0.001(3) 0.003(2) -0.003(2) C10 0.023(3) 0.017(3) 0.024(3) 0.000(3) 0.005(2) -0.002(2) C11 0.030(3) 0.023(4) 0.029(4) -0.002(3) 0.013(2) -0.003(2) O11 0.034(2) 0.054(3) 0.033(3) -0.007(3) 0.0150(18) -0.005(2) C12 0.019(3) 0.028(4) 0.033(4) -0.001(3) 0.006(2) -0.001(2) C13 0.024(3) 0.019(4) 0.036(4) 0.006(3) -0.002(2) -0.008(2) O13 0.025(2) 0.049(3) 0.028(3) -0.008(2) -0.0006(17) -0.0048(19) C14 0.025(3) 0.027(4) 0.023(3) 0.006(3) 0.001(2) -0.008(2) C15 0.022(3) 0.027(4) 0.026(4) -0.002(3) 0.004(2) -0.006(2) C16 0.020(3) 0.022(4) 0.033(4) 0.005(3) 0.004(2) -0.001(2) C17 0.017(2) 0.021(3) 0.022(3) -0.001(3) 0.001(2) -0.004(2) C18 0.031(3) 0.028(4) 0.025(4) -0.002(3) 0.010(2) 0.001(2) O18 0.059(3) 0.045(4) 0.045(3) -0.003(3) 0.011(2) 0.022(2) C19 0.035(3) 0.020(4) 0.042(4) 0.012(3) 0.010(3) 0.006(3) C20 0.028(3) 0.022(4) 0.033(4) 0.010(3) 0.004(2) -0.004(2) O20 0.047(3) 0.041(3) 0.031(3) 0.012(2) 0.000(2) 0.014(2) C21 0.024(3) 0.031(4) 0.020(3) -0.005(3) 0.001(2) 0.001(2) C22 0.019(3) 0.038(4) 0.018(3) -0.003(3) -0.002(2) 0.005(2) C23 0.024(3) 0.034(4) 0.015(3) -0.011(3) -0.002(2) 0.006(2) C24 0.023(3) 0.035(4) 0.016(3) -0.004(3) 0.000(2) 0.000(2) O25 0.061(3) 0.051(4) 0.043(3) -0.018(3) 0.036(2) -0.015(2) C25 0.033(3) 0.048(5) 0.014(3) -0.011(3) 0.004(2) -0.007(3) C26 0.031(3) 0.045(5) 0.025(4) -0.012(3) 0.011(2) -0.001(3) C27 0.021(3) 0.032(4) 0.028(4) -0.012(3) -0.003(2) 0.005(2) O27 0.036(2) 0.037(3) 0.037(3) -0.016(2) 0.0093(18) 0.001(2) C28 0.028(3) 0.033(4) 0.022(3) -0.004(3) 0.001(2) 0.002(3) C29 0.036(3) 0.017(4) 0.033(4) -0.006(3) 0.005(2) 0.002(2) C30 0.049(4) 0.056(6) 0.056(5) 0.002(4) -0.002(3) 0.000(3) C31 0.067(5) 0.040(6) 0.069(6) 0.000(5) -0.011(4) 0.002(4) C32 0.056(5) 0.084(7) 0.067(6) -0.010(5) 0.000(4) 0.018(4) C33 0.103(7) 0.086(9) 0.096(8) -0.031(7) -0.002(6) 0.041(6) C35 0.029(3) 0.045(5) 0.023(4) -0.008(3) 0.007(2) -0.003(3) C36 0.038(4) 0.065(6) 0.069(6) -0.010(5) 0.022(3) -0.013(4) C37 0.052(5) 0.086(8) 0.115(8) -0.017(6) 0.048(5) -0.018(5) C38 0.065(6) 0.103(9) 0.155(11) -0.033(8) 0.065(6) -0.041(6) C39 0.060(10) 0.125(18) 0.18(2) -0.028(14) 0.043(11) -0.023(10) C40 0.077(13) 0.112(18) 0.19(2) -0.008(15) 0.057(13) -0.040(12) C39B 0.023(13) 0.11(3) 0.09(2) -0.04(2) 0.027(13) -0.028(14) C40B 0.06(2) 0.13(4) 0.09(3) 0.02(3) -0.005(17) -0.01(2) C41 0.025(3) 0.046(5) 0.027(4) -0.001(3) 0.002(2) 0.004(3) C42 0.024(3) 0.047(5) 0.057(5) 0.008(4) 0.009(3) 0.004(3) C43 0.027(3) 0.064(6) 0.071(6) -0.006(5) 0.008(3) 0.002(3) C44 0.033(4) 0.074(7) 0.078(6) 0.014(5) 0.010(3) -0.003(4) C45 0.040(4) 0.090(8) 0.093(7) 0.005(6) 0.012(4) 0.008(4) C46 0.063(5) 0.083(8) 0.101(8) -0.012(6) 0.025(5) -0.011(5) C47 0.033(3) 0.036(4) 0.023(4) -0.002(3) 0.000(2) -0.004(3) C48 0.040(3) 0.041(5) 0.035(4) 0.002(3) 0.001(3) 0.004(3) C49 0.053(4) 0.042(5) 0.043(5) -0.003(4) 0.002(3) 0.016(3) C50 0.059(4) 0.069(6) 0.058(6) 0.005(5) 0.016(4) 0.023(4) C51 0.079(6) 0.065(7) 0.100(8) 0.001(6) 0.018(5) 0.036(5) C52 0.100(8) 0.140(12) 0.163(12) 0.019(10) 0.056(8) 0.061(8) C34 0.125(10) 0.182(16) 0.121(11) -0.018(11) 0.024(8) 0.060(10) Br1 0.0299(3) 0.0451(5) 0.0572(5) -0.0239(4) 0.0166(3) -0.0087(3) Br2 0.0401(4) 0.0479(5) 0.0713(6) -0.0147(4) 0.0211(3) -0.0060(3) Br3 0.0342(7) 0.0307(9) 0.0366(9) 0.0032(7) 0.0002(6) -0.0021(6) O1A 0.037(6) 0.048(8) 0.044(6) 0.007(5) 0.000(5) 0.005(5) Br4 0.0274(6) 0.0505(11) 0.0333(9) 0.0124(8) -0.0024(5) -0.0149(6) O2A 0.054(6) 0.052(8) 0.022(6) -0.009(5) 0.005(4) -0.014(5) N1 0.027(2) 0.028(3) 0.036(3) -0.006(3) 0.010(2) -0.007(2) N2 0.022(2) 0.029(3) 0.046(4) 0.003(3) 0.004(2) -0.001(2) C1C 0.044(4) 0.057(6) 0.040(5) 0.006(4) -0.009(3) 0.011(3) C2C 0.051(4) 0.057(6) 0.037(5) -0.005(4) 0.006(3) -0.014(3) C3C 0.028(3) 0.026(4) 0.052(5) -0.002(3) 0.013(3) -0.007(3) C4C 0.027(3) 0.033(4) 0.049(4) 0.011(3) 0.009(3) -0.011(3) C5C 0.029(3) 0.014(3) 0.048(4) -0.004(3) 0.011(3) -0.002(2) C6C 0.035(3) 0.016(4) 0.037(4) 0.000(3) 0.007(3) -0.003(2) C7C 0.028(3) 0.038(5) 0.066(5) -0.023(4) 0.021(3) -0.008(3) C8C 0.028(3) 0.024(4) 0.062(5) -0.002(4) 0.011(3) 0.005(3) N3 0.040(3) 0.058(5) 0.026(3) -0.015(3) 0.002(2) 0.017(3) C9C 0.038(4) 0.024(4) 0.131(9) -0.031(5) -0.016(4) 0.007(3) C10C 0.029(3) 0.033(4) 0.052(5) 0.005(4) 0.015(3) 0.006(3) C11C 0.106(8) 0.246(17) 0.033(6) -0.041(8) 0.005(5) 0.053(9) C12C 0.024(3) 0.028(4) 0.039(4) -0.002(3) 0.000(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.385(8) . ? C1 C6 1.423(7) . ? C1 C14 1.526(7) . ? C2 C3 1.407(8) . ? C2 H2 0.9500 . ? C3 C4 1.400(7) . ? C3 C7 1.499(8) . ? C4 O4 1.386(7) . ? C4 C5 1.390(8) . ? O4 H4 0.83(2) . ? C5 C6 1.380(8) . ? C5 H5 0.9500 . ? C6 O6 1.373(7) . ? O6 H6 0.84(2) . ? C7 C8 1.535(8) . ? C7 C29 1.544(7) . ? C7 H7 1.0000 . ? C8 C9 1.391(7) . ? C8 C13 1.409(7) . ? C9 C10 1.385(7) . ? C9 H9 0.9500 . ? C10 C11 1.395(7) . ? C10 C28 1.522(7) . ? C11 O11 1.376(7) . ? C11 C12 1.396(8) . ? O11 H11 0.84(2) . ? C12 C13 1.368(8) . ? C12 H12 0.9500 . ? C13 O13 1.379(7) . ? O13 H13 0.82(2) . ? C14 C15 1.519(8) . ? C14 C35 1.537(8) . ? C14 H14 1.0000 . ? C15 C16 1.394(8) . ? C15 C20 1.401(8) . ? C16 C17 1.385(8) . ? C16 H16 0.9500 . ? C17 C18 1.416(8) . ? C17 C21 1.520(7) . ? C18 O18 1.361(7) . ? C18 C19 1.373(8) . ? O18 H18 0.85(2) . ? C19 C20 1.380(8) . ? C19 H19 0.9500 . ? C20 O20 1.375(7) . ? O20 H20 0.85(2) . ? C21 C41 1.531(7) . ? C21 C22 1.537(8) . ? C21 H21 1.0000 . ? C22 C23 1.395(8) . ? C22 C27 1.404(8) . ? C23 C24 1.386(8) . ? C23 H23 0.9500 . ? C24 C25 1.400(8) . ? C24 C28 1.524(8) . ? O25 C25 1.392(7) . ? O25 H25 0.8400 . ? C25 C26 1.374(9) . ? C26 C27 1.385(8) . ? C26 H26 0.9500 . ? C27 O27 1.379(7) . ? O27 H27 0.84(2) . ? C28 C47 1.528(8) . ? C28 H28 1.0000 . ? C29 C30 1.484(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.557(10) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.489(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.537(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.532(13) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C35 C36 1.527(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.468(10) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.512(11) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39B 1.331(18) . ? C38 C39 1.403(14) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.525(16) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C39B C40B 1.53(2) . ? C39B H39C 0.9900 . ? C39B H39D 0.9900 . ? C40B H40D 0.9800 . ? C40B H40E 0.9800 . ? C40B H40F 0.9800 . ? C41 C42 1.512(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.515(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.509(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.536(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.446(11) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.523(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.540(8) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.472(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.538(10) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.494(12) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? N1 C2C 1.485(8) . ? N1 C6C 1.496(7) . ? N1 C3C 1.504(7) . ? N1 C7C 1.517(7) . ? N2 C5C 1.491(7) . ? N2 C8C 1.497(7) . ? N2 C1C 1.498(8) . ? N2 C4C 1.508(7) . ? C1C H1CA 0.9800 . ? C1C H1CB 0.9800 . ? C1C H1CC 0.9800 . ? C2C H2CA 0.9800 . ? C2C H2CB 0.9800 . ? C2C H2CC 0.9800 . ? C3C C4C 1.529(9) . ? C3C H3CA 0.9900 . ? C3C H3CB 0.9900 . ? C4C H4CA 0.9900 . ? C4C H4CB 0.9900 . ? C5C C6C 1.519(8) . ? C5C H5CA 0.9900 . ? C5C H5CB 0.9900 . ? C6C H6CA 0.9900 . ? C6C H6CB 0.9900 . ? C7C C8C 1.528(9) . ? C7C H7CA 0.9900 . ? C7C H7CB 0.9900 . ? C8C H8CA 0.9900 . ? C8C H8CB 0.9900 . ? N3 C9C 1.497(9) . ? N3 C10C 1.497(8) . ? N3 C11C 1.505(10) . ? N3 C12C 1.506(7) . ? C9C C9C 1.455(16) 2 ? C9C H9CA 0.9900 . ? C9C H9CB 0.9900 . ? C10C C12C 1.502(8) 2 ? C10C H10A 0.9900 . ? C10C H10B 0.9900 . ? C11C H11A 0.9800 . ? C11C H11B 0.9800 . ? C11C H11C 0.9800 . ? C12C C10C 1.502(8) 2 ? C12C H12A 0.9900 . ? C12C H12B 0.9900 . ? O1E C2E 1.450(9) . ? O1E H1E 0.8400 . ? C2E C3EB 1.351(17) . ? C2E C3E 1.451(12) . ? C2E H2EA 0.9900 . ? C2E H2EB 0.9900 . ? C2E H2ED 0.9900 . ? C2E H2EC 0.9900 . ? C3E H3EA 0.9800 . ? C3E H3EB 0.9800 . ? C3E H3EC 0.9800 . ? C3EB H3ED 0.9800 . ? C3EB H3EE 0.9800 . ? C3EB H3EF 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 C2 C1 C6 116.4(5) . . ? C2 C1 C14 121.8(5) . . ? C6 C1 C14 121.7(5) . . ? C1 C2 C3 125.3(5) . . ? C1 C2 H2 117.4 . . ? C3 C2 H2 117.4 . . ? C4 C3 C2 114.9(5) . . ? C4 C3 C7 123.4(5) . . ? C2 C3 C7 121.6(5) . . ? O4 C4 C5 119.9(5) . . ? O4 C4 C3 117.4(5) . . ? C5 C4 C3 122.6(5) . . ? C4 O4 H4 106(5) . . ? C6 C5 C4 119.9(5) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? O6 C6 C5 120.3(5) . . ? O6 C6 C1 118.9(5) . . ? C5 C6 C1 120.7(5) . . ? C6 O6 H6 114(5) . . ? C3 C7 C8 113.5(5) . . ? C3 C7 C29 109.9(4) . . ? C8 C7 C29 113.9(5) . . ? C3 C7 H7 106.3 . . ? C8 C7 H7 106.3 . . ? C29 C7 H7 106.3 . . ? C9 C8 C13 115.6(5) . . ? C9 C8 C7 124.4(4) . . ? C13 C8 C7 119.9(5) . . ? C10 C9 C8 125.0(5) . . ? C10 C9 H9 117.5 . . ? C8 C9 H9 117.5 . . ? C9 C10 C11 117.0(5) . . ? C9 C10 C28 122.4(4) . . ? C11 C10 C28 120.6(5) . . ? O11 C11 C10 124.5(5) . . ? O11 C11 C12 115.4(5) . . ? C10 C11 C12 120.1(5) . . ? C11 O11 H11 110(5) . . ? C13 C12 C11 120.9(5) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 O13 117.8(5) . . ? C12 C13 C8 121.3(5) . . ? O13 C13 C8 120.9(5) . . ? C13 O13 H13 112(5) . . ? C15 C14 C1 111.6(4) . . ? C15 C14 C35 114.4(5) . . ? C1 C14 C35 111.0(5) . . ? C15 C14 H14 106.4 . . ? C1 C14 H14 106.4 . . ? C35 C14 H14 106.4 . . ? C16 C15 C20 115.6(5) . . ? C16 C15 C14 125.0(5) . . ? C20 C15 C14 119.4(5) . . ? C17 C16 C15 124.8(5) . . ? C17 C16 H16 117.6 . . ? C15 C16 H16 117.6 . . ? C16 C17 C18 116.7(5) . . ? C16 C17 C21 122.9(5) . . ? C18 C17 C21 120.4(5) . . ? O18 C18 C19 116.4(5) . . ? O18 C18 C17 123.3(5) . . ? C19 C18 C17 120.3(6) . . ? C18 O18 H18 114(6) . . ? C18 C19 C20 120.6(6) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? O20 C20 C19 121.9(5) . . ? O20 C20 C15 116.1(6) . . ? C19 C20 C15 121.9(6) . . ? C20 O20 H20 104(5) . . ? C17 C21 C41 114.6(5) . . ? C17 C21 C22 111.4(4) . . ? C41 C21 C22 112.3(5) . . ? C17 C21 H21 105.9 . . ? C41 C21 H21 105.9 . . ? C22 C21 H21 105.9 . . ? C23 C22 C27 116.5(5) . . ? C23 C22 C21 123.0(5) . . ? C27 C22 C21 120.5(6) . . ? C24 C23 C22 124.7(5) . . ? C24 C23 H23 117.7 . . ? C22 C23 H23 117.7 . . ? C23 C24 C25 115.9(6) . . ? C23 C24 C28 122.8(5) . . ? C25 C24 C28 121.2(5) . . ? C25 O25 H25 109.5 . . ? C26 C25 O25 121.9(5) . . ? C26 C25 C24 121.9(6) . . ? O25 C25 C24 116.1(6) . . ? C25 C26 C27 120.3(6) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? O27 C27 C26 121.7(5) . . ? O27 C27 C22 117.6(5) . . ? C26 C27 C22 120.7(6) . . ? C27 O27 H27 112(5) . . ? C10 C28 C24 109.8(5) . . ? C10 C28 C47 115.1(5) . . ? C24 C28 C47 113.0(5) . . ? C10 C28 H28 106.1 . . ? C24 C28 H28 106.1 . . ? C47 C28 H28 106.1 . . ? C30 C29 C7 115.5(5) . . ? C30 C29 H29A 108.4 . . ? C7 C29 H29A 108.4 . . ? C30 C29 H29B 108.4 . . ? C7 C29 H29B 108.4 . . ? H29A C29 H29B 107.5 . . ? C29 C30 C31 113.6(6) . . ? C29 C30 H30A 108.8 . . ? C31 C30 H30A 108.8 . . ? C29 C30 H30B 108.8 . . ? C31 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C30 114.6(6) . . ? C32 C31 H31A 108.6 . . ? C30 C31 H31A 108.6 . . ? C32 C31 H31B 108.6 . . ? C30 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? C31 C32 C33 113.5(7) . . ? C31 C32 H32A 108.9 . . ? C33 C32 H32A 108.9 . . ? C31 C32 H32B 108.9 . . ? C33 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C34 C33 C32 112.2(8) . . ? C34 C33 H33A 109.2 . . ? C32 C33 H33A 109.2 . . ? C34 C33 H33B 109.2 . . ? C32 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C36 C35 C14 111.7(6) . . ? C36 C35 H35A 109.3 . . ? C14 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? C14 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? C37 C36 C35 115.4(7) . . ? C37 C36 H36A 108.4 . . ? C35 C36 H36A 108.4 . . ? C37 C36 H36B 108.4 . . ? C35 C36 H36B 108.4 . . ? H36A C36 H36B 107.5 . . ? C36 C37 C38 115.4(8) . . ? C36 C37 H37A 108.4 . . ? C38 C37 H37A 108.4 . . ? C36 C37 H37B 108.4 . . ? C38 C37 H37B 108.4 . . ? H37A C37 H37B 107.5 . . ? C39B C38 C39 62.6(13) . . ? C39B C38 C37 126.6(13) . . ? C39 C38 C37 118.7(11) . . ? C39B C38 H38A 45.2 . . ? C39 C38 H38A 107.6 . . ? C37 C38 H38A 107.6 . . ? C39B C38 H38B 123.1 . . ? C39 C38 H38B 107.6 . . ? C37 C38 H38B 107.6 . . ? H38A C38 H38B 107.1 . . ? C38 C39 C40 118.5(14) . . ? C38 C39 H39A 107.7 . . ? C40 C39 H39A 107.7 . . ? C38 C39 H39B 107.7 . . ? C40 C39 H39B 107.7 . . ? H39A C39 H39B 107.1 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C39B C40B 115.4(16) . . ? C38 C39B H39C 108.4 . . ? C40B C39B H39C 108.4 . . ? C38 C39B H39D 108.4 . . ? C40B C39B H39D 108.4 . . ? H39C C39B H39D 107.5 . . ? C39B C40B H40D 109.5 . . ? C39B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C39B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C42 C41 C21 114.0(5) . . ? C42 C41 H41A 108.8 . . ? C21 C41 H41A 108.8 . . ? C42 C41 H41B 108.8 . . ? C21 C41 H41B 108.8 . . ? H41A C41 H41B 107.6 . . ? C41 C42 C43 113.1(6) . . ? C41 C42 H42A 109.0 . . ? C43 C42 H42A 109.0 . . ? C41 C42 H42B 109.0 . . ? C43 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? C44 C43 C42 115.0(7) . . ? C44 C43 H43A 108.5 . . ? C42 C43 H43A 108.5 . . ? C44 C43 H43B 108.5 . . ? C42 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? C43 C44 C45 113.4(7) . . ? C43 C44 H44A 108.9 . . ? C45 C44 H44A 108.9 . . ? C43 C44 H44B 108.9 . . ? C45 C44 H44B 108.9 . . ? H44A C44 H44B 107.7 . . ? C46 C45 C44 114.4(8) . . ? C46 C45 H45A 108.7 . . ? C44 C45 H45A 108.7 . . ? C46 C45 H45B 108.7 . . ? C44 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? 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 . . ? C48 C47 C28 112.4(5) . . ? C48 C47 H47A 109.1 . . ? C28 C47 H47A 109.1 . . ? C48 C47 H47B 109.1 . . ? C28 C47 H47B 109.1 . . ? H47A C47 H47B 107.9 . . ? C47 C48 C49 114.4(6) . . ? C47 C48 H48A 108.7 . . ? C49 C48 H48A 108.7 . . ? C47 C48 H48B 108.7 . . ? C49 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? C50 C49 C48 114.0(6) . . ? C50 C49 H49A 108.7 . . ? C48 C49 H49A 108.7 . . ? C50 C49 H49B 108.7 . . ? C48 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? C49 C50 C51 113.4(7) . . ? C49 C50 H50A 108.9 . . ? C51 C50 H50A 108.9 . . ? C49 C50 H50B 108.9 . . ? C51 C50 H50B 108.9 . . ? H50A C50 H50B 107.7 . . ? C52 C51 C50 114.3(8) . . ? C52 C51 H51A 108.7 . . ? C50 C51 H51A 108.7 . . ? C52 C51 H51B 108.7 . . ? C50 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? 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 . . ? C2C N1 C6C 110.2(5) . . ? C2C N1 C3C 110.8(5) . . ? C6C N1 C3C 108.2(4) . . ? C2C N1 C7C 110.9(5) . . ? C6C N1 C7C 109.2(4) . . ? C3C N1 C7C 107.4(5) . . ? C5C N2 C8C 109.3(5) . . ? C5C N2 C1C 110.2(5) . . ? C8C N2 C1C 109.2(5) . . ? C5C N2 C4C 108.0(4) . . ? C8C N2 C4C 109.1(5) . . ? C1C N2 C4C 111.1(5) . . ? N2 C1C H1CA 109.5 . . ? N2 C1C H1CB 109.5 . . ? H1CA C1C H1CB 109.5 . . ? N2 C1C H1CC 109.5 . . ? H1CA C1C H1CC 109.5 . . ? H1CB C1C H1CC 109.5 . . ? N1 C2C H2CA 109.5 . . ? N1 C2C H2CB 109.5 . . ? H2CA C2C H2CB 109.5 . . ? N1 C2C H2CC 109.5 . . ? H2CA C2C H2CC 109.5 . . ? H2CB C2C H2CC 109.5 . . ? N1 C3C C4C 108.4(5) . . ? N1 C3C H3CA 110.0 . . ? C4C C3C H3CA 110.0 . . ? N1 C3C H3CB 110.0 . . ? C4C C3C H3CB 110.0 . . ? H3CA C3C H3CB 108.4 . . ? N2 C4C C3C 109.5(5) . . ? N2 C4C H4CA 109.8 . . ? C3C C4C H4CA 109.8 . . ? N2 C4C H4CB 109.8 . . ? C3C C4C H4CB 109.8 . . ? H4CA C4C H4CB 108.2 . . ? N2 C5C C6C 109.3(5) . . ? N2 C5C H5CA 109.8 . . ? C6C C5C H5CA 109.8 . . ? N2 C5C H5CB 109.8 . . ? C6C C5C H5CB 109.8 . . ? H5CA C5C H5CB 108.3 . . ? N1 C6C C5C 109.4(5) . . ? N1 C6C H6CA 109.8 . . ? C5C C6C H6CA 109.8 . . ? N1 C6C H6CB 109.8 . . ? C5C C6C H6CB 109.8 . . ? H6CA C6C H6CB 108.2 . . ? N1 C7C C8C 110.2(5) . . ? N1 C7C H7CA 109.6 . . ? C8C C7C H7CA 109.6 . . ? N1 C7C H7CB 109.6 . . ? C8C C7C H7CB 109.6 . . ? H7CA C7C H7CB 108.1 . . ? N2 C8C C7C 108.2(5) . . ? N2 C8C H8CA 110.1 . . ? C7C C8C H8CA 110.1 . . ? N2 C8C H8CB 110.1 . . ? C7C C8C H8CB 110.1 . . ? H8CA C8C H8CB 108.4 . . ? C9C N3 C10C 108.0(5) . . ? C9C N3 C11C 113.4(7) . . ? C10C N3 C11C 109.8(6) . . ? C9C N3 C12C 108.9(5) . . ? C10C N3 C12C 108.3(5) . . ? C11C N3 C12C 108.4(6) . . ? C9C C9C N3 109.5(4) 2 . ? C9C C9C H9CA 109.8 2 . ? N3 C9C H9CA 109.8 . . ? C9C C9C H9CB 109.8 2 . ? N3 C9C H9CB 109.8 . . ? H9CA C9C H9CB 108.2 . . ? N3 C10C C12C 108.7(4) . 