# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Jerry L. Atwood' _publ_contact_author_address ; Department of Chemistry University of Missouri-Columbia Columbia MO 65211 USA ; _publ_contact_author_phone '+1 (573)882 8371' _publ_contact_author_fax '+1 (573)882 2754' _publ_contact_author_email atwoodj@missouri.edu _publ_contact_letter ; The following 4 sets of data are supplementary data for the the crystal structure included in the paper, details of which are given below ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and structural characterisation of lower rim halogenated pyrogallol[4]arenes: bi-layers and hexameric nano-capsules ; loop_ _publ_author_name _publ_author_address 'Scott J. Dalgarno' ; Department of Chemistry University of Missouri-Columbia Columbia MO 65211 USA ; 'Nicholas P. Power' ; Department of Chemistry University of Missouri-Columbia Columbia MO 65211 USA ; 'Jcohen Antesberger' ; Department of Chemistry University of Missouri-Columbia Columbia MO 65211 USA ; 'Robert M. McKinlay' ; Department of Chemistry University of Missouri-Columbia Columbia MO 65211 USA ; 'Jerry L. Atwood' ; Department of Chemistry University of Missouri-Columbia Columbia MO 65211 USA ; #================================================================= data_PgC4ClMeOH _database_code_depnum_ccdc_archive 'CCDC 604862' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H64 Cl4 O15' _chemical_formula_sum 'C47 H64 Cl4 O15' _chemical_formula_weight 1010.78 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.607(11) _cell_length_b 12.792(7) _cell_length_c 19.014(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.721(9) _cell_angle_gamma 90.00 _cell_volume 4967(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9333 _exptl_absorpt_correction_T_max 0.9558 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _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 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33805 _diffrn_reflns_av_R_equivalents 0.1695 _diffrn_reflns_av_sigmaI/netI 0.2350 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.31 _reflns_number_total 10945 _reflns_number_gt 4950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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^)+(0.1149P)^2^+33.0377P] 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 10945 _refine_ls_number_parameters 629 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2562 _refine_ls_R_factor_gt 0.1352 _refine_ls_wR_factor_ref 0.3464 _refine_ls_wR_factor_gt 0.2988 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.056 _refine_ls_shift/su_mean 0.002 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 Cl1 Cl 0.056(2) 0.539(3) 0.423(2) 0.032(2) Uani 0.25 1 d P A 3 O1 O 0.4134(3) 0.3239(5) 0.8008(3) 0.0298(15) Uani 1 1 d . . . H100 H 0.4513 0.3489 0.8034 0.036 Uiso 1 1 calc R . . C1 C 0.3266(4) 0.2586(6) 0.7133(4) 0.0166(17) Uani 1 1 d . . . Cl2 Cl 0.0635(9) 0.5548(14) 0.4070(7) 0.032(2) Uani 0.60 1 d P A 2 O2 O 0.4876(3) 0.3763(5) 0.6967(3) 0.0292(14) Uani 1 1 d . . . H101 H 0.5044 0.3937 0.6606 0.035 Uiso 1 1 calc R . . C2 C 0.3882(4) 0.3077(6) 0.7294(4) 0.0202(18) Uani 1 1 d . . . Cl3 Cl 0.0590(19) 0.562(3) 0.4316(17) 0.032(2) Uani 0.15 1 d P A 1 O3 O 0.4446(3) 0.3398(4) 0.5560(3) 0.0218(13) Uani 1 1 d . . . H102 H 0.4337 0.3072 0.5179 0.026 Uiso 1 1 calc R . . C3 C 0.4262(4) 0.3337(6) 0.6760(4) 0.0172(17) Uani 1 1 d . . . Cl4 Cl -0.088(4) -0.135(6) 0.414(5) 0.043(3) Uani 0.15 1 d P B 1 O4 O 0.4405(3) 0.1620(4) 0.4754(3) 0.0187(12) Uani 1 1 d . . . H103 H 0.4761 0.1301 0.4757 0.022 Uiso 1 1 calc R . . C4 C 0.4022(4) 0.3128(6) 0.6052(4) 0.0181(17) Uani 1 1 d . . . Cl5 Cl -0.0974(9) -0.1380(11) 0.4259(8) 0.043(3) Uani 0.70 1 d P B 2 O5 O 0.4609(2) -0.0471(4) 0.4411(3) 0.0208(13) Uani 1 1 d . . . H104 H 0.4551 -0.0827 0.4036 0.025 Uiso 1 1 calc R . . C5 C 0.3406(4) 0.2640(6) 0.5860(4) 0.0163(17) Uani 1 1 d . . . Cl6 Cl -0.088(2) -0.153(3) 0.449(2) 0.043(3) Uani 0.15 1 d P B 3 O6 O 0.3685(3) -0.1930(4) 0.4508(3) 0.0204(12) Uani 1 1 d . . . H105 H 0.3363 -0.2329 0.4517 0.025 Uiso 1 1 calc R . . C6 C 0.3048(4) 0.2397(6) 0.6413(4) 0.0179(17) Uani 1 1 d . . . H6 H 0.2630 0.2082 0.6293 0.021 Uiso 1 1 calc R . . Cl7 Cl -0.0478(3) -0.3324(6) 0.7297(4) 0.0430(16) Uani 0.50 1 d P C 2 O7 O 0.2906(3) -0.3471(4) 0.4954(3) 0.0214(13) Uani 1 1 d . . . H106 H 0.2587 -0.3632 0.4649 0.026 Uiso 1 1 calc R . . C7 C 0.3160(4) 0.2392(6) 0.5075(4) 0.0154(17) Uani 1 1 d . . . H7 H 0.3436 0.2810 0.4784 0.018 Uiso 1 1 calc R . . Cl8 Cl -0.0372(4) -0.3854(8) 0.7516(4) 0.067(2) Uani 0.50 1 d P D 1 O8 O 0.3009(3) -0.4514(5) 0.6239(3) 0.0307(15) Uani 1 1 d . . . H107 H 0.3112 -0.4685 0.5841 0.037 Uiso 1 1 calc R . . C8 C 0.3273(4) 0.1232(6) 0.4909(4) 0.0147(16) Uani 1 1 d . . . Cl9 Cl 0.124(3) 0.455(3) 0.622(2) 0.061(11) Uani 0.25 1 d P E 2 O9 O 0.2575(3) -0.3665(5) 0.7409(3) 0.0344(15) Uani 1 1 d . . . H108 H 0.2749 -0.4242 0.7337 0.041 Uiso 1 1 calc R . . C9 C 0.3887(4) 0.0883(6) 0.4755(4) 0.0134(16) Uani 1 1 d . . . Cl10 Cl 0.1249(15) 0.495(3) 0.6238(12) 0.057(11) Uani 0.50 1 d P E 2 O10 O 0.3147(3) -0.2133(5) 0.8217(3) 0.0352(16) Uani 1 1 d . . . H109 H 0.3504 -0.2258 0.8470 0.042 Uiso 1 1 calc R . . C10 C 0.4001(4) -0.0164(6) 0.4594(4) 0.0169(17) Uani 1 1 d . . . Cl11 Cl 0.117(3) 0.520(7) 0.631(3) 0.074(17) Uani 0.25 1 d P F 1 O11 O 0.4132(3) -0.0827(4) 0.8787(3) 0.0225(13) Uani 1 1 d . . . H110 H 0.4124 -0.0743 0.9224 0.027 Uiso 1 1 calc R . . C11 C 0.3499(4) -0.0897(6) 0.4631(4) 0.0133(16) Uani 1 1 d . . . O12 O 0.4010(3) 0.1298(5) 0.8627(3) 0.0262(14) Uani 1 1 d . . . H111 H 0.3933 0.1932 0.8537 0.031 Uiso 1 1 calc R . . C12 C 0.2878(4) -0.0594(6) 0.4755(4) 0.0143(16) Uani 1 1 d . . . O13 O 0.4495(3) 0.6733(5) 0.8289(3) 0.0384(17) Uani 1 1 d . . . C13 C 0.2786(4) 0.0477(6) 0.4900(4) 0.0159(17) Uani 1 1 d . . . H13 H 0.2367 0.0693 0.4997 0.019 Uiso 1 1 calc R . . O14 O 0.5328(3) 0.1015(5) 0.3617(3) 0.0376(16) Uani 1 1 d . . . C14 C 0.2325(4) -0.1407(6) 0.4750(4) 0.0210(18) Uani 1 1 d . . . H14 H 0.2385 -0.1934 0.4376 0.025 Uiso 1 1 calc R . . O15 O 0.4077(3) 0.9600(5) 0.0122(3) 0.0258(14) Uani 1 1 d . . . C15 C 0.2395(4) -0.1988(6) 0.5467(4) 0.0188(18) Uani 1 1 d . . . C16 C 0.2672(4) -0.2990(6) 0.5541(4) 0.0225(18) Uani 1 1 d . . . C17 C 0.2726(4) -0.3528(6) 0.6192(4) 0.0241(19) Uani 1 1 d . . . C18 C 0.2511(4) -0.3055(7) 0.6774(4) 0.0237(19) Uani 1 1 d . . . C19 C 0.2245(4) -0.2060(7) 0.6733(4) 0.0224(19) Uani 1 1 d . . . C20 C 0.2199(4) -0.1539(6) 0.6071(4) 0.0211(18) Uani 1 1 d . . . H20 H 0.2026 -0.0850 0.6038 0.025 Uiso 1 1 calc R . . C21 C 0.1993(4) -0.1504(7) 0.7380(4) 0.0234(19) Uani 1 1 d . . . H21 H 0.1967 -0.2056 0.7748 0.028 Uiso 1 1 calc R . . C22 C 0.2505(4) -0.0717(6) 0.7704(4) 0.0169(7) Uani 1 1 d . . . C23 C 0.3080(4) -0.1080(6) 0.8115(4) 0.0169(7) Uani 1 1 d . . . C24 C 0.3573(4) -0.0389(6) 0.8408(4) 0.0169(7) Uani 1 1 d . . . C25 C 0.3501(4) 0.0695(6) 0.8294(4) 0.0169(7) Uani 1 1 d . . . C26 C 0.2945(4) 0.1096(6) 0.7880(4) 0.0169(7) Uani 1 1 d . . . C27 C 0.2465(4) 0.0384(6) 0.7593(4) 0.0169(7) Uani 1 1 d . . . H27 H 0.2089 0.0652 0.7305 0.020 Uiso 1 1 calc R . . C28 C 0.2871(4) 0.2276(6) 0.7745(4) 0.0175(17) Uani 1 1 d . . . H28 H 0.3086 0.2634 0.8183 0.021 Uiso 1 1 calc R . . C29 C 0.2445(4) 0.2717(6) 0.4837(4) 0.0181(17) Uani 1 1 d . . . H29A H 0.2167 0.2423 0.5174 0.022 Uiso 1 1 calc R . . H29B H 0.2299 0.2407 0.4365 0.022 Uiso 1 1 calc R . . C30 C 0.2337(4) 0.3908(6) 0.4791(4) 0.0191(18) Uani 1 1 d . . . H30A H 0.2441 0.4222 0.5269 0.023 Uiso 1 1 calc R . . H30B H 0.2632 0.4220 0.4478 0.023 Uiso 1 1 calc R . . C31 C 0.1622(4) 0.4142(7) 0.4494(5) 0.029(2) Uani 1 1 d . A . H31A H 0.1521 0.3818 0.4019 0.034 Uiso 1 1 calc R . . H31B H 0.1331 0.3822 0.4808 0.034 Uiso 1 1 calc R . . C32 C 0.1482(4) 0.5317(7) 0.4434(5) 0.034(2) Uani 1 1 d . . . C33 C 0.1627(4) -0.0928(6) 0.4562(4) 0.0219(18) Uani 1 1 d . . . H33A H 0.1550 -0.0425 0.4938 0.026 Uiso 1 1 calc R . . H33B H 0.1609 -0.0535 0.4112 0.026 Uiso 1 1 calc R . . C34 C 0.1070(4) -0.1755(7) 0.4485(5) 0.0249(19) Uani 1 1 d . . . H34A H 0.1103 -0.2199 0.4064 0.030 Uiso 1 1 calc R . . H34B H 0.1114 -0.2210 0.4909 0.030 Uiso 1 1 calc R . . C35 C 0.0401(4) -0.1206(7) 0.4401(5) 0.034(2) Uani 1 1 d . B . H35A H 0.0374 -0.0742 0.4813 0.041 Uiso 1 1 calc R . . H35B H 0.0350 -0.0770 0.3967 0.041 Uiso 1 1 calc R . . C36 C -0.0143(4) -0.2009(8) 0.4353(7) 0.039(3) Uani 1 1 d . . . C37 C 0.1306(4) -0.1068(10) 0.7202(5) 0.040(3) Uani 1 1 d D . . C38 C 0.0864(9) -0.2091(17) 0.7030(10) 0.025(2) Uani 0.50 1 d P C 2 H38A H 0.1059 -0.2542 0.6690 0.031 Uiso 0.50 1 calc PR C 2 H38B H 0.0845 -0.2496 0.7471 0.031 Uiso 0.50 1 calc PR C 2 C39 C 0.0164(8) -0.1754(14) 0.6707(9) 0.025(2) Uani 0.50 1 d P C 2 H39A H -0.0018 -0.1301 0.7054 0.031 Uiso 0.50 1 calc PR C 2 H39B H 0.0198 -0.1326 0.6280 0.031 Uiso 0.50 1 calc PR C 2 C40 C -0.0310(8) -0.2615(15) 0.6504(9) 0.025(2) Uani 0.50 1 d P C 2 H40A H -0.0127 -0.3102 0.6176 0.031 Uiso 0.50 1 calc PR C 2 H40B H -0.0723 -0.2323 0.6254 0.031 Uiso 0.50 1 calc PR C 2 C41 C 0.0726(15) -0.163(2) 0.6774(16) 0.065(4) Uani 0.50 1 d P D 1 H41A H 0.0351 -0.1148 0.6654 0.078 Uiso 0.50 1 calc PR D 1 H41B H 0.0850 -0.1928 0.6331 0.078 Uiso 0.50 1 calc PR D 1 C42 C 0.0569(13) -0.2452(19) 0.7258(15) 0.065(4) Uani 0.50 1 d P D 1 H42A H 0.0486 -0.2146 0.7716 0.078 Uiso 0.50 1 calc PR D 1 H42B H 0.0938 -0.2951 0.7351 0.078 Uiso 0.50 1 calc PR D 1 C43 C -0.0091(13) -0.3049(19) 0.6869(15) 0.065(4) Uani 0.50 1 d P D 1 H43A H 0.0016 -0.3475 0.6465 0.078 Uiso 0.50 1 calc PR D 1 H43B H -0.0431 -0.2532 0.6689 0.078 Uiso 0.50 1 calc PR D 1 C44 C 0.2165(4) 0.2668(6) 0.7618(4) 0.0202(18) Uani 1 1 d . . . H44A H 0.1918 0.2371 0.7983 0.024 Uiso 1 1 calc R . . H44B H 0.1955 0.2423 0.7148 0.024 Uiso 1 1 calc R . . C45 C 0.2131(5) 0.3884(7) 0.7645(6) 0.042(3) Uani 1 1 d . . . H45A H 0.2412 0.4129 0.8077 0.050 Uiso 1 1 calc R . . H45B H 0.2314 0.4171 0.7230 0.050 Uiso 1 1 calc R . . C46 C 0.1441(6) 0.4329(11) 0.7649(6) 0.064(4) Uani 1 1 d . . . C47 C 0.1003(6) 0.4170(11) 0.7000(6) 0.038(3) Uani 0.75 1 d P E 2 C48 C 0.1047(19) 0.506(4) 0.7159(19) 0.038(3) Uani 0.25 1 d P F 1 H48A H 0.1099 0.5765 0.7379 0.046 Uiso 0.25 1 calc PR F 1 H48B H 0.0582 0.4864 0.7154 0.046 Uiso 0.25 1 calc PR F 1 C49 C 0.4444(7) 0.6247(10) 0.7601(5) 0.068(4) Uani 1 1 d . . . H49A H 0.4324 0.6775 0.7233 0.102 Uiso 1 1 calc R . . H49B H 0.4107 0.5702 0.7566 0.102 Uiso 1 1 calc R . . H49C H 0.4866 0.5934 0.7536 0.102 Uiso 1 1 calc R . . C50 C 0.5950(5) 0.0744(10) 0.3423(5) 0.056(3) Uani 1 1 d . . . H50A H 0.6118 0.1329 0.3168 0.084 Uiso 1 1 calc R . . H50B H 0.5904 0.0126 0.3116 0.084 Uiso 1 1 calc R . . H50C H 0.6255 0.0591 0.3851 0.084 Uiso 1 1 calc R . . C51 C 0.4444(5) 0.8939(8) 0.0656(5) 0.037(2) Uani 1 1 d . . . H51A H 0.4914 0.9052 0.0654 0.056 Uiso 1 1 calc R . . H51B H 0.4338 0.8204 0.0550 0.056 Uiso 1 1 calc R . . H51C H 0.4327 0.9115 0.1125 0.056 Uiso 1 1 calc R . . H36A H -0.019(5) -0.244(8) 0.392(5) 0.05(3) Uiso 1 1 d . . . H36B H -0.010(4) -0.243(7) 0.480(4) 0.03(2) Uiso 1 1 d . . . H37A H 0.136(4) -0.040(3) 0.697(4) 0.03(2) Uiso 1 1 d D . . H37B H 0.114(6) -0.067(8) 0.759(4) 0.08(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.022(4) 0.026(4) 0.045(7) -0.008(4) -0.009(4) 0.009(3) O1 0.027(3) 0.042(4) 0.018(3) 0.000(3) -0.004(2) -0.011(3) C1 0.018(4) 0.019(4) 0.012(4) 0.004(3) -0.001(3) 0.004(3) Cl2 0.022(4) 0.026(4) 0.045(7) -0.008(4) -0.009(4) 0.009(3) O2 0.023(3) 0.044(4) 0.020(3) 0.001(3) 0.000(2) -0.018(3) C2 0.024(4) 0.021(5) 0.014(4) 0.004(3) -0.003(3) 0.009(4) Cl3 0.022(4) 0.026(4) 0.045(7) -0.008(4) -0.009(4) 0.009(3) O3 0.022(3) 0.034(4) 0.010(2) 0.003(2) 0.003(2) -0.006(3) C3 0.023(4) 0.018(4) 0.010(3) -0.004(3) -0.002(3) -0.001(3) Cl4 0.012(6) 0.045(3) 0.069(11) 0.003(5) -0.003(3) 0.006(3) O4 0.015(3) 0.010(3) 0.030(3) -0.002(2) 0.002(2) -0.003(2) C4 0.020(4) 0.019(4) 0.017(4) 0.002(3) 0.008(3) -0.005(3) Cl5 0.012(6) 0.045(3) 0.069(11) 0.003(5) -0.003(3) 0.006(3) O5 0.020(3) 0.027(3) 0.016(3) -0.008(2) 0.003(2) 0.002(2) C5 0.020(4) 0.013(4) 0.016(4) 0.004(3) 0.002(3) 0.012(3) Cl6 0.012(6) 0.045(3) 0.069(11) 0.003(5) -0.003(3) 0.006(3) O6 0.017(3) 0.015(3) 0.029(3) -0.008(2) 0.003(2) -0.002(2) C6 0.015(4) 0.018(4) 0.021(4) -0.004(3) 0.001(3) -0.002(3) Cl7 0.031(3) 0.052(5) 0.046(4) 0.002(3) 0.006(3) -0.020(3) O7 0.019(3) 0.027(3) 0.018(3) -0.002(2) 0.000(2) -0.002(2) C7 0.019(4) 0.013(4) 0.013(4) 0.002(3) 0.003(3) 0.010(3) Cl8 0.052(4) 0.090(7) 0.059(5) -0.016(4) 0.007(4) -0.008(5) O8 0.037(4) 0.029(4) 0.024(3) -0.003(3) -0.004(3) 0.003(3) C8 0.017(4) 0.017(4) 0.010(3) -0.002(3) 0.003(3) 0.001(3) Cl9 0.08(2) 0.05(2) 0.050(13) 0.019(14) 0.001(12) 0.017(18) O9 0.052(4) 0.020(3) 0.032(3) 0.011(3) 0.008(3) -0.004(3) C9 0.019(4) 0.012(4) 0.009(3) -0.001(3) -0.001(3) -0.001(3) Cl10 0.066(13) 0.08(3) 0.019(5) -0.007(11) 0.007(7) -0.032(17) O10 0.048(4) 0.028(4) 0.024(3) 0.003(3) -0.017(3) 0.004(3) C10 0.017(4) 0.025(5) 0.008(3) -0.007(3) 0.000(3) 0.000(3) Cl11 0.076(16) 0.08(3) 0.07(3) 0.02(3) -0.007(17) 0.010(14) O11 0.027(3) 0.029(3) 0.009(3) 0.003(2) -0.006(2) 0.011(3) C11 0.018(4) 0.012(4) 0.009(3) 0.003(3) -0.004(3) 0.001(3) O12 0.016(3) 0.025(3) 0.034(3) -0.003(3) -0.011(2) 0.003(3) C12 0.020(4) 0.015(4) 0.006(3) -0.002(3) -0.006(3) 0.003(3) O13 0.055(4) 0.038(4) 0.024(3) 0.003(3) 0.010(3) -0.009(3) C13 0.013(4) 0.019(4) 0.016(4) 0.002(3) 0.005(3) 0.006(3) O14 0.020(3) 0.056(5) 0.037(4) 0.004(3) 0.005(3) 0.012(3) C14 0.019(4) 0.020(5) 0.023(4) 0.002(4) 0.000(3) 0.007(4) O15 0.027(3) 0.031(4) 0.018(3) 0.003(3) -0.001(2) 0.004(3) C15 0.014(4) 0.022(5) 0.020(4) -0.001(3) -0.003(3) -0.010(3) C16 0.024(5) 0.015(4) 0.027(4) 0.005(4) -0.001(4) 0.000(4) C17 0.031(5) 0.017(5) 0.022(4) 0.001(4) -0.008(4) -0.003(4) C18 0.025(5) 0.021(5) 0.024(4) 0.003(4) 0.004(4) -0.008(4) C19 0.020(4) 0.023(5) 0.024(4) -0.001(4) 0.004(3) -0.007(4) C20 0.016(4) 0.015(4) 0.031(5) -0.001(4) -0.001(3) -0.004(3) C21 0.033(5) 0.025(5) 0.013(4) -0.003(3) 0.006(3) -0.011(4) C22 0.0164(16) 0.0237(18) 0.0104(14) 0.0013(13) 0.0009(12) 0.0027(14) C23 0.0164(16) 0.0237(18) 0.0104(14) 0.0013(13) 0.0009(12) 0.0027(14) C24 0.0164(16) 0.0237(18) 0.0104(14) 0.0013(13) 0.0009(12) 0.0027(14) C25 0.0164(16) 0.0237(18) 0.0104(14) 0.0013(13) 0.0009(12) 0.0027(14) C26 0.0164(16) 0.0237(18) 0.0104(14) 0.0013(13) 0.0009(12) 0.0027(14) C27 0.0164(16) 0.0237(18) 0.0104(14) 0.0013(13) 0.0009(12) 0.0027(14) C28 0.021(4) 0.021(5) 0.010(4) 0.004(3) 0.004(3) 0.004(3) C29 0.022(4) 0.021(5) 0.010(4) -0.002(3) -0.001(3) 0.003(4) C30 0.022(4) 0.022(5) 0.014(4) -0.001(3) 0.004(3) 0.000(4) C31 0.020(5) 0.022(5) 0.041(5) -0.001(4) -0.004(4) 0.003(4) C32 0.011(4) 0.028(5) 0.060(6) -0.007(5) -0.005(4) 0.007(4) C33 0.019(4) 0.024(5) 0.023(4) -0.010(4) 0.003(3) -0.001(4) C34 0.015(4) 0.021(5) 0.035(5) 0.000(4) -0.008(4) 0.001(4) C35 0.021(5) 0.026(5) 0.053(6) -0.005(4) -0.004(4) 0.007(4) C36 0.011(5) 0.038(6) 0.064(8) 0.005(6) -0.001(5) -0.001(4) C37 0.020(5) 0.073(8) 0.027(5) -0.012(5) 0.006(4) -0.013(5) C38 0.020(6) 0.028(7) 0.027(6) 0.002(5) -0.001(4) -0.017(5) C39 0.020(6) 0.028(7) 0.027(6) 0.002(5) -0.001(4) -0.017(5) C40 0.020(6) 0.028(7) 0.027(6) 0.002(5) -0.001(4) -0.017(5) C41 0.064(11) 0.038(9) 0.093(13) -0.007(8) 0.012(10) -0.022(8) C42 0.064(11) 0.038(9) 0.093(13) -0.007(8) 0.012(10) -0.022(8) C43 0.064(11) 0.038(9) 0.093(13) -0.007(8) 0.012(10) -0.022(8) C44 0.012(4) 0.021(5) 0.029(4) 0.011(4) 0.007(3) -0.001(3) C45 0.047(6) 0.029(6) 0.054(6) 0.016(5) 0.026(5) 0.019(5) C46 0.058(8) 0.095(10) 0.041(6) 0.029(6) 0.013(6) 0.049(7) C47 0.039(7) 0.051(9) 0.026(6) 0.004(6) 0.011(5) 0.008(7) C48 0.039(7) 0.051(9) 0.026(6) 0.004(6) 0.011(5) 0.008(7) C49 0.100(11) 0.068(9) 0.035(6) -0.003(6) 0.001(6) 0.031(8) C50 0.034(6) 0.108(10) 0.027(5) 0.016(6) 0.008(4) 0.020(6) C51 0.032(5) 0.044(6) 0.035(5) 0.003(5) -0.001(4) 0.005(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 Cl1 C32 1.89(4) . ? O1 C2 1.402(9) . ? C1 C6 1.404(10) . ? C1 C2 1.413(11) . ? C1 C28 1.558(10) . ? Cl2 C32 1.81(2) . ? O2 C3 1.386(9) . ? C2 C3 1.403(11) . ? Cl3 C32 1.86(4) . ? O3 C4 1.406(8) . ? C3 C4 1.396(10) . ? Cl4 C36 1.74(10) . ? O4 C9 1.424(9) . ? C4 C5 1.418(11) . ? Cl5 C36 1.88(2) . ? O5 C10 1.401(9) . ? C5 C6 1.398(10) . ? C5 C7 1.543(10) . ? Cl6 C36 1.69(5) . ? O6 C11 1.405(9) . ? Cl7 C40 1.832(18) . ? O7 C16 1.414(9) . ? C7 C29 1.538(10) . ? C7 C8 1.542(11) . ? Cl8 C43 1.76(3) . ? O8 C17 1.388(10) . ? C8 C13 1.391(11) . ? C8 C9 1.408(10) . ? Cl9 Cl10 0.51(5) . ? Cl9 C47 1.70(4) . ? O9 C18 1.429(10) . ? C9 C10 1.401(11) . ? Cl10 C47 1.88(3) . ? O10 C23 1.366(10) . ? C10 C11 1.405(11) . ? Cl11 C48 1.68(6) . ? O11 C24 1.393(9) . ? C11 C12 1.387(10) . ? O12 C25 1.385(9) . ? C12 C13 1.415(10) . ? C12 C14 1.541(11) . ? O13 C49 1.440(12) . ? O14 C50 1.423(11) . ? C14 C15 1.543(11) . ? C14 C33 1.561(11) . ? O15 C51 1.453(10) . ? C15 C16 1.402(11) . ? C15 C20 1.391(11) . ? C16 C17 1.409(11) . ? C17 C18 1.384(11) . ? C18 C19 1.383(12) . ? C19 C20 1.416(11) . ? C19 C21 1.570(11) . ? C21 C37 1.517(13) . ? C21 C22 1.527(11) . ? C22 C23 1.408(10) . ? C22 C27 1.425(11) . ? C23 C24 1.404(11) . ? C24 C25 1.408(11) . ? C25 C26 1.397(10) . ? C26 C27 1.400(11) . ? C26 C28 1.535(11) . ? C28 C44 1.527(10) . ? C29 C30 1.541(11) . ? C30 C31 1.534(11) . ? C31 C32 1.532(12) . ? C33 C34 1.554(11) . ? C34 C35 1.536(11) . ? C35 C36 1.514(13) . ? C37 C41 1.53(3) . ? C37 C38 1.60(2) . ? C38 C39 1.55(3) . ? C39 C40 1.49(2) . ? C41 C42 1.46(3) . ? C42 C43 1.65(3) . ? C44 C45 1.559(12) . ? C45 C46 1.532(14) . ? C46 C47 1.442(17) . ? C46 C48 1.49(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 C6 C1 C2 116.6(7) . . ? C6 C1 C28 123.7(7) . . ? C2 C1 C28 119.7(6) . . ? C3 C2 O1 119.7(7) . . ? C3 C2 C1 121.4(7) . . ? O1 C2 C1 118.8(7) . . ? O2 C3 C2 117.6(6) . . ? O2 C3 C4 122.8(7) . . ? C2 C3 C4 119.6(7) . . ? C3 C4 C5 121.4(6) . . ? C3 C4 O3 115.0(7) . . ? C5 C4 O3 123.5(6) . . ? C6 C5 C4 116.6(7) . . ? C6 C5 C7 123.0(7) . . ? C4 C5 C7 120.4(6) . . ? C5 C6 C1 124.4(7) . . ? C29 C7 C5 114.0(6) . . ? C29 C7 C8 111.4(6) . . ? C5 C7 C8 110.9(6) . . ? C13 C8 C9 116.3(7) . . ? C13 C8 C7 122.8(7) . . ? C9 C8 C7 120.9(7) . . ? Cl10 Cl9 C47 103(7) . . ? C10 C9 C8 122.1(7) . . ? C10 C9 O4 119.0(6) . . ? C8 C9 O4 118.9(6) . . ? Cl9 Cl10 C47 62(6) . . ? O5 C10 C9 120.3(7) . . ? O5 C10 C11 121.0(7) . . ? C9 C10 C11 118.7(7) . . ? C12 C11 C10 121.7(7) . . ? C12 C11 O6 124.8(7) . . ? C10 C11 O6 113.5(6) . . ? C11 C12 C13 117.0(7) . . ? C11 C12 C14 120.5(7) . . ? C13 C12 C14 122.4(7) . . ? C8 C13 C12 124.0(7) . . ? C12 C14 C15 109.8(6) . . ? C12 C14 C33 113.2(7) . . ? C15 C14 C33 111.4(6) . . ? C16 C15 C20 117.0(7) . . ? C16 C15 C14 121.1(7) . . ? C20 C15 C14 121.9(7) . . ? C15 C16 O7 119.7(7) . . ? C15 C16 C17 121.1(8) . . ? O7 C16 C17 119.1(7) . . ? O8 C17 C18 121.6(7) . . ? O8 C17 C16 118.9(7) . . ? C18 C17 C16 119.5(8) . . ? C19 C18 C17 121.6(7) . . ? C19 C18 O9 122.7(7) . . ? C17 C18 O9 115.7(7) . . ? C18 C19 C20 117.5(7) . . ? C18 C19 C21 123.0(7) . . ? C20 C19 C21 119.6(7) . . ? C15 C20 C19 123.2(8) . . ? C37 C21 C22 114.9(7) . . ? C37 C21 C19 112.9(7) . . ? C22 C21 C19 109.4(6) . . ? C23 C22 C27 115.8(7) . . ? C23 C22 C21 119.4(7) . . ? C27 C22 C21 124.7(7) . . ? O10 C23 C24 120.8(7) . . ? O10 C23 C22 117.7(7) . . ? C24 C23 C22 121.5(7) . . ? O11 C24 C23 117.1(7) . . ? O11 C24 C25 122.7(7) . . ? C23 C24 C25 120.2(7) . . ? O12 C25 C26 124.5(7) . . ? O12 C25 C24 114.8(6) . . ? C26 C25 C24 120.7(7) . . ? C25 C26 C27 117.6(7) . . ? C25 C26 C28 120.7(7) . . ? C27 C26 C28 121.7(7) . . ? C26 C27 C22 124.1(7) . . ? C44 C28 C26 114.9(6) . . ? C44 C28 C1 112.3(6) . . ? C26 C28 C1 109.0(6) . . ? C7 C29 C30 114.2(6) . . ? C31 C30 C29 109.8(7) . . ? C32 C31 C30 112.4(7) . . ? C31 C32 Cl2 110.5(8) . . ? C31 C32 Cl1 104.0(14) . . ? Cl2 C32 Cl1 12.3(12) . . ? C31 C32 Cl3 112.9(14) . . ? Cl2 C32 Cl3 15.5(10) . . ? Cl1 C32 Cl3 10.4(15) . . ? C34 C33 C14 113.7(7) . . ? C35 C34 C33 109.9(7) . . ? C36 C35 C34 110.0(7) . . ? C35 C36 Cl6 114.6(14) . . ? C35 C36 Cl4 108(2) . . ? Cl6 C36 Cl4 24(4) . . ? C35 C36 Cl5 111.9(8) . . ? Cl6 C36 Cl5 14.9(11) . . ? Cl4 C36 Cl5 9(3) . . ? C21 C37 C41 125.8(14) . . ? C21 C37 C38 103.4(11) . . ? C41 C37 C38 29.2(10) . . ? C39 C38 C37 109.0(15) . . ? C40 C39 C38 116.1(16) . . ? C39 C40 Cl7 110.0(12) . . ? C42 C41 C37 103(2) . . ? C41 C42 C43 107(2) . . ? C42 C43 Cl8 106.7(19) . . ? C28 C44 C45 111.6(7) . . ? C46 C45 C44 114.6(9) . . ? C47 C46 C48 47.7(17) . . ? C47 C46 C45 114.7(10) . . ? C48 C46 C45 131.4(16) . . ? C46 C47 Cl9 119(2) . . ? C46 C47 Cl10 112.4(13) . . ? Cl9 C47 Cl10 15.4(17) . . ? C46 C48 Cl11 122(4) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.31 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.690 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.118 #===END data_PgC4ClEtOAc _database_code_depnum_ccdc_archive 'CCDC 604863' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H64 Cl4 O15' _chemical_formula_sum 'C50 H64 Cl4 O15' _chemical_formula_weight 1046.81 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.048(4) _cell_length_b 12.069(4) _cell_length_c 18.233(6) _cell_angle_alpha 95.141(5) _cell_angle_beta 93.711(6) _cell_angle_gamma 106.383(5) _cell_volume 2522.1(14) _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 Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.302 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9094 _exptl_absorpt_correction_T_max 0.9392 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _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 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14554 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.12 _reflns_number_total 10780 _reflns_number_gt 7993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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^)+(0.0789P)^2^+2.6762P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10780 _refine_ls_number_parameters 648 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1669 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Cl1 Cl 0.16576(7) 0.45335(7) 0.39423(4) 0.03739(19) Uani 1 1 d . . . Cl2 Cl -0.31147(10) 0.07067(10) 0.42439(5) 0.0619(3) Uani 1 1 d . . . Cl3 Cl -0.59982(10) 0.25319(10) 0.45497(5) 0.0668(3) Uani 1 1 d . . . Cl4 Cl 0.06993(8) 1.15668(9) 0.56126(6) 0.0598(3) Uani 1 1 d . . . O1 O 0.08732(17) 0.99207(16) 0.91809(10) 0.0267(4) Uani 1 1 d . . . H100 H 0.0864 0.9815 0.9630 0.032 Uiso 