2 ? N3 C10C H10A 109.9 . . ? C12C C10C H10A 109.9 2 . ? N3 C10C H10B 109.9 . . ? C12C C10C H10B 109.9 2 . ? H10A C10C H10B 108.3 . . ? N3 C11C H11A 109.5 . . ? N3 C11C H11B 109.5 . . ? H11A C11C H11B 109.5 . . ? N3 C11C H11C 109.5 . . ? H11A C11C H11C 109.5 . . ? H11B C11C H11C 109.5 . . ? C10C C12C N3 108.0(5) 2 . ? C10C C12C H12A 110.1 2 . ? N3 C12C H12A 110.1 . . ? C10C C12C H12B 110.1 2 . ? N3 C12C H12B 110.1 . . ? H12A C12C H12B 108.4 . . ? C2E O1E H1E 109.5 . . ? C3EB C2E O1E 112.6(14) . . ? C3EB C2E C3E 44.8(12) . . ? O1E C2E C3E 115.6(8) . . ? C3EB C2E H2EA 138.1 . . ? O1E C2E H2EA 108.4 . . ? C3E C2E H2EA 108.4 . . ? C3EB C2E H2EB 67.5 . . ? O1E C2E H2EB 108.4 . . ? C3E C2E H2EB 108.4 . . ? H2EA C2E H2EB 107.4 . . ? C3EB C2E H2ED 109.1 . . ? O1E C2E H2ED 109.1 . . ? C3E C2E H2ED 134.4 . . ? H2EA C2E H2ED 63.6 . . ? H2EB C2E H2ED 45.9 . . ? C3EB C2E H2EC 109.1 . . ? O1E C2E H2EC 109.1 . . ? C3E C2E H2EC 66.1 . . ? H2EA C2E H2EC 47.1 . . ? H2EB C2E H2EC 140.2 . . ? H2ED C2E H2EC 107.8 . . ? C2E C3E H3EA 109.5 . . ? C2E C3E H3EB 109.5 . . ? H3EA C3E H3EB 109.5 . . ? C2E C3E H3EC 109.5 . . ? H3EA C3E H3EC 109.5 . . ? H3EB C3E H3EC 109.5 . . ? C2E C3EB H3ED 109.5 . . ? C2E C3EB H3EE 109.5 . . ? H3ED C3EB H3EE 109.5 . . ? C2E C3EB H3EF 109.5 . . ? H3ED C3EB H3EF 109.5 . . ? H3EE C3EB H3EF 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 C6 C1 C2 C3 1.1(8) . . . . ? C14 C1 C2 C3 -177.0(5) . . . . ? C1 C2 C3 C4 -3.4(8) . . . . ? C1 C2 C3 C7 173.1(5) . . . . ? C2 C3 C4 O4 -177.4(5) . . . . ? C7 C3 C4 O4 6.2(8) . . . . ? C2 C3 C4 C5 2.6(8) . . . . ? C7 C3 C4 C5 -173.8(5) . . . . ? O4 C4 C5 C6 -179.5(5) . . . . ? C3 C4 C5 C6 0.4(9) . . . . ? C4 C5 C6 O6 177.9(5) . . . . ? C4 C5 C6 C1 -3.0(9) . . . . ? C2 C1 C6 O6 -178.6(5) . . . . ? C14 C1 C6 O6 -0.5(8) . . . . ? C2 C1 C6 C5 2.2(8) . . . . ? C14 C1 C6 C5 -179.7(5) . . . . ? C4 C3 C7 C8 -109.3(6) . . . . ? C2 C3 C7 C8 74.5(6) . . . . ? C4 C3 C7 C29 121.8(6) . . . . ? C2 C3 C7 C29 -54.3(7) . . . . ? C3 C7 C8 C9 -100.2(6) . . . . ? C29 C7 C8 C9 26.5(8) . . . . ? C3 C7 C8 C13 78.4(6) . . . . ? C29 C7 C8 C13 -154.9(5) . . . . ? C13 C8 C9 C10 1.8(9) . . . . ? C7 C8 C9 C10 -179.6(6) . . . . ? C8 C9 C10 C11 -0.5(9) . . . . ? C8 C9 C10 C28 -179.4(6) . . . . ? C9 C10 C11 O11 179.6(6) . . . . ? C28 C10 C11 O11 -1.5(9) . . . . ? C9 C10 C11 C12 0.3(9) . . . . ? C28 C10 C11 C12 179.2(6) . . . . ? O11 C11 C12 C13 179.1(6) . . . . ? C10 C11 C12 C13 -1.6(9) . . . . ? C11 C12 C13 O13 -178.3(5) . . . . ? C11 C12 C13 C8 3.0(9) . . . . ? C9 C8 C13 C12 -3.0(9) . . . . ? C7 C8 C13 C12 178.3(6) . . . . ? C9 C8 C13 O13 178.4(5) . . . . ? C7 C8 C13 O13 -0.3(8) . . . . ? C2 C1 C14 C15 -67.0(7) . . . . ? C6 C1 C14 C15 115.0(6) . . . . ? C2 C1 C14 C35 62.0(7) . . . . ? C6 C1 C14 C35 -116.0(6) . . . . ? C1 C14 C15 C16 95.4(6) . . . . ? C35 C14 C15 C16 -31.8(8) . . . . ? C1 C14 C15 C20 -86.1(6) . . . . ? C35 C14 C15 C20 146.8(5) . . . . ? C20 C15 C16 C17 -0.2(8) . . . . ? C14 C15 C16 C17 178.4(5) . . . . ? C15 C16 C17 C18 -0.3(8) . . . . ? C15 C16 C17 C21 -179.2(5) . . . . ? C16 C17 C18 O18 -178.8(5) . . . . ? C21 C17 C18 O18 0.2(8) . . . . ? C16 C17 C18 C19 1.3(8) . . . . ? C21 C17 C18 C19 -179.8(5) . . . . ? O18 C18 C19 C20 178.2(5) . . . . ? C17 C18 C19 C20 -1.8(9) . . . . ? C18 C19 C20 O20 178.3(5) . . . . ? C18 C19 C20 C15 1.4(9) . . . . ? C16 C15 C20 O20 -177.5(5) . . . . ? C14 C15 C20 O20 3.8(7) . . . . ? C16 C15 C20 C19 -0.4(8) . . . . ? C14 C15 C20 C19 -179.1(5) . . . . ? C16 C17 C21 C41 31.4(8) . . . . ? C18 C17 C21 C41 -147.5(5) . . . . ? C16 C17 C21 C22 -97.5(6) . . . . ? C18 C17 C21 C22 83.6(6) . . . . ? C17 C21 C22 C23 79.8(7) . . . . ? C41 C21 C22 C23 -50.3(7) . . . . ? C17 C21 C22 C27 -97.9(6) . . . . ? C41 C21 C22 C27 132.0(6) . . . . ? C27 C22 C23 C24 -1.1(8) . . . . ? C21 C22 C23 C24 -178.8(5) . . . . ? C22 C23 C24 C25 1.6(8) . . . . ? C22 C23 C24 C28 179.0(5) . . . . ? C23 C24 C25 C26 -0.7(8) . . . . ? C28 C24 C25 C26 -178.1(5) . . . . ? C23 C24 C25 O25 179.2(5) . . . . ? C28 C24 C25 O25 1.7(8) . . . . ? O25 C25 C26 C27 179.5(5) . . . . ? C24 C25 C26 C27 -0.6(9) . . . . ? C25 C26 C27 O27 -178.8(5) . . . . ? C25 C26 C27 C22 1.2(9) . . . . ? C23 C22 C27 O27 179.6(5) . . . . ? C21 C22 C27 O27 -2.6(7) . . . . ? C23 C22 C27 C26 -0.4(8) . . . . ? C21 C22 C27 C26 177.5(5) . . . . ? C9 C10 C28 C24 93.9(6) . . . . ? C11 C10 C28 C24 -84.9(6) . . . . ? C9 C10 C28 C47 -34.9(8) . . . . ? C11 C10 C28 C47 146.2(6) . . . . ? C23 C24 C28 C10 -77.8(6) . . . . ? C25 C24 C28 C10 99.5(6) . . . . ? C23 C24 C28 C47 52.2(7) . . . . ? C25 C24 C28 C47 -130.5(6) . . . . ? C3 C7 C29 C30 -168.5(5) . . . . ? C8 C7 C29 C30 62.9(7) . . . . ? C7 C29 C30 C31 175.5(6) . . . . ? C29 C30 C31 C32 -67.8(9) . . . . ? C30 C31 C32 C33 176.3(8) . . . . ? C31 C32 C33 C34 180.0(10) . . . . ? C15 C14 C35 C36 -70.6(7) . . . . ? C1 C14 C35 C36 161.9(5) . . . . ? C14 C35 C36 C37 -173.9(7) . . . . ? C35 C36 C37 C38 172.2(8) . . . . ? C36 C37 C38 C39B -92.7(19) . . . . ? C36 C37 C38 C39 -168.4(13) . . . . ? C39B C38 C39 C40 50(2) . . . . ? C37 C38 C39 C40 168.6(14) . . . . ? C39 C38 C39B C40B -64(2) . . . . ? C37 C38 C39B C40B -170(2) . . . . ? C17 C21 C41 C42 60.1(7) . . . . ? C22 C21 C41 C42 -171.5(5) . . . . ? C21 C41 C42 C43 170.5(6) . . . . ? C41 C42 C43 C44 172.2(7) . . . . ? C42 C43 C44 C45 177.0(7) . . . . ? C43 C44 C45 C46 173.0(8) . . . . ? C10 C28 C47 C48 -65.0(7) . . . . ? C24 C28 C47 C48 167.7(5) . . . . ? C28 C47 C48 C49 -170.6(5) . . . . ? C47 C48 C49 C50 -67.7(9) . . . . ? C48 C49 C50 C51 -179.4(7) . . . . ? C49 C50 C51 C52 -177.6(9) . . . . ? C2C N1 C3C C4C -169.0(5) . . . . ? C6C N1 C3C C4C -48.0(6) . . . . ? C7C N1 C3C C4C 69.8(6) . . . . ? C5C N2 C4C C3C 69.8(6) . . . . ? C8C N2 C4C C3C -48.8(7) . . . . ? C1C N2 C4C C3C -169.2(5) . . . . ? N1 C3C C4C N2 -18.6(7) . . . . ? C8C N2 C5C C6C 70.8(5) . . . . ? C1C N2 C5C C6C -169.2(5) . . . . ? C4C N2 C5C C6C -47.7(6) . . . . ? C2C N1 C6C C5C -168.2(5) . . . . ? C3C N1 C6C C5C 70.4(6) . . . . ? C7C N1 C6C C5C -46.2(6) . . . . ? N2 C5C C6C N1 -18.8(6) . . . . ? C2C N1 C7C C8C -171.2(5) . . . . ? C6C N1 C7C C8C 67.2(6) . . . . ? C3C N1 C7C C8C -49.9(7) . . . . ? C5C N2 C8C C7C -49.3(6) . . . . ? C1C N2 C8C C7C -169.9(5) . . . . ? C4C N2 C8C C7C 68.5(6) . . . . ? N1 C7C C8C N2 -16.5(7) . . . . ? C10C N3 C9C C9C 46.8(9) . . . 2 ? C11C N3 C9C C9C 168.7(7) . . . 2 ? C12C N3 C9C C9C -70.5(8) . . . 2 ? C9C N3 C10C C12C -71.3(7) . . . 2 ? C11C N3 C10C C12C 164.6(7) . . . 2 ? C12C N3 C10C C12C 46.5(6) . . . 2 ? C9C N3 C12C C10C 45.1(6) . . . 2 ? C10C N3 C12C C10C -72.1(6) . . . 2 ? C11C N3 C12C C10C 168.9(7) . . . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O1A 0.83(2) 1.82(3) 2.641(11) 167(6) . O4 H4 Br3 0.83(2) 2.60(3) 3.402(4) 162(6) . O6 H6 O1E 0.84(2) 1.83(2) 2.666(6) 176(7) . O11 H11 O25 0.84(2) 1.97(3) 2.784(6) 165(8) . O13 H13 O4 0.82(2) 2.10(3) 2.897(6) 164(7) . O18 H18 O27 0.85(2) 1.89(2) 2.736(7) 177(8) . O20 H20 Br1 0.85(2) 2.40(3) 3.201(4) 158(7) 6_575 O25 H25 Br1 0.84 2.37 3.192(4) 167.3 . O27 H27 O6 0.84(2) 1.98(4) 2.738(6) 150(7) 6_576 O20 H20 Br1 0.85(2) 2.40(3) 3.201(4) 158(7) 6_575 O1E H1E Br2 0.84 2.58 3.306(4) 145.4 . _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.843 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.086 #==END data_Complex6 _database_code_depnum_ccdc_archive 'CCDC 254963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 2C40H48O8*1.5C20H26N3Br*0.5H20*7CH4O _chemical_formula_sum 'C117 H164 Br3 N3 O23.50' _chemical_formula_weight 2228.24 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 15.8558(3) _cell_length_b 17.8230(4) _cell_length_c 20.2560(4) _cell_angle_alpha 85.6930(10) _cell_angle_beta 88.5400(10) _cell_angle_gamma 86.6320(10) _cell_volume 5697.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description colorless _exptl_crystal_colour block _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3026 _exptl_absorpt_correction_T_max 0.3145 _exptl_absorpt_process_details ' R. H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38.' _exptl_special_details ; dx = 35, 15 sec./deg., 1 deg., mos.=0.396+/-0.001 ; _diffrn_ambient_temperature 173(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 'rotation in phi and omega, 1 deg.' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 32249 _diffrn_reflns_av_R_equivalents 0.0936 _diffrn_reflns_av_sigmaI/netI 0.2046 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.08 _reflns_number_total 17331 _reflns_number_gt 8271 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELX97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17331 _refine_ls_number_parameters 1343 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1874 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1388 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 C1 C 0.5855(4) 0.5659(3) -0.2184(3) 0.0158(15) Uani 1 1 d . . . C2 C 0.5005(3) 0.5736(3) -0.2316(3) 0.0172(15) Uani 1 1 d . . . H2 H 0.4847 0.5920 -0.2750 0.021 Uiso 1 1 calc R . . C3 C 0.4355(3) 0.5563(3) -0.1859(3) 0.0167(16) Uani 1 1 d . . . C4 C 0.4602(4) 0.5295(3) -0.1230(3) 0.0173(16) Uani 1 1 d . . . O4 O 0.4043(2) 0.5133(3) -0.07086(19) 0.0264(12) Uani 1 1 d . . . H4 H 0.3545 0.5196 -0.0843 0.040 Uiso 1 1 calc R . . C5 C 0.5450(4) 0.5179(3) -0.1076(3) 0.0192(16) Uani 1 1 d . . . H5 H 0.5606 0.4965 -0.0650 0.023 Uiso 1 1 calc R . . C6 C 0.6072(4) 0.5374(3) -0.1543(3) 0.0194(16) Uani 1 1 d . . . O6 O 0.6887(3) 0.5304(3) -0.1315(2) 0.0259(13) Uani 1 1 d . . . H6 H 0.720(4) 0.535(4) -0.157(3) 0.039 Uiso 1 1 d . . . C7 C 0.3424(4) 0.5687(3) -0.2035(3) 0.0188(16) Uani 1 1 d . . . H7 H 0.3126 0.5270 -0.1789 0.023 Uiso 1 1 calc R . . C8 C 0.3047(3) 0.6416(4) -0.1776(3) 0.0183(16) Uani 1 1 d . . . C9 C 0.3247(3) 0.7113(4) -0.2076(3) 0.0180(16) Uani 1 1 d . . . H9A H 0.3868 0.7133 -0.2050 0.022 Uiso 1 1 calc R . . H9B H 0.3121 0.7101 -0.2551 0.022 Uiso 1 1 calc R . . C10 C 0.2907(3) 0.7792(4) -0.1885(3) 0.0145(15) Uani 1 1 d . . . C11 C 0.2357(4) 0.7780(4) -0.1335(3) 0.0208(16) Uani 1 1 d . . . O11 O 0.1975(3) 0.8410(2) -0.1090(2) 0.0299(12) Uani 1 1 d . . . H11 H 0.2343 0.8712 -0.1016 0.045 Uiso 1 1 calc R . . C12 C 0.2151(4) 0.7103(4) -0.1017(3) 0.0235(17) Uani 1 1 d . . . H12A H 0.1530 0.7080 -0.1038 0.028 Uiso 1 1 calc R . . H12B H 0.2287 0.7121 -0.0545 0.028 Uiso 1 1 calc R . . C13 C 0.2509(4) 0.6425(4) -0.1223(3) 0.0183(16) Uani 1 1 d . . . O13 O 0.2344(3) 0.5738(3) -0.0893(2) 0.0276(12) Uani 1 1 d . . . H13 H 0.207(4) 0.584(4) -0.054(3) 0.041 Uiso 1 1 d . . . C14 C 0.3113(4) 0.8541(4) -0.2280(3) 0.0217(17) Uani 1 1 d . . . C15 C 0.4001(4) 0.8773(3) -0.2115(3) 0.0198(16) Uani 1 1 d . . . C16 C 0.4734(3) 0.8643(3) -0.2510(3) 0.0185(16) Uani 1 1 d . . . H16 H 0.4678 0.8395 -0.2904 0.022 Uiso 1 1 calc R . . C17 C 0.5520(4) 0.8852(3) -0.2361(3) 0.0187(16) Uani 1 1 d . . . C18 C 0.5592(4) 0.9207(4) -0.1781(3) 0.0226(17) Uani 1 1 d . . . O18 O 0.6384(3) 0.9411(3) -0.1620(2) 0.0270(13) Uani 1 1 d . . . H18 H 0.640(5) 0.964(4) -0.134(3) 0.041 Uiso 1 1 d . . . C19 C 0.4887(4) 0.9358(4) -0.1366(3) 0.0236(17) Uani 1 1 d . . . H19 H 0.4942 0.9606 -0.0972 0.028 Uiso 1 1 calc R . . C20 C 0.4117(4) 0.9135(4) -0.1549(3) 0.0219(17) Uani 1 1 d . . . O20 O 0.3402(3) 0.9272(3) -0.1154(2) 0.0308(13) Uani 1 1 d . . . H20 H 0.346(4) 0.956(4) -0.084(3) 0.046 Uiso 1 1 d . . . C21 C 0.6316(3) 0.8717(3) -0.2799(3) 0.0158(15) Uani 1 1 d . . . H21 H 0.6687 0.9141 -0.2742 0.019 Uiso 1 1 calc R . . C22 C 0.6819(4) 0.7992(4) -0.2570(3) 0.0171(16) Uani 1 1 d . . . C23 C 0.6490(4) 0.7290(4) -0.2653(3) 0.0151(15) Uani 1 1 d . . . H23 H 0.5928 0.7291 -0.2804 0.018 Uiso 1 1 calc R . . C24 C 0.6917(4) 0.6605(4) -0.2533(3) 0.0158(15) Uani 1 1 d . . . C25 C 0.7737(3) 0.6612(4) -0.2283(3) 0.0173(16) Uani 1 1 d . . . O25 O 0.8150(3) 0.5928(3) -0.2138(2) 0.0253(12) Uani 1 1 d . . . H25 H 0.862(4) 0.599(4) -0.193(3) 0.038 Uiso 1 1 d . . . C26 C 0.8081(4) 0.7289(4) -0.2171(3) 0.0196(16) Uani 1 1 d . . . H26 H 0.8628 0.7287 -0.1989 0.023 Uiso 1 1 calc R . . C27 C 0.7631(4) 0.7967(4) -0.2324(3) 0.0171(16) Uani 1 1 d . . . O27 O 0.8000(3) 0.8632(3) -0.2227(2) 0.0267(13) Uani 1 1 d . . . H27 H 0.833(4) 0.859(5) -0.202(4) 0.040 Uiso 1 1 d . . . C28 C 0.6545(4) 0.5881(4) -0.2689(3) 0.0187(16) Uani 1 1 d . . . H28 H 0.7010 0.5478 -0.2640 0.022 Uiso 1 1 calc R . . C29 C 0.3257(4) 0.5630(4) -0.2765(3) 0.0239(17) Uani 1 1 d . . . H29A H 0.3556 0.5167 -0.2912 0.029 Uiso 1 1 calc R . . H29B H 0.3492 0.6066 -0.3023 0.029 Uiso 1 1 calc R . . C30 C 0.2310(4) 0.5612(4) -0.2913(3) 0.0292(18) Uani 1 1 d . . . H30A H 0.2083 0.5159 -0.2676 0.035 Uiso 1 1 calc R . . H30B H 0.2006 0.6060 -0.2740 0.035 Uiso 1 1 calc R . . C31 C 0.2140(4) 0.5602(5) -0.3644(3) 0.046(2) Uani 1 1 d . . . H31A H 0.2309 0.6075 -0.3876 0.070 Uiso 1 1 calc R . . H31B H 0.1536 0.5549 -0.3705 0.070 Uiso 1 1 calc R . . H31C H 0.2466 0.5177 -0.3824 0.070 Uiso 1 1 calc R . . C32 C 0.2992(4) 0.8495(4) -0.3023(3) 0.0259(18) Uani 1 1 d . . . H32A H 0.3150 0.8973 -0.3262 0.031 Uiso 1 1 calc R . . H32B H 0.3374 0.8084 -0.3182 0.031 Uiso 1 1 calc R . . C33 C 0.2091(4) 0.8351(5) -0.3181(3) 0.044(2) Uani 1 1 d . . . H33A H 0.1713 0.8774 -0.3039 0.053 Uiso 1 1 calc R . . H33B H 0.1925 0.7886 -0.2925 0.053 Uiso 1 1 calc R . . C34 C 0.1968(5) 0.8267(6) -0.3927(4) 0.083(4) Uani 1 1 d . . . H34A H 0.1375 0.8178 -0.4002 0.125 Uiso 1 1 calc R . . H34B H 0.2329 0.7841 -0.4067 0.125 Uiso 1 1 calc R . . H34C H 0.2122 0.8730 -0.4182 0.125 Uiso 1 1 calc R . . C35 C 0.6120(4) 0.8743(4) -0.3537(3) 0.0209(16) Uani 1 1 d . . . H35A H 0.5780 0.8311 -0.3616 0.025 Uiso 1 1 calc R . . H35B H 0.5774 0.9211 -0.3659 0.025 Uiso 1 1 calc R . . C36 C 0.6912(4) 0.8717(4) -0.3982(3) 0.0334(19) Uani 1 1 d . . . H36A H 0.7249 0.9152 -0.3906 0.040 Uiso 1 1 calc R . . H36B H 0.7260 0.8251 -0.3857 0.040 Uiso 1 1 calc R . . C37 C 0.6713(4) 0.8737(5) -0.4710(3) 0.045(2) Uani 1 1 d . . . H37A H 0.7242 0.8720 -0.4972 0.067 Uiso 1 1 calc R . . H37B H 0.6378 0.9202 -0.4839 0.067 Uiso 1 1 calc R . . H37C H 0.6392 0.8301 -0.4791 0.067 Uiso 1 1 calc R . . C38 C 0.6261(4) 0.5907(4) -0.3411(3) 0.0218(17) Uani 1 1 d . . . H38A H 0.5988 0.5435 -0.3484 0.026 Uiso 1 1 calc R . . H38B H 0.5837 0.6332 -0.3493 0.026 Uiso 1 1 calc R . . C39 C 0.7000(4) 0.6001(4) -0.3901(3) 0.0295(18) Uani 1 1 d . . . H39A H 0.7404 0.5558 -0.3837 0.035 Uiso 1 1 calc R . . H39B H 0.7296 0.6453 -0.3805 0.035 Uiso 1 1 calc R . . C40 C 0.6730(4) 0.6082(5) -0.4623(3) 0.045(2) Uani 1 1 d . . . H40A H 0.6379 0.5667 -0.4708 0.067 Uiso 1 1 calc R . . H40B H 0.7233 0.6068 -0.4914 0.067 Uiso 1 1 calc R . . H40C H 0.6406 0.6563 -0.4709 0.067 Uiso 1 1 calc R . . C1B C -0.0683(4) 0.6929(4) 0.4144(3) 0.0187(16) Uani 1 1 d . . . C2B C -0.0335(4) 0.7602(4) 0.4276(3) 0.0197(16) Uani 1 1 d . . . H2B H 0.0208 0.7577 0.4466 0.024 Uiso 1 1 calc R . . C3B C -0.0748(3) 0.8311(4) 0.4142(3) 0.0157(15) Uani 1 1 d . . . C4B C -0.1522(4) 0.8339(4) 0.3827(3) 0.0208(17) Uani 1 1 d . . . O4B O -0.1914(3) 0.9034(3) 0.3681(2) 0.0251(12) Uani 1 1 d . . . H4B H -0.238(4) 0.903(4) 0.349(3) 0.038 Uiso 1 1 d . . . C5B C -0.1883(4) 0.7679(4) 0.3659(3) 0.0221(16) Uani 1 1 d . . . H5B H -0.2401 0.7708 0.3431 0.027 Uiso 1 1 calc R . . C6B C -0.1465(4) 0.6974(4) 0.3834(3) 0.0205(16) Uani 1 1 d . . . O6B O -0.1795(3) 0.6322(3) 0.3680(2) 0.0268(12) Uani 1 1 d . . . H6B H -0.223(4) 0.643(4) 0.349(3) 0.040 Uiso 1 1 d . . . C7B C -0.0366(3) 0.9023(3) 0.4359(3) 0.0185(16) Uani 1 1 d . . . H7B H -0.0824 0.9433 0.4335 0.022 Uiso 1 1 calc R . . C8B C 0.0334(4) 0.9274(3) 0.3880(3) 0.0188(16) Uani 1 1 d . . . C9B C 0.1191(4) 0.9095(3) 0.4010(3) 0.0201(16) Uani 1 1 d . . . H9B' H 0.1327 0.8815 0.4415 0.024 Uiso 1 1 calc R . . C10B C 0.1854(4) 0.9303(3) 0.3583(3) 0.0204(16) Uani 1 1 d . . . C11B C 0.1628(4) 0.9696(4) 0.2998(3) 0.0250(17) Uani 1 1 d . . . O11B O 0.2277(3) 0.9860(3) 0.2541(3) 0.0324(14) Uani 1 1 d . . . H11B H 0.222(5) 1.022(4) 0.244(4) 0.049 Uiso 1 1 d . . . C12B C 0.0793(4) 0.9901(4) 0.2849(3) 0.0284(18) Uani 1 1 d . . . H12B' H 0.0659 1.0195 0.2450 0.034 Uiso 1 1 calc R . . C13B C 0.0162(4) 0.9673(4) 0.3285(3) 0.0235(17) Uani 1 1 d . . . O13B O -0.0652(3) 0.9882(3) 0.3089(2) 0.0309(13) Uani 1 1 d . . . H13B H -0.098(4) 0.962(4) 0.335(3) 0.046 Uiso 1 1 d . . . C14B C 0.2776(4) 0.9099(4) 0.3732(3) 0.0237(17) Uani 1 1 d . . . H14B H 0.3102 0.9516 0.3514 0.028 Uiso 1 1 calc R . . C15B C 0.3097(3) 0.8380(4) 0.3408(3) 0.0194(16) Uani 1 1 d . . . C16B C 0.2870(4) 0.7680(4) 0.3677(3) 0.0205(17) Uani 1 1 d . . . H16B H 0.2473 0.7665 0.4036 0.025 Uiso 1 1 calc R . . C17B C 0.3191(4) 0.6995(4) 0.3452(3) 0.0203(16) Uani 1 1 d . . . C18B C 0.3770(4) 0.7041(4) 0.2928(3) 0.0223(17) Uani 1 1 d . . . O18B O 0.4072(3) 0.6365(3) 0.2689(2) 0.0337(14) Uani 1 1 d . . . H18B H 0.442(4) 0.638(4) 0.241(3) 0.051 Uiso 1 1 d . . . C19B C 0.3989(4) 0.7734(4) 0.2626(3) 0.0226(17) Uani 1 1 d . . . H19B H 0.4380 0.7752 0.2263 0.027 Uiso 1 1 calc R . . C20B C 0.3643(4) 0.8388(4) 0.2854(3) 0.0220(17) Uani 1 1 d . . . O20B O 0.3889(3) 0.9053(3) 0.2531(3) 0.0310(14) Uani 1 1 d . . . H20B H 0.356(4) 0.933(4) 0.244(4) 0.046 Uiso 1 1 d . . . C21B C 0.2928(4) 0.6245(4) 0.3786(3) 0.0232(17) Uani 1 1 d . . . H21B H 0.3311 0.5847 0.3595 0.028 Uiso 1 1 calc R . . C22B C 0.2036(4) 0.6082(3) 0.3596(3) 0.0199(16) Uani 1 1 d . . . C23B C 0.1341(4) 0.6167(3) 0.4034(3) 0.0201(16) Uani 1 1 d . . . H23B H 0.1440 0.6325 0.4462 0.024 Uiso 1 1 calc R . . C24B C 0.0511(4) 0.6032(3) 0.3876(3) 0.0168(16) Uani 1 1 d . . . C25B C 0.0392(4) 0.5794(4) 0.3250(3) 0.0252(17) Uani 1 1 d . . . O25B O -0.0387(3) 0.5640(3) 0.3026(2) 0.0315(12) Uani 1 1 d . . . H25' H -0.0767 0.5825 0.3271 0.047 Uiso 1 1 calc R . . C26B C 0.1066(4) 0.5705(3) 0.2805(3) 0.0234(17) Uani 1 1 d . . . H26B H 0.0973 0.5535 0.2381 0.028 Uiso 1 1 calc R . . C27B C 0.1868(4) 0.5861(3) 0.2976(3) 0.0220(17) Uani 1 1 d . . . O27B O 0.2483(3) 0.5776(3) 0.2484(3) 0.0312(15) Uani 1 1 d . . . H27B H 0.284(5) 0.582(5) 0.260(4) 0.047 Uiso 1 1 d . . . C28B C -0.0235(3) 0.6176(4) 0.4351(3) 0.0178(16) Uani 1 1 d . . . H28B H -0.0642 0.5780 0.4293 0.021 Uiso 1 1 calc R . . C29B C -0.0106(4) 0.8901(4) 0.5085(3) 0.0193(16) Uani 1 1 d . . . H29C H 0.0300 0.8457 0.5135 0.023 Uiso 1 1 calc R . . H29D H 0.0186 0.9345 0.5206 0.023 Uiso 1 1 calc R . . C30B C -0.0853(4) 0.8777(4) 0.5560(3) 0.0311(19) Uani 1 1 d . . . H30C H -0.1184 0.9262 0.5596 0.037 Uiso 1 1 calc R . . H30D H -0.1225 0.8419 0.5379 0.037 Uiso 1 1 calc R . . C31B C -0.0579(4) 0.8474(4) 0.6238(3) 0.043(2) Uani 1 1 d . . . H31D H -0.1079 0.8396 0.6525 0.064 Uiso 1 1 calc R . . H31E H -0.0228 0.8836 0.6426 0.064 Uiso 1 1 calc R . . H31F H -0.0253 0.7994 0.6206 0.064 Uiso 1 1 calc R . . C32B C 0.2986(4) 0.9057(4) 0.4464(3) 0.0246(17) Uani 1 1 d . . . H32C H 0.2723 0.9508 0.4662 0.029 Uiso 1 1 calc R . . H32D H 0.2735 0.8608 0.4690 0.029 Uiso 1 1 calc R . . C33B C 0.3928(4) 0.9012(4) 0.4587(3) 0.038(2) Uani 1 1 d . . . H33C H 0.4194 0.8574 0.4372 0.045 Uiso 1 1 calc R . . H33D H 0.4174 0.9472 0.4377 0.045 Uiso 1 1 calc R . . C34B C 0.4139(5) 0.8938(6) 0.5311(4) 0.067(3) Uani 1 1 d . . . H34D H 0.4754 0.8918 0.5358 0.100 Uiso 1 1 calc R . . H34E H 0.3915 0.8474 0.5520 0.100 Uiso 1 1 calc R . . H34F H 0.3884 0.9373 0.5527 0.100 Uiso 1 1 calc R . . C35B C 0.3090(4) 0.6185(4) 0.4529(3) 0.0289(18) Uani 1 1 d . . . H35C H 0.2771 0.6605 0.4734 0.035 Uiso 1 1 calc R . . H35D H 0.2875 0.5707 0.4729 0.035 Uiso 1 1 calc R . . C36B C 0.4016(4) 0.6207(5) 0.4685(4) 0.050(2) Uani 1 1 d . . . H36C H 0.4230 0.6685 0.4485 0.060 Uiso 1 1 calc R . . H36D H 0.4335 0.5788 0.4479 0.060 Uiso 1 1 calc R . . C37B C 0.4177(5) 0.6146(6) 0.5420(4) 0.094(4) Uani 1 1 d . . . H37D H 0.4785 0.6157 0.5492 0.141 Uiso 1 1 calc R . . H37E H 0.3972 0.5671 0.5620 0.141 Uiso 1 1 calc R . . H37F H 0.3880 0.6570 0.5625 0.141 Uiso 1 1 calc R . . C38B C -0.0008(3) 0.6117(4) 0.5077(3) 0.0217(17) Uani 1 1 d . . . H38C H 0.0329 0.5638 0.5177 0.026 Uiso 1 1 calc R . . H38D H 0.0351 0.6535 0.5159 0.026 Uiso 1 1 calc R . . C39B C -0.0768(4) 0.6143(4) 0.5546(3) 0.0317(19) Uani 1 1 d . . . H39C H -0.1097 0.5696 0.5497 0.038 Uiso 1 1 calc R . . H39D H -0.1135 0.6597 0.5418 0.038 Uiso 1 1 calc R . . C40B C -0.0534(4) 0.6161(4) 0.6267(3) 0.040(2) Uani 1 1 d . . . H40D H -0.1050 0.6184 0.6543 0.060 Uiso 1 1 calc R . . H40E H -0.0215 0.6605 0.6320 0.060 Uiso 1 1 calc R . . H40F H -0.0188 0.5704 0.6402 0.060 Uiso 1 1 calc R . . Br1 Br 0.57531(4) 0.66291(4) 0.17462(3) 0.0277(2) Uani 1 1 d . . . Br2 Br 0.97211(5) 0.71821(5) -0.05478(4) 0.0531(3) Uani 1 1 d . . . N1C N 0.5027(3) 0.7299(3) -0.0364(2) 0.0148(12) Uani 1 1 d . . . N2C N 0.6639(3) 0.7152(3) -0.0242(2) 0.0184(13) Uani 1 1 d . . . C1C C 0.5341(4) 0.7927(4) -0.0004(3) 0.0222(16) Uani 1 1 d . . . H1C1 H 0.4993 0.7992 0.0403 0.027 Uiso 1 1 calc R . . H1C2 H 0.5288 0.8404 -0.0288 0.027 Uiso 1 1 calc R . . C2C C 0.6267(3) 0.7753(3) 0.0180(3) 0.0195(16) Uani 1 1 d . . . H2C1 H 0.6586 0.8214 0.0104 0.023 Uiso 1 1 calc R . . H2C2 H 0.6304 0.7576 0.0654 0.023 Uiso 1 1 calc R . . C3C C 0.5468(4) 0.7293(4) -0.1035(3) 0.0231(17) Uani 1 1 d . . . H3C1 H 0.5238 0.7719 -0.1332 0.028 Uiso 1 1 calc R . . H3C2 H 0.5372 0.6818 -0.1238 0.028 Uiso 1 1 calc R . . C4C C 0.6412(4) 0.7363(4) -0.0948(3) 0.0239(17) Uani 1 1 d . . . H4C1 H 0.6737 0.7028 -0.1242 0.029 Uiso 1 1 calc R . . H4C2 H 0.6560 0.7888 -0.1072 0.029 Uiso 1 1 calc R . . C5C C 0.5287(3) 0.6564(3) 0.0024(3) 0.0200(16) Uani 1 1 d . . . H5C1 H 0.5010 0.6143 -0.0158 0.024 Uiso 1 1 calc R . . H5C2 H 0.5105 0.6588 0.0493 0.024 Uiso 1 1 calc R . . C6C C 0.6242(3) 0.6428(3) -0.0023(3) 0.0219(16) Uani 1 1 d . . . H6C1 H 0.6461 0.6233 0.0414 0.026 Uiso 1 1 calc R . . H6C2 H 0.6390 0.6047 -0.0345 0.026 Uiso 1 1 calc R . . C7C C 0.4073(3) 0.7384(4) -0.0457(3) 0.0220(16) Uani 1 1 d . . . H7C1 H 0.3930 0.7874 -0.0703 0.026 Uiso 1 1 calc R . . H7C2 H 0.3901 0.6981 -0.0727 0.026 Uiso 1 1 calc R . . C8C C 0.3580(4) 0.7345(4) 0.0191(3) 0.0227(17) Uani 1 1 d . . . C9C C 0.3410(4) 0.7995(4) 0.0526(3) 0.0240(17) Uani 1 1 d . . . H9C H 0.3584 0.8466 0.0335 0.029 Uiso 1 1 calc R . . C10C C 0.2987(4) 0.7959(4) 0.1136(3) 0.0314(18) Uani 1 1 d . . . H10C H 0.2888 0.8397 0.1372 0.038 Uiso 1 1 calc R . . C11C C 0.2711(4) 0.7270(4) 0.1393(3) 0.0333(19) Uani 1 1 d . . . H11C H 0.2412 0.7238 0.1806 0.040 Uiso 1 1 calc R . . C12C C 0.2868(4) 0.6633(4) 0.1057(3) 0.0298(18) Uani 1 1 d . . . H12C H 0.2678 0.6164 0.1238 0.036 Uiso 1 1 calc R . . C13C C 0.3303(4) 0.6673(4) 0.0453(3) 0.0284(18) Uani 1 1 d . . . H13C H 0.3409 0.6232 0.0221 0.034 Uiso 1 1 calc R . . C14C C 0.7606(3) 0.7076(4) -0.0193(3) 0.0257(18) Uani 1 1 d . . . H14A H 0.7831 0.6681 -0.0480 0.031 Uiso 1 1 calc R . . H14B' H 0.7844 0.7557 -0.0358 0.031 Uiso 1 1 calc R . . C15C C 0.7880(4) 0.6875(4) 0.0501(3) 0.0238(17) Uani 1 1 d . . . C16C C 0.7954(4) 0.7402(4) 0.0957(4) 0.0362(19) Uani 1 1 d . . . H16C H 0.7856 0.7921 0.0822 0.043 Uiso 1 1 calc R . . C17C C 0.8167(4) 0.7196(5) 0.1600(4) 0.046(2) Uani 1 1 d . . . H17C H 0.8187 0.7568 0.1910 0.055 Uiso 1 1 calc R . . C18C C 0.8353(5) 0.6447(6) 0.1798(4) 0.056(3) Uani 1 1 d . . . H18C H 0.8503 0.6298 0.2241 0.067 Uiso 1 1 calc R . . C19C C 0.8314(4) 0.5921(5) 0.1336(5) 0.048(2) Uani 1 1 d . . . H19C H 0.8439 0.5402 0.1459 0.057 Uiso 1 1 calc R . . C20C C 0.8091(3) 0.6151(3) 0.0687(2) 0.038(2) Uani 1 1 d . . . H20C H 0.8089 0.5786 0.0369 0.045 Uiso 1 1 calc R . . N1E N 0.0614(3) 0.9606(3) 0.0237(2) 0.026(3) Uiso 0.50 1 d PR . 1 C3E C 0.0306(3) 1.0025(3) 0.0788(2) 0.039(6) Uiso 0.50 1 d PR . 1 C4E C 0.1277(3) 0.8956(3) 0.0502(2) 0.022(3) Uiso 0.50 1 d PR A 1 C1E C -0.1135(3) 0.9819(3) 0.0232(2) 0.039(4) Uiso 0.50 1 d PR . 1 C2E C -0.0017(3) 0.9337(3) -0.0160(2) 0.044(4) Uiso 0.50 1 d PR . 1 C8E C 0.0970(7) 0.8475(5) 0.1007(5) 0.023(3) Uiso 0.50 1 d PG A 1 C9E C 0.0577(7) 0.7842(6) 0.0837(4) 0.038(4) Uiso 0.50 1 d PG A 1 C10E C 0.0262(8) 0.7342(5) 0.1330(6) 0.057(5) Uiso 0.50 1 d PG A 1 C11E C 0.0340(8) 0.7476(6) 0.1993(5) 0.055(6) Uiso 0.50 1 d PG A 1 C12E C 0.0733(8) 0.8109(7) 0.2162(4) 0.054(5) Uiso 0.50 1 d PG A 1 C13E C 0.1048(8) 0.8609(6) 0.1669(5) 0.032(7) Uiso 0.50 1 d PG A 1 N1G N 0.0365(7) 0.9274(7) 0.0273(6) 0.043(3) Uiso 0.50 1 d P B 2 C1G C -0.0545(8) 0.9064(8) 0.0377(6) 0.028(3) Uiso 0.50 1 d P B 2 C2G C 0.0480(8) 0.9422(8) -0.0456(7) 0.038(4) Uiso 0.50 1 d P . 2 C3G C 0.0488(11) 1.0068(9) 0.0598(9) 0.046(4) Uiso 0.50 1 d P . 2 C4G C 0.0991(9) 0.8604(9) 0.0503(8) 0.044(4) Uiso 0.50 1 d P B 2 C8G C 0.0832(8) 0.8307(6) 0.1210(4) 0.037(4) Uiso 0.50 1 d PG B 2 C9G C 0.0413(7) 0.7641(6) 0.1261(4) 0.055(5) Uiso 0.50 1 d PG B 2 C10G C 0.0276(7) 0.7269(5) 0.1879(5) 0.033(5) Uiso 0.50 1 d PG B 2 C11G C 0.0558(6) 0.7562(5) 0.2445(4) 0.030(3) Uiso 0.50 1 d PG B 2 C12G C 0.0977(7) 0.8228(6) 0.2394(4) 0.035(4) Uiso 0.50 1 d PG B 2 C13G C 0.1114(8) 0.8601(5) 0.1776(5) 0.040(8) Uiso 0.50 1 d PG B 2 Br3 Br 0.3037(8) 1.02583(18) 0.01098(15) 0.0413(18) Uani 0.360(13) 1 d P C 1 Br3B Br 0.3571(5) 1.01757(14) 0.01101(8) 0.0473(13) Uani 0.640(13) 1 d P C 2 O1M O 0.9640(3) 0.5978(3) -0.1646(3) 0.0528(17) Uani 1 1 d . . . H1M H 0.963(6) 0.628(5) -0.136(4) 0.079 Uiso 1 1 d . . . C2M C 1.0391(4) 0.5985(5) -0.2026(4) 0.057(3) Uani 1 1 d . . . H2M1 H 1.0415 0.6468 -0.2288 0.085 Uiso 1 1 calc R . . H2M2 H 1.0408 0.5575 -0.2323 0.085 Uiso 1 1 calc R . . H2M3 H 1.0876 0.5917 -0.1732 0.085 Uiso 1 1 calc R . . O3M O 0.9528(3) 0.8498(3) -0.1691(3) 0.0412(14) Uani 1 1 d . . . H3M H 0.957(4) 0.810(4) -0.129(4) 0.062 Uiso 1 1 d . . . C4M C 1.0253(4) 0.8318(5) -0.2088(4) 0.050(2) Uani 1 1 d . . . H4M1 H 1.0451 0.8779 -0.2320 0.074 Uiso 1 1 calc R . . H4M2 H 1.0107 0.7968 -0.2412 0.074 Uiso 1 1 calc R . . H4M3 H 1.0702 0.8081 -0.1806 0.074 Uiso 1 1 calc R . . C6M C 0.5824(5) 0.9200(6) 0.3443(5) 0.082(3) Uani 1 1 d . . . H6M1 H 0.5912 0.9440 0.3853 0.123 Uiso 1 1 calc R . . H6M2 H 0.5490 0.8757 0.3541 0.123 Uiso 1 1 calc R . . H6M3 H 0.5521 0.9559 0.3130 0.123 Uiso 1 1 calc R . . O5M O 0.6598(3) 0.8978(3) 0.3167(3) 0.0546(16) Uani 1 1 d . . . H5M H 0.6529 0.8662 0.2889 0.082 Uiso 1 1 calc R . . C8M C 0.5987(5) 0.6570(6) 0.3576(4) 0.090(4) Uani 1 1 d . . . H8M1 H 0.6166 0.6584 0.4034 0.135 Uiso 1 1 calc R . . H8M2 H 0.5624 0.6148 0.3545 0.135 Uiso 1 1 calc R . . H8M3 H 0.5672 0.7044 0.3440 0.135 Uiso 1 1 calc R . . O7M O 0.6694(3) 0.6479(3) 0.3163(2) 0.0495(15) Uani 1 1 d D . . H7M H 0.659(5) 0.651(5) 0.2759(13) 0.074 Uiso 1 1 d D . . O9M O 0.6359(4) 0.8290(3) 0.2067(3) 0.0540(17) Uani 1 1 d . . . H9M H 0.633(6) 0.788(5) 0.200(5) 0.081 Uiso 1 1 d . . . C10M C 0.5847(5) 0.8770(5) 0.1660(4) 0.056(3) Uani 1 1 d . . . H10A H 0.5741 0.9251 0.1861 0.085 Uiso 1 1 calc R . . H10B H 0.5308 0.8542 0.1604 0.085 Uiso 1 1 calc R . . H10D H 0.6128 0.8858 0.1227 0.085 Uiso 1 1 calc R . . O11M O -0.1259(4) 0.9919(4) 0.1788(3) 0.084(2) Uani 1 1 d . . . H11M H -0.0994 0.9920 0.2142 0.126 Uiso 1 1 calc R . . C12M C -0.1799(6) 0.9334(6) 0.1838(6) 0.100(4) Uani 1 1 d . . . H12A' H -0.2310 0.9483 0.2088 0.149 Uiso 1 1 calc R . . H12B'' H -0.1516 0.8888 0.2067 0.149 Uiso 1 1 calc R . . H12D H -0.1952 0.9215 0.1393 0.149 Uiso 1 1 calc R . . O13M O 0.8915(3) 0.4169(3) 0.0030(3) 0.066(2) Uani 1 1 d . . . H13M H 0.935(5) 0.379(5) 0.012(4) 0.099 Uiso 1 1 d . . . C14M C 0.9067(5) 0.4546(5) -0.0580(4) 0.070(3) Uani 1 1 d . . . H14C H 0.8675 0.4991 -0.0637 0.105 Uiso 1 1 calc R . . H14D H 0.8984 0.4210 -0.0931 0.105 Uiso 1 1 calc R . . H14E H 0.9650 0.4703 -0.0603 0.105 Uiso 1 1 calc R . . O1W O 0.7921(6) 0.8883(6) -0.0797(5) 0.063(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.017(4) 0.014(4) 0.018(4) -0.007(3) -0.006(3) -0.001(3) C2 0.022(4) 0.006(4) 0.022(4) 0.001(3) -0.004(3) 0.005(3) C3 0.017(3) 0.013(4) 0.020(4) -0.003(3) 0.001(3) 0.005(3) C4 0.017(4) 0.013(4) 0.022(4) -0.003(3) 0.003(3) -0.005(3) O4 0.022(2) 0.036(3) 0.021(3) 0.003(2) 0.002(2) -0.004(2) C5 0.029(4) 0.012(4) 0.017(4) 0.003(3) -0.005(3) -0.008(3) C6 0.017(4) 0.016(4) 0.025(4) -0.003(3) 0.000(3) 0.001(3) O6 0.019(3) 0.032(3) 0.025(3) 0.001(2) 0.001(2) -0.001(2) C7 0.021(4) 0.017(4) 0.017(4) 0.003(3) 0.005(3) -0.001(3) C8 0.014(3) 0.021(4) 0.021(4) -0.004(3) 0.001(3) -0.007(3) C9 0.009(3) 0.028(5) 0.017(4) 0.001(3) -0.011(3) 0.001(3) C10 0.010(3) 0.019(4) 0.015(4) -0.003(3) -0.002(3) 0.000(3) C11 0.018(3) 0.026(5) 0.017(4) 0.001(3) -0.002(3) 0.000(3) O11 0.033(3) 0.020(3) 0.037(3) -0.007(2) 0.015(3) -0.002(2) C12 0.018(3) 0.038(5) 0.015(4) -0.001(4) -0.006(3) -0.005(3) C13 0.016(3) 0.025(5) 0.013(4) 0.006(3) -0.005(3) -0.002(3) O13 0.028(3) 0.027(3) 0.026(3) 0.003(2) 0.010(2) -0.002(2) C14 0.020(4) 0.026(4) 0.017(4) 0.011(3) -0.001(3) -0.006(3) C15 0.026(4) 0.010(4) 0.023(4) 0.002(3) -0.003(3) -0.003(3) C16 0.019(4) 0.013(4) 0.022(4) 0.002(3) 0.008(3) 0.000(3) C17 0.025(4) 0.011(4) 0.020(4) 0.002(3) 0.005(3) 0.001(3) C18 0.025(4) 0.020(4) 0.022(4) 0.009(3) 0.001(3) -0.006(3) O18 0.025(3) 0.033(4) 0.026(3) -0.011(2) -0.001(2) -0.010(2) C19 0.025(4) 0.022(4) 0.023(4) -0.001(3) 0.003(3) 0.002(3) C20 0.023(4) 0.017(4) 0.025(4) -0.002(3) 0.013(3) -0.002(3) O20 0.030(3) 0.029(3) 0.036(3) -0.017(2) 0.012(3) -0.001(2) C21 0.019(3) 0.010(4) 0.020(4) -0.006(3) 0.003(3) -0.007(3) C22 0.016(3) 0.023(4) 0.011(3) 0.003(3) 0.002(3) -0.002(3) C23 0.011(3) 0.021(4) 0.013(3) 0.001(3) 0.000(3) -0.005(3) C24 0.020(4) 0.015(4) 0.012(3) 0.002(3) -0.002(3) 0.002(3) C25 0.009(3) 0.019(4) 0.024(4) -0.001(3) 0.006(3) 0.003(3) O25 0.014(2) 0.021(3) 0.039(3) 0.005(2) -0.007(2) 0.005(2) C26 0.010(3) 0.024(5) 0.024(4) 0.004(3) 0.004(3) -0.002(3) C27 0.017(4) 0.011(4) 0.023(4) 0.000(3) 0.005(3) -0.006(3) O27 0.026(3) 0.025(3) 0.030(3) 0.001(2) -0.006(2) -0.008(3) C28 0.014(3) 0.024(4) 0.018(4) -0.001(3) 0.001(3) 0.002(3) C29 0.025(4) 0.025(4) 0.023(4) -0.003(3) -0.001(3) -0.006(3) C30 0.025(4) 0.036(5) 0.029(4) -0.005(4) -0.002(3) -0.011(3) C31 0.033(4) 0.069(6) 0.041(5) -0.007(4) -0.008(4) -0.024(4) C32 0.015(3) 0.039(5) 0.023(4) 0.002(3) 0.001(3) 0.000(3) C33 0.024(4) 0.073(7) 0.032(5) 0.015(4) -0.002(4) 0.000(4) C34 0.034(5) 0.183(12) 0.035(5) -0.002(6) -0.017(4) -0.021(6) C35 0.022(4) 0.023(4) 0.018(4) 0.000(3) 0.001(3) 0.001(3) C36 0.034(4) 0.040(5) 0.024(4) 0.007(4) 0.001(4) -0.003(4) C37 0.040(4) 0.070(6) 0.025(4) -0.001(4) 0.002(4) -0.006(4) C38 0.022(4) 0.015(4) 0.029(4) -0.011(3) 0.006(3) -0.005(3) C39 0.032(4) 0.034(5) 0.022(4) -0.001(3) 0.007(3) 0.001(3) C40 0.037(4) 0.065(6) 0.033(5) -0.004(4) 0.006(4) -0.008(4) C1B 0.011(3) 0.030(5) 0.014(4) 0.000(3) -0.005(3) 0.003(3) C2B 0.012(3) 0.024(5) 0.024(4) -0.006(3) 0.000(3) -0.008(3) C3B 0.009(3) 0.018(4) 0.019(4) -0.001(3) 0.005(3) 0.000(3) C4B 0.018(4) 0.023(5) 0.019(4) 0.007(3) 0.002(3) 0.007(3) O4B 0.017(2) 0.020(3) 0.037(3) 0.004(2) -0.008(2) 0.003(2) C5B 0.016(3) 0.020(5) 0.031(4) -0.002(3) -0.005(3) -0.002(3) C6B 0.026(4) 0.016(4) 0.020(4) -0.008(3) 0.003(3) -0.003(3) O6B 0.019(3) 0.021(3) 0.042(3) -0.007(2) -0.012(2) -0.002(2) C7B 0.013(3) 0.014(4) 0.028(4) 0.002(3) 0.004(3) 0.002(3) C8B 0.015(3) 0.014(4) 0.027(4) 0.001(3) 0.000(3) 0.001(3) C9B 0.026(4) 0.017(4) 0.017(4) -0.003(3) 0.001(3) -0.002(3) C10B 0.020(4) 0.013(4) 0.028(4) -0.001(3) -0.003(3) 0.000(3) C11B 0.018(4) 0.021(4) 0.035(4) 0.004(3) 0.009(4) -0.005(3) O11B 0.028(3) 0.025(3) 0.040(3) 0.016(3) 0.006(2) 0.001(3) C12B 0.027(4) 0.022(4) 0.035(4) 0.011(3) 0.004(4) -0.003(3) C13B 0.021(4) 0.017(4) 0.031(4) 0.007(3) -0.005(3) 0.007(3) O13B 0.021(3) 0.033(3) 0.035(3) 0.015(2) -0.001(2) 0.004(2) C14B 0.013(3) 0.027(5) 0.029(4) 0.003(3) 0.002(3) 0.002(3) C15B 0.011(3) 0.023(4) 0.023(4) 0.003(3) 0.001(3) 0.002(3) C16B 0.014(3) 0.032(5) 0.016(4) 0.001(3) 0.003(3) -0.002(3) C17B 0.018(3) 0.020(4) 0.022(4) 0.004(3) 0.003(3) 0.005(3) C18B 0.018(3) 0.023(5) 0.027(4) -0.005(3) 0.003(3) -0.004(3) O18B 0.032(3) 0.029(3) 0.038(3) -0.002(3) 0.022(2) 0.003(2) C19B 0.016(3) 0.035(5) 0.017(4) -0.005(3) 0.008(3) -0.004(3) C20B 0.020(4) 0.029(5) 0.017(4) -0.001(3) -0.002(3) -0.007(3) O20B 0.026(3) 0.025(4) 0.040(3) 0.007(3) 0.007(3) -0.001(2) C21B 0.017(3) 0.023(4) 0.027(4) 0.004(3) 0.005(3) 0.008(3) C22B 0.021(4) 0.010(4) 0.028(4) 0.002(3) 0.003(3) 0.005(3) C23B 0.024(4) 0.013(4) 0.022(4) -0.005(3) 0.003(3) 0.005(3) C24B 0.019(4) 0.007(4) 0.023(4) 0.010(3) -0.002(3) 0.000(3) C25B 0.020(4) 0.026(5) 0.028(4) 0.004(3) -0.003(4) 0.003(3) O25B 0.030(3) 0.036(3) 0.030(3) -0.012(2) -0.004(2) 0.002(2) C26B 0.041(4) 0.012(4) 0.017(4) -0.006(3) 0.000(4) 0.001(3) C27B 0.030(4) 0.011(4) 0.024(4) 0.005(3) 0.004(4) 0.004(3) O27B 0.030(3) 0.027(3) 0.034(3) -0.002(2) 0.008(3) 0.006(3) C28B 0.011(3) 0.024(4) 0.018(4) 0.001(3) -0.002(3) -0.001(3) C29B 0.020(3) 0.016(4) 0.021(4) 0.003(3) 0.007(3) -0.002(3) C30B 0.028(4) 0.035(5) 0.033(4) -0.014(4) 0.002(4) -0.011(4) C31B 0.043(5) 0.050(6) 0.035(5) -0.001(4) 0.016(4) -0.006(4) C32B 0.023(4) 0.028(5) 0.024(4) -0.008(3) -0.001(3) -0.001(3) C33B 0.022(4) 0.054(6) 0.039(5) -0.008(4) 0.000(4) -0.004(4) C34B 0.034(5) 0.123(9) 0.045(6) -0.009(6) -0.014(4) -0.017(5) C35B 0.021(4) 0.033(5) 0.032(4) 0.004(4) -0.001(3) -0.006(3) C36B 0.026(4) 0.080(7) 0.039(5) 0.018(5) -0.003(4) 0.000(4) C37B 0.032(5) 0.184(12) 0.061(7) 0.033(7) -0.015(5) -0.020(6) C38B 0.016(3) 0.018(4) 0.030(4) 0.001(3) -0.001(3) 0.002(3) C39B 0.023(4) 0.047(5) 0.023(4) 0.004(4) 0.007(3) -0.002(4) C40B 0.038(4) 0.044(5) 0.036(5) 0.008(4) 0.011(4) 0.001(4) Br1 0.0283(4) 0.0324(5) 0.0230(4) -0.0045(3) 0.0042(3) -0.0052(3) Br2 0.0343(4) 0.0817(7) 0.0389(5) 0.0109(5) 0.0053(4) 0.0101(4) N1C 0.021(3) 0.013(3) 0.011(3) -0.003(2) -0.004(2) -0.002(2) N2C 0.017(3) 0.017(3) 0.020(3) 0.001(3) 0.002(2) -0.004(2) C1C 0.026(4) 0.018(4) 0.022(4) 0.000(3) 0.001(3) 0.002(3) C2C 0.018(3) 0.018(4) 0.023(4) 0.000(3) 0.003(3) -0.007(3) C3C 0.032(4) 0.019(4) 0.017(4) -0.001(3) 0.002(3) -0.002(3) C4C 0.026(4) 0.021(4) 