1 1 calc R . . O2 O 0.26614(15) 0.91396(15) 0.96730(9) 0.0214(4) Uani 1 1 d . . . H101 H 0.2456 0.8755 1.0028 0.026 Uiso 1 1 calc R . . O3 O 0.31242(15) 0.72504(15) 0.88828(10) 0.0236(4) Uani 1 1 d . . . H102 H 0.3460 0.7652 0.9277 0.028 Uiso 1 1 calc R . . O4 O 0.31141(15) 0.49849(15) 0.85374(11) 0.0265(4) Uani 1 1 d . . . H103 H 0.3233 0.5704 0.8639 0.032 Uiso 1 1 calc R . . O5 O 0.21160(17) 0.29274(17) 0.90124(11) 0.0322(5) Uani 1 1 d . . . H104 H 0.2798 0.3371 0.9097 0.039 Uiso 1 1 calc R . . O6 O -0.01452(16) 0.17674(15) 0.86300(11) 0.0274(4) Uani 1 1 d . . . H105 H -0.0097 0.1884 0.9094 0.033 Uiso 1 1 calc R . . O7 O -0.24745(17) 0.16092(17) 0.89541(11) 0.0291(4) Uani 1 1 d . . . H106 H -0.1895 0.1555 0.8737 0.035 Uiso 1 1 calc R . . O8 O -0.41112(15) 0.23197(16) 0.96954(9) 0.0223(4) Uani 1 1 d . . . H107 H -0.4611 0.1677 0.9566 0.027 Uiso 1 1 calc R . . O9 O -0.50058(15) 0.39500(15) 0.92197(10) 0.0228(4) Uani 1 1 d . . . H108 H -0.5067 0.4603 0.9133 0.027 Uiso 1 1 calc R . . O10 O -0.46709(16) 0.63027(15) 0.92742(10) 0.0270(4) Uani 1 1 d . . . H109 H -0.4724 0.6698 0.9667 0.032 Uiso 1 1 calc R . . O11 O -0.3345(2) 0.84075(17) 0.99260(12) 0.0389(5) Uani 1 1 d . . . H110 H -0.2877 0.9062 1.0072 0.047 Uiso 1 1 calc R . . O12 O -0.14149(16) 0.96321(15) 0.92953(10) 0.0237(4) Uani 1 1 d . . . H111 H -0.0721 0.9752 0.9201 0.028 Uiso 1 1 calc R . . O13 O 0.5306(3) -0.0325(2) 0.10949(16) 0.0714(9) Uani 1 1 d . . . O14 O 0.5583(2) 0.0291(2) 0.23044(13) 0.0517(6) Uani 1 1 d . . . C53 C -0.1128(11) 0.5999(12) 0.9327(8) 0.061(4) Uani 0.50 1 d P . . O16 O 0.0000 0.5000 1.0000 0.0595(11) Uani 1 2 d S . . C1 C 0.0332(2) 0.8418(2) 0.81398(13) 0.0163(5) Uani 1 1 d . . . C2 C 0.1054(2) 0.8968(2) 0.87786(13) 0.0181(5) Uani 1 1 d . . . C3 C 0.1976(2) 0.8579(2) 0.90306(13) 0.0184(5) Uani 1 1 d . . . C4 C 0.2218(2) 0.7647(2) 0.86376(13) 0.0186(5) Uani 1 1 d . . . C5 C 0.1550(2) 0.7101(2) 0.79795(13) 0.0173(5) Uani 1 1 d . . . C6 C 0.0613(2) 0.7497(2) 0.77550(13) 0.0177(5) Uani 1 1 d . . . H6 H 0.0141 0.7118 0.7316 0.021 Uiso 1 1 calc R . . C7 C 0.1867(2) 0.6117(2) 0.75347(13) 0.0182(5) Uani 1 1 d . . . H7 H 0.2728 0.6276 0.7627 0.022 Uiso 1 1 calc R . . C8 C 0.1314(2) 0.4942(2) 0.78121(13) 0.0177(5) Uani 1 1 d . . . C9 C 0.1961(2) 0.4475(2) 0.82905(14) 0.0203(5) Uani 1 1 d . . . C10 C 0.1475(2) 0.3408(2) 0.85475(14) 0.0222(5) Uani 1 1 d . . . C11 C 0.0316(2) 0.2809(2) 0.83460(14) 0.0210(5) Uani 1 1 d . . . C12 C -0.0362(2) 0.3237(2) 0.78617(14) 0.0193(5) Uani 1 1 d . . . C13 C 0.0155(2) 0.4305(2) 0.76066(14) 0.0195(5) Uani 1 1 d . . . H13 H -0.0301 0.4611 0.7280 0.023 Uiso 1 1 calc R . . C14 C -0.1617(2) 0.2536(2) 0.76134(14) 0.0199(5) Uani 1 1 d . . . H14 H -0.1697 0.1728 0.7736 0.024 Uiso 1 1 calc R . . C15 C -0.2478(2) 0.2977(2) 0.80551(13) 0.0182(5) Uani 1 1 d . . . C16 C -0.2872(2) 0.2478(2) 0.86926(14) 0.0206(5) Uani 1 1 d . . . C17 C -0.3710(2) 0.2829(2) 0.90678(13) 0.0194(5) Uani 1 1 d . . . C18 C -0.4145(2) 0.3699(2) 0.88286(14) 0.0187(5) Uani 1 1 d . . . C19 C -0.3749(2) 0.4244(2) 0.82105(13) 0.0167(5) Uani 1 1 d . . . C20 C -0.2911(2) 0.3864(2) 0.78439(13) 0.0180(5) Uani 1 1 d . . . H20 H -0.2623 0.4234 0.7428 0.022 Uiso 1 1 calc R . . C21 C -0.4226(2) 0.5194(2) 0.79345(13) 0.0177(5) Uani 1 1 d . . . H21 H -0.5009 0.5082 0.8121 0.021 Uiso 1 1 calc R . . C22 C -0.3476(2) 0.6400(2) 0.82693(13) 0.0169(5) Uani 1 1 d . . . C23 C -0.3727(2) 0.6900(2) 0.89361(14) 0.0208(5) Uani 1 1 d . . . C24 C -0.3042(2) 0.7980(2) 0.92628(14) 0.0244(5) Uani 1 1 d . . . C25 C -0.2077(2) 0.8577(2) 0.89290(13) 0.0187(5) Uani 1 1 d . . . C26 C -0.1801(2) 0.8122(2) 0.82552(13) 0.0171(5) Uani 1 1 d . . . C27 C -0.2508(2) 0.7031(2) 0.79453(13) 0.0180(5) Uani 1 1 d . . . H27 H -0.2324 0.6703 0.7493 0.022 Uiso 1 1 calc R . . C28 C -0.0734(2) 0.8792(2) 0.78958(13) 0.0179(5) Uani 1 1 d . . . H28 H -0.0567 0.9629 0.8092 0.022 Uiso 1 1 calc R . . C29 C 0.1600(2) 0.6118(2) 0.66977(14) 0.0222(5) Uani 1 1 d . . . H29A H 0.0747 0.5902 0.6581 0.027 Uiso 1 1 calc R . . H29B H 0.1928 0.6917 0.6568 0.027 Uiso 1 1 calc R . . C30 C 0.2079(3) 0.5295(3) 0.62179(15) 0.0284(6) Uani 1 1 d . . . H30A H 0.1761 0.4493 0.6344 0.034 Uiso 1 1 calc R . . H30B H 0.2935 0.5519 0.6317 0.034 Uiso 1 1 calc R . . C31 C 0.1754(3) 0.5336(3) 0.53986(16) 0.0364(7) Uani 1 1 d . . . H31A H 0.0900 0.5171 0.5314 0.044 Uiso 1 1 calc R . . H31B H 0.2111 0.6132 0.5272 0.044 Uiso 1 1 calc R . . C32 C 0.2127(3) 0.4499(3) 0.48952(16) 0.0374(7) Uani 1 1 d . . . H32A H 0.1800 0.3704 0.5033 0.045 Uiso 1 1 calc R . . H32B H 0.2984 0.4688 0.4956 0.045 Uiso 1 1 calc R . . C33 C -0.1912(2) 0.2438(2) 0.67697(15) 0.0247(6) Uani 1 1 d . . . H33A H -0.1985 0.3192 0.6633 0.030 Uiso 1 1 calc R . . H33B H -0.1267 0.2268 0.6515 0.030 Uiso 1 1 calc R . . C34 C -0.3038(3) 0.1487(3) 0.65068(17) 0.0391(7) Uani 1 1 d . . . H34A H -0.3669 0.1651 0.6779 0.047 Uiso 1 1 calc R . . H34B H -0.2950 0.0738 0.6641 0.047 Uiso 1 1 calc R . . C35 C -0.3412(3) 0.1347(3) 0.56786(19) 0.0448(8) Uani 1 1 d . . . H35A H -0.4202 0.0796 0.5581 0.054 Uiso 1 1 calc R . . H35B H -0.3451 0.2107 0.5533 0.054 Uiso 1 1 calc R . . C36 C -0.2614(3) 0.0918(4) 0.5212(2) 0.0535(10) Uani 1 1 d . . . H36A H -0.2549 0.0173 0.5369 0.064 Uiso 1 1 calc R . . H36B H -0.1831 0.1486 0.5290 0.064 Uiso 1 1 calc R . . C37 C -0.4413(2) 0.5094(2) 0.70837(14) 0.0206(5) Uani 1 1 d . . . H37A H -0.4725 0.5729 0.6942 0.025 Uiso 1 1 calc R . . H37B H -0.3652 0.5203 0.6881 0.025 Uiso 1 1 calc R . . C38 C -0.5242(2) 0.3933(2) 0.67337(15) 0.0254(6) Uani 1 1 d . . . H38A H -0.5015 0.3290 0.6941 0.031 Uiso 1 1 calc R . . H38B H -0.6042 0.3885 0.6856 0.031 Uiso 1 1 calc R . . C39 C -0.5220(2) 0.3800(3) 0.58952(16) 0.0304(6) Uani 1 1 d . . . H39A H -0.5434 0.4452 0.5691 0.036 Uiso 1 1 calc R . . H39B H -0.4420 0.3842 0.5775 0.036 Uiso 1 1 calc R . . C40 C -0.6040(3) 0.2670(3) 0.55361(17) 0.0385(7) Uani 1 1 d . . . H40A H -0.6841 0.2627 0.5654 0.046 Uiso 1 1 calc R . . H40B H -0.5827 0.2016 0.5739 0.046 Uiso 1 1 calc R . . C41 C -0.0978(2) 0.8716(2) 0.70484(14) 0.0215(5) Uani 1 1 d . . . H41A H -0.1161 0.7893 0.6839 0.026 Uiso 1 1 calc R . . H41B H -0.1673 0.8977 0.6938 0.026 Uiso 1 1 calc R . . C42 C 0.0030(2) 0.9442(2) 0.66600(15) 0.0273(6) Uani 1 1 d . . . H42A H 0.0700 0.9125 0.6719 0.033 Uiso 1 1 calc R . . H42B H -0.0213 0.9369 0.6124 0.033 Uiso 1 1 calc R . . C43 C 0.0409(3) 1.0714(3) 0.69610(18) 0.0353(7) Uani 1 1 d . . . H43A H 0.0744 1.0788 0.7480 0.042 Uiso 1 1 calc R . . H43B H -0.0286 1.0998 0.6965 0.042 Uiso 1 1 calc R . . C44 C 0.1293(3) 1.1491(3) 0.65322(19) 0.0463(8) Uani 1 1 d . . . H44A H 0.1974 1.1190 0.6501 0.056 Uiso 1 1 calc R . . H44B H 0.1563 1.2283 0.6801 0.056 Uiso 1 1 calc R . . C45 C 0.5757(3) -0.0338(3) 0.1729(2) 0.0540(10) Uani 1 1 d . . . C46 C 0.6526(4) -0.1063(4) 0.1929(3) 0.0715(13) Uani 1 1 d . . . H46A H 0.6111 -0.1674 0.2215 0.107 Uiso 1 1 calc R . . H46B H 0.7228 -0.0573 0.2226 0.107 Uiso 1 1 calc R . . H46C H 0.6744 -0.1419 0.1477 0.107 Uiso 1 1 calc R . . C47 C 0.4780(4) 0.0995(4) 0.2172(2) 0.0548(10) Uani 1 1 d . . . H47A H 0.5052 0.1519 0.1792 0.066 Uiso 1 1 calc R . . H47B H 0.3990 0.0484 0.1998 0.066 Uiso 1 1 calc R . . C48 C 0.4763(4) 0.1669(4) 0.2875(2) 0.0591(10) Uani 1 1 d . . . H48A H 0.4490 0.1140 0.3245 0.089 Uiso 1 1 calc R . . H48B H 0.4240 0.2151 0.2810 0.089 Uiso 1 1 calc R . . H48C H 0.5550 0.2168 0.3041 0.089 Uiso 1 1 calc R . . C49 C -0.0033(6) 0.5998(6) 0.9790(4) 0.0402(15) Uani 0.50 1 d P . . O50 O 