0.023(4) 0.005(3) -0.001(3) -0.005(3) C5C 0.020(3) 0.016(4) 0.023(4) 0.000(3) -0.002(3) 0.000(3) C6C 0.026(4) 0.009(4) 0.030(4) 0.005(3) -0.001(3) -0.003(3) C7C 0.022(4) 0.018(4) 0.028(4) -0.004(3) -0.012(3) -0.007(3) C8C 0.016(3) 0.026(5) 0.025(4) 0.010(4) -0.003(3) -0.005(3) C9C 0.026(4) 0.013(4) 0.032(4) -0.003(3) -0.002(3) 0.002(3) C10C 0.025(4) 0.032(5) 0.037(5) -0.010(4) -0.003(4) 0.006(4) C11C 0.024(4) 0.048(6) 0.026(4) 0.004(4) 0.000(3) 0.006(4) C12C 0.032(4) 0.021(5) 0.035(4) 0.004(4) 0.004(4) 0.000(3) C13C 0.024(4) 0.034(5) 0.027(4) -0.002(4) -0.002(3) -0.005(3) C14C 0.014(3) 0.033(5) 0.030(4) 0.003(3) 0.005(3) -0.007(3) C15C 0.020(4) 0.015(4) 0.035(4) 0.002(4) 0.001(3) 0.003(3) C16C 0.031(4) 0.032(5) 0.046(5) -0.002(4) -0.013(4) 0.001(4) C17C 0.034(5) 0.058(7) 0.049(6) -0.017(5) -0.008(4) -0.012(4) C18C 0.041(5) 0.074(8) 0.048(6) 0.025(6) -0.008(4) 0.003(5) C19C 0.036(5) 0.025(5) 0.079(7) 0.020(5) -0.007(5) -0.004(4) C20C 0.030(4) 0.049(6) 0.034(5) 0.000(4) -0.007(4) 0.005(4) Br3 0.060(5) 0.0343(17) 0.0297(14) -0.0075(11) 0.0061(17) -0.0049(18) Br3B 0.080(4) 0.0370(10) 0.0275(8) -0.0112(7) 0.0059(11) -0.0177(13) O1M 0.027(3) 0.072(5) 0.060(4) -0.006(3) -0.006(3) -0.002(3) C2M 0.030(4) 0.060(6) 0.083(7) -0.020(5) 0.009(5) -0.011(4) O3M 0.033(3) 0.035(3) 0.055(4) -0.002(3) -0.005(3) -0.001(2) C4M 0.032(4) 0.059(6) 0.055(5) 0.003(5) 0.005(4) 0.004(4) C6M 0.043(5) 0.126(10) 0.081(7) -0.046(7) -0.008(5) 0.010(6) O5M 0.025(3) 0.070(5) 0.072(4) -0.033(3) -0.015(3) 0.015(3) C8M 0.055(6) 0.168(12) 0.044(6) 0.005(7) 0.000(5) -0.006(7) O7M 0.029(3) 0.085(5) 0.035(3) -0.004(3) -0.007(3) -0.004(3) O9M 0.062(4) 0.031(4) 0.070(4) -0.011(4) -0.014(3) 0.004(3) C10M 0.089(7) 0.038(6) 0.040(5) 0.005(4) 0.011(5) -0.004(5) O11M 0.103(5) 0.117(6) 0.039(4) -0.006(4) 0.002(4) -0.060(5) C12M 0.094(8) 0.063(8) 0.145(11) 0.001(7) -0.032(8) -0.031(7) O13M 0.054(4) 0.069(5) 0.062(4) 0.044(3) 0.036(3) 0.020(3) C14M 0.079(6) 0.076(7) 0.048(6) 0.020(5) 0.017(5) 0.011(6) O1W 0.056(7) 0.067(9) 0.063(8) 0.002(7) -0.013(6) 0.004(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 C1 C2 1.378(8) . ? C1 C6 1.400(8) . ? C1 C28 1.528(7) . ? C2 C3 1.399(7) . ? C2 H2 0.9500 . ? C3 C4 1.384(8) . ? C3 C7 1.527(8) . ? C4 O4 1.386(6) . ? C4 C5 1.387(8) . ? O4 H4 0.8400 . ? C5 C6 1.390(8) . ? C5 H5 0.9500 . ? C6 O6 1.380(7) . ? O6 H6 0.71(6) . ? C7 C29 1.520(8) . ? C7 C8 1.521(8) . ? C7 H7 1.0000 . ? C8 C13 1.391(8) . ? C8 C9 1.391(8) . ? C9 C10 1.375(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.397(8) . ? C10 C14 1.551(8) . ? C11 O11 1.365(7) . ? C11 C12 1.377(8) . ? O11 H11 0.8400 . ? C12 C13 1.392(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O13 1.387(7) . ? O13 H13 0.85(6) . ? C14 C32 1.532(8) . ? C14 C15 1.542(8) . ? C15 C20 1.378(9) . ? C15 C16 1.412(8) . ? C16 C17 1.368(8) . ? C16 H16 0.9500 . ? C17 C18 1.386(9) . ? C17 C21 1.542(7) . ? C18 O18 1.382(8) . ? C18 C19 1.407(8) . ? O18 H18 0.72(7) . ? C19 C20 1.374(8) . ? C19 H19 0.9500 . ? C20 O20 1.393(7) . ? O20 H20 0.86(7) . ? C21 C22 1.527(8) . ? C21 C35 1.530(8) . ? C21 H21 1.0000 . ? C22 C27 1.388(8) . ? C22 C23 1.407(8) . ? C23 C24 1.369(8) . ? C23 H23 0.9500 . ? C24 C25 1.408(8) . ? C24 C28 1.507(8) . ? C25 O25 1.364(7) . ? C25 C26 1.390(8) . ? O25 H25 0.88(6) . ? C26 C27 1.385(8) . ? C26 H26 0.9500 . ? C27 O27 1.383(8) . ? O27 H27 0.68(7) . ? C28 C38 1.538(8) . ? C28 H28 1.0000 . ? C29 C30 1.541(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.514(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.513(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.548(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.528(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.515(9) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.524(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.527(9) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C1B C2B 1.394(8) . ? C1B C6B 1.400(8) . ? C1B C28B 1.518(8) . ? C2B C3B 1.400(8) . ? C2B H2B 0.9500 . ? C3B C4B 1.394(8) . ? C3B C7B 1.535(8) . ? C4B O4B 1.368(7) . ? C4B C5B 1.405(9) . ? O4B H4B 0.84(6) . ? C5B C6B 1.411(8) . ? C5B H5B 0.9500 . ? C6B O6B 1.362(7) . ? O6B H6B 0.81(6) . ? C7B C8B 1.520(7) . ? C7B C29B 1.535(8) . ? C7B H7B 1.0000 . ? C8B C13B 1.379(8) . ? C8B C9B 1.404(8) . ? C9B C10B 1.394(8) . ? C9B H9B 0.9500 . ? C10B C11B 1.374(8) . ? C10B C14B 1.518(8) . ? C11B C12B 1.388(8) . ? C11B O11B 1.396(7) . ? O11B H11B 0.67(7) . ? C12B C13B 1.377(8) . ? C12B H12B 0.9500 . ? C13B O13B 1.381(7) . ? O13B H13B 0.87(6) . ? C14B C32B 1.525(8) . ? C14B C15B 1.536(9) . ? C14B H14B 1.0000 . ? C15B C16B 1.387(8) . ? C15B C20B 1.400(8) . ? C16B C17B 1.399(8) . ? C16B H16B 0.9500 . ? C17B C18B 1.387(8) . ? C17B C21B 1.527(8) . ? C18B O18B 1.386(8) . ? C18B C19B 1.396(8) . ? O18B H18B 0.78(6) . ? C19B C20B 1.365(9) . ? C19B H19B 0.9500 . ? C20B O20B 1.382(7) . ? O20B H20B 0.72(7) . ? C21B C22B 1.524(8) . ? C21B C35B 1.530(9) . ? C21B H21B 1.0000 . ? C22B C27B 1.381(9) . ? C22B C23B 1.405(8) . ? C23B C24B 1.402(8) . ? C23B H23B 0.9500 . ? C24B C25B 1.389(9) . ? C24B C28B 1.527(8) . ? C25B O25B 1.375(7) . ? C25B C26B 1.390(8) . ? O25B H25 0.8400 . ? C26B C27B 1.376(9) . ? C26B H26B 0.9500 . ? C27B O27B 1.386(8) . ? O27B H27B 0.63(8) . ? C28B C38B 1.518(8) . ? C28B H28B 1.0000 . ? C29B C30B 1.522(7) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C30B C31B 1.503(9) . ? C30B H30C 0.9900 . ? C30B H30D 0.9900 . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? C32B C33B 1.518(8) . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C33B C34B 1.507(9) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? C35B C36B 1.512(9) . ? C35B H35C 0.9900 . ? C35B H35D 0.9900 . ? C36B C37B 1.513(10) . ? C36B H36C 0.9900 . ? C36B H36D 0.9900 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? C38B C39B 1.515(7) . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? C39B C40B 1.518(9) . ? C39B H39C 0.9900 . ? C39B H39D 0.9900 . ? C40B H40D 0.9800 . ? C40B H40E 0.9800 . ? C40B H40F 0.9800 . ? N1C C1C 1.498(8) . ? N1C C3C 1.513(7) . ? N1C C5C 1.517(7) . ? N1C C7C 1.526(7) . ? N2C C4C 1.498(7) . ? N2C C6C 1.502(7) . ? N2C C2C 1.503(7) . ? N2C C14C 1.536(7) . ? C1C C2C 1.533(8) . ? C1C H1C1 0.9900 . ? C1C H1C2 0.9900 . ? C2C H2C1 0.9900 . ? C2C H2C2 0.9900 . ? C3C C4C 1.526(8) . ? C3C H3C1 0.9900 . ? C3C H3C2 0.9900 . ? C4C H4C1 0.9900 . ? C4C H4C2 0.9900 . ? C5C C6C 1.522(8) . ? C5C H5C1 0.9900 . ? C5C H5C2 0.9900 . ? C6C H6C1 0.9900 . ? C6C H6C2 0.9900 . ? C7C C8C 1.509(8) . ? C7C H7C1 0.9900 . ? C7C H7C2 0.9900 . ? C8C C13C 1.365(8) . ? C8C C9C 1.395(9) . ? C9C C10C 1.389(8) . ? C9C H9C 0.9500 . ? C10C C11C 1.388(9) . ? C10C H10C 0.9500 . ? C11C C12C 1.375(9) . ? C11C H11C 0.9500 . ? C12C C13C 1.388(8) . ? C12C H12C 0.9500 . ? C13C H13C 0.9500 . ? C14C C15C 1.495(9) . ? C14C H14A 0.9900 . ? C14C H14B 0.9900 . ? C15C C20C 1.342(8) . ? C15C C16C 1.376(9) . ? C16C C17C 1.372(10) . ? C16C H16C 0.9500 . ? C17C C18C 1.381(11) . ? C17C H17C 0.9500 . ? C18C C19C 1.378(11) . ? C18C H18C 0.9500 . ? C19C C20C 1.395(9) . ? C19C H19C 0.9500 . ? C20C H20C 0.9500 . ? N1E C2E 1.4257 . ? N1E C3E 1.4476 . ? N1E C4E 1.5891 . ? N1E C1E 1.596(9) 2_575 ? C3E C2E 1.696(10) 2_575 ? C4E C8E 1.383(8) . ? C1E N1E 1.596(9) 2_575 ? C2E C3E 1.696(10) 2_575 ? C8E C9E 1.3900 . ? C8E C13E 1.3900 . ? C9E C10E 1.3900 . ? C10E C11E 1.3900 . ? C11E C12E 1.3900 . ? C12E C13E 1.3900 . ? N1G C2G 1.490(17) . ? N1G C1G 1.518(16) . ? N1G C4G 1.559(18) . ? N1G C3G 1.63(2) . ? C2G C3G 1.76(2) 2_575 ? C3G C2G 1.76(2) 2_575 ? C4G C8G 1.508(16) . ? C8G C9G 1.3900 . ? C8G C13G 1.3900 . ? C9G C10G 1.3900 . ? C10G C11G 1.3900 . ? C11G C12G 1.3900 . ? C12G C13G 1.3900 . ? O1M C2M 1.402(8) . ? O1M H1M 0.83(8) . ? C2M H2M1 0.9800 . ? C2M H2M2 0.9800 . ? C2M H2M3 0.9800 . ? O3M C4M 1.422(7) . ? O3M H3M 1.04(7) . ? C4M H4M1 0.9800 . ? C4M H4M2 0.9800 . ? C4M H4M3 0.9800 . ? C6M O5M 1.385(8) . ? C6M H6M1 0.9800 . ? C6M H6M2 0.9800 . ? C6M H6M3 0.9800 . ? O5M H5M 0.8400 . ? C8M O7M 1.390(9) . ? C8M H8M1 0.9800 . ? C8M H8M2 0.9800 . ? C8M H8M3 0.9800 . ? O7M H7M 0.84(2) . ? O9M C10M 1.384(9) . ? O9M H9M 0.75(9) . ? C10M H10A 0.9800 . ? C10M H10B 0.9800 . ? C10M H10D 0.9800 . ? O11M C12M 1.384(9) . ? O11M H11M 0.8400 . ? C12M H12A 0.9800 . ? C12M H12B 0.9800 . ? C12M H12D 0.9800 . ? O13M C14M 1.383(8) . ? O13M H13M 0.95(9) . ? C14M H14C 0.9800 . ? C14M H14D 0.9800 . ? C14M H14E 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 C2 C1 C6 116.5(5) . . ? C2 C1 C28 123.4(6) . . ? C6 C1 C28 120.1(5) . . ? C1 C2 C3 125.0(6) . . ? C1 C2 H2 117.5 . . ? C3 C2 H2 117.5 . . ? C4 C3 C2 116.3(5) . . ? C4 C3 C7 121.6(5) . . ? C2 C3 C7 122.0(5) . . ? C3 C4 O4 123.9(5) . . ? C3 C4 C5 121.1(5) . . ? O4 C4 C5 114.9(5) . . ? C4 O4 H4 109.5 . . ? C4 C5 C6 120.3(6) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? O6 C6 C5 115.1(6) . . ? O6 C6 C1 124.1(5) . . ? C5 C6 C1 120.6(6) . . ? C6 O6 H6 114(6) . . ? C29 C7 C8 112.7(5) . . ? C29 C7 C3 113.8(5) . . ? C8 C7 C3 110.8(5) . . ? C29 C7 H7 106.3 . . ? C8 C7 H7 106.3 . . ? C3 C7 H7 106.3 . . ? C13 C8 C9 116.6(6) . . ? C13 C8 C7 122.4(6) . . ? C9 C8 C7 121.0(5) . . ? C10 C9 C8 124.2(5) . . ? C10 C9 H9A 106.3 . . ? C8 C9 H9A 106.3 . . ? C10 C9 H9B 106.3 . . ? C8 C9 H9B 106.3 . . ? H9A C9 H9B 106.4 . . ? C9 C10 C11 117.6(6) . . ? C9 C10 C14 120.8(5) . . ? C11 C10 C14 121.6(6) . . ? O11 C11 C12 115.9(5) . . ? O11 C11 C10 124.0(6) . . ? C12 C11 C10 120.1(6) . . ? C11 O11 H11 109.5 . . ? C11 C12 C13 120.7(6) . . ? C11 C12 H12A 107.2 . . ? C13 C12 H12A 107.2 . . ? C11 C12 H12B 107.2 . . ? C13 C12 H12B 107.2 . . ? H12A C12 H12B 106.8 . . ? O13 C13 C8 117.4(6) . . ? O13 C13 C12 121.9(5) . . ? C8 C13 C12 120.7(6) . . ? C13 O13 H13 106(5) . . ? C32 C14 C15 113.0(5) . . ? C32 C14 C10 111.2(5) . . ? C15 C14 C10 110.7(5) . . ? C20 C15 C16 115.6(6) . . ? C20 C15 C14 120.0(5) . . ? C16 C15 C14 124.5(6) . . ? C17 C16 C15 124.2(6) . . ? C17 C16 H16 117.9 . . ? C15 C16 H16 117.9 . . ? C16 C17 C18 117.1(6) . . ? C16 C17 C21 123.9(6) . . ? C18 C17 C21 118.9(6) . . ? O18 C18 C17 117.8(5) . . ? O18 C18 C19 120.6(6) . . ? C17 C18 C19 121.7(6) . . ? C18 O18 H18 116(6) . . ? C20 C19 C18 117.9(6) . . ? C20 C19 H19 121.0 . . ? C18 C19 H19 121.0 . . ? C19 C20 C15 123.5(6) . . ? C19 C20 O20 120.0(6) . . ? C15 C20 O20 116.5(6) . . ? C20 O20 H20 116(5) . . ? C22 C21 C35 111.8(5) . . ? C22 C21 C17 111.8(4) . . ? C35 C21 C17 112.8(5) . . ? C22 C21 H21 106.7 . . ? C35 C21 H21 106.7 . . ? C17 C21 H21 106.7 . . ? C27 C22 C23 115.8(6) . . ? C27 C22 C21 124.2(6) . . ? C23 C22 C21 119.8(5) . . ? C24 C23 C22 125.1(6) . . ? C24 C23 H23 117.4 . . ? C22 C23 H23 117.4 . . ? C23 C24 C25 116.7(6) . . ? C23 C24 C28 121.7(6) . . ? C25 C24 C28 121.5(6) . . ? O25 C25 C26 122.7(6) . . ? O25 C25 C24 116.7(6) . . ? C26 C25 C24 120.5(6) . . ? C25 O25 H25 110(4) . . ? C27 C26 C25 120.3(6) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? O27 C27 C26 119.0(6) . . ? O27 C27 C22 119.5(6) . . ? C26 C27 C22 121.6(6) . . ? C27 O27 H27 114(7) . . ? C24 C28 C1 111.2(5) . . ? C24 C28 C38 112.0(5) . . ? C1 C28 C38 113.6(5) . . ? C24 C28 H28 106.5 . . ? C1 C28 H28 106.5 . . ? C38 C28 H28 106.5 . . ? C7 C29 C30 113.1(5) . . ? C7 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? C7 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C31 C30 C29 113.1(5) . . ? 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 . . ? C33 C32 C14 112.1(5) . . ? C33 C32 H32A 109.2 . . ? C14 C32 H32A 109.2 . . ? C33 C32 H32B 109.2 . . ? C14 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C34 112.7(5) . . ? C32 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? C32 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? 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 C21 113.2(5) . . ? C36 C35 H35A 108.9 . . ? C21 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C21 C35 H35B 108.9 . . ? H35A C35 H35B 107.8 . . ? C37 C36 C35 112.9(6) . . ? C37 C36 H36A 109.0 . . ? C35 C36 H36A 109.0 . . ? C37 C36 H36B 109.0 . . ? C35 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C28 112.0(5) . . ? C39 C38 H38A 109.2 . . ? C28 C38 H38A 109.2 . . ? C39 C38 H38B 109.2 . . ? C28 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C38 C39 C40 113.3(6) . . ? C38 C39 H39A 108.9 . . ? C40 C39 H39A 108.9 . . ? C38 C39 H39B 108.9 . . ? C40 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C2B C1B C6B 117.9(6) . . ? C2B C1B C28B 120.6(6) . . ? C6B C1B C28B 121.5(6) . . ? C1B C2B C3B 123.3(6) . . ? C1B C2B H2B 118.4 . . ? C3B C2B H2B 118.4 . . ? C4B C3B C2B 117.5(6) . . ? C4B C3B C7B 122.0(6) . . ? C2B C3B C7B 120.5(5) . . ? O4B C4B C3B 117.5(6) . . ? O4B C4B C5B 121.2(6) . . ? C3B C4B C5B 121.4(6) . . ? C4B O4B H4B 115(5) . . ? C4B C5B C6B 119.1(6) . . ? C4B C5B H5B 120.4 . . ? C6B C5B H5B 120.4 . . ? O6B C6B C1B 118.3(6) . . ? O6B C6B C5B 120.9(6) . . ? C1B C6B C5B 120.7(6) . . ? C6B O6B H6B 108(5) . . ? C8B C7B C29B 114.7(5) . . ? C8B C7B C3B 110.9(5) . . ? C29B C7B C3B 109.9(5) . . ? C8B C7B H7B 107.0 . . ? C29B C7B H7B 107.0 . . ? C3B C7B H7B 107.0 . . ? C13B C8B C9B 116.2(5) . . ? C13B C8B C7B 121.8(5) . . ? C9B C8B C7B 122.0(6) . . ? C10B C9B C8B 124.1(6) . . ? C10B C9B H9B 117.9 . . ? C8B C9B H9B 117.9 . . ? C11B C10B C9B 116.0(6) . . ? C11B C10B C14B 120.7(5) . . ? C9B C10B C14B 123.2(6) . . ? C10B C11B C12B 122.4(6) . . ? C10B C11B O11B 117.1(6) . . ? C12B C11B O11B 120.5(6) . . ? C11B O11B H11B 107(7) . . ? C13B C12B C11B 119.1(6) . . ? C13B C12B H12B 120.4 . . ? C11B C12B H12B 120.4 . . ? C12B C13B C8B 122.1(6) . . ? C12B C13B O13B 115.5(6) . . ? C8B C13B O13B 122.5(5) . . ? C13B O13B H13B 106(4) . . ? C10B C14B C32B 114.6(5) . . ? C10B C14B C15B 111.7(5) . . ? C32B C14B C15B 111.6(5) . . ? C10B C14B H14B 106.1 . . ? C32B C14B H14B 106.1 . . ? C15B C14B H14B 106.1 . . ? C16B C15B C20B 116.8(6) . . ? C16B C15B C14B 120.1(5) . . ? C20B C15B C14B 123.1(6) . . ? C15B C16B C17B 124.0(5) . . ? C15B C16B H16B 118.0 . . ? C17B C16B H16B 118.0 . . ? C18B C17B C16B 116.2(6) . . ? C18B C17B C21B 122.8(6) . . ? C16B C17B C21B 121.0(5) . . ? C17B C18B O18B 116.6(6) . . ? C17B C18B C19B 121.5(6) . . ? O18B C18B C19B 121.7(5) . . ? C18B O18B H18B 118(5) . . ? C20B C19B C18B 120.0(6) . . ? C20B C19B H19B 120.0 . . ? C18B C19B H19B 120.0 . . ? C19B C20B O20B 116.8(5) . . ? C19B C20B C15B 121.2(6) . . ? O20B C20B C15B 121.9(6) . . ? C20B O20B H20B 116(6) . . ? C22B C21B C17B 111.1(5) . . ? C22B C21B C35B 115.3(5) . . ? C17B C21B C35B 111.8(6) . . ? C22B C21B H21B 106.0 . . ? C17B C21B H21B 106.0 . . ? C35B C21B H21B 106.0 . . ? C27B C22B C23B 116.6(6) . . ? C27B C22B C21B 121.4(5) . . ? C23B C22B C21B 121.9(6) . . ? C24B C23B C22B 123.7(6) . . ? C24B C23B H23B 118.1 . . ? C22B C23B H23B 118.1 . . ? C25B C24B C23B 116.5(6) . . ? C25B C24B C28B 121.3(6) . . ? C23B C24B C28B 122.1(6) . . ? O25B C25B C24B 123.0(5) . . ? O25B C25B C26B 115.9(6) . . ? C24B C25B C26B 121.1(6) . . ? C25B O25B H25 109.5 . . ? C27B C26B C25B 120.4(6) . . ? C27B C26B H26B 119.8 . . ? C25B C26B H26B 119.8 . . ? C26B C27B C22B 121.6(6) . . ? C26B C27B O27B 115.1(6) . . ? C22B C27B O27B 123.3(6) . . ? C27B O27B H27B 110(9) . . ? C1B C28B C38B 111.9(5) . . ? C1B C28B C24B 109.1(4) . . ? C38B C28B C24B 114.5(5) . . ? C1B C28B H28B 107.0 . . ? C38B C28B H28B 107.0 . . ? C24B C28B H28B 107.0 . . ? C30B C29B C7B 113.0(5) . . ? C30B C29B H29C 109.0 . . ? C7B C29B H29C 109.0 . . ? C30B C29B H29D 109.0 . . ? C7B C29B H29D 109.0 . . ? H29C C29B H29D 107.8 . . ? C31B C30B C29B 112.2(5) . . ? C31B C30B H30C 109.2 . . ? C29B C30B H30C 109.2 . . ? C31B C30B H30D 109.2 . . ? C29B C30B H30D 109.2 . . ? H30C C30B H30D 107.9 . . ? C30B C31B H31D 109.5 . . ? C30B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C30B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C33B C32B C14B 113.2(5) . . ? C33B C32B H32C 108.9 . . ? C14B C32B H32C 108.9 . . ? C33B C32B H32D 108.9 . . ? C14B C32B H32D 108.9 . . ? H32C C32B H32D 107.8 . . ? C34B C33B C32B 113.4(6) . . ? C34B C33B H33C 108.9 . . ? C32B C33B H33C 108.9 . . ? C34B C33B H33D 108.9 . . ? C32B C33B H33D 108.9 . . ? H33C C33B H33D 107.7 . . ? C33B C34B H34D 109.5 . . ? C33B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C33B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C36B C35B C21B 112.9(5) . . ? C36B C35B H35C 109.0 . . ? C21B C35B H35C 109.0 . . ? C36B C35B H35D 109.0 . . ? C21B C35B H35D 109.0 . . ? H35C C35B H35D 107.8 . . ? C35B C36B C37B 112.9(6) . . ? C35B C36B H36C 109.0 . . ? C37B C36B H36C 109.0 . . ? C35B C36B H36D 109.0 . . ? C37B C36B H36D 109.0 . . ? H36C C36B H36D 107.8 . . ? C36B C37B H37D 109.5 . . ? C36B C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? C36B C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? C39B C38B C28B 113.8(5) . . ? C39B C38B H38C 108.8 . . ? C28B C38B H38C 108.8 . . ? C39B C38B H38D 108.8 . . ? C28B C38B H38D 108.8 . . ? H38C C38B H38D 107.7 . . ? C38B C39B C40B 113.4(5) . . ? C38B C39B H39C 108.9 . . ? C40B C39B H39C 108.9 . . ? C38B C39B H39D 108.9 . . ? C40B C39B H39D 108.9 . . ? H39C C39B H39D 107.7 . . ? C39B C40B H40D 109.5 . . ? C39B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C39B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C1C N1C C3C 108.8(4) . . ? C1C N1C C5C 107.6(5) . . ? C3C N1C C5C 107.4(4) . . ? C1C N1C C7C 111.9(4) . . ? C3C N1C C7C 109.3(4) . . ? C5C N1C C7C 111.7(4) . . ? C4C N2C C6C 108.4(5) . . ? C4C N2C C2C 108.6(5) . . ? C6C N2C C2C 107.9(4) . . ? C4C N2C C14C 108.9(4) . . ? C6C N2C C14C 111.7(5) . . ? C2C N2C C14C 111.2(5) . . ? N1C C1C C2C 110.0(5) . . ? N1C C1C H1C1 109.7 . . ? C2C C1C H1C1 109.7 . . ? N1C C1C H1C2 109.7 . . ? C2C C1C H1C2 109.7 . . ? H1C1 C1C H1C2 108.2 . . ? N2C C2C C1C 108.8(5) . . ? N2C C2C H2C1 109.9 . . ? C1C C2C H2C1 109.9 . . ? N2C C2C H2C2 109.9 . . ? C1C C2C H2C2 109.9 . . ? H2C1 C2C H2C2 108.3 . . ? N1C C3C C4C 108.9(5) . . ? N1C C3C H3C1 109.9 . . ? C4C C3C H3C1 109.9 . . ? N1C C3C H3C2 109.9 . . ? C4C C3C H3C2 109.9 . . ? H3C1 C3C H3C2 108.3 . . ? N2C C4C C3C 109.9(4) . . ? N2C C4C H4C1 109.7 . . ? C3C C4C H4C1 109.7 . . ? N2C C4C H4C2 109.7 . . ? C3C C4C H4C2 109.7 . . ? H4C1 C4C H4C2 108.2 . . ? N1C C5C C6C 109.5(4) . . ? N1C C5C H5C1 109.8 . . ? C6C C5C H5C1 109.8 . . ? N1C C5C H5C2 109.8 . . ? C6C C5C H5C2 109.8 . . ? H5C1 C5C H5C2 108.2 . . ? N2C C6C C5C 109.6(5) . . ? N2C C6C H6C1 109.7 . . ? C5C C6C H6C1 109.7 . . ? N2C C6C H6C2 109.7 . . ? C5C C6C H6C2 109.7 . . ? H6C1 C6C H6C2 108.2 . . ? C8C C7C N1C 112.8(5) . . ? C8C C7C H7C1 109.0 . . ? N1C C7C H7C1 109.0 . . ? C8C C7C H7C2 109.0 . . ? N1C C7C H7C2 109.0 . . ? H7C1 C7C H7C2 107.8 . . ? C13C C8C C9C 119.8(6) . . ? C13C C8C C7C 120.1(6) . . ? C9C C8C C7C 120.1(6) . . ? C10C C9C C8C 120.5(6) . . ? C10C C9C H9C 119.8 . . ? C8C C9C H9C 119.8 . . ? C11C C10C C9C 118.8(7) . . ? C11C C10C H10C 120.6 . . ? C9C C10C H10C 120.6 . . ? C12C C11C C10C 120.5(6) . . ? C12C C11C H11C 119.7 . . ? C10C C11C H11C 119.7 . . ? C11C C12C C13C 120.2(6) . . ? C11C C12C H12C 119.9 . . ? C13C C12C H12C 119.9 . . ? C8C C13C C12C 120.1(7) . . ? C8C C13C H13C 119.9 . . ? C12C C13C H13C 119.9 . . ? C15C C14C N2C 111.9(5) . . ? C15C C14C H14A 109.2 . . ? N2C C14C H14A 109.2 . . ? C15C C14C H14B 109.2 . . ? N2C C14C H14B 109.2 . . ? H14A C14C H14B 107.9 . . ? C20C C15C C16C 118.0(7) . . ? C20C C15C C14C 118.8(6) . . ? C16C C15C C14C 123.2(6) . . ? C17C C16C C15C 121.7(7) . . ? C17C C16C H16C 119.2 . . ? C15C C16C H16C 119.2 . . ? C16C C17C C18C 120.1(8) . . ? C16C C17C H17C 119.9 . . ? C18C C17C H17C 119.9 . . ? C19C C18C C17C 118.4(8) . . ? C19C C18C H18C 120.8 . . ? C17C C18C H18C 120.8 . . ? C18C C19C C20C 119.9(7) . . ? C18C C19C H19C 120.1 . . ? C20C C19C H19C 120.1 . . ? C15C C20C C19C 121.7(6) . . ? C15C C20C H20C 119.1 . . ? C19C C20C H20C 119.1 . . ? C2E N1E C3E 115.9 . . ? C2E N1E C4E 112.6 . . ? C3E N1E C4E 108.9 . . ? C2E N1E C1E 106.8(4) . 2_575 ? C3E N1E C1E 105.7(4) . 2_575 ? C4E N1E C1E 106.3(3) . 2_575 ? N1E C3E C2E 81.2(3) . 2_575 ? C8E C4E N1E 114.4(5) . . ? N1E C2E C3E 111.8(3) . 2_575 ? C4E C8E C9E 118.1(8) . . ? C4E C8E C13E 121.9(8) . . ? C9E C8E C13E 120.0 . . ? C10E C9E C8E 120.0 . . ? C9E C10E C11E 120.0 . . ? C12E C11E C10E 120.0 . . ? C11E C12E C13E 120.0 . . ? C12E C13E C8E 120.0 . . ? C2G N1G C1G 105.3(11) . . ? C2G N1G C4G 107.8(10) . . ? C1G N1G C4G 111.1(11) . . ? C2G N1G C3G 106.6(12) . . ? C1G N1G C3G 109.3(11) . . ? C4G N1G C3G 116.0(12) . . ? N1G C2G C3G 97.0(11) . 2_575 ? N1G C3G C2G 103.5(11) . 2_575 ? C8G C4G N1G 113.0(11) . . ? C9G C8G C13G 120.0 . . ? C9G C8G C4G 113.2(9) . . ? C13G C8G C4G 126.6(9) . . ? C10G C9G C8G 120.0 . . ? C9G C10G C11G 120.0 . . ? C12G C11G C10G 120.0 . . ? C11G C12G C13G 120.0 . . ? C12G C13G C8G 120.0 . . ? C2M O1M H1M 112(6) . . ? O1M C2M H2M1 109.5 . . ? O1M C2M H2M2 109.5 . . ? H2M1 C2M H2M2 109.5 . . ? O1M C2M H2M3 109.5 . . ? H2M1 C2M H2M3 109.5 . . ? H2M2 C2M H2M3 109.5 . . ? C4M O3M H3M 104(4) . . ? O3M C4M H4M1 109.5 . . ? O3M C4M H4M2 109.5 . . ? H4M1 C4M H4M2 109.5 . . ? O3M C4M H4M3 109.5 . . ? H4M1 C4M H4M3 109.5 . . ? H4M2 C4M H4M3 109.5 . . ? O5M C6M H6M1 109.5 . . ? O5M C6M H6M2 109.5 . . ? H6M1 C6M H6M2 109.5 . . ? O5M C6M H6M3 109.5 . . ? H6M1 C6M H6M3 109.5 . . ? H6M2 C6M H6M3 109.5 . . ? C6M O5M H5M 109.5 . . ? O7M C8M H8M1 109.5 . . ? O7M C8M H8M2 109.5 . . ? H8M1 C8M H8M2 109.5 . . ? O7M C8M H8M3 109.5 . . ? H8M1 C8M H8M3 109.5 . . ? H8M2 C8M H8M3 109.5 . . ? C8M O7M H7M 115(6) . . ? C10M O9M H9M 113(8) . . ? O9M C10M H10A 109.5 . . ? O9M C10M H10B 109.5 . . ? H10A C10M H10B 109.5 . . ? O9M C10M H10D 109.5 . . ? H10A C10M H10D 109.5 . . ? H10B C10M H10D 109.5 . . ? C12M O11M H11M 109.5 . . ? O11M C12M H12A 109.5 . . ? O11M C12M H12B 109.5 . . ? H12A C12M H12B 109.5 . . ? O11M C12M H12D 109.5 . . ? H12A C12M H12D 109.5 . . ? H12B C12M H12D 109.5 . . ? C14M O13M H13M 110(5) . . ? O13M C14M H14C 109.5 . . ? O13M C14M H14D 109.5 . . ? H14C C14M H14D 109.5 . . ? O13M C14M H14E 109.5 . . ? H14C C14M H14E 109.5 . . ? H14D C14M H14E 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 C6 C1 C2 C3 1.0(9) . . . . ? C28 C1 C2 C3 -177.7(6) . . . . ? C1 C2 C3 C4 0.0(9) . . . . ? C1 C2 C3 C7 177.9(6) . . . . ? C2 C3 C4 O4 176.6(6) . . . . ? C7 C3 C4 O4 -1.4(9) . . . . ? C2 C3 C4 C5 -2.5(9) . . . . ? C7 C3 C4 C5 179.6(6) . . . . ? C3 C4 C5 C6 4.0(10) . . . . ? O4 C4 C5 C6 -175.2(5) . . . . ? C4 C5 C6 O6 173.8(6) . . . . ? C4 C5 C6 C1 -2.9(9) . . . . ? C2 C1 C6 O6 -175.9(6) . . . . ? C28 C1 C6 O6 2.9(9) . . . . ? C2 C1 C6 C5 0.4(9) . . . . ? C28 C1 C6 C5 179.2(6) . . . . ? C4 C3 C7 C29 -153.5(6) . . . . ? C2 C3 C7 C29 28.6(8) . . . . ? C4 C3 C7 C8 78.2(7) . . . . ? C2 C3 C7 C8 -99.6(7) . . . . ? C29 C7 C8 C13 126.2(6) . . . . ? C3 C7 C8 C13 -104.9(6) . . . . ? C29 C7 C8 C9 -55.6(8) . . . . ? C3 C7 C8 C9 73.3(7) . . . . ? C13 C8 C9 C10 -4.2(9) . . . . ? C7 C8 C9 C10 177.5(6) . . . . ? C8 C9 C10 C11 3.1(9) . . . . ? C8 C9 C10 C14 -175.3(6) . . . . ? C9 C10 C11 O11 179.9(6) . . . . ? C14 C10 C11 O11 -1.6(9) . . . . ? C9 C10 C11 C12 -2.0(9) . . . . ? C14 C10 C11 C12 176.4(6) . . . . ? O11 C11 C12 C13 -179.5(6) . . . . ? C10 C11 C12 C13 2.3(10) . . . . ? C9 C8 C13 O13 -176.1(5) . . . . ? C7 C8 C13 O13 2.2(9) . . . . ? C9 C8 C13 C12 4.2(9) . . . . ? C7 C8 C13 C12 -177.5(6) . . . . ? C11 C12 C13 O13 176.8(6) . . . . ? C11 C12 C13 C8 -3.4(10) . . . . ? C9 C10 C14 C32 49.2(7) . . . . ? C11 C10 C14 C32 -129.2(6) . . . . ? C9 C10 C14 C15 -77.4(7) . . . . ? C11 C10 C14 C15 104.2(6) . . . . ? C32 C14 C15 C20 153.3(6) . . . . ? C10 C14 C15 C20 -81.2(7) . . . . ? C32 C14 C15 C16 -26.6(8) . . . . ? C10 C14 C15 C16 98.9(7) . . . . ? C20 C15 C16 C17 0.0(9) . . . . ? C14 C15 C16 C17 179.8(6) . . . . ? C15 C16 C17 C18 0.6(9) . . . . ? C15 C16 C17 C21 -179.2(6) . . . . ? C16 C17 C18 O18 179.0(5) . . . . ? C21 C17 C18 O18 -1.1(8) . . . . ? C16 C17 C18 C19 -0.9(9) . . . . ? C21 C17 C18 C19 179.0(5) . . . . ? O18 C18 C19 C20 -179.3(6) . . . . ? C17 C18 C19 C20 0.6(9) . . . . ? C18 C19 C20 C15 0.0(10) . . . . ? C18 C19 C20 O20 -180.0(5) . . . . ? C16 C15 C20 C19 -0.3(9) . . . . ? C14 C15 C20 C19 179.8(6) . . . . ? C16 C15 C20 O20 179.7(5) . . . . ? C14 C15 C20 O20 -0.2(9) . . . . ? C16 C17 C21 C22 -95.3(7) . . . . ? C18 C17 C21 C22 84.8(7) . . . . ? C16 C17 C21 C35 31.6(8) . . . . ? C18 C17 C21 C35 -148.2(6) . . . . ? C35 C21 C22 C27 117.1(6) . . . . ? C17 C21 C22 C27 -115.5(6) . . . . ? C35 C21 C22 C23 -57.5(6) . . . . ? C17 C21 C22 C23 70.0(7) . . . . ? C27 C22 C23 C24 -2.3(8) . . . . ? C21 C22 C23 C24 172.7(5) . . . . ? C22 C23 C24 C25 2.6(8) . . . . ? C22 C23 C24 C28 -174.8(5) . . . . ? C23 C24 C25 O25 177.4(5) . . . . ? C28 C24 C25 O25 -5.2(8) . . . . ? C23 C24 C25 C26 -0.4(8) . . . . ? C28 C24 C25 C26 177.0(5) . . . . ? O25 C25 C26 C27 -179.6(5) . . . . ? C24 C25 C26 C27 -2.0(8) . . . . ? C25 C26 C27 O27 -178.0(5) . . . . ? C25 C26 C27 C22 2.2(9) . . . . ? C23 C22 C27 O27 -179.9(5) . . . . ? C21 C22 C27 O27 5.3(9) . . . . ? C23 C22 C27 C26 -0.2(8) . . . . ? C21 C22 C27 C26 -174.9(5) . . . . ? C23 C24 C28 C1 -74.8(7) . . . . ? C25 C24 C28 C1 107.9(6) . . . . ? C23 C24 C28 C38 53.5(7) . . . . ? C25 C24 C28 C38 -123.8(6) . . . . ? C2 C1 C28 C24 105.2(7) . . . . ? C6 C1 C28 C24 -73.4(7) . . . . ? C2 C1 C28 C38 -22.2(9) . . . . ? C6 C1 C28 C38 159.2(6) . . . . ? C8 C7 C29 C30 -63.3(7) . . . . ? C3 C7 C29 C30 169.5(5) . . . . ? C7 C29 C30 C31 176.6(6) . . . . ? C15 C14 C32 C33 -173.7(6) . . . . ? C10 C14 C32 C33 61.0(7) . . . . ? C14 C32 C33 C34 -177.4(7) . . . . ? C22 C21 C35 C36 -60.9(7) . . . . ? C17 C21 C35 C36 172.1(5) . . . . ? C21 C35 C36 C37 179.5(6) . . . . ? C24 C28 C38 C39 62.5(7) . . . . ? C1 C28 C38 C39 -170.5(5) . . . . ? C28 C38 C39 C40 -176.1(6) . . . . ? C6B C1B C2B C3B 3.1(8) . . . . ? C28B C1B C2B C3B -175.0(5) . . . . ? C1B C2B C3B C4B -3.8(8) . . . . ? C1B C2B C3B C7B 174.3(5) . . . . ? C2B C3B C4B O4B -178.4(5) . . . . ? C7B C3B C4B O4B 3.6(8) . . . . ? C2B C3B C4B C5B 1.0(8) . . . . ? C7B C3B C4B C5B -177.0(5) . . . . ? O4B C4B C5B C6B -178.5(5) . . . . ? C3B C4B C5B C6B 2.1(8) . . . . ? C2B C1B C6B O6B 177.6(5) . . . . ? C28B C1B C6B O6B -4.3(8) . . . . ? C2B C1B C6B C5B 0.3(8) . . . . ? C28B C1B C6B C5B 178.4(5) . . . . ? C4B C5B C6B O6B 180.0(5) . . . . ? C4B C5B C6B C1B -2.8(8) . . . . ? C4B C3B C7B C8B -102.4(6) . . . . ? C2B C3B C7B C8B 79.6(7) . . . . ? C4B C3B C7B C29B 129.7(6) . . . . ? C2B C3B C7B C29B -48.3(7) . . . . ? C29B C7B C8B C13B -154.9(6) . . . . ? C3B C7B C8B C13B 79.8(7) . . . . ? C29B C7B C8B C9B 26.8(9) . . . . ? C3B C7B C8B C9B -98.5(7) . . . . ? C13B C8B C9B C10B 0.7(10) . . . . ? C7B C8B C9B C10B 179.1(6) . . . . ? C8B C9B C10B C11B -1.1(10) . . . . ? C8B C9B C10B C14B -179.5(6) . . . . ? C9B C10B C11B C12B 2.4(10) . . . . ? C14B C10B C11B C12B -179.1(6) . . . . ? C9B C10B C11B O11B -175.2(6) . . . . ? C14B C10B C11B O11B 3.2(9) . . . . ? C10B C11B C12B C13B -3.3(11) . . . . ? O11B C11B C12B C13B 174.3(6) . . . . ? C11B C12B C13B C8B 2.8(10) . . . . ? C11B C12B C13B O13B -178.1(6) . . . . ? C9B C8B C13B C12B -1.5(10) . . . . ? C7B C8B C13B C12B -179.9(6) . . . . ? C9B C8B C13B O13B 179.4(6) . . . . ? C7B C8B C13B O13B 1.0(10) . . . . ? C11B C10B C14B C32B 149.3(6) . . . . ? C9B C10B C14B C32B -32.4(9) . . . . ? C11B C10B C14B C15B -82.7(7) . . . . ? C9B C10B C14B C15B 95.6(7) . . . . ? C10B C14B C15B C16B -75.5(7) . . . . ? C32B C14B C15B C16B 54.1(8) . . . . ? C10B C14B C15B C20B 106.5(7) . . . . ? C32B C14B C15B C20B -123.8(6) . . . . ? C20B C15B C16B C17B 3.9(9) . . . . ? C14B C15B C16B C17B -174.1(6) . . . . ? C15B C16B C17B C18B 0.1(10) . . . . ? C15B C16B C17B C21B 178.4(6) . . . . ? C16B C17B C18B O18B -178.1(5) . . . . ? C21B C17B C18B O18B 3.7(9) . . . . ? C16B C17B C18B C19B -2.8(9) . . . . ? C21B C17B C18B C19B 179.0(6) . . . . ? C17B C18B C19B C20B 1.2(10) . . . . ? O18B C18B C19B C20B 176.3(6) . . . . ? C18B C19B C20B O20B 179.9(6) . . . . ? C18B C19B C20B C15B 3.1(10) . . . . ? C16B C15B C20B C19B -5.5(9) . . . . ? C14B C15B C20B C19B 172.5(6) . . . . ? C16B C15B C20B O20B 177.8(6) . . . . ? C14B C15B C20B O20B -4.2(9) . . . . ? C18B C17B C21B C22B -106.7(7) . . . . ? C16B C17B C21B C22B 75.2(8) . . . . ? C18B C17B C21B C35B 123.0(7) . . . . ? C16B C17B C21B C35B -55.1(8) . . . . ? C17B C21B C22B C27B 74.1(8) . . . . ? C35B C21B C22B C27B -157.4(6) . . . . ? C17B C21B C22B C23B -104.3(7) . . . . ? C35B C21B C22B C23B 24.2(9) . . . . ? C27B C22B C23B C24B 0.7(9) . . . . ? C21B C22B C23B C24B 179.2(6) . . . . ? C22B C23B C24B C25B 0.7(9) . . . . ? C22B C23B C24B C28B -176.3(6) . . . . ? C23B C24B C25B O25B 180.0(5) . . . . ? C28B C24B C25B O25B -3.0(9) . . . . ? C23B C24B C25B C26B -0.7(9) . . . . ? C28B C24B C25B C26B 176.3(6) . . . . ? O25B C25B C26B C27B 178.6(6) . . . . ? C24B C25B C26B C27B -0.8(10) . . . . ? C25B C26B C27B C22B 2.4(10) . . . . ? C25B C26B C27B O27B -177.9(6) . . . . ? C23B C22B C27B C26B -2.3(9) . . . . ? C21B C22B C27B C26B 179.2(6) . . . . ? C23B C22B C27B O27B 178.0(6) . . . . ? C21B C22B C27B O27B -0.5(10) . . . . ? C2B C1B C28B C38B 51.9(7) . . . . ? C6B C1B C28B C38B -126.2(6) . . . . ? C2B C1B C28B C24B -75.9(7) . . . . ? C6B C1B C28B C24B 106.0(6) . . . . ? C25B C24B C28B C1B -77.5(7) . . . . ? C23B C24B C28B C1B 99.4(7) . . . . ? C25B C24B C28B C38B 156.2(6) . . . . ? C23B C24B C28B C38B -27.0(8) . . . . ? C8B C7B C29B C30B 170.5(5) . . . . ? C3B C7B C29B C30B -63.8(7) . . . . ? C7B C29B C30B C31B 166.0(6) . . . . ? C10B C14B C32B C33B -168.1(6) . . . . ? C15B C14B C32B C33B 63.8(7) . . . . ? C14B C32B C33B C34B -177.6(7) . . . . ? C22B C21B C35B C36B 169.3(6) . . . . ? C17B C21B C35B C36B -62.5(8) . . . . ? C21B C35B C36B C37B -179.9(7) . . . . ? C1B C28B C38B C39B 63.9(7) . . . . ? C24B C28B C38B C39B -171.3(5) . . . . ? C28B C38B C39B C40B -174.4(6) . . . . ? C3C N1C C1C C2C -68.5(6) . . . . ? C5C N1C C1C C2C 47.6(6) . . . . ? C7C N1C C1C C2C 170.6(5) . . . . ? C4C N2C C2C C1C 47.7(6) . . . . ? C6C N2C C2C C1C -69.7(6) . . . . ? C14C N2C C2C C1C 167.5(5) . . . . ? N1C C1C C2C N2C 18.3(6) . . . . ? C1C N1C C3C C4C 46.6(6) . . . . ? C5C N1C C3C C4C -69.6(6) . . . . ? C7C N1C C3C C4C 169.0(5) . . . . ? C6C N2C C4C C3C 47.2(6) . . . . ? C2C N2C C4C C3C -69.8(6) . . . . ? C14C N2C C4C C3C 169.0(5) . . . . ? N1C C3C C4C N2C 19.3(7) . . . . ? C1C N1C C5C C6C -68.8(6) . . . . ? C3C N1C C5C C6C 48.2(6) . . . . ? C7C N1C C5C C6C 168.0(5) . . . . ? C4C N2C C6C C5C -68.9(6) . . . . ? C2C N2C C6C C5C 48.6(6) . . . . ? C14C N2C C6C C5C 171.1(5) . . . . ? N1C C5C C6C N2C 17.9(7) . . . . ? C1C N1C C7C C8C -63.1(6) . . . . ? C3C N1C C7C C8C 176.3(5) . . . . ? C5C N1C C7C C8C 57.6(7) . . . . ? N1C C7C C8C C13C -92.9(7) . . . . ? N1C C7C C8C C9C 86.7(7) . . . . ? C13C C8C C9C C10C 2.3(10) . . . . ? C7C C8C C9C C10C -177.3(6) . . . . ? C8C C9C C10C C11C -2.3(10) . . . . ? C9C C10C C11C C12C 1.2(10) . . . . ? C10C C11C C12C C13C -0.2(10) . . . . ? C9C C8C C13C C12C -1.3(10) . . . . ? C7C C8C C13C C12C 178.4(6) . . . . ? C11C C12C C13C C8C 0.2(10) . . . . ? C4C N2C C14C C15C 179.2(5) . . . . ? C6C N2C C14C C15C -61.1(7) . . . . ? C2C N2C C14C C15C 59.5(7) . . . . ? N2C C14C C15C C20C 98.2(6) . . . . ? N2C C14C C15C C16C -84.0(7) . . . . ? C20C C15C C16C C17C -5.5(10) . . . . ? C14C C15C C16C C17C 176.7(6) . . . . ? C15C C16C C17C C18C 3.1(11) . . . . ? C16C C17C C18C C19C -0.3(11) . . . . ? C17C C18C C19C C20C -0.1(11) . . . . ? C16C C15C C20C C19C 5.2(8) . . . . ? C14C C15C C20C C19C -176.9(5) . . . . ? C18C C19C C20C C15C -2.5(10) . . . . ? C2E N1E C3E C2E -69.9(3) . . . 2_575 ? C4E N1E C3E C2E 161.9(3) . . . 2_575 ? C1E N1E C3E C2E 48.2(3) 2_575 . . 2_575 ? C2E N1E C4E C8E -74.2(5) . . . . ? C3E N1E C4E C8E 55.8(5) . . . . ? C1E N1E C4E C8E 169.2(8) 2_575 . . . ? C3E N1E C2E C3E 89.3(3) . . . 2_575 ? C4E N1E C2E C3E -144.4(3) . . . 2_575 ? C1E N1E C2E C3E -28.10(17) 2_575 . . 2_575 ? N1E C4E C8E C9E 89.3(7) . . . . ? N1E C4E C8E C13E -90.9(6) . . . . ? C4E C8E C9E C10E 179.8(9) . . . . ? C13E C8E C9E C10E 0.0 . . . . ? C8E C9E C10E C11E 0.0 . . . . ? C9E C10E C11E C12E 0.0 . . . . ? C10E C11E C12E C13E 0.0 . . . . ? C11E C12E C13E C8E 0.0 . . . . ? C4E C8E C13E C12E -179.8(10) . . . . ? C9E C8E C13E C12E 0.0 . . . . ? C1G N1G C2G C3G 42.5(12) . . . 2_575 ? C4G N1G C2G C3G 161.2(11) . . . 2_575 ? C3G N1G C2G C3G -73.6(13) . . . 2_575 ? C2G N1G C3G C2G 78.3(13) . . . 2_575 ? C1G N1G C3G C2G -35.1(14) . . . 2_575 ? C4G N1G C3G C2G -161.6(11) . . . 