0.0731(5) 0.6843(4) 1.0044(3) 0.0574(14) Uani 0.50 1 d P . . C51 C -0.0999(7) 0.5161(6) 0.9656(5) 0.053(2) Uani 0.50 1 d P . . C52 C -0.0712(10) 0.6363(11) 0.9469(6) 0.045(2) 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 Cl1 0.0412(4) 0.0499(5) 0.0213(3) 0.0002(3) 0.0020(3) 0.0150(3) Cl2 0.0721(7) 0.0739(7) 0.0357(5) -0.0054(4) 0.0009(4) 0.0193(5) Cl3 0.0843(7) 0.0752(7) 0.0309(5) -0.0199(4) -0.0004(5) 0.0161(6) Cl4 0.0466(5) 0.0713(6) 0.0594(6) 0.0412(5) 0.0068(4) 0.0028(4) O1 0.0395(11) 0.0233(10) 0.0198(9) -0.0045(7) -0.0005(8) 0.0159(8) O2 0.0262(9) 0.0190(9) 0.0172(9) 0.0002(7) -0.0016(7) 0.0049(7) O3 0.0243(9) 0.0239(9) 0.0240(10) -0.0027(7) -0.0047(7) 0.0121(8) O4 0.0192(9) 0.0176(9) 0.0415(11) 0.0019(8) -0.0038(8) 0.0054(7) O5 0.0310(10) 0.0256(10) 0.0403(12) 0.0099(8) -0.0080(9) 0.0092(8) O6 0.0311(10) 0.0194(9) 0.0325(11) 0.0082(8) 0.0073(8) 0.0062(8) O7 0.0321(10) 0.0350(11) 0.0314(11) 0.0153(8) 0.0137(8) 0.0220(9) O8 0.0220(9) 0.0245(9) 0.0198(9) 0.0077(7) 0.0048(7) 0.0039(7) O9 0.0259(9) 0.0221(9) 0.0251(10) 0.0070(7) 0.0113(7) 0.0110(7) O10 0.0303(10) 0.0211(9) 0.0252(10) -0.0038(7) 0.0138(8) 0.0000(8) O11 0.0541(13) 0.0214(10) 0.0330(12) -0.0083(8) 0.0269(10) -0.0036(9) O12 0.0262(9) 0.0171(9) 0.0244(10) -0.0030(7) 0.0031(7) 0.0022(7) O13 0.097(2) 0.0470(16) 0.0500(18) -0.0090(13) 0.0266(16) -0.0111(15) O14 0.0581(15) 0.0624(16) 0.0386(14) -0.0058(12) 0.0021(11) 0.0279(13) C53 0.058(8) 0.057(8) 0.065(7) 0.004(5) -0.024(6) 0.019(6) O16 0.055(2) 0.0350(19) 0.089(3) 0.0176(18) -0.018(2) 0.0153(17) C1 0.0159(11) 0.0152(11) 0.0165(12) 0.0021(9) 0.0025(9) 0.0021(9) C2 0.0218(12) 0.0151(11) 0.0185(12) 0.0002(9) 0.0051(9) 0.0071(9) C3 0.0203(12) 0.0168(11) 0.0164(12) 0.0010(9) 0.0002(9) 0.0035(9) C4 0.0200(12) 0.0166(12) 0.0194(12) 0.0043(9) 0.0024(9) 0.0046(10) C5 0.0191(12) 0.0142(11) 0.0181(12) 0.0021(9) 0.0038(9) 0.0034(9) C6 0.0185(11) 0.0166(11) 0.0164(12) 0.0007(9) 0.0018(9) 0.0026(9) C7 0.0183(12) 0.0165(12) 0.0197(12) 0.0006(9) 0.0040(9) 0.0047(9) C8 0.0203(12) 0.0152(11) 0.0189(12) 0.0011(9) 0.0043(9) 0.0067(9) C9 0.0172(12) 0.0185(12) 0.0241(13) -0.0022(10) 0.0007(9) 0.0052(10) C10 0.0270(13) 0.0187(12) 0.0231(13) 0.0030(10) 0.0008(10) 0.0102(10) C11 0.0253(13) 0.0161(12) 0.0231(13) 0.0028(10) 0.0054(10) 0.0073(10) C12 0.0182(12) 0.0173(12) 0.0232(13) 0.0007(9) 0.0048(9) 0.0064(10) C13 0.0206(12) 0.0181(12) 0.0214(12) 0.0011(9) 0.0027(9) 0.0082(10) C14 0.0185(12) 0.0167(12) 0.0260(13) 0.0040(10) 0.0059(10) 0.0060(10) C15 0.0149(11) 0.0186(12) 0.0190(12) 0.0011(9) 0.0021(9) 0.0018(9) C16 0.0191(12) 0.0217(12) 0.0217(13) 0.0061(10) 0.0007(10) 0.0065(10) C17 0.0174(11) 0.0219(12) 0.0172(12) 0.0037(9) 0.0020(9) 0.0021(10) C18 0.0154(11) 0.0198(12) 0.0196(12) -0.0001(9) 0.0018(9) 0.0035(9) C19 0.0154(11) 0.0158(11) 0.0166(12) -0.0010(9) -0.0014(9) 0.0021(9) C20 0.0167(11) 0.0182(12) 0.0169(12) 0.0017(9) 0.0018(9) 0.0012(9) C21 0.0164(11) 0.0179(12) 0.0181(12) 0.0009(9) 0.0033(9) 0.0036(9) C22 0.0172(11) 0.0168(11) 0.0181(12) 0.0018(9) -0.0002(9) 0.0076(9) C23 0.0202(12) 0.0201(12) 0.0211(13) 0.0026(10) 0.0050(10) 0.0036(10) C24 0.0319(14) 0.0205(13) 0.0196(13) -0.0012(10) 0.0094(11) 0.0052(11) C25 0.0216(12) 0.0151(11) 0.0184(12) 0.0000(9) 0.0005(9) 0.0045(10) C26 0.0170(11) 0.0179(12) 0.0185(12) 0.0048(9) 0.0014(9) 0.0075(9) C27 0.0197(12) 0.0208(12) 0.0149(11) 0.0013(9) 0.0020(9) 0.0082(10) C28 0.0184(12) 0.0173(12) 0.0187(12) 0.0026(9) 0.0029(9) 0.0058(9) C29 0.0253(13) 0.0225(13) 0.0199(13) 0.0017(10) 0.0051(10) 0.0084(10) C30 0.0351(15) 0.0308(15) 0.0223(14) 0.0002(11) 0.0048(11) 0.0149(12) C31 0.0471(18) 0.0451(18) 0.0239(15) -0.0002(13) 0.0051(13) 0.0254(15) C32 0.057(2) 0.0402(17) 0.0206(14) 0.0044(12) 0.0049(13) 0.0229(15) C33 0.0252(13) 0.0250(13) 0.0238(14) -0.0014(10) 0.0041(10) 0.0078(11) C34 0.0325(16) 0.0440(18) 0.0322(17) -0.0058(14) 0.0027(13) 0.0002(14) C35 0.0338(17) 0.055(2) 0.0400(19) -0.0081(16) -0.0040(14) 0.0097(15) C36 0.057(2) 0.071(3) 0.0360(19) -0.0086(17) -0.0043(16) 0.030(2) C37 0.0199(12) 0.0198(12) 0.0211(13) 0.0024(9) -0.0009(9) 0.0046(10) C38 0.0251(13) 0.0243(13) 0.0236(14) -0.0004(10) -0.0022(10) 0.0038(11) C39 0.0294(14) 0.0311(15) 0.0272(15) -0.0016(11) -0.0012(11) 0.0058(12) C40 0.0405(17) 0.0401(18) 0.0296(16) -0.0055(13) -0.0028(13) 0.0073(14) C41 0.0245(13) 0.0203(12) 0.0195(13) 0.0019(10) 0.0011(10) 0.0067(10) C42 0.0310(14) 0.0295(14) 0.0240(14) 0.0077(11) 0.0070(11) 0.0103(12) C43 0.0362(16) 0.0322(16) 0.0383(17) 0.0095(13) 0.0112(13) 0.0080(13) C44 0.0445(19) 0.046(2) 0.043(2) 0.0151(15) 0.0097(15) -0.0002(16) C45 0.051(2) 0.041(2) 0.059(3) -0.0057(17) 0.0229(19) -0.0052(17) C46 0.055(2) 0.053(2) 0.107(4) -0.004(2) 0.025(2) 0.018(2) C47 0.058(2) 0.066(3) 0.047(2) 0.0133(19) 0.0031(18) 0.026(2) C48 0.067(3) 0.049(2) 0.069(3) 0.0071(19) 0.010(2) 0.029(2) C49 0.054(4) 0.031(3) 0.030(3) 0.002(3) 0.002(3) 0.004(3) O50 0.073(4) 0.041(3) 0.042(3) 0.007(2) -0.006(3) -0.008(3) C51 0.048(4) 0.041(4) 0.067(5) 0.005(3) -0.022(4) 0.014(3) C52 0.045(6) 0.058(7) 0.041(6) 0.022(5) -0.004(4) 0.025(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 Cl1 C32 1.800(3) . ? Cl2 C36 1.800(4) . ? Cl3 C40 1.796(3) . ? Cl4 C44 1.800(4) . ? O1 C2 1.385(3) . ? O2 C3 1.389(3) . ? O3 C4 1.376(3) . ? O4 C9 1.377(3) . ? O5 C10 1.381(3) . ? O6 C11 1.384(3) . ? O7 C16 1.378(3) . ? O8 C17 1.397(3) . ? O9 C18 1.382(3) . ? O10 C23 1.379(3) . ? O11 C24 1.383(3) . ? O12 C25 1.382(3) . ? O13 C45 1.248(5) . ? O14 C45 1.303(4) . ? O14 C47 1.479(4) . ? C53 C52 0.592(12) . ? C53 C51 1.262(17) . ? C53 C49 1.520(13) . ? O16 C49 1.307(7) 2_567 ? O16 C49 1.307(7) . ? O16 C51 1.391(7) 2_567 ? O16 C51 1.391(7) . ? C1 C6 1.395(3) . ? C1 C2 1.399(3) . ? C1 C28 1.529(3) . ? C2 C3 1.390(3) . ? C3 C4 1.390(3) . ? C4 C5 1.398(3) . ? C5 C6 1.397(3) . ? C5 C7 1.528(3) . ? C7 C8 1.533(3) . ? C7 C29 1.539(3) . ? C8 C9 1.391(3) . ? C8 C13 1.399(3) . ? C9 C10 1.393(4) . ? C10 C11 1.387(4) . ? C11 C12 1.393(4) . ? C12 C13 1.399(3) . ? C12 C14 1.526(3) . ? C14 C15 1.533(3) . ? C14 C33 1.542(4) . ? C15 C20 1.389(3) . ? C15 C16 1.405(3) . ? C16 C17 1.395(3) . ? C17 C18 1.389(4) . ? C18 C19 1.399(3) . ? C19 C20 1.404(3) . ? C19 C21 1.529(3) . ? C21 C22 1.528(3) . ? C21 C37 1.542(3) . ? C22 C23 1.397(3) . ? C22 C27 1.399(3) . ? C23 C24 1.388(4) . ? C24 C25 1.392(4) . ? C25 C26 1.399(3) . ? C26 C27 1.396(3) . ? C26 C28 1.534(3) . ? C28 C41 1.544(3) . ? C29 C30 1.522(4) . ? C30 C31 1.528(4) . ? C31 C32 1.486(4) . ? C33 C34 1.525(4) . ? C34 C35 1.528(5) . ? C35 C36 1.491(5) . ? C37 C38 1.528(3) . ? C38 C39 1.526(4) . ? C39 C40 1.504(4) . ? C41 C42 1.538(4) . ? C42 C43 1.513(4) . ? C43 C44 1.517(4) . ? C45 C46 1.493(6) . ? C47 C48 1.460(6) . ? C49 C52 1.180(13) . ? C49 O50 1.198(8) . ? C49 C51 1.300(10) . ? O50 C52 1.883(11) . ? C51 C52 1.470(14) . ? 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 C45 O14 C47 116.2(3) . . ? C52 C53 C51 98(2) . . ? C52 C53 C49 45(2) . . ? C51 C53 C49 54.8(7) . . ? C49 O16 C49 180.0(5) 2_567 . ? C49 O16 C51 57.5(4) 2_567 2_567 ? C49 O16 C51 122.5(4) . 