2_575 ? C2G N1G C4G C8G -169.8(11) . . . . ? C1G N1G C4G C8G -54.8(15) . . . . ? C3G N1G C4G C8G 70.9(15) . . . . ? N1G C4G C8G C9G 102.4(12) . . . . ? N1G C4G C8G C13G -82.7(13) . . . . ? C13G C8G C9G C10G 0.0 . . . . ? C4G C8G C9G C10G 175.3(10) . . . . ? C8G C9G C10G C11G 0.0 . . . . ? C9G C10G C11G C12G 0.0 . . . . ? C10G C11G C12G C13G 0.0 . . . . ? C11G C12G C13G C8G 0.0 . . . . ? C9G C8G C13G C12G 0.0 . . . . ? C4G C8G C13G C12G -174.6(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O18 H18 Br3B 0.72(7) 2.55(7) 3.202(5) 153(8) 2_675 O18 H18 Br3 0.72(7) 2.70(7) 3.320(6) 146(8) 2_675 O4B H4B O5M 0.84(6) 1.77(6) 2.613(6) 174(6) 1_455 O6B H6B O7M 0.81(6) 1.84(7) 2.631(6) 166(7) 1_455 O11B H11B O27 0.67(7) 2.07(7) 2.728(7) 173(10) 2_675 O13M H13M Br2 0.95(9) 2.34(9) 3.272(5) 169(7) 2_765 O13 H13 O13M 0.85(6) 1.86(6) 2.626(6) 150(6) 2_665 O4 H4 O13 0.84 2.09 2.865(6) 154.2 . O6 H6 O25 0.71(6) 2.13(6) 2.799(5) 156(8) . O11 H11 O20 0.84 2.01 2.802(6) 158.1 . O20 H20 Br3B 0.86(7) 2.30(7) 3.150(5) 172(6) . O20 H20 Br3 0.86(7) 2.42(7) 3.233(6) 157(6) . O25 H25 O1M 0.88(6) 1.73(7) 2.596(7) 167(6) . O27 H27 O3M 0.68(7) 2.02(7) 2.671(6) 161(8) . O27 H27 O1W 0.68(7) 2.63(8) 2.963(12) 114(7) . O18B H18B Br1 0.78(6) 2.52(6) 3.276(4) 163(7) . O13B H13B O4B 0.87(6) 1.93(6) 2.772(6) 163(6) . O25B H25 O6B 0.84 2.00 2.826(6) 168.2 . O20B H20B O11B 0.72(7) 2.20(7) 2.859(6) 153(8) . O27B H27B O18B 0.63(8) 2.25(8) 2.838(6) 157(11) . O1M H1M Br2 0.83(8) 2.39(9) 3.214(6) 175(8) . O3M H3M Br2 1.04(7) 2.14(7) 3.177(5) 173(6) . O7M H7M Br1 0.84(2) 2.46(4) 3.254(5) 158(7) . O9M H9M Br1 0.75(9) 2.55(9) 3.280(5) 162(10) . O5M H5M O9M 0.84 1.87 2.670(8) 158.6 . O11M H11M O13B 0.84 2.00 2.823(7) 165.5 . _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 24.08 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.709 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.087 #==END data_Complex7 _database_code_depnum_ccdc_archive 'CCDC 254964' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C72H2112O8*0.5C20H23N2Br2*2.5C2H6O _chemical_formula_sum 'C87 H140 Br N O10.50' _chemical_formula_weight 1447.91 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 9.82460(10) _cell_length_b 15.7155(2) _cell_length_c 26.8439(4) _cell_angle_alpha 91.3870(10) _cell_angle_beta 91.4380(10) _cell_angle_gamma 92.6860(10) _cell_volume 4137.46(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30522 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 21336 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.05 _reflns_number_total 14265 _reflns_number_gt 9062 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELX97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+5.2952P] 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 14265 _refine_ls_number_parameters 1004 _refine_ls_number_restraints 215 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2648(3) 0.4516(2) 0.16874(12) 0.0291(8) Uani 1 1 d . . . C2 C 0.3917(3) 0.4162(2) 0.17185(12) 0.0267(8) Uani 1 1 d . . . H2 H 0.4063 0.3760 0.1971 0.032 Uiso 1 1 calc R . . C3 C 0.4986(3) 0.4357(2) 0.14040(12) 0.0270(8) Uani 1 1 d . . . C4 C 0.4727(4) 0.4920(2) 0.10215(13) 0.0344(9) Uani 1 1 d . . . C5 C 0.3475(4) 0.5288(2) 0.09800(14) 0.0407(9) Uani 1 1 d . . . H5 H 0.3315 0.5674 0.0720 0.049 Uiso 1 1 calc R . . O4 O 0.5674(3) 0.51428(16) 0.06747(10) 0.0484(7) Uani 1 1 d D . . H4 H 0.619(4) 0.474(2) 0.0631(17) 0.073 Uiso 1 1 d D . . C6 C 0.2463(4) 0.5103(2) 0.13090(13) 0.0370(9) Uani 1 1 d . . . O6 O 0.1197(3) 0.54572(18) 0.12779(10) 0.0515(8) Uani 1 1 d D . . H6 H 0.122(5) 0.575(3) 0.1027(12) 0.077 Uiso 1 1 d D . . C7 C 0.6364(3) 0.3956(2) 0.14715(12) 0.0276(8) Uani 1 1 d . . . H7 H 0.7003 0.4264 0.1246 0.033 Uiso 1 1 calc R . . C8 C 0.6271(3) 0.3029(2) 0.12886(12) 0.0248(7) Uani 1 1 d . . . C9 C 0.6096(3) 0.2343(2) 0.16039(12) 0.0236(7) Uani 1 1 d . . . H9 H 0.6028 0.2460 0.1951 0.028 Uiso 1 1 calc R . . C10 C 0.6015(3) 0.1493(2) 0.14371(12) 0.0235(7) Uani 1 1 d . . . C11 C 0.6071(3) 0.1346(2) 0.09241(12) 0.0253(8) Uani 1 1 d . . . O11 O 0.5965(2) 0.05347(14) 0.07041(9) 0.0326(6) Uani 1 1 d D . . H11 H 0.575(4) 0.017(2) 0.0913(12) 0.049 Uiso 1 1 d D . . C12 C 0.6268(3) 0.2005(2) 0.05987(12) 0.0271(8) Uani 1 1 d . . . H12 H 0.6327 0.1889 0.0251 0.032 Uiso 1 1 calc R . . C13 C 0.6379(3) 0.2835(2) 0.07835(12) 0.0259(8) Uani 1 1 d . . . O13 O 0.6614(2) 0.35053(15) 0.04664(9) 0.0336(6) Uani 1 1 d D . . H13 H 0.689(4) 0.330(2) 0.0203(10) 0.050 Uiso 1 1 d D . . C14 C 0.5893(3) 0.0746(2) 0.17841(12) 0.0250(7) Uani 1 1 d . . . H14 H 0.6437 0.0287 0.1635 0.030 Uiso 1 1 calc R . . C15 C 0.4423(3) 0.0390(2) 0.17878(12) 0.0244(7) Uani 1 1 d . . . C16 C 0.3408(3) 0.0837(2) 0.20159(12) 0.0254(7) Uani 1 1 d . . . H16 H 0.3653 0.1380 0.2164 0.030 Uiso 1 1 calc R . . C17 C 0.2059(3) 0.0539(2) 0.20399(12) 0.0265(8) Uani 1 1 d . . . C18 C 0.1708(3) -0.0244(2) 0.18017(13) 0.0337(9) Uani 1 1 d . . . O18 O 0.0354(2) -0.05239(16) 0.18095(10) 0.0444(7) Uani 1 1 d D . . H18 H 0.019(4) -0.0957(19) 0.1630(14) 0.067 Uiso 1 1 d D . . C19 C 0.2670(3) -0.0700(2) 0.15583(14) 0.0360(9) Uani 1 1 d . . . H19 H 0.2413 -0.1228 0.1395 0.043 Uiso 1 1 calc R . . C20 C 0.4010(3) -0.0387(2) 0.15532(13) 0.0324(8) Uani 1 1 d . . . O20 O 0.4991(2) -0.08250(15) 0.13076(10) 0.0423(7) Uani 1 1 d D . . H20 H 0.486(4) -0.1355(13) 0.1301(16) 0.063 Uiso 1 1 d D . . C21 C 0.1022(3) 0.1043(2) 0.23213(12) 0.0284(8) Uani 1 1 d . . . H21 H 0.0167 0.0673 0.2324 0.034 Uiso 1 1 calc R . . C22 C 0.0676(3) 0.1832(2) 0.20383(12) 0.0272(8) Uani 1 1 d . . . C23 C 0.1196(3) 0.2652(2) 0.21694(12) 0.0281(8) Uani 1 1 d . . . H23 H 0.1775 0.2720 0.2458 0.034 Uiso 1 1 calc R . . C24 C 0.0914(3) 0.3372(2) 0.19027(12) 0.0279(8) Uani 1 1 d . . . C25 C 0.0067(3) 0.3249(2) 0.14727(13) 0.0326(9) Uani 1 1 d . . . O25 O -0.0310(3) 0.38973(18) 0.11762(10) 0.0438(7) Uani 1 1 d . . . H25 H 0.016(4) 0.436(3) 0.1255(17) 0.066 Uiso 1 1 d . . . C26 C -0.0464(3) 0.2447(2) 0.13339(13) 0.0322(9) Uani 1 1 d . . . H26 H -0.1039 0.2375 0.1045 0.039 Uiso 1 1 calc R . . C27 C -0.0167(3) 0.1752(2) 0.16095(13) 0.0319(9) Uani 1 1 d . . . O27 O -0.0736(2) 0.09736(16) 0.14361(9) 0.0382(6) Uani 1 1 d D . . H27 H -0.049(4) 0.059(2) 0.1616(14) 0.057 Uiso 1 1 d D . . C28 C 0.1515(3) 0.4260(2) 0.20415(12) 0.0285(8) Uani 1 1 d . . . H28 H 0.0770 0.4662 0.1984 0.034 Uiso 1 1 calc R . . C29 C 0.6962(3) 0.4101(2) 0.20028(12) 0.0299(8) Uani 1 1 d . . . H29A H 0.6265 0.3937 0.2247 0.036 Uiso 1 1 calc R . . H29B H 0.7748 0.3738 0.2052 0.036 Uiso 1 1 calc R . . C30 C 0.7424(4) 0.5037(2) 0.20918(14) 0.0407(9) Uani 1 1 d . . . H30A H 0.6629 0.5391 0.2038 0.049 Uiso 1 1 calc R . . H30B H 0.8103 0.5194 0.1839 0.049 Uiso 1 1 calc R . . C31 C 0.8049(4) 0.5258(2) 0.26086(14) 0.0427(10) Uani 1 1 d . . . H31A H 0.8721 0.4830 0.2691 0.051 Uiso 1 1 calc R . . H31B H 0.8551 0.5818 0.2595 0.051 Uiso 1 1 calc R . . C32 C 0.7039(4) 0.5297(2) 0.30282(14) 0.0411(10) Uani 1 1 d . . . H32A H 0.6294 0.5666 0.2929 0.049 Uiso 1 1 calc R . . H32B H 0.6633 0.4718 0.3078 0.049 Uiso 1 1 calc R . . C33 C 0.7681(4) 0.5638(2) 0.35191(13) 0.0378(9) Uani 1 1 d . . . H33A H 0.8427 0.5268 0.3616 0.045 Uiso 1 1 calc R . . H33B H 0.8092 0.6215 0.3466 0.045 Uiso 1 1 calc R . . C34 C 0.6708(4) 0.5690(2) 0.39469(14) 0.0400(9) Uani 1 1 d . . . H34A H 0.5945 0.6043 0.3846 0.048 Uiso 1 1 calc R . . H34B H 0.6321 0.5110 0.4008 0.048 Uiso 1 1 calc R . . C35 C 0.7343(4) 0.6058(2) 0.44303(13) 0.0375(9) Uani 1 1 d . . . H35A H 0.7742 0.6635 0.4369 0.045 Uiso 1 1 calc R . . H35B H 0.8095 0.5699 0.4535 0.045 Uiso 1 1 calc R . . C36 C 0.6348(4) 0.6118(2) 0.48532(14) 0.0387(9) Uani 1 1 d . . . H36A H 0.5972 0.5538 0.4920 0.046 Uiso 1 1 calc R . . H36B H 0.5580 0.6460 0.4743 0.046 Uiso 1 1 calc R . . C37 C 0.6958(4) 0.6512(2) 0.53365(13) 0.0374(9) Uani 1 1 d . . . H37A H 0.7723 0.6170 0.5449 0.045 Uiso 1 1 calc R . . H37B H 0.7333 0.7093 0.5271 0.045 Uiso 1 1 calc R . . C38 C 0.5951(4) 0.6566(2) 0.57503(14) 0.0440(10) Uani 1 1 d . . . H38A H 0.5590 0.5983 0.5819 0.053 Uiso 1 1 calc R . . H38B H 0.5176 0.6897 0.5634 0.053 Uiso 1 1 calc R . . C39 C 0.6538(5) 0.6976(3) 0.62350(15) 0.0589(12) Uani 1 1 d . . . H39A H 0.5824 0.6988 0.6483 0.088 Uiso 1 1 calc R . . H39B H 0.6877 0.7560 0.6174 0.088 Uiso 1 1 calc R . . H39C H 0.7289 0.6644 0.6360 0.088 Uiso 1 1 calc R . . C40 C 0.6490(3) 0.0926(2) 0.23113(12) 0.0263(8) Uani 1 1 d . . . H40A H 0.7373 0.1252 0.2290 0.032 Uiso 1 1 calc R . . H40B H 0.5864 0.1280 0.2501 0.032 Uiso 1 1 calc R . . C41 C 0.6704(4) 0.0106(2) 0.25866(13) 0.0356(9) Uani 1 1 d . . . H41A H 0.7363 -0.0231 0.2402 0.043 Uiso 1 1 calc R . . H41B H 0.5829 -0.0232 0.2587 0.043 Uiso 1 1 calc R . . C42 C 0.7227(4) 0.0243(2) 0.31240(13) 0.0382(9) Uani 1 1 d . . . H42A H 0.7540 -0.0305 0.3248 0.046 Uiso 1 1 calc R . . H42B H 0.8027 0.0651 0.3128 0.046 Uiso 1 1 calc R . . C43 C 0.6183(4) 0.0576(2) 0.34783(13) 0.0369(9) Uani 1 1 d . . . H43A H 0.5377 0.0173 0.3470 0.044 Uiso 1 1 calc R . . H43B H 0.5883 0.1129 0.3358 0.044 Uiso 1 1 calc R . . C44 C 0.6706(4) 0.0698(2) 0.40168(13) 0.0370(9) Uani 1 1 d . . . H44A H 0.7038 0.0150 0.4134 0.044 Uiso 1 1 calc R . . H44B H 0.7488 0.1119 0.4028 0.044 Uiso 1 1 calc R . . C45 C 0.5632(4) 0.0999(2) 0.43680(13) 0.0380(9) Uani 1 1 d . . . H45A H 0.4859 0.0571 0.4360 0.046 Uiso 1 1 calc R . . H45B H 0.5286 0.1538 0.4244 0.046 Uiso 1 1 calc R . . C46 C 0.6126(4) 0.1143(2) 0.49054(13) 0.0382(9) Uani 1 1 d . . . H46A H 0.6875 0.1587 0.4918 0.046 Uiso 1 1 calc R . . H46B H 0.6498 0.0610 0.5028 0.046 Uiso 1 1 calc R . . C47 C 0.5009(4) 0.1416(2) 0.52491(14) 0.0405(9) Uani 1 1 d . . . H47A H 0.4266 0.0967 0.5237 0.049 Uiso 1 1 calc R . . H47B H 0.4628 0.1942 0.5120 0.049 Uiso 1 1 calc R . . C48 C 0.5463(4) 0.1579(2) 0.57901(14) 0.0431(10) Uani 1 1 d . . . H48A H 0.5863 0.1059 0.5919 0.052 Uiso 1 1 calc R . . H48B H 0.6185 0.2041 0.5806 0.052 Uiso 1 1 calc R . . C49 C 0.4316(5) 0.1826(3) 0.61221(15) 0.0541(11) Uani 1 1 d . . . H49A H 0.3597 0.1362 0.6107 0.065 Uiso 1 1 calc R . . H49B H 0.3913 0.2344 0.5991 0.065 Uiso 1 1 calc R . . C50 C 0.4758(5) 0.1997(3) 0.66633(17) 0.0732(15) Uani 1 1 d . . . H50A H 0.3969 0.2151 0.6856 0.110 Uiso 1 1 calc R . . H50B H 0.5452 0.2466 0.6683 0.110 Uiso 1 1 calc R . . H50C H 0.5139 0.1483 0.6799 0.110 Uiso 1 1 calc R . . C51 C 0.1470(3) 0.1205(2) 0.28680(12) 0.0301(8) Uani 1 1 d . . . H51A H 0.2355 0.1534 0.2884 0.036 Uiso 1 1 calc R . . H51B H 0.0791 0.1549 0.3037 0.036 Uiso 1 1 calc R . . C52 C 0.1611(4) 0.0370(2) 0.31392(13) 0.0375(9) Uani 1 1 d . . . H52A H 0.0732 0.0036 0.3110 0.045 Uiso 1 1 calc R . . H52B H 0.2305 0.0036 0.2972 0.045 Uiso 1 1 calc R . . C53 C 0.2013(4) 0.0484(2) 0.36863(13) 0.0361(9) Uani 1 1 d . . . H53A H 0.2842 0.0867 0.3717 0.043 Uiso 1 1 calc R . . H53B H 0.2250 -0.0076 0.3816 0.043 Uiso 1 1 calc R . . C54 C 0.0924(3) 0.0846(2) 0.40083(13) 0.0355(9) Uani 1 1 d . . . H54A H 0.0088 0.0470 0.3974 0.043 Uiso 1 1 calc R . . H54B H 0.0702 0.1413 0.3885 0.043 Uiso 1 1 calc R . . C55 C 0.1338(4) 0.0936(2) 0.45565(13) 0.0372(9) Uani 1 1 d . . . H55A H 0.1568 0.0370 0.4678 0.045 Uiso 1 1 calc R . . H55B H 0.2172 0.1314 0.4590 0.045 Uiso 1 1 calc R . . C56 C 0.0265(4) 0.1291(2) 0.48872(13) 0.0388(9) Uani 1 1 d . . . H56A H -0.0567 0.0911 0.4859 0.047 Uiso 1 1 calc R . . H56B H 0.0028 0.1856 0.4766 0.047 Uiso 1 1 calc R . . C57 C 0.0713(4) 0.1381(2) 0.54300(13) 0.0396(9) Uani 1 1 d . . . H57A H 0.0970 0.0816 0.5546 0.048 Uiso 1 1 calc R . . H57B H 0.1539 0.1767 0.5456 0.048 Uiso 1 1 calc R . . C58 C -0.0339(4) 0.1719(3) 0.57752(14) 0.0485(10) Uani 1 1 d . . . H58A H -0.1166 0.1333 0.5752 0.058 Uiso 1 1 calc R . . H58B H -0.0597 0.2285 0.5661 0.058 Uiso 1 1 calc R . . C59 C 0.0134(4) 0.1804(3) 0.63158(15) 0.0518(11) Uani 1 1 d . . . H59A H 0.0427 0.1242 0.6425 0.062 Uiso 1 1 calc R . . H59B H 0.0942 0.2205 0.6340 0.062 Uiso 1 1 calc R . . C60 C -0.0915(6) 0.2111(3) 0.66696(17) 0.0780(16) Uani 1 1 d . . . H60A H -0.1716 0.1704 0.6654 0.094 Uiso 1 1 calc R . . H60B H -0.1221 0.2669 0.6559 0.094 Uiso 1 1 calc R . . C61 C -0.0395(7) 0.2204(4) 0.72062(19) 0.107(2) Uani 1 1 d . . . H61A H -0.1121 0.2406 0.7416 0.161 Uiso 1 1 calc R . . H61B H 0.0387 0.2615 0.7227 0.161 Uiso 1 1 calc R . . H61C H -0.0114 0.1651 0.7322 0.161 Uiso 1 1 calc R . . C62 C 0.1979(3) 0.4388(2) 0.25915(12) 0.0307(8) Uani 1 1 d . . . H62A H 0.1227 0.4200 0.2808 0.037 Uiso 1 1 calc R . . H62B H 0.2762 0.4031 0.2661 0.037 Uiso 1 1 calc R . . C63 C 0.2391(4) 0.5316(2) 0.27148(13) 0.0422(10) Uani 1 1 d . . . H63A H 0.1583 0.5661 0.2662 0.051 Uiso 1 1 calc R . . H63B H 0.3085 0.5509 0.2476 0.051 Uiso 1 1 calc R . . C64 C 0.2960(4) 0.5502(2) 0.32416(13) 0.0413(10) Uani 1 1 d . . . H64A H 0.3675 0.5095 0.3312 0.050 Uiso 1 1 calc R . . H64B H 0.3404 0.6081 0.3253 0.050 Uiso 1 1 calc R . . C65 C 0.1931(4) 0.5450(2) 0.36555(13) 0.0380(9) Uani 1 1 d . . . H65A H 0.1622 0.4848 0.3696 0.046 Uiso 1 1 calc R . . H65B H 0.1125 0.5771 0.3559 0.046 Uiso 1 1 calc R . . C66 C 0.2522(4) 0.5809(2) 0.41512(13) 0.0364(9) Uani 1 1 d . . . H66A H 0.3291 0.5461 0.4253 0.044 Uiso 1 1 calc R . . H66B H 0.2897 0.6395 0.4099 0.044 Uiso 1 1 calc R . . C67 C 0.1538(4) 0.5839(2) 0.45743(13) 0.0361(9) Uani 1 1 d . . . H67A H 0.1208 0.5250 0.4645 0.043 Uiso 1 1 calc R . . H67B H 0.0741 0.6159 0.4469 0.043 Uiso 1 1 calc R . . C68 C 0.2169(4) 0.6253(2) 0.50497(13) 0.0382(9) Uani 1 1 d . . . H68A H 0.2965 0.5929 0.5152 0.046 Uiso 1 1 calc R . . H68B H 0.2509 0.6838 0.4974 0.046 Uiso 1 1 calc R . . C69 C 0.1219(4) 0.6305(2) 0.54876(14) 0.0374(9) Uani 1 1 d . . . H69A H 0.0419 0.6628 0.5388 0.045 Uiso 1 1 calc R . . H69B H 0.0885 0.5722 0.5568 0.045 Uiso 1 1 calc R . . C70 C 0.1890(4) 0.6728(2) 0.59515(13) 0.0389(9) Uani 1 1 d . . . H70A H 0.2698 0.6409 0.6045 0.047 Uiso 1 1 calc R . . H70B H 0.2216 0.7312 0.5869 0.047 Uiso 1 1 calc R . . C71 C 0.0988(4) 0.6784(3) 0.63973(14) 0.0444(10) Uani 1 1 d . . . H71A H 0.0645 0.6202 0.6478 0.053 Uiso 1 1 calc R . . H71B H 0.0191 0.7118 0.6309 0.053 Uiso 1 1 calc R . . C72 C 0.1707(4) 0.7193(3) 0.68562(15) 0.0550(11) Uani 1 1 d . . . H72A H 0.1071 0.7210 0.7131 0.083 Uiso 1 1 calc R . . H72B H 0.2030 0.7775 0.6782 0.083 Uiso 1 1 calc R . . H72C H 0.2486 0.6859 0.6952 0.083 Uiso 1 1 calc R . . Br1 Br 0.82285(5) 0.26516(3) -0.049613(18) 0.06627(17) Uani 1 1 d . . . N1 N 0.1201(3) 0.03006(18) 0.01326(13) 0.0489(9) Uani 1 1 d D . . C1C C 0.0086(9) 0.0969(6) 0.0193(4) 0.037(2) Uani 0.486(7) 1 d PDU . 1 H1CA H -0.0124 0.1273 -0.0116 0.045 Uiso 0.486(7) 1 calc PR . 1 H1CB H 0.0265 0.1375 0.0478 0.045 Uiso 0.486(7) 1 calc PR . 1 C2C C 0.0549(7) -0.0361(4) 0.0549(3) 0.033(2) Uani 0.486(7) 1 d PDU . 1 H2CA H 0.0821 -0.0224 0.0900 0.039 Uiso 0.486(7) 1 calc PR . 1 H2CB H 0.0601 -0.0975 0.0464 0.039 Uiso 0.486(7) 1 calc PR . 1 C3C C 0.1068(8) -0.0155(6) -0.0314(3) 0.046(3) Uani 0.486(7) 1 d PDU . 1 H3C1 H 0.1951 -0.0378 -0.0412 0.055 Uiso 0.486(7) 1 calc PR . 1 H3C2 H 0.0724 0.0204 -0.0583 0.055 Uiso 0.486(7) 1 calc PR . 1 C1CB C 0.0273(10) 0.0648(8) 0.0434(4) 0.062(4) Uani 0.514(7) 1 d PDU . 2 H1CC H 0.0557 0.1237 0.0545 0.075 Uiso 0.514(7) 1 calc PR . 2 H1CD H 0.0090 0.0296 0.0728 0.075 Uiso 0.514(7) 1 calc PR . 2 C2CB C 0.1329(7) -0.0622(4) 0.0045(4) 0.050(3) Uani 0.514(7) 1 d PDU . 2 H2CC H 0.1169 -0.0964 0.0345 0.060 Uiso 0.514(7) 1 calc PR . 2 H2CD H 0.2193 -0.0767 -0.0111 0.060 Uiso 0.514(7) 1 calc PR . 2 C3CB C 0.0985(7) 0.0625(5) -0.0430(2) 0.040(2) Uani 0.514(7) 1 d PDU . 2 H3C3 H 0.1152 0.1250 -0.0446 0.048 Uiso 0.514(7) 1 calc PR . 2 H3C4 H 0.1592 0.0339 -0.0663 0.048 Uiso 0.514(7) 1 calc PR . 2 C4C C 0.2658(4) 0.0623(3) 0.03043(19) 0.0629(14) Uani 1 1 d . . . H4C1 H 0.2799 0.0486 0.0659 0.075 Uiso 1 1 calc R . . H4C2 H 0.3328 0.0312 0.0110 0.075 Uiso 1 1 calc R . . C5C C 0.2927(3) 0.1547(2) 0.02465(14) 0.0363(9) Uani 1 1 d . . . C6C C 0.3451(4) 0.1865(3) -0.01932(16) 0.0567(13) Uani 1 1 d . . . H6C H 0.3654 0.1478 -0.0455 0.068 Uiso 1 1 calc R . . C7C C 0.3682(4) 0.2731(4) -0.02572(19) 0.0665(14) Uani 1 1 d . . . H7C H 0.4042 0.2936 -0.0559 0.080 Uiso 1 1 calc R . . C8C C 0.3387(4) 0.3280(3) 0.01172(19) 0.0565(12) Uani 1 1 d . . . H8C H 0.3525 0.3875 0.0071 0.068 Uiso 1 1 calc R . . C9C C 0.2900(4) 0.3004(2) 0.05562(16) 0.0434(10) Uani 1 1 d . . . H9C H 0.2719 0.3402 0.0815 0.052 Uiso 1 1 calc R . . C10C C 0.2666(3) 0.2133(2) 0.06258(14) 0.0402(9) Uani 1 1 d . . . H10C H 0.2327 0.1938 0.0933 0.048 Uiso 1 1 calc R . . O1E O 0.5783(15) 0.2462(11) -0.1281(3) 0.036(2) Uani 0.611(13) 1 d PDU A 1 H1E H 0.6356 0.2587 -0.1050 0.053 Uiso 0.611(13) 1 calc PR A 1 C2E C 0.6137(12) 0.2934(6) -0.1721(3) 0.062(3) Uani 0.611(13) 1 d PDU A 1 H2E1 H 0.7138 0.2952 -0.1757 0.074 Uiso 0.611(13) 1 calc PR A 1 H2E2 H 0.5852 0.3527 -0.1681 0.074 Uiso 0.611(13) 1 calc PR A 1 C3E C 0.5464(16) 0.2535(8) -0.2181(3) 0.133(6) Uani 0.611(13) 1 d PDU A 1 H3E1 H 0.5742 0.2858 -0.2472 0.200 Uiso 0.611(13) 1 calc PR A 1 H3E2 H 0.4472 0.2539 -0.2152 0.200 Uiso 0.611(13) 1 calc PR A 1 H3E3 H 0.5738 0.1946 -0.2220 0.200 Uiso 0.611(13) 1 calc PR A 1 O1EB O 0.541(2) 0.249(2) -0.1329(7) 0.055(6) Uani 0.389(13) 1 d PDU A 2 H1EB H 0.6180 0.2567 -0.1190 0.083 Uiso 0.389(13) 1 calc PR A 2 C2EB C 0.5433(17) 0.2844(13) -0.1823(8) 0.101(8) Uani 0.389(13) 1 d PDU A 2 H2E3 H 0.5300 0.3464 -0.1799 0.122 Uiso 0.389(13) 1 calc PR A 2 H2E4 H 0.4676 0.2576 -0.2032 0.122 Uiso 0.389(13) 1 calc PR A 2 C3EB C 0.678(2) 0.2690(11) -0.2066(6) 0.129(9) Uani 0.389(13) 1 d PDU A 2 H3E4 H 0.6789 0.2949 -0.2394 0.193 Uiso 0.389(13) 1 calc PR A 2 H3E5 H 0.6888 0.2075 -0.2105 0.193 Uiso 0.389(13) 1 calc PR A 2 H3E6 H 0.7527 0.2945 -0.1856 0.193 Uiso 0.389(13) 1 calc PR A 2 O4E O -0.0515(9) -0.1723(6) 0.1179(5) 0.063(3) Uani 0.519(10) 1 d PDU B 1 H4E H -0.0071 -0.2081 0.1022 0.094 Uiso 0.519(10) 1 calc PR B 1 C5E C -0.1680(9) -0.2146(5) 0.1393(4) 0.068(3) Uani 0.519(10) 1 d PDU B 1 H5E1 H -0.2510 -0.2008 0.1200 0.081 Uiso 0.519(10) 1 calc PR B 1 H5E2 H -0.1774 -0.1927 0.1739 0.081 Uiso 0.519(10) 1 calc PR B 1 C6E C -0.1586(13) -0.3094(5) 0.1399(6) 0.109(5) Uani 0.519(10) 1 d PDU B 1 H6E1 H -0.2394 -0.3348 0.1555 0.163 Uiso 0.519(10) 1 calc PR B 1 H6E2 H -0.0767 -0.3235 0.1590 0.163 Uiso 0.519(10) 1 calc PR B 1 H6E3 H -0.1534 -0.3318 0.1057 0.163 Uiso 0.519(10) 1 calc PR B 1 O4EB O -0.0135(9) -0.2029(7) 0.1313(6) 0.066(4) Uani 0.481(10) 1 d PDU B 2 H4EB H 0.0494 -0.2221 0.1143 0.099 Uiso 0.481(10) 1 calc PR B 2 C5EB C -0.1000(10) -0.2724(6) 0.1478(5) 0.063(4) Uani 0.481(10) 1 d PDU B 2 H5E3 H -0.0476 -0.3075 0.1708 0.075 Uiso 0.481(10) 1 calc PR B 2 H5E4 H -0.1308 -0.3088 0.1187 0.075 Uiso 0.481(10) 1 calc PR B 2 C6EB C -0.2225(10) -0.2405(8) 0.1739(5) 0.095(5) Uani 0.481(10) 1 d PDU B 2 H6E4 H -0.2796 -0.2892 0.1846 0.142 Uiso 0.481(10) 1 calc PR B 2 H6E5 H -0.2753 -0.2064 0.1510 0.142 Uiso 0.481(10) 1 calc PR B 2 H6E6 H -0.1922 -0.2052 0.2031 0.142 Uiso 0.481(10) 1 calc PR B 2 O7E O -0.0158(6) 0.5765(4) 0.0441(2) 0.0578(15) Uiso 0.50 1 d PU C 1 H7E H 0.0409 0.6098 0.0307 0.087 Uiso 0.50 1 calc PR C 1 C8E C -0.0637(5) 0.5157(4) 0.0098(2) 0.0819(16) Uiso 1 1 d U . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0343(19) 0.030(2) 0.0230(18) -0.0055(15) 0.0008(15) 0.0086(16) C2 0.036(2) 0.0234(18) 0.0211(18) 0.0012(14) 0.0008(15) 0.0044(15) C3 0.038(2) 0.0193(18) 0.0244(18) -0.0019(15) 0.0065(15) 0.0025(15) C4 0.052(2) 0.026(2) 0.026(2) 0.0039(16) 0.0126(17) 0.0041(17) C5 0.065(3) 0.029(2) 0.030(2) 0.0043(17) 0.0033(19) 0.0156(19) O4 0.0659(19) 0.0365(16) 0.0462(17) 0.0168(13) 0.0260(15) 0.0150(13) C6 0.048(2) 0.033(2) 0.031(2) -0.0003(17) -0.0011(18) 0.0180(18) O6 0.0617(18) 0.0569(19) 0.0389(17) 0.0051(14) -0.0009(14) 0.0344(15) C7 0.0306(19) 0.0240(19) 0.0284(19) -0.0005(15) 0.0072(15) -0.0002(15) C8 0.0196(17) 0.0267(19) 0.0283(19) -0.0041(15) 0.0012(14) 0.0030(14) C9 0.0202(17) 0.030(2) 0.0207(17) -0.0020(15) 0.0018(14) 0.0013(14) C10 0.0135(16) 0.0271(19) 0.0298(19) -0.0019(15) 0.0034(14) 0.0003(13) C11 0.0177(16) 0.0274(19) 0.0308(19) -0.0069(16) 0.0007(14) 0.0038(14) O11 0.0402(14) 0.0265(14) 0.0310(14) -0.0050(11) 0.0048(11) 0.0004(11) C12 0.0264(18) 0.032(2) 0.0225(18) -0.0046(16) 0.0017(14) 0.0042(15) C13 0.0217(17) 0.031(2) 0.0256(19) 0.0029(16) 0.0019(14) 0.0052(14) O13 0.0453(15) 0.0312(14) 0.0252(13) 0.0046(11) 0.0063(11) 0.0064(11) C14 0.0220(17) 0.0249(18) 0.0284(19) -0.0023(15) 0.0056(14) 0.0021(14) C15 0.0237(17) 0.0225(18) 0.0273(18) -0.0018(14) 0.0060(14) 0.0005(14) C16 0.0267(18) 0.0233(18) 0.0256(18) -0.0026(14) 0.0016(15) -0.0031(14) C17 0.0219(17) 0.0282(19) 0.0290(19) -0.0057(15) 0.0036(14) -0.0005(14) C18 0.0257(19) 0.039(2) 0.036(2) -0.0087(17) 0.0072(16) -0.0070(16) O18 0.0265(13) 0.0471(17) 0.0575(18) -0.0245(13) 0.0092(12) -0.0119(12) C19 0.031(2) 0.030(2) 0.045(2) -0.0177(17) 0.0077(17) -0.0070(16) C20 0.031(2) 0.029(2) 0.037(2) -0.0084(16) 0.0105(16) 0.0029(16) O20 0.0365(14) 0.0288(14) 0.0614(18) -0.0157(14) 0.0201(13) -0.0017(12) C21 0.0258(18) 0.033(2) 0.0258(19) -0.0078(15) 0.0041(15) -0.0011(15) C22 0.0201(17) 0.040(2) 0.0219(18) -0.0079(16) 0.0053(14) 0.0023(15) C23 0.0217(17) 0.042(2) 0.0207(18) -0.0080(16) 0.0004(14) 0.0065(15) C24 0.0182(17) 0.040(2) 0.0261(19) -0.0077(16) 0.0040(14) 0.0067(15) C25 0.0227(18) 0.048(2) 0.028(2) -0.0023(18) 0.0012(15) 0.0137(17) O25 0.0406(16) 0.0518(18) 0.0390(16) -0.0030(14) -0.0117(12) 0.0132(13) C26 0.0195(17) 0.049(2) 0.0277(19) -0.0118(18) -0.0048(15) 0.0078(16) C27 0.0197(17) 0.044(2) 0.032(2) -0.0144(18) 0.0058(15) 0.0020(16) O27 0.0307(14) 0.0486(17) 0.0340(15) -0.0127(12) -0.0027(11) -0.0043(12) C28 0.0276(18) 0.034(2) 0.0247(18) -0.0036(15) 0.0011(15) 0.0122(15) C29 0.0310(19) 0.0275(19) 0.031(2) -0.0021(15) 0.0048(15) -0.0003(15) C30 0.046(2) 0.036(2) 0.039(2) -0.0097(18) 0.0069(18) -0.0106(18) C31 0.043(2) 0.040(2) 0.044(2) -0.0116(18) 0.0080(18) -0.0126(18) C32 0.038(2) 0.041(2) 0.043(2) -0.0133(18) 0.0043(18) -0.0047(18) C33 0.038(2) 0.037(2) 0.037(2) -0.0045(17) 0.0055(17) -0.0016(17) C34 0.036(2) 0.036(2) 0.047(2) -0.0107(18) 0.0017(18) -0.0004(17) C35 0.039(2) 0.032(2) 0.042(2) -0.0018(17) -0.0005(17) 0.0027(16) C36 0.039(2) 0.034(2) 0.043(2) -0.0075(18) 0.0052(18) 0.0003(17) C37 0.040(2) 0.031(2) 0.041(2) 0.0009(17) 0.0009(18) 0.0018(17) C38 0.049(2) 0.039(2) 0.044(2) -0.0077(19) 0.0064(19) -0.0006(18) C39 0.072(3) 0.062(3) 0.043(3) -0.004(2) 0.001(2) 0.011(2) C40 0.0238(17) 0.0302(19) 0.0250(18) 0.0011(15) 0.0026(14) 0.0009(14) C41 0.040(2) 0.033(2) 0.035(2) 0.0015(17) 0.0021(17) 0.0061(16) C42 0.042(2) 0.037(2) 0.037(2) 0.0060(17) -0.0024(18) 0.0088(17) C43 0.035(2) 0.040(2) 0.036(2) 0.0075(17) -0.0030(17) 0.0066(17) C44 0.035(2) 0.038(2) 0.039(2) 0.0065(17) -0.0033(17) 0.0059(17) C45 0.042(2) 0.034(2) 0.038(2) 0.0076(17) -0.0048(18) 0.0033(17) C46 0.040(2) 0.034(2) 0.040(2) 0.0026(17) -0.0056(18) 0.0008(17) C47 0.045(2) 0.037(2) 0.039(2) 0.0062(18) -0.0026(18) 0.0054(18) C48 0.047(2) 0.035(2) 0.047(2) 0.0002(18) -0.002(2) -0.0024(18) C49 0.072(3) 0.044(3) 0.048(3) 0.003(2) 0.013(2) 0.009(2) C50 0.100(4) 0.066(3) 0.052(3) -0.012(2) 0.020(3) -0.014(3) C51 0.0286(18) 0.032(2) 0.0298(19) -0.0044(16) 0.0068(15) 0.0006(15) C52 0.038(2) 0.036(2) 0.038(2) -0.0010(17) 0.0058(17) 0.0037(17) C53 0.038(2) 0.034(2) 0.037(2) 0.0028(17) -0.0008(17) 0.0074(17) C54 0.035(2) 0.041(2) 0.031(2) 0.0056(17) 0.0010(16) 0.0022(17) C55 0.038(2) 0.039(2) 0.035(2) 0.0029(17) -0.0013(17) 0.0029(17) C56 0.043(2) 0.042(2) 0.032(2) 0.0075(17) 0.0003(17) 0.0046(18) C57 0.044(2) 0.040(2) 0.035(2) 0.0035(18) -0.0002(18) -0.0029(18) C58 0.065(3) 0.044(2) 0.038(2) 0.0062(19) 0.007(2) 0.012(2) C59 0.072(3) 0.044(2) 0.039(2) -0.0001(19) 0.007(2) -0.008(2) C60 0.131(5) 0.061(3) 0.045(3) 0.002(2) 0.026(3) 0.021(3) C61 0.192(7) 0.081(4) 0.048(3) -0.015(3) 0.033(4) -0.010(4) C62 0.0316(19) 0.034(2) 0.0266(19) -0.0045(16) 0.0034(15) 0.0043(16) C63 0.056(2) 0.039(2) 0.031(2) -0.0053(17) 0.0035(18) -0.0011(19) C64 0.046(2) 0.038(2) 0.038(2) -0.0088(18) 0.0008(18) -0.0100(18) C65 0.038(2) 0.036(2) 0.039(2) -0.0066(17) 0.0006(17) -0.0037(17) C66 0.042(2) 0.033(2) 0.033(2) -0.0076(17) -0.0009(17) -0.0017(17) C67 0.037(2) 0.033(2) 0.038(2) -0.0079(17) 0.0011(17) 0.0006(16) C68 0.042(2) 0.037(2) 0.036(2) -0.0037(17) 0.0022(17) -0.0039(17) C69 0.041(2) 0.029(2) 0.043(2) -0.0049(17) 0.0030(18) 0.0008(16) C70 0.046(2) 0.036(2) 0.035(2) -0.0040(17) 0.0073(18) -0.0030(17) C71 0.046(2) 0.044(2) 0.044(2) -0.0044(19) 0.0120(19) 0.0060(19) C72 0.068(3) 0.059(3) 0.039(2) -0.010(2) 0.013(2) 0.004(2) Br1 0.0740(3) 0.0736(3) 0.0522(3) -0.0220(2) 0.0089(2) 0.0224(3) N1 0.048(2) 0.0266(18) 0.071(3) -0.0063(17) -0.0312(19) 0.0083(15) C1C 0.035(5) 0.044(6) 0.033(6) -0.001(4) 0.005(5) 0.000(4) C2C 0.030(4) 0.026(4) 0.042(5) 0.000(3) -0.011(3) -0.005(3) C3C 0.026(4) 0.075(8) 0.034(5) 0.002(5) -0.002(4) -0.004(4) C1CB 0.048(6) 0.097(10) 0.038(6) -0.027(6) 0.021(5) -0.044(6) C2CB 0.026(4) 0.024(4) 0.098(8) 0.008(4) -0.005(4) -0.003(3) C3CB 0.037(4) 0.049(5) 0.033(4) 0.011(4) -0.013(3) -0.009(4) C4C 0.045(3) 0.046(3) 0.095(4) -0.011(2) -0.040(3) 0.006(2) C5C 0.0291(19) 0.041(2) 0.039(2) -0.0130(18) -0.0048(17) 0.0041(16) C6C 0.038(2) 0.090(4) 0.042(3) -0.023(3) 0.002(2) 0.011(2) C7C 0.038(3) 0.107(5) 0.054(3) 0.024(3) 0.002(2) -0.009(3) C8C 0.040(2) 0.059(3) 0.069(3) 0.014(3) -0.006(2) -0.008(2) C9C 0.037(2) 0.037(2) 0.054(3) -0.013(2) -0.001(2) -0.0043(18) C10C 0.031(2) 0.052(3) 0.037(2) -0.0075(19) 0.0021(17) -0.0043(18) O1E 0.041(6) 0.033(4) 0.032(4) -0.010(3) -0.002(3) 0.001(5) C2E 0.090(8) 0.058(6) 0.036(5) -0.001(4) 0.003(6) -0.017(6) C3E 0.207(15) 0.136(11) 0.046(6) -0.002(6) -0.029(8) -0.073(10) O1EB 0.051(13) 0.060(8) 0.054(8) 0.001(6) -0.005(6) 0.003(9) C2EB 0.118(17) 0.087(11) 0.091(17) -0.026(11) 0.008(15) -0.064(12) C3EB 0.25(3) 0.065(11) 0.072(13) -0.013(9) -0.027(15) 0.001(14) O4E 0.041(5) 0.062(7) 0.082(7) -0.040(5) 0.018(5) -0.016(4) C5E 0.061(7) 0.062(7) 0.077(7) 0.000(6) -0.011(6) -0.019(6) C6E 0.095(11) 0.079(10) 0.157(14) 0.018(9) 0.060(10) 0.005(8) O4EB 0.043(6) 0.053(7) 0.099(9) -0.038(5) 0.034(6) -0.018(5) C5EB 0.048(7) 0.043(8) 0.095(8) -0.015(6) 0.019(6) -0.022(5) C6EB 0.087(9) 0.094(10) 0.104(10) 0.016(8) 0.037(8) -0.023(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.390(4) . ? C1 C6 1.402(5) . ? C1 C28 1.528(5) . ? C2 C3 1.392(5) . ? C2 H2 0.9500 . ? C3 C4 1.397(5) . ? C3 C7 1.528(4) . ? C4 O4 1.373(4) . ? C4 C5 1.387(5) . ? C5 C6 1.372(5) . ? C5 H5 0.9500 . ? O4 H4 0.836(19) . ? C6 O6 1.387(4) . ? O6 H6 0.83(2) . ? C7 C8 1.525(4) . ? C7 C29 1.537(4) . ? C7 H7 1.0000 . ? C8 C13 1.390(4) . ? C8 C9 1.394(5) . ? C9 C10 1.397(4) . ? C9 H9 0.9500 . ? C10 C11 1.394(4) . ? C10 C14 1.519(5) . ? C11 C12 1.381(5) . ? C11 O11 1.390(4) . ? O11 H11 0.835(19) . ? C12 C13 1.384(4) . ? C12 H12 0.9500 . ? C13 O13 1.384(4) . ? O13 H13 0.828(19) . ? C14 C15 1.524(4) . ? C14 C40 1.533(4) . ? C14 H14 1.0000 . ? C15 C16 1.393(4) . ? C15 C20 1.398(4) . ? C16 C17 1.388(4) . ? C16 H16 0.9500 . ? C17 C18 1.398(4) . ? C17 C21 1.523(4) . ? C18 O18 1.383(4) . ? C18 C19 1.380(5) . ? O18 H18 0.832(19) . ? C19 C20 1.384(5) . ? C19 H19 0.9500 . ? C20 O20 1.382(4) . ? O20 H20 0.836(19) . ? C21 C22 1.517(5) . ? C21 C51 1.533(4) . ? C21 H21 1.0000 . ? C22 C23 1.397(5) . ? C22 C27 1.401(4) . ? C23 C24 1.389(5) . ? C23 H23 0.9500 . ? C24 C25 1.410(4) . ? C24 C28 1.524(5) . ? C25 O25 1.367(4) . ? C25 C26 1.380(5) . ? O25 H25 0.86(4) . ? C26 C27 1.373(5) . ? C26 H26 0.9500 . ? C27 O27 1.385(4) . ? O27 H27 0.829(19) . ? C28 C62 1.540(4) . ? C28 H28 1.0000 . ? C29 C30 1.529(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.529(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.522(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.521(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.516(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.516(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.521(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.521(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.509(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.526(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.521(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.526(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.518(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.526(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.516(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.519(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.521(5) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.521(5) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.513(5) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.520(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.526(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.516(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.515(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.518(5) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.512(5) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.513(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.512(5) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.513(5) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.507(6) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.518(7) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.522(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.524(5) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.522(5) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.523(5) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.511(5) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.523(5) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.522(5) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.518(5) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.510(5) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.518(5) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? N1 C1CB 1.359(9) . ? N1 C3C 1.382(7) . ? N1 C2CB 1.475(7) . ? N1 C1C 1.561(8) . ? N1 C4C 1.551(5) . ? N1 C3CB 1.617(7) . ? N1 C2C 1.663(7) . ? C1C C3C 1.712(13) 2 ? C1C H1CA 0.9900 . ? C1C H1CB 0.9900 . ? C2C C3C 1.917(11) 2 ? C2C H2CA 0.9900 . ? C2C H2CB 0.9900 . ? C3C C1C 1.712(13) 2 ? C3C H3C1 0.9900 . ? C3C H3C2 0.9900 . ? C1CB C2CB 2.007(14) 2 ? C1CB H1CC 0.9900 . ? C1CB H1CD 0.9900 . ? C2CB C1CB 2.007(14) 2 ? C2CB H2CC 0.9900 . ? C2CB H2CD 0.9900 . ? C3CB C2C 1.567(9) 2 ? C3CB H3C3 0.9900 . ? C3CB H3C4 0.9900 . ? C4C C5C 1.476(5) . ? C4C H4C1 0.9900 . ? C4C H4C2 0.9900 . ? C5C C10C 1.393(5) . ? C5C C6C 1.394(6) . ? C6C C7C 1.385(7) . ? C6C H6C 0.9500 . ? C7C C8C 1.355(7) . ? C7C H7C 0.9500 . ? C8C C9C 1.356(6) . ? C8C H8C 0.9500 . ? C9C C10C 1.395(5) . ? C9C H9C 0.9500 . ? C10C H10C 0.9500 . ? O1E C2E 1.451(7) . ? O1E H1E 0.8400 . ? C2E C3E 1.496(7) . ? C2E H2E1 0.9900 . ? C2E H2E2 0.9900 . ? C3E H3E1 0.9800 . ? C3E H3E2 0.9800 . ? C3E H3E3 0.9800 . ? O1EB C2EB 1.451(9) . ? O1EB H1EB 0.8400 . ? C2EB C3EB 1.515(9) . ? C2EB H2E3 0.9900 . ? C2EB H2E4 0.9900 . ? C3EB H3E4 0.9800 . ? C3EB H3E5 0.9800 . ? C3EB H3E6 0.9800 . ? O4E C5E 1.436(8) . ? O4E H4E 0.8400 . ? C5E C6E 1.497(8) . ? C5E H5E1 0.9900 . ? C5E H5E2 0.9900 . ? C6E H6E1 0.9800 . ? C6E H6E2 0.9800 . ? C6E H6E3 0.9800 . ? O4EB C5EB 1.437(8) . ? O4EB H4EB 0.8400 . ? C5EB C6EB 1.507(8) . ? C5EB H5E3 0.9900 . ? C5EB H5E4 0.9900 . ? C6EB H6E4 0.9800 . ? C6EB H6E5 0.9800 . ? C6EB H6E6 0.9800 . ? O7E C8E 1.370(7) . ? O7E H7E 0.8400 . ? C8E C8E 1.471(10) 2_565 ? 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 C2 C1 C6 116.4(3) . . ? C2 C1 C28 121.3(3) . . ? C6 C1 C28 122.3(3) . . ? C1 C2 C3 124.3(3) . . ? C1 C2 H2 117.9 . . ? C3 C2 H2 117.9 . . ? C2 C3 C4 116.8(3) . . ? C2 C3 C7 121.0(3) . . ? C4 C3 C7 122.1(3) . . ? O4 C4 C5 116.7(3) . . ? O4 C4 C3 122.9(3) . . ? C5 C4 C3 120.4(3) . . ? C6 C5 C4 120.9(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C4 O4 H4 109(3) . . ? C5 C6 O6 122.5(3) . . ? C5 C6 C1 121.1(3) . . ? O6 C6 C1 116.5(3) . . ? C6 O6 H6 105(3) . . ? C8 C7 C3 110.4(3) . . ? C8 C7 C29 114.8(3) . . ? C3 C7 C29 112.1(3) . . ? C8 C7 H7 106.3 . . ? C3 C7 H7 106.3 . . ? C29 C7 H7 106.3 . . ? C13 C8 C9 116.8(3) . . ? C13 C8 C7 119.8(3) . . ? C9 C8 C7 123.5(3) . . ? C8 C9 C10 123.5(3) . . ? C8 C9 H9 118.2 . . ? C10 C9 H9 118.2 . . ? C11 C10 C9 116.7(3) . . ? C11 C10 C14 119.9(3) . . ? C9 C10 C14 123.4(3) . . ? C12 C11 O11 115.3(3) . . ? C12 C11 C10 121.7(3) . . ? O11 C11 C10 123.0(3) . . ? C11 O11 H11 111(3) . . ? C11 C12 C13 119.4(3) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C12 C13 O13 120.5(3) . . ? C12 C13 C8 121.8(3) . . ? O13 C13 C8 117.7(3) . . ? C13 O13 H13 107(3) . . ? C10 C14 C15 110.3(2) . . ? C10 C14 C40 114.7(3) . . ? C15 C14 C40 112.3(3) . . ? C10 C14 H14 106.3 . . ? C15 C14 H14 106.3 . . ? C40 C14 H14 106.3 . . ? C16 C15 C20 116.3(3) . . ? C16 C15 C14 121.4(3) . . ? C20 C15 C14 122.3(3) . . ? C17 C16 C15 124.0(3) . . ? C17 C16 H16 118.0 . . ? C15 C16 H16 118.0 . . ? C16 C17 C18 117.0(3) . . ? C16 C17 C21 121.0(3) . . ? C18 C17 C21 122.0(3) . . ? O18 C18 C19 122.0(3) . . ? O18 C18 C17 116.9(3) . . ? C19 C18 C17 121.1(3) . . ? C18 O18 H18 112(3) . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? O20 C20 C19 121.1(3) . . ? O20 C20 C15 117.3(3) . . ? C19 C20 C15 121.6(3) . . ? C20 O20 H20 115(3) . . ? C22 C21 C17 110.4(3) . . ? C22 C21 C51 115.2(3) . . ? C17 C21 C51 111.4(3) . . ? C22 C21 H21 106.4 . . ? C17 C21 H21 106.4 . . ? C51 C21 H21 106.4 . . ? C23 C22 C27 116.7(3) . . ? C23 C22 C21 123.6(3) . . ? C27 C22 C21 119.7(3) . . ? C24 C23 C22 123.8(3) . . ? C24 C23 H23 118.1 . . ? C22 C23 H23 118.1 . . ? C23 C24 C25 116.8(3) . . ? C23 C24 C28 123.3(3) . . ? C25 C24 C28 119.8(3) . . ? O25 C25 C26 115.8(3) . . ? O25 C25 C24 123.5(3) . . ? C26 C25 C24 120.7(3) . . ? C25 O25 H25 111(3) . . ? C27 C26 C25 120.6(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 O27 116.2(3) . . ? C26 C27 C22 121.3(3) . . ? O27 C27 C22 122.4(3) . . ? C27 O27 H27 110(3) . . ? C1 C28 C24 110.5(3) . . ? C1 C28 C62 111.8(3) . . ? C24 C28 C62 114.8(3) . . ? C1 C28 H28 106.4 . . ? C24 C28 H28 106.4 . . ? C62 C28 H28 106.4 . . ? C30 C29 C7 110.6(3) . . ? C30 C29 H29A 109.5 . . ? C7 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? C7 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C31 115.4(3) . . ? C29 C30 H30A 108.4 . . ? C31 C30 H30A 108.4 . . ? C29 C30 H30B 108.4 . . ? C31 C30 H30B 108.4 . . ? H30A C30 H30B 107.5 . . ? C32 C31 C30 115.3(3) . . ? C32 C31 H31A 108.4 . . ? C30 C31 H31A 108.4 . . ? C32 C31 H31B 108.4 . . ? C30 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? C33 C32 C31 113.2(3) . . ? C33 C32 H32A 108.9 . . ? C31 C32 H32A 108.9 . . ? C33 C32 H32B 108.9 . . ? C31 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C34 C33 C32 114.9(3) . . ? C34 C33 H33A 108.5 . . ? C32 C33 H33A 108.5 . . ? C34 C33 H33B 108.5 . . ? C32 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C35 C34 C33 114.6(3) . . ? C35 C34 H34A 108.6 . . ? C33 C34 H34A 108.6 . . ? C35 C34 H34B 108.6 . . ? C33 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? C34 C35 C36 114.0(3) . . ? C34 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? C34 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C35 C36 C37 114.7(3) . . ? C35 C36 H36A 108.6 . . ? C37 C36 H36A 108.6 . . ? C35 C36 H36B 108.6 . . ? C37 C36 H36B 108.6 . . ? H36A C36 H36B 107.6 . . ? C38 C37 C36 113.7(3) . . ? 