2_567 ? C49 O16 C51 122.5(4) 2_567 . ? C49 O16 C51 57.5(4) . . ? C51 O16 C51 180.000(4) 2_567 . ? C6 C1 C2 116.8(2) . . ? C6 C1 C28 122.1(2) . . ? C2 C1 C28 121.1(2) . . ? O1 C2 C3 117.7(2) . . ? O1 C2 C1 121.0(2) . . ? C3 C2 C1 121.3(2) . . ? O2 C3 C4 120.4(2) . . ? O2 C3 C2 119.4(2) . . ? C4 C3 C2 120.2(2) . . ? O3 C4 C3 120.8(2) . . ? O3 C4 C5 118.6(2) . . ? C3 C4 C5 120.6(2) . . ? C6 C5 C4 117.4(2) . . ? C6 C5 C7 122.7(2) . . ? C4 C5 C7 119.8(2) . . ? C1 C6 C5 123.7(2) . . ? C5 C7 C8 111.31(19) . . ? C5 C7 C29 111.6(2) . . ? C8 C7 C29 113.4(2) . . ? C9 C8 C13 117.4(2) . . ? C9 C8 C7 120.3(2) . . ? C13 C8 C7 122.3(2) . . ? O4 C9 C8 124.6(2) . . ? O4 C9 C10 114.3(2) . . ? C8 C9 C10 121.1(2) . . ? O5 C10 C11 118.4(2) . . ? O5 C10 C9 121.5(2) . . ? C11 C10 C9 120.0(2) . . ? O6 C11 C10 118.3(2) . . ? O6 C11 C12 120.9(2) . . ? C10 C11 C12 120.8(2) . . ? C11 C12 C13 117.8(2) . . ? C11 C12 C14 120.1(2) . . ? C13 C12 C14 122.1(2) . . ? C8 C13 C12 122.8(2) . . ? C12 C14 C15 111.7(2) . . ? C12 C14 C33 112.9(2) . . ? C15 C14 C33 112.9(2) . . ? C20 C15 C16 117.3(2) . . ? C20 C15 C14 122.2(2) . . ? C16 C15 C14 120.5(2) . . ? O7 C16 C17 118.0(2) . . ? O7 C16 C15 121.5(2) . . ? C17 C16 C15 120.5(2) . . ? C18 C17 C16 120.5(2) . . ? C18 C17 O8 119.2(2) . . ? C16 C17 O8 120.3(2) . . ? O9 C18 C17 116.0(2) . . ? O9 C18 C19 123.1(2) . . ? C17 C18 C19 120.8(2) . . ? C18 C19 C20 117.1(2) . . ? C18 C19 C21 121.5(2) . . ? C20 C19 C21 121.3(2) . . ? C15 C20 C19 123.7(2) . . ? C22 C21 C19 111.10(19) . . ? C22 C21 C37 112.3(2) . . ? C19 C21 C37 112.81(19) . . ? C23 C22 C27 117.4(2) . . ? C23 C22 C21 120.0(2) . . ? C27 C22 C21 122.6(2) . . ? O10 C23 C24 119.7(2) . . ? O10 C23 C22 119.1(2) . . ? C24 C23 C22 121.2(2) . . ? O11 C24 C23 117.5(2) . . ? O11 C24 C25 122.7(2) . . ? C23 C24 C25 119.8(2) . . ? O12 C25 C24 116.7(2) . . ? O12 C25 C26 122.1(2) . . ? C24 C25 C26 121.1(2) . . ? C27 C26 C25 117.3(2) . . ? C27 C26 C28 122.3(2) . . ? C25 C26 C28 120.4(2) . . ? C26 C27 C22 123.1(2) . . ? C1 C28 C26 110.55(19) . . ? C1 C28 C41 113.7(2) . . ? C26 C28 C41 111.9(2) . . ? C30 C29 C7 114.2(2) . . ? C29 C30 C31 110.6(2) . . ? C32 C31 C30 113.8(2) . . ? C31 C32 Cl1 111.8(2) . . ? C34 C33 C14 112.1(2) . . ? C33 C34 C35 115.7(3) . . ? C36 C35 C34 113.4(3) . . ? C35 C36 Cl2 112.1(3) . . ? C38 C37 C21 113.8(2) . . ? C39 C38 C37 111.1(2) . . ? C40 C39 C38 112.2(2) . . ? C39 C40 Cl3 111.4(2) . . ? C42 C41 C28 114.5(2) . . ? C43 C42 C41 112.9(2) . . ? C42 C43 C44 114.8(3) . . ? C43 C44 Cl4 112.0(2) . . ? O13 C45 O14 122.4(4) . . ? O13 C45 C46 125.7(4) . . ? O14 C45 C46 111.9(4) . . ? C48 C47 O14 106.9(3) . . ? C52 C49 O50 104.7(8) . . ? C52 C49 C51 72.6(7) . . ? O50 C49 C51 165.1(8) . . ? C52 C49 O16 137.0(8) . . ? O50 C49 O16 117.5(6) . . ? C51 C49 O16 64.5(4) . . ? C52 C49 C53 20.9(9) . . ? O50 C49 C53 125.6(8) . . ? C51 C49 C53 52.5(7) . . ? O16 C49 C53 116.4(7) . . ? C49 O50 C52 37.3(6) . . ? C53 C51 C49 72.7(7) . . ? C53 C51 O16 129.9(8) . . ? C49 C51 O16 58.0(4) . . ? C53 C51 C52 23.5(5) . . ? C49 C51 C52 49.9(6) . . ? O16 C51 C52 107.9(6) . . ? C53 C52 C49 114(3) . . ? C53 C52 C51 58(2) . . ? C49 C52 C51 57.5(7) . . ? C53 C52 O50 152(3) . . ? C49 C52 O50 38.0(5) . . ? C51 C52 O50 94.4(6) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.718 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.073 #===END data_PgC8BrMeCN _database_code_depnum_ccdc_archive 'CCDC 604864' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62.70 H88.05 Br4 N1.35 O12' _chemical_formula_sum 'C62.70 H88.05 Br4 N1.35 O12' _chemical_formula_weight 1372.33 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 Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 36.984(3) _cell_length_b 36.984(3) _cell_length_c 25.824(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 30590(6) _cell_formula_units_Z 18 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12775 _exptl_absorpt_coefficient_mu 2.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5939 _exptl_absorpt_correction_T_max 0.6300 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _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 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 89238 _diffrn_reflns_av_R_equivalents 0.0874 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 27.11 _reflns_number_total 14967 _reflns_number_gt 7039 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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. The Crystals were weakly diffracting and one of the bromooctyl chains was badly disordered near the end. It was not possible to fully model the chain over all positions but this was attempted with limited success. Some of the upper rim pyrogallol- arene hydroxyl groups were disordered over two positions and modelled as such. The encapsulated acetonitrile molecules were modelled as effectively as possible, but again with limited success. The difference in reported and calculated formulae is due to the difference in the calculated formula and the modelled atoms of the disordered MeCN mmolecules and the bromo- octyl chain mentioned above. The largest residual peak is located near the end of another bromooctyl group and is consistent with possibly disordered bromine at the chain end. It was not possible to model this effectively and the assigned bromine atom was refined at full occupancy. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14967 _refine_ls_number_parameters 691 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.2856 _refine_ls_R_factor_gt 0.1743 _refine_ls_wR_factor_ref 0.4637 _refine_ls_wR_factor_gt 0.4286 _refine_ls_goodness_of_fit_ref 2.606 _refine_ls_restrained_S_all 2.614 _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 Br1 Br 0.28975(5) 0.03994(6) 0.78495(7) 0.1109(7) Uani 1 1 d . A . O1 O 0.3590(3) -0.1613(3) 0.9369(3) 0.0185(13) Uani 0.70 1 d P A 1 H1 H 0.3379 -0.1681 0.9555 0.022 Uiso 0.70 1 calc PR A 1 C1 C 0.4348(2) -0.1197(2) 0.9398(3) 0.0172(15) Uani 1 1 d . A 1 N300 N 0.411(2) -0.248(2) 1.334(2) 0.048(16) Uiso 0.13 1 d P . . Br2 Br 0.86397(6) 0.16259(7) 0.97844(11) 0.1680(11) Uani 1 1 d . A . O2 O 0.3593(7) -0.1583(7) 0.9551(7) 0.0185(13) Uani 0.30 1 d P A 2 H2 H 0.3494 -0.1787 0.9755 0.022 Uiso 0.30 1 calc PR A 2 N2 N 0.4950(12) -0.2367(12) 1.1733(15) 0.076(11) Uiso 0.25 1 d PD . . C2 C 0.3965(2) -0.1342(2) 0.9659(3) 0.0226(17) Uani 1 1 d . . . Br3 Br 0.9366(6) 0.0342(6) 1.0703(7) 0.286(8) Uiso 0.25 1 d P . . O3 O 0.3539(3) -0.1402(4) 1.0333(4) 0.0185(13) Uani 0.50 1 d P A 1 H3 H 0.3375 -0.1546 1.0096 0.022 Uiso 0.50 1 calc PR A 1 C3 C 0.3958(2) -0.1224(2) 1.0157(3) 0.0271(18) Uani 1 1 d . A . O4 O 0.3620(3) -0.1339(4) 1.0496(4) 0.0185(13) Uani 0.50 1 d P A 2 H4 H 0.3396 -0.1504 1.0345 0.022 Uiso 0.50 1 calc PR A 2 C4 C 0.4317(2) -0.0960(2) 1.0419(3) 0.0233(17) Uani 1 1 d . . . Br5 Br 0.87792(17) 0.03302(16) 0.90351(18) 0.1572(16) Uani 0.50 1 d P . . O5 O 0.4224(3) -0.0870(4) 1.0883(5) 0.0185(13) Uani 0.50 1 d P A 1 H5 H 0.3964 -0.0996 1.0921 0.022 Uiso 0.50 1 calc PR A 1 C5 C 0.4704(2) -0.08051(19) 1.0179(3) 0.0179(15) Uani 1 1 d . A 1 Br6 Br 0.8372(3) -0.0542(3) 0.9078(4) 0.1572(16) Uani 0.25 1 d P . . O6 O 0.4354(3) -0.0799(4) 1.0955(5) 0.0185(13) Uani 0.50 1 d P A 2 H6 H 0.4250 -0.1000 1.1163 0.022 Uiso 0.50 1 calc PR A 2 C6 C 0.47033(19) -0.09349(18) 0.9677(3) 0.0141(14) Uani 1 1 d . . . H8 H 0.4966 -0.0837 0.9512 0.017 Uiso 1 1 calc R A 1 O7 O 0.48877(19) -0.08044(17) 1.1519(2) 0.0447(11) Uani 1 1 d . A . H15 H 0.4853 -0.0900 1.1821 0.054 Uiso 1 1 calc R . . C7 C 0.5113(2) -0.05080(19) 1.0466(3) 0.0188(15) Uani 1 1 d . . . H7 H 0.5042 -0.0359 1.0735 0.023 Uiso 1 1 calc R A 1 Br8 Br 0.8360(11) -0.0416(12) 1.0317(14) 0.265(13) Uiso 0.15 1 d P . 