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 114.5(3) . . ? C37 C38 H38A 108.6 . . ? C39 C38 H38A 108.6 . . ? C37 C38 H38B 108.6 . . ? C39 C38 H38B 108.6 . . ? H38A C38 H38B 107.6 . . ? 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 C14 111.6(3) . . ? C41 C40 H40A 109.3 . . ? C14 C40 H40A 109.3 . . ? C41 C40 H40B 109.3 . . ? C14 C40 H40B 109.3 . . ? H40A C40 H40B 108.0 . . ? C40 C41 C42 114.2(3) . . ? C40 C41 H41A 108.7 . . ? C42 C41 H41A 108.7 . . ? C40 C41 H41B 108.7 . . ? C42 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C43 C42 C41 114.4(3) . . ? C43 C42 H42A 108.7 . . ? C41 C42 H42A 108.7 . . ? C43 C42 H42B 108.7 . . ? C41 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? C42 C43 C44 114.1(3) . . ? C42 C43 H43A 108.7 . . ? C44 C43 H43A 108.7 . . ? C42 C43 H43B 108.7 . . ? C44 C43 H43B 108.7 . . ? H43A C43 H43B 107.6 . . ? C45 C44 C43 113.3(3) . . ? C45 C44 H44A 108.9 . . ? C43 C44 H44A 108.9 . . ? C45 C44 H44B 108.9 . . ? C43 C44 H44B 108.9 . . ? H44A C44 H44B 107.7 . . ? C44 C45 C46 114.7(3) . . ? C44 C45 H45A 108.6 . . ? C46 C45 H45A 108.6 . . ? C44 C45 H45B 108.6 . . ? C46 C45 H45B 108.6 . . ? H45A C45 H45B 107.6 . . ? C45 C46 C47 113.1(3) . . ? C45 C46 H46A 109.0 . . ? C47 C46 H46A 109.0 . . ? C45 C46 H46B 109.0 . . ? C47 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C46 C47 C48 114.9(3) . . ? C46 C47 H47A 108.6 . . ? C48 C47 H47A 108.6 . . ? C46 C47 H47B 108.6 . . ? C48 C47 H47B 108.6 . . ? H47A C47 H47B 107.5 . . ? C49 C48 C47 113.2(3) . . ? C49 C48 H48A 108.9 . . ? C47 C48 H48A 108.9 . . ? C49 C48 H48B 108.9 . . ? C47 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? C48 C49 C50 113.8(4) . . ? C48 C49 H49A 108.8 . . ? C50 C49 H49A 108.8 . . ? C48 C49 H49B 108.8 . . ? C50 C49 H49B 108.8 . . ? H49A C49 H49B 107.7 . . ? 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 C21 111.3(3) . . ? C52 C51 H51A 109.4 . . ? C21 C51 H51A 109.4 . . ? C52 C51 H51B 109.4 . . ? C21 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? C53 C52 C51 114.0(3) . . ? C53 C52 H52A 108.7 . . ? C51 C52 H52A 108.7 . . ? C53 C52 H52B 108.7 . . ? C51 C52 H52B 108.7 . . ? H52A C52 H52B 107.6 . . ? C52 C53 C54 114.6(3) . . ? C52 C53 H53A 108.6 . . ? C54 C53 H53A 108.6 . . ? C52 C53 H53B 108.6 . . ? C54 C53 H53B 108.6 . . ? H53A C53 H53B 107.6 . . ? C53 C54 C55 113.6(3) . . ? C53 C54 H54A 108.8 . . ? C55 C54 H54A 108.8 . . ? C53 C54 H54B 108.8 . . ? C55 C54 H54B 108.8 . . ? H54A C54 H54B 107.7 . . ? C56 C55 C54 114.7(3) . . ? C56 C55 H55A 108.6 . . ? C54 C55 H55A 108.6 . . ? C56 C55 H55B 108.6 . . ? C54 C55 H55B 108.6 . . ? H55A C55 H55B 107.6 . . ? C55 C56 C57 113.5(3) . . ? C55 C56 H56A 108.9 . . ? C57 C56 H56A 108.9 . . ? C55 C56 H56B 108.9 . . ? C57 C56 H56B 108.9 . . ? H56A C56 H56B 107.7 . . ? C58 C57 C56 115.2(3) . . ? C58 C57 H57A 108.5 . . ? C56 C57 H57A 108.5 . . ? C58 C57 H57B 108.5 . . ? C56 C57 H57B 108.5 . . ? H57A C57 H57B 107.5 . . ? C57 C58 C59 114.1(3) . . ? C57 C58 H58A 108.7 . . ? C59 C58 H58A 108.7 . . ? C57 C58 H58B 108.7 . . ? C59 C58 H58B 108.7 . . ? H58A C58 H58B 107.6 . . ? C60 C59 C58 115.0(4) . . ? C60 C59 H59A 108.5 . . ? C58 C59 H59A 108.5 . . ? C60 C59 H59B 108.5 . . ? C58 C59 H59B 108.5 . . ? H59A C59 H59B 107.5 . . ? C59 C60 C61 113.5(5) . . ? C59 C60 H60A 108.9 . . ? C61 C60 H60A 108.9 . . ? C59 C60 H60B 108.9 . . ? C61 C60 H60B 108.9 . . ? H60A C60 H60B 107.7 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C63 C62 C28 111.5(3) . . ? C63 C62 H62A 109.3 . . ? C28 C62 H62A 109.3 . . ? C63 C62 H62B 109.3 . . ? C28 C62 H62B 109.3 . . ? H62A C62 H62B 108.0 . . ? C62 C63 C64 115.7(3) . . ? C62 C63 H63A 108.4 . . ? C64 C63 H63A 108.4 . . ? C62 C63 H63B 108.4 . . ? C64 C63 H63B 108.4 . . ? H63A C63 H63B 107.4 . . ? C65 C64 C63 115.9(3) . . ? C65 C64 H64A 108.3 . . ? C63 C64 H64A 108.3 . . ? C65 C64 H64B 108.3 . . ? C63 C64 H64B 108.3 . . ? H64A C64 H64B 107.4 . . ? C64 C65 C66 112.3(3) . . ? C64 C65 H65A 109.1 . . ? C66 C65 H65A 109.1 . . ? C64 C65 H65B 109.1 . . ? C66 C65 H65B 109.1 . . ? H65A C65 H65B 107.9 . . ? C67 C66 C65 115.7(3) . . ? C67 C66 H66A 108.3 . . ? C65 C66 H66A 108.3 . . ? C67 C66 H66B 108.3 . . ? C65 C66 H66B 108.3 . . ? H66A C66 H66B 107.4 . . ? C66 C67 C68 113.1(3) . . ? C66 C67 H67A 109.0 . . ? C68 C67 H67A 109.0 . . ? C66 C67 H67B 109.0 . . ? C68 C67 H67B 109.0 . . ? H67A C67 H67B 107.8 . . ? C69 C68 C67 115.3(3) . . ? C69 C68 H68A 108.4 . . ? C67 C68 H68A 108.4 . . ? C69 C68 H68B 108.4 . . ? C67 C68 H68B 108.4 . . ? H68A C68 H68B 107.5 . . ? C70 C69 C68 113.4(3) . . ? C70 C69 H69A 108.9 . . ? C68 C69 H69A 108.9 . . ? C70 C69 H69B 108.9 . . ? C68 C69 H69B 108.9 . . ? H69A C69 H69B 107.7 . . ? C71 C70 C69 115.2(3) . . ? C71 C70 H70A 108.5 . . ? C69 C70 H70A 108.5 . . ? C71 C70 H70B 108.5 . . ? C69 C70 H70B 108.5 . . ? H70A C70 H70B 107.5 . . ? C70 C71 C72 113.5(3) . . ? C70 C71 H71A 108.9 . . ? C72 C71 H71A 108.9 . . ? C70 C71 H71B 108.9 . . ? C72 C71 H71B 108.9 . . ? H71A C71 H71B 107.7 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C1CB N1 C3C 132.4(6) . . ? C1CB N1 C2CB 124.6(7) . . ? C3C N1 C2CB 52.0(5) . . ? C1CB N1 C1C 33.0(5) . . ? C3C N1 C1C 112.7(6) . . ? C2CB N1 C1C 140.4(5) . . ? C1CB N1 C4C 109.5(5) . . ? C3C N1 C4C 117.3(4) . . ? C2CB N1 C4C 103.7(4) . . ? C1C N1 C4C 114.7(4) . . ? C1CB N1 C3CB 109.8(7) . . ? C3C N1 C3CB 49.7(5) . . ? C2CB N1 C3CB 101.5(5) . . ? C1C N1 C3CB 77.3(5) . . ? C4C N1 C3CB 106.2(4) . . ? C1CB N1 C2C 65.5(7) . . ? C3C N1 C2C 104.2(5) . . ? C2CB N1 C2C 61.9(5) . . ? C1C N1 C2C 94.9(5) . . ? C4C N1 C2C 109.9(3) . . ? C3CB N1 C2C 142.9(4) . . ? N1 C1C C3C 89.0(6) . 2 ? N1 C1C H1CA 113.8 . . ? C3C C1C H1CA 113.8 2 . ? N1 C1C H1CB 113.8 . . ? C3C C1C H1CB 113.8 2 . ? H1CA C1C H1CB 111.0 . . ? N1 C2C C3C 79.4(4) . 2 ? N1 C2C H2CA 115.3 . . ? C3C C2C H2CA 115.3 2 . ? N1 C2C H2CB 115.3 . . ? C3C C2C H2CB 115.3 2 . ? H2CA C2C H2CB 112.4 . . ? N1 C3C C1C 103.8(6) . 2 ? N1 C3C H3C1 111.0 . . ? C1C C3C H3C1 111.0 2 . ? N1 C3C H3C2 111.0 . . ? C1C C3C H3C2 111.0 2 . ? H3C1 C3C H3C2 109.0 . . ? N1 C1CB C2CB 99.0(6) . 2 ? N1 C1CB H1CC 112.0 . . ? C2CB C1CB H1CC 112.0 2 . ? N1 C1CB H1CD 112.0 . . ? C2CB C1CB H1CD 112.0 2 . ? H1CC C1CB H1CD 109.6 . . ? N1 C2CB C1CB 90.1(5) . 2 ? N1 C2CB H2CC 113.6 . . ? C1CB C2CB H2CC 113.6 2 . ? N1 C2CB H2CD 113.6 . . ? C1CB C2CB H2CD 113.6 2 . ? H2CC C2CB H2CD 110.9 . . ? C2C C3CB N1 102.6(5) 2 . ? C2C C3CB H3C3 111.2 2 . ? N1 C3CB H3C3 111.2 . . ? C2C C3CB H3C4 111.2 2 . ? N1 C3CB H3C4 111.2 . . ? H3C3 C3CB H3C4 109.2 . . ? C5C C4C N1 113.8(3) . . ? C5C C4C H4C1 108.8 . . ? N1 C4C H4C1 108.8 . . ? C5C C4C H4C2 108.8 . . ? N1 C4C H4C2 108.8 . . ? H4C1 C4C H4C2 107.7 . . ? C10C C5C C6C 117.5(4) . . ? C10C C5C C4C 121.6(4) . . ? C6C C5C C4C 120.9(4) . . ? C7C C6C C5C 121.6(4) . . ? C7C C6C H6C 119.2 . . ? C5C C6C H6C 119.2 . . ? C8C C7C C6C 119.0(4) . . ? C8C C7C H7C 120.5 . . ? C6C C7C H7C 120.5 . . ? C7C C8C C9C 121.8(4) . . ? C7C C8C H8C 119.1 . . ? C9C C8C H8C 119.1 . . ? C8C C9C C10C 119.7(4) . . ? C8C C9C H9C 120.1 . . ? C10C C9C H9C 120.1 . . ? C5C C10C C9C 120.3(4) . . ? C5C C10C H10C 119.8 . . ? C9C C10C H10C 119.8 . . ? O1E C2E C3E 111.4(7) . . ? O1E C2E H2E1 109.3 . . ? C3E C2E H2E1 109.3 . . ? O1E C2E H2E2 109.3 . . ? C3E C2E H2E2 109.3 . . ? H2E1 C2E H2E2 108.0 . . ? C2E C3E H3E1 109.5 . . ? C2E C3E H3E2 109.5 . . ? H3E1 C3E H3E2 109.5 . . ? C2E C3E H3E3 109.5 . . ? H3E1 C3E H3E3 109.5 . . ? H3E2 C3E H3E3 109.5 . . ? C2EB O1EB H1EB 109.5 . . ? O1EB C2EB C3EB 110.6(9) . . ? O1EB C2EB H2E3 109.5 . . ? C3EB C2EB H2E3 109.5 . . ? O1EB C2EB H2E4 109.5 . . ? C3EB C2EB H2E4 109.5 . . ? H2E3 C2EB H2E4 108.1 . . ? C2EB C3EB H3E4 109.5 . . ? C2EB C3EB H3E5 109.5 . . ? H3E4 C3EB H3E5 109.5 . . ? C2EB C3EB H3E6 109.5 . . ? H3E4 C3EB H3E6 109.5 . . ? H3E5 C3EB H3E6 109.5 . . ? O4E C5E C6E 112.9(7) . . ? O4E C5E H5E1 109.0 . . ? C6E C5E H5E1 109.0 . . ? O4E C5E H5E2 109.0 . . ? C6E C5E H5E2 109.0 . . ? H5E1 C5E H5E2 107.8 . . ? C5E C6E H6E1 109.5 . . ? C5E C6E H6E2 109.5 . . ? H6E1 C6E H6E2 109.5 . . ? C5E C6E H6E3 109.5 . . ? H6E1 C6E H6E3 109.5 . . ? H6E2 C6E H6E3 109.5 . . ? C5EB O4EB H4EB 109.5 . . ? O4EB C5EB C6EB 111.3(7) . . ? O4EB C5EB H5E3 109.4 . . ? C6EB C5EB H5E3 109.4 . . ? O4EB C5EB H5E4 109.4 . . ? C6EB C5EB H5E4 109.4 . . ? H5E3 C5EB H5E4 108.0 . . ? C5EB C6EB H6E4 109.5 . . ? C5EB C6EB H6E5 109.5 . . ? H6E4 C6EB H6E5 109.5 . . ? C5EB C6EB H6E6 109.5 . . ? H6E4 C6EB H6E6 109.5 . . ? H6E5 C6EB H6E6 109.5 . . ? O7E C8E C8E 101.7(6) . 2_565 ? 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 C6 C1 C2 C3 0.4(5) . . . . ? C28 C1 C2 C3 179.1(3) . . . . ? C1 C2 C3 C4 -2.8(5) . . . . ? C1 C2 C3 C7 178.4(3) . . . . ? C2 C3 C4 O4 -177.6(3) . . . . ? C7 C3 C4 O4 1.1(5) . . . . ? C2 C3 C4 C5 2.9(5) . . . . ? C7 C3 C4 C5 -178.3(3) . . . . ? O4 C4 C5 C6 179.9(3) . . . . ? C3 C4 C5 C6 -0.7(5) . . . . ? C4 C5 C6 O6 -179.8(3) . . . . ? C4 C5 C6 C1 -2.0(5) . . . . ? C2 C1 C6 C5 2.1(5) . . . . ? C28 C1 C6 C5 -176.6(3) . . . . ? C2 C1 C6 O6 -180.0(3) . . . . ? C28 C1 C6 O6 1.4(5) . . . . ? C2 C3 C7 C8 74.6(4) . . . . ? C4 C3 C7 C8 -104.1(4) . . . . ? C2 C3 C7 C29 -54.6(4) . . . . ? C4 C3 C7 C29 126.6(3) . . . . ? C3 C7 C8 C13 82.4(4) . . . . ? C29 C7 C8 C13 -149.8(3) . . . . ? C3 C7 C8 C9 -98.4(3) . . . . ? C29 C7 C8 C9 29.4(4) . . . . ? C13 C8 C9 C10 -0.6(4) . . . . ? C7 C8 C9 C10 -179.8(3) . . . . ? C8 C9 C10 C11 -2.2(4) . . . . ? C8 C9 C10 C14 177.0(3) . . . . ? C9 C10 C11 C12 3.3(4) . . . . ? C14 C10 C11 C12 -175.9(3) . . . . ? C9 C10 C11 O11 -178.2(3) . . . . ? C14 C10 C11 O11 2.6(4) . . . . ? O11 C11 C12 C13 179.7(3) . . . . ? C10 C11 C12 C13 -1.7(5) . . . . ? C11 C12 C13 O13 178.2(3) . . . . ? C11 C12 C13 C8 -1.3(5) . . . . ? C9 C8 C13 C12 2.4(4) . . . . ? C7 C8 C13 C12 -178.4(3) . . . . ? C9 C8 C13 O13 -177.2(3) . . . . ? C7 C8 C13 O13 2.0(4) . . . . ? C11 C10 C14 C15 -79.2(3) . . . . ? C9 C10 C14 C15 101.6(3) . . . . ? C11 C10 C14 C40 152.7(3) . . . . ? C9 C10 C14 C40 -26.4(4) . . . . ? C10 C14 C15 C16 -71.4(4) . . . . ? C40 C14 C15 C16 58.0(4) . . . . ? C10 C14 C15 C20 106.9(4) . . . . ? C40 C14 C15 C20 -123.7(3) . . . . ? C20 C15 C16 C17 2.9(5) . . . . ? C14 C15 C16 C17 -178.7(3) . . . . ? C15 C16 C17 C18 -2.5(5) . . . . ? C15 C16 C17 C21 176.5(3) . . . . ? C16 C17 C18 O18 -177.6(3) . . . . ? C21 C17 C18 O18 3.4(5) . . . . ? C16 C17 C18 C19 0.6(5) . . . . ? C21 C17 C18 C19 -178.5(3) . . . . ? O18 C18 C19 C20 178.9(3) . . . . ? C17 C18 C19 C20 0.8(6) . . . . ? C18 C19 C20 O20 -179.2(3) . . . . ? C18 C19 C20 C15 -0.4(6) . . . . ? C16 C15 C20 O20 177.5(3) . . . . ? C14 C15 C20 O20 -0.9(5) . . . . ? C16 C15 C20 C19 -1.4(5) . . . . ? C14 C15 C20 C19 -179.8(3) . . . . ? C16 C17 C21 C22 72.1(4) . . . . ? C18 C17 C21 C22 -108.9(4) . . . . ? C16 C17 C21 C51 -57.3(4) . . . . ? C18 C17 C21 C51 121.8(4) . . . . ? C17 C21 C22 C23 -102.8(3) . . . . ? C51 C21 C22 C23 24.5(4) . . . . ? C17 C21 C22 C27 74.7(4) . . . . ? C51 C21 C22 C27 -158.0(3) . . . . ? C27 C22 C23 C24 0.4(5) . . . . ? C21 C22 C23 C24 178.0(3) . . . . ? C22 C23 C24 C25 -0.9(5) . . . . ? C22 C23 C24 C28 -178.4(3) . . . . ? C23 C24 C25 O25 179.3(3) . . . . ? C28 C24 C25 O25 -3.1(5) . . . . ? C23 C24 C25 C26 0.9(5) . . . . ? C28 C24 C25 C26 178.5(3) . . . . ? O25 C25 C26 C27 -179.1(3) . . . . ? C24 C25 C26 C27 -0.6(5) . . . . ? C25 C26 C27 O27 -179.2(3) . . . . ? C25 C26 C27 C22 0.1(5) . . . . ? C23 C22 C27 C26 0.0(5) . . . . ? C21 C22 C27 C26 -177.7(3) . . . . ? C23 C22 C27 O27 179.3(3) . . . . ? C21 C22 C27 O27 1.6(5) . . . . ? C2 C1 C28 C24 -73.9(4) . . . . ? C6 C1 C28 C24 104.7(4) . . . . ? C2 C1 C28 C62 55.4(4) . . . . ? C6 C1 C28 C62 -126.0(3) . . . . ? C23 C24 C28 C1 104.4(4) . . . . ? C25 C24 C28 C1 -73.0(4) . . . . ? C23 C24 C28 C62 -23.2(4) . . . . ? C25 C24 C28 C62 159.4(3) . . . . ? C8 C7 C29 C30 162.3(3) . . . . ? C3 C7 C29 C30 -70.7(4) . . . . ? C7 C29 C30 C31 -179.6(3) . . . . ? C29 C30 C31 C32 -74.8(4) . . . . ? C30 C31 C32 C33 -172.0(3) . . . . ? C31 C32 C33 C34 179.8(3) . . . . ? C32 C33 C34 C35 -178.0(3) . . . . ? C33 C34 C35 C36 179.1(3) . . . . ? C34 C35 C36 C37 -178.2(3) . . . . ? C35 C36 C37 C38 179.9(3) . . . . ? C36 C37 C38 C39 -178.8(3) . . . . ? C10 C14 C40 C41 -163.6(3) . . . . ? C15 C14 C40 C41 69.4(3) . . . . ? C14 C40 C41 C42 -176.9(3) . . . . ? C40 C41 C42 C43 71.5(4) . . . . ? C41 C42 C43 C44 179.0(3) . . . . ? C42 C43 C44 C45 -177.8(3) . . . . ? C43 C44 C45 C46 -178.8(3) . . . . ? C44 C45 C46 C47 -178.1(3) . . . . ? C45 C46 C47 C48 -179.2(3) . . . . ? C46 C47 C48 C49 -178.5(3) . . . . ? C47 C48 C49 C50 -179.6(4) . . . . ? C22 C21 C51 C52 172.4(3) . . . . ? C17 C21 C51 C52 -60.9(4) . . . . ? C21 C51 C52 C53 -178.3(3) . . . . ? C51 C52 C53 C54 68.9(4) . . . . ? C52 C53 C54 C55 178.7(3) . . . . ? C53 C54 C55 C56 -179.6(3) . . . . ? C54 C55 C56 C57 -179.4(3) . . . . ? C55 C56 C57 C58 -179.0(3) . . . . ? C56 C57 C58 C59 -179.9(3) . . . . ? C57 C58 C59 C60 -177.9(4) . . . . ? C58 C59 C60 C61 -178.9(4) . . . . ? C1 C28 C62 C63 60.6(4) . . . . ? C24 C28 C62 C63 -172.5(3) . . . . ? C28 C62 C63 C64 -175.9(3) . . . . ? C62 C63 C64 C65 -72.4(4) . . . . ? C63 C64 C65 C66 -168.8(3) . . . . ? C64 C65 C66 C67 175.9(3) . . . . ? C65 C66 C67 C68 -176.5(3) . . . . ? C66 C67 C68 C69 179.6(3) . . . . ? C67 C68 C69 C70 -179.6(3) . . . . ? C68 C69 C70 C71 -179.3(3) . . . . ? C69 C70 C71 C72 178.7(3) . . . . ? C1CB N1 C1C C3C -58.7(11) . . . 2 ? C3C N1 C1C C3C 75.5(7) . . . 2 ? C2CB N1 C1C C3C 18.2(12) . . . 2 ? C4C N1 C1C C3C -146.8(5) . . . 2 ? C3CB N1 C1C C3C 111.0(5) . . . 2 ? C2C N1 C1C C3C -32.2(5) . . . 2 ? C1CB N1 C2C C3C 44.4(5) . . . 2 ? C3C N1 C2C C3C -86.0(5) . . . 2 ? C2CB N1 C2C C3C -117.2(5) . . . 2 ? C1C N1 C2C C3C 29.0(5) . . . 2 ? C4C N1 C2C C3C 147.5(4) . . . 2 ? C3CB N1 C2C C3C -46.4(8) . . . 2 ? C1CB N1 C3C C1C -53.3(13) . . . 2 ? C2CB N1 C3C C1C 51.9(6) . . . 2 ? C1C N1 C3C C1C -85.3(8) . . . 2 ? C4C N1 C3C C1C 138.1(5) . . . 2 ? C3CB N1 C3C C1C -133.3(8) . . . 2 ? C2C N1 C3C C1C 16.4(6) . . . 2 ? C3C N1 C1CB C2CB -16.1(13) . . . 2 ? C2CB N1 C1CB C2CB -83.6(9) . . . 2 ? C1C N1 C1CB C2CB 47.5(10) . . . 2 ? C4C N1 C1CB C2CB 153.1(4) . . . 2 ? C3CB N1 C1CB C2CB 36.8(7) . . . 2 ? C2C N1 C1CB C2CB -103.3(6) . . . 2 ? C1CB N1 C2CB C1CB 78.9(9) . . . 2 ? C3C N1 C2CB C1CB -41.1(5) . . . 2 ? C1C N1 C2CB C1CB 38.8(12) . . . 2 ? C4C N1 C2CB C1CB -155.2(4) . . . 2 ? C3CB N1 C2CB C1CB -45.1(5) . . . 2 ? C2C N1 C2CB C1CB 99.3(5) . . . 2 ? C1CB N1 C3CB C2C -55.7(7) . . . 2 ? C3C N1 C3CB C2C 73.6(6) . . . 2 ? C2CB N1 C3CB C2C 77.8(6) . . . 2 ? C1C N1 C3CB C2C -61.7(6) . . . 2 ? C4C N1 C3CB C2C -174.1(5) . . . 2 ? C2C N1 C3CB C2C 19.5(11) . . . 2 ? C1CB N1 C4C C5C -65.5(8) . . . . ? C3C N1 C4C C5C 105.6(6) . . . . ? C2CB N1 C4C C5C 159.6(5) . . . . ? C1C N1 C4C C5C -30.2(7) . . . . ? C3CB N1 C4C C5C 53.0(5) . . . . ? C2C N1 C4C C5C -135.7(4) . . . . ? N1 C4C C5C C10C 89.9(5) . . . . ? N1 C4C C5C C6C -89.9(5) . . . . ? C10C C5C C6C C7C -1.2(6) . . . . ? C4C C5C C6C C7C 178.7(4) . . . . ? C5C C6C C7C C8C -0.2(6) . . . . ? C6C C7C C8C C9C 1.5(6) . . . . ? C7C C8C C9C C10C -1.3(6) . . . . ? C6C C5C C10C C9C 1.3(5) . . . . ? C4C C5C C10C C9C -178.5(3) . . . . ? C8C C9C C10C C5C -0.2(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O13 0.836(19) 2.05(3) 2.823(3) 154(4) . O6 H6 O7E 0.83(2) 2.05(4) 2.650(6) 129(4) . O11 H11 O20 0.835(19) 2.03(2) 2.857(4) 168(4) . O13 H13 Br1 0.828(19) 2.54(2) 3.351(2) 167(4) . O18 H18 O4E 0.832(19) 1.79(3) 2.601(12) 165(4) . O18 H18 O4EB 0.832(19) 1.88(2) 2.703(13) 171(4) . O25 H25 O6 0.86(4) 1.96(4) 2.808(4) 168(4) . O27 H27 O18 0.829(19) 2.04(2) 2.826(4) 159(4) . O6 H6 Br1 0.83(2) 2.95(3) 3.710(3) 153(4) 2_665 O20 H20 O1EB 0.836(19) 1.80(4) 2.63(4) 176(5) 2_655 O20 H20 O1E 0.836(19) 1.82(3) 2.646(17) 168(4) 2_655 O7E H7E Br1 0.84 2.36 3.055(6) 140.1 2_665 O4E H4E Br1 0.84 2.51 3.304(11) 158.6 2_655 O1EB H1EB Br1 0.84 2.70 3.51(2) 162.2 . O1E H1E Br1 0.84 2.33 3.154(14) 165.6 . O4EB H4EB Br1 0.84 2.28 3.090(12) 163.2 2_655 _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.915 _refine_diff_density_min -1.069 _refine_diff_density_rms 0.053 #==END