2 O8 O 0.52000(19) -0.12385(17) 1.2025(2) 0.0447(11) Uani 1 1 d . . . H54 H 0.5317 -0.1367 1.2138 0.054 Uiso 1 1 calc R . . C8 C 0.5275(2) -0.07585(19) 1.0751(3) 0.0187(15) Uani 1 1 d . A . O9 O 0.5719(6) -0.1414(6) 1.1604(5) 0.0447(11) Uani 0.50 1 d P A 1 H9 H 0.5591 -0.1454 1.1886 0.054 Uiso 0.50 1 calc PR A 1 C9 C 0.5157(2) -0.0896(2) 1.1254(3) 0.0252(17) Uani 1 1 d . . . O10 O 0.5773(6) -0.1431(6) 1.1486(6) 0.0447(11) Uani 0.50 1 d P A 2 H10 H 0.5684 -0.1501 1.1790 0.054 Uiso 0.50 1 calc PR A 2 C10 C 0.5320(3) -0.1121(2) 1.1509(3) 0.036(2) Uani 1 1 d . A . O11 O 0.58179(18) -0.19688(17) 1.0957(2) 0.0437(13) Uani 1 1 d . . . H11 H 0.5745 -0.2213 1.1052 0.052 Uiso 1 1 calc R B 1 C11 C 0.5594(2) -0.1204(2) 1.1261(3) 0.0263(17) Uani 1 1 d . . . O12 O 0.5430(4) -0.2686(4) 1.0498(5) 0.0437(13) Uani 0.60 1 d P C 1 H12 H 0.5301 -0.2910 1.0330 0.052 Uiso 0.60 1 calc PR C 1 C12 C 0.5720(2) -0.1079(2) 1.0770(3) 0.0199(16) Uani 1 1 d . A . O13 O 0.5334(6) -0.2750(6) 1.0330(7) 0.0437(13) Uani 0.40 1 d P C 2 H13 H 0.5407 -0.2756 1.0636 0.052 Uiso 0.40 1 calc PR C 2 C13 C 0.5554(2) -0.08609(19) 1.0513(3) 0.0182(15) Uani 1 1 d . . . H16 H 0.5633 -0.0779 1.0164 0.022 Uiso 1 1 calc R A . O14 O 0.5162(5) -0.2752(5) 0.9513(6) 0.0437(13) Uani 0.50 1 d P A 1 H14 H 0.5160 -0.2907 0.9752 0.052 Uiso 0.50 1 calc PR A 1 C14 C 0.6020(2) -0.1185(2) 1.0496(3) 0.0298(19) Uani 1 1 d . A 1 H17 H 0.6182 -0.1231 1.0773 0.036 Uiso 1 1 calc R A 1 O15 O 0.5122(5) -0.2731(5) 0.9355(6) 0.0437(13) Uani 0.50 1 d P A 2 H15A H 0.4893 -0.2898 0.9496 0.052 Uiso 0.50 1 calc PR A 2 C15 C 0.5776(2) -0.1600(2) 1.0202(3) 0.0244(17) Uani 1 1 d . A 1 O16 O 0.45039(18) -0.28056(17) 0.8855(3) 0.0530(11) Uani 1 1 d . . . H18 H 0.4755 -0.2746 0.8856 0.064 Uiso 1 1 calc R . . C16 C 0.5687(2) -0.1975(3) 1.0439(3) 0.036(2) Uani 1 1 d . A 1 O17 O 0.37379(17) -0.28691(17) 0.8858(3) 0.0530(11) Uani 1 1 d . . . H36 H 0.3804 -0.3056 0.8859 0.064 Uiso 1 1 calc R . . C17 C 0.5478(3) -0.2347(3) 1.0185(4) 0.039(2) Uani 1 1 d . . . O18 O 0.36493(18) -0.21936(17) 0.8850(3) 0.0530(11) Uani 1 1 d . . . H26 H 0.3478 -0.2451 0.8852 0.064 Uiso 1 1 calc R . . C18 C 0.5348(2) -0.2355(2) 0.9681(4) 0.034(2) Uani 1 1 d . A . C19 C 0.5424(2) -0.1995(2) 0.9426(3) 0.0247(18) Uani 1 1 d . A 1 C20 C 0.5639(2) -0.1621(2) 0.9708(3) 0.0221(17) Uani 1 1 d . A 1 H29 H 0.5691 -0.1369 0.9545 0.027 Uiso 1 1 calc R A 1 C21 C 0.5283(2) -0.1999(2) 0.8872(3) 0.0266(18) Uani 1 1 d . . . H21 H 0.5258 -0.2254 0.8704 0.032 Uiso 1 1 calc R A 1 C22 C 0.4844(2) -0.2048(2) 0.8863(3) 0.0223(16) Uani 1 1 d . A . C23 C 0.4484(2) -0.2435(2) 0.8859(3) 0.0305(19) Uani 1 1 d . . . C24 C 0.4101(2) -0.2476(2) 0.8859(3) 0.034(2) Uani 1 1 d . A . C25 C 0.4052(2) -0.2127(2) 0.8856(3) 0.0256(17) Uani 1 1 d . . . C26 C 0.4397(2) -0.1734(2) 0.8858(3) 0.0200(15) Uani 1 1 d . A . C27 C 0.4789(2) -0.1705(2) 0.8875(3) 0.0174(15) Uani 1 1 d . . . H19 H 0.5029 -0.1435 0.8895 0.021 Uiso 1 1 calc R A . C28 C 0.4353(2) -0.1339(2) 0.8852(3) 0.0200(16) Uani 1 1 d . . . H28 H 0.4076 -0.1420 0.8694 0.024 Uiso 1 1 calc R A 1 C29 C 0.5442(2) -0.0173(2) 1.0113(3) 0.0227(16) Uani 1 1 d . A . H59A H 0.5530 -0.0310 0.9853 0.027 Uiso 1 1 calc R . . H59B H 0.5314 -0.0033 0.9924 0.027 Uiso 1 1 calc R . . C30 C 0.5827(2) 0.0155(2) 1.0403(3) 0.0260(17) Uani 1 1 d . . . H32A H 0.5767 0.0370 1.0542 0.031 Uiso 1 1 calc R A . H32B H 0.5881 0.0020 1.0701 0.031 Uiso 1 1 calc R . . C31 C 0.6215(2) 0.0367(2) 1.0073(3) 0.0259(17) Uani 1 1 d . A . H27A H 0.6167 0.0518 0.9789 0.031 Uiso 1 1 calc R . . H27B H 0.6261 0.0150 0.9912 0.031 Uiso 1 1 calc R . . C32 C 0.6611(2) 0.0674(2) 1.0359(3) 0.0316(19) Uani 1 1 d . . . H39A H 0.6652 0.0531 1.0657 0.038 Uiso 1 1 calc R A . H39B H 0.6577 0.0906 1.0495 0.038 Uiso 1 1 calc R . . C33 C 0.6994(2) 0.0851(2) 1.0012(3) 0.0330(19) Uani 1 1 d . A . H44A H 0.6960 0.1014 0.9731 0.040 Uiso 1 1 calc R . . H44B H 0.7008 0.0616 0.9849 0.040 Uiso 1 1 calc R . . C34 C 0.7410(2) 0.1133(2) 1.0290(3) 0.037(2) Uani 1 1 d . . . H52A H 0.7411 0.1386 1.0421 0.044 Uiso 1 1 calc R A . H52B H 0.7437 0.0982 1.0591 0.044 Uiso 1 1 calc R . . C35 C 0.7781(2) 0.1263(3) 0.9924(4) 0.044(2) Uani 1 1 d . A . H46A H 0.7776 0.1009 0.9793 0.053 Uiso 1 1 calc R . . H46B H 0.7751 0.1412 0.9623 0.053 Uiso 1 1 calc R . . C36 C 0.8193(3) 0.1538(3) 1.0180(5) 0.065(3) Uani 1 1 d . . . H60A H 0.8202 0.1410 1.0513 0.078 Uiso 1 1 calc R A . H60B H 0.8216 0.1811 1.0259 0.078 Uiso 1 1 calc R . . C37 C 0.5588(2) -0.1629(2) 0.8550(3) 0.0289(18) Uani 1 1 d . A . H33A H 0.5616 -0.1371 0.8703 0.035 Uiso 1 1 calc R . . H33B H 0.5473 -0.1658 0.8197 0.035 Uiso 1 1 calc R . . C38 C 0.6027(2) -0.1584(3) 0.8512(4) 0.042(2) Uani 1 1 d . . . H48A H 0.6076 -0.1706 0.8826 0.050 Uiso 1 1 calc R A . H48B H 0.6032 -0.1747 0.8211 0.050 Uiso 1 1 calc R . . C39 C 0.6377(3) -0.1142(3) 0.8456(4) 0.048(3) Uani 1 1 d . A . H49A H 0.6351 -0.0972 0.8734 0.058 Uiso 1 1 calc R . . H49B H 0.6346 -0.1031 0.8121 0.058 Uiso 1 1 calc R . . C40 C 0.6813(3) -0.1087(3) 0.8482(4) 0.048(2) Uani 1 1 d . . . H58A H 0.6828 -0.1239 0.8789 0.057 Uiso 1 1 calc R A . H58B H 0.6855 -0.1219 0.8171 0.057 Uiso 1 1 calc R . . C41 C 0.7159(3) -0.0653(3) 0.8510(5) 0.058(3) Uani 1 1 d . A . H57A H 0.7116 -0.0516 0.8814 0.070 Uiso 1 1 calc R . . H57B H 0.7154 -0.0502 0.8196 0.070 Uiso 1 1 calc R . . C42 C 0.7603(4) -0.0616(4) 0.8555(6) 0.096(5) Uani 1 1 d . . . H64A H 0.7588 -0.0813 0.8825 0.115 Uiso 1 1 calc R A . H64B H 0.7665 -0.0706 0.8222 0.115 Uiso 1 1 calc R . . C43 C 0.7964(4) -0.0187(4) 0.8684(6) 0.089(4) Uani 1 1 d . A . H61A H 0.7869 -0.0088 0.8984 0.107 Uiso 1 1 calc R . . H61B H 0.7987 -0.0006 0.8389 0.107 Uiso 1 1 calc R . . C44 C 0.8409(4) -0.0079(7) 0.8810(7) 0.146(8) Uani 1 1 d . . . C45 C 0.4692(2) -0.0998(2) 0.8502(3) 0.0233(16) Uani 1 1 d . A . H47A H 0.4971 -0.0928 0.8636 0.028 Uiso 1 1 calc R . . H47B H 0.4666 -0.1113 0.8149 0.028 Uiso 1 1 calc R . . C46 C 0.4670(2) -0.0592(2) 0.8466(3) 0.0288(18) Uani 1 1 d . . . H42A H 0.4726 -0.0461 0.8813 0.035 Uiso 1 1 calc R A . H42B H 0.4895 -0.0395 0.8232 0.035 Uiso 1 1 calc R . . C47 C 0.4270(2) -0.0648(2) 0.8278(3) 0.0309(19) Uani 1 1 d . A . H56A H 0.4047 -0.0820 0.8529 0.037 Uiso 1 1 calc R . . H56B H 0.4199 -0.0800 0.7944 0.037 Uiso 1 1 calc R . . C48 C 0.4285(2) -0.0227(2) 0.8203(3) 0.0323(19) Uani 1 1 d . . . H51A H 0.4479 -0.0073 0.7915 0.039 Uiso 1 1 calc R A . H51B H 0.4398 -0.0058 0.8522 0.039 Uiso 1 1 calc R . . C49 C 0.3854(2) -0.0278(2) 0.8084(3) 0.035(2) Uani 1 1 d . A . H41A H 0.3760 -0.0412 0.7740 0.041 Uiso 1 1 calc R . . H41B H 0.3651 -0.0467 0.8344 0.041 Uiso 1 1 calc R . . C50 C 0.3850(2) 0.0124(2) 0.8083(3) 0.0330(19) Uani 1 1 d . . . H43A H 0.4054 0.0314 0.7824 0.040 Uiso 1 1 calc R A . H43B H 0.3942 0.0257 0.8428 0.040 Uiso 1 1 calc R . . C51 C 0.3424(2) 0.0070(2) 0.7962(4) 0.038(2) Uani 1 1 d . A . H50A H 0.3339 -0.0050 0.7611 0.045 Uiso 1 1 calc R . . H50B H 0.3217 -0.0131 0.8210 0.045 Uiso 1 1 calc R . . C52 C 0.3412(3) 0.0469(3) 0.7986(4) 0.048(2) Uani 1 1 d . . . H53A H 0.3615 0.0669 0.7733 0.057 Uiso 1 1 calc R A . H53B H 0.3501 0.0592 0.8336 0.057 Uiso 1 1 calc R . . C53 C 0.6344(3) -0.0833(3) 1.0144(4) 0.0597(18) Uani 1 1 d . . . C54 C 0.6611(7) -0.0406(8) 1.0455(12) 0.0597(18) Uani 0.50 1 d P . 1 C55 C 0.6678(7) -0.0505(8) 1.0477(12) 0.0597(18) Uani 0.50 1 d P . 2 H55A H 0.6746 -0.0638 1.0765 0.072 Uiso 0.50 1 calc PR . 2 H55B H 0.6579 -0.0324 1.0628 0.072 Uiso 0.50 1 calc PR . 2 C56 C 0.6974(11) -0.0392(13) 1.0696(18) 0.0597(18) Uani 0.25 1 d P . 1 H56C H 0.6902 -0.0675 1.0810 0.072 Uiso 0.25 1 calc PR . 1 H56D H 0.7057 -0.0209 1.1005 0.072 Uiso 0.25 1 calc PR . 1 C57 C 0.7080(7) -0.0234(7) 1.0137(9) 0.0597(18) Uani 0.50 1 d P . 2 H57C H 0.7186 -0.0411 0.9991 0.072 Uiso 0.50 1 calc PR . 2 H57D H 0.7014 -0.0100 0.9847 0.072 Uiso 0.50 1 calc PR . 2 C58 C 0.7357(6) -0.0217(7) 1.0293(9) 0.0597(18) Uani 0.50 1 d P . 1 C59 C 0.7407(6) 0.0101(7) 1.0501(9) 0.0597(18) Uani 0.50 1 d P . 2 H59C H 0.7330 0.0319 1.0549 0.072 Uiso 0.50 1 calc PR . 2 H59D H 0.7380 -0.0032 1.0843 0.072 Uiso 0.50 1 calc PR . 2 C60 C 0.7661(6) -0.0225(7) 1.0547(9) 0.0597(18) Uani 0.50 1 d P . 1 H60C H 0.7537 -0.0484 1.0757 0.072 Uiso 0.50 1 calc PR . 1 H60D H 0.7782 0.0013 1.0792 0.072 Uiso 0.50 1 calc PR . 1 C61 C 0.7844(5) 0.0308(6) 1.0358(9) 0.0597(18) Uani 0.50 1 d P . 2 H61C H 0.8001 0.0566 1.0566 0.072 Uiso 0.50 1 calc PR . 2 H61D H 0.7874 0.0389 0.9988 0.072 Uiso 0.50 1 calc PR . 2 C62 C 0.8032(11) 0.0021(12) 1.0447(14) 0.113(11) Uiso 0.50 1 d P . 2 C63 C 0.828(3) -0.028(3) 1.063(3) 0.14(3) Uiso 0.25 1 d PD . 1 C64 C 0.854(2) -0.0118(18) 1.076(2) 0.16(2) Uiso 0.50 1 d P . . C65 C 0.7053(13) -0.0134(15) 1.034(2) 0.0597(18) Uani 0.25 1 d P . 1 H65A H 0.7055 0.0000 1.0003 0.072 Uiso 0.25 1 calc PR . 1 H65B H 0.7153 0.0090 1.0599 0.072 Uiso 0.25 1 calc PR . 1 C66 C 0.8718(9) -0.0112(8) 1.0865(10) 0.061(7) Uiso 0.50 1 d P . 1 C67 C 0.8904(11) 0.0228(12) 1.0921(12) 0.101(9) Uiso 0.50 1 d P . . C68 C 0.8499(14) 0.0198(14) 1.0521(17) 0.061(11) Uiso 0.25 1 d P . 2 C69 C 0.870(3) -0.011(3) 1.030(3) 0.14(3) Uiso 0.25 1 d P . . C70 C 0.8012(14) -0.0208(16) 1.0238(18) 0.156(16) Uiso 0.50 1 d PD . 1 H70A H 0.8176 0.0067 1.0067 0.187 Uiso 0.50 1 calc PR . 1 H70B H 0.7905 -0.0429 0.9971 0.187 Uiso 0.50 1 calc PR . 1 C301 C 0.382(3) -0.272(3) 1.332(3) 0.06(2) Uiso 0.13 1 d P . . N101 N 0.4601(4) -0.1894(3) 1.0277(5) 0.102(4) Uani 1 1 d . D 1 C101 C 0.4297(15) -0.2329(15) 1.222(2) 0.079(14) Uiso 0.25 1 d PD . . H10A H 0.4024 -0.2501 1.2054 0.119 Uiso 0.25 1 calc PR . . H10B H 0.4410 -0.2036 1.2113 0.119 Uiso 0.25 1 calc PR . . H10C H 0.4267 -0.2352 1.2594 0.119 Uiso 0.25 1 calc PR . . C102 C 0.460(3) -0.248(3) 1.204(4) 0.24(5) Uiso 0.25 1 d PD . . Br7 Br 0.8430(6) -0.0657(7) 1.0574(8) 0.283(8) Uiso 0.25 1 d P . . Br13 Br 0.8926(4) 0.0504(4) 1.0705(5) 0.179(4) Uiso 0.25 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 Br1 0.0991(12) 0.1276(14) 0.1382(16) 0.0407(11) 0.0184(10) 0.0809(11) O1 0.002(2) 0.023(2) 0.019(3) -0.004(2) 0.001(3) -0.0026(19) C1 0.013(3) 0.014(3) 0.028(4) 0.008(3) 0.003(3) 0.009(3) Br2 0.0903(14) 0.1445(19) 0.229(3) -0.0416(17) 0.0196(15) 0.0286(13) O2 0.002(2) 0.023(2) 0.019(3) -0.004(2) 0.001(3) -0.0026(19) C2 0.011(3) 0.014(4) 0.039(5) 0.009(3) 0.005(3) 0.004(3) O3 0.002(2) 0.023(2) 0.019(3) -0.004(2) 0.001(3) -0.0026(19) C3 0.020(4) 0.022(4) 0.039(5) 0.008(4) 0.017(3) 0.011(3) O4 0.002(2) 0.023(2) 0.019(3) -0.004(2) 0.001(3) -0.0026(19) C4 0.025(4) 0.018(4) 0.028(4) 0.010(3) 0.015(3) 0.011(3) Br5 0.158(4) 0.163(4) 0.144(3) 0.030(3) -0.004(3) 0.075(3) O5 0.002(2) 0.023(2) 0.019(3) -0.004(2) 0.001(3) -0.0026(19) C5 0.016(3) 0.010(3) 0.026(4) 0.006(3) 0.006(3) 0.005(3) Br6 0.158(4) 0.163(4) 0.144(3) 0.030(3) -0.004(3) 0.075(3) O6 0.002(2) 0.023(2) 0.019(3) -0.004(2) 0.001(3) -0.0026(19) C6 0.010(3) 0.009(3) 0.024(4) 0.006(3) 0.007(3) 0.005(3) O7 0.060(3) 0.038(2) 0.024(2) 0.0116(17) 0.0106(18) 0.0146(19) C7 0.020(4) 0.009(3) 0.025(4) 0.005(3) 0.010(3) 0.006(3) O8 0.060(3) 0.038(2) 0.024(2) 0.0116(17) 0.0106(18) 0.0146(19) C8 0.018(4) 0.008(3) 0.020(4) 0.002(3) 0.002(3) -0.001(3) O9 0.060(3) 0.038(2) 0.024(2) 0.0116(17) 0.0106(18) 0.0146(19) C9 0.024(4) 0.017(4) 0.022(4) -0.002(3) 0.004(3) 0.001(3) O10 0.060(3) 0.038(2) 0.024(2) 0.0116(17) 0.0106(18) 0.0146(19) C10 0.048(5) 0.021(4) 0.018(4) 0.009(3) -0.003(4) 0.002(4) O11 0.054(3) 0.035(2) 0.055(4) 0.033(2) 0.014(2) 0.032(2) C11 0.024(4) 0.018(4) 0.030(5) 0.004(3) -0.010(3) 0.005(3) O12 0.054(3) 0.035(2) 0.055(4) 0.033(2) 0.014(2) 0.032(2) C12 0.011(3) 0.011(3) 0.027(4) 0.005(3) -0.007(3) -0.002(3) O13 0.054(3) 0.035(2) 0.055(4) 0.033(2) 0.014(2) 0.032(2) C13 0.013(3) 0.011(3) 0.026(4) 0.003(3) 0.000(3) 0.002(3) O14 0.054(3) 0.035(2) 0.055(4) 0.033(2) 0.014(2) 0.032(2) C14 0.014(4) 0.028(4) 0.044(5) 0.014(4) 0.002(3) 0.008(3) O15 0.054(3) 0.035(2) 0.055(4) 0.033(2) 0.014(2) 0.032(2) C15 0.017(4) 0.019(4) 0.044(5) 0.020(3) 0.015(3) 0.014(3) O16 0.033(2) 0.0223(18) 0.084(3) -0.0046(18) 0.0129(19) -0.0011(16) C16 0.034(5) 0.039(5) 0.047(6) 0.025(4) 0.017(4) 0.025(4) O17 0.033(2) 0.0223(18) 0.084(3) -0.0046(18) 0.0129(19) -0.0011(16) C17 0.039(5) 0.026(5) 0.062(7) 0.028(4) 0.022(5) 0.024(4) O18 0.033(2) 0.0223(18) 0.084(3) -0.0046(18) 0.0129(19) -0.0011(16) C18 0.028(4) 0.008(4) 0.071(7) 0.011(4) 0.016(4) 0.012(3) C19 0.017(4) 0.012(3) 0.051(5) 0.010(3) 0.015(3) 0.011(3) C20 0.012(3) 0.016(4) 0.044(5) 0.012(3) 0.010(3) 0.011(3) C21 0.022(4) 0.012(4) 0.045(5) -0.001(3) 0.013(4) 0.008(3) C22 0.019(4) 0.014(4) 0.032(4) 0.002(3) 0.011(3) 0.007(3) C23 0.028(4) 0.008(3) 0.051(5) -0.002(3) 0.009(4) 0.006(3) C24 0.023(4) 0.014(4) 0.053(6) -0.006(4) 0.005(4) -0.001(3) C25 0.010(3) 0.023(4) 0.037(5) -0.002(3) 0.001(3) 0.003(3) C26 0.019(4) 0.018(4) 0.019(4) -0.002(3) -0.001(3) 0.006(3) C27 0.014(3) 0.011(3) 0.024(4) 0.002(3) 0.006(3) 0.004(3) C28 0.014(3) 0.021(4) 0.022(4) 0.003(3) 0.003(3) 0.006(3) C29 0.023(4) 0.013(3) 0.026(4) 0.006(3) 0.008(3) 0.005(3) C30 0.025(4) 0.010(3) 0.030(4) 0.003(3) 0.006(3) -0.001(3) C31 0.025(4) 0.011(3) 0.030(4) 0.006(3) 0.012(3) 0.000(3) C32 0.031(4) 0.020(4) 0.033(5) -0.003(3) 0.003(4) 0.005(3) C33 0.020(4) 0.023(4) 0.043(5) -0.001(4) 0.001(4) 0.001(3) C34 0.032(5) 0.028(4) 0.039(5) 0.003(4) 0.001(4) 0.006(4) C35 0.026(5) 0.035(5) 0.061(6) -0.005(4) 0.001(4) 0.007(4) C36 0.042(6) 0.050(6) 0.093(9) 0.000(6) -0.007(6) 0.015(5) C37 0.032(4) 0.021(4) 0.039(5) 0.007(3) 0.018(4) 0.016(4) C38 0.031(5) 0.035(5) 0.066(6) 0.015(4) 0.028(4) 0.021(4) C39 0.042(5) 0.033(5) 0.072(7) 0.023(5) 0.026(5) 0.020(4) C40 0.039(5) 0.040(5) 0.069(7) 0.003(5) 0.011(5) 0.023(5) C41 0.042(6) 0.044(6) 0.091(8) 0.001(5) 0.009(5) 0.023(5) C42 0.057(8) 0.062(8) 0.161(14) -0.001(8) 0.035(8) 0.024(7) C43 0.073(9) 0.057(8) 0.140(13) 0.015(8) -0.002(8) 0.035(7) C44 0.050(9) 0.24(2) 0.150(16) 0.102(16) 0.041(9) 0.071(12) C45 0.016(4) 0.024(4) 0.025(4) 0.009(3) 0.008(3) 0.006(3) C46 0.025(4) 0.024(4) 0.032(5) 0.016(3) 0.006(3) 0.007(3) C47 0.027(4) 0.026(4) 0.039(5) 0.007(4) -0.007(4) 0.012(4) C48 0.030(4) 0.029(4) 0.037(5) 0.007(4) 0.004(4) 0.013(4) C49 0.032(5) 0.033(5) 0.043(5) 0.000(4) -0.005(4) 0.020(4) C50 0.034(5) 0.038(5) 0.031(5) 0.005(4) -0.003(4) 0.021(4) C51 0.033(5) 0.028(4) 0.051(6) 0.005(4) -0.004(4) 0.015(4) C52 0.055(6) 0.043(6) 0.047(6) 0.011(4) 0.004(5) 0.027(5) C53 0.028(3) 0.052(4) 0.075(5) 0.008(3) -0.001(3) 0.003(3) C54 0.028(3) 0.052(4) 0.075(5) 0.008(3) -0.001(3) 0.003(3) C55 0.028(3) 0.052(4) 0.075(5) 0.008(3) -0.001(3) 0.003(3) C56 0.028(3) 0.052(4) 0.075(5) 0.008(3) -0.001(3) 0.003(3) C57 0.028(3) 0.052(4) 0.075(5) 0.008(3) -0.001(3) 0.003(3) C58 0.028(3) 0.052(4) 0.075(5) 0.008(3) -0.001(3) 0.003(3) C59 0.028(3) 0.052(4) 0.075(5) 0.008(3) -0.001(3) 0.003(3) C60 0.028(3) 0.052(4) 0.075(5) 0.008(3) -0.001(3) 0.003(3) C61 0.028(3) 0.052(4) 0.075(5) 0.008(3) -0.001(3) 0.003(3) C65 0.028(3) 0.052(4) 0.075(5) 0.008(3) -0.001(3) 0.003(3) N101 0.083(8) 0.082(8) 0.118(10) 0.014(7) 0.011(7) 0.024(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 Br1 C52 1.823(9) . ? O1 C2 1.449(11) . ? C1 C6 1.382(9) . ? C1 C2 1.412(9) . ? C1 C28 1.508(10) . ? N300 C301 1.01(9) . ? Br2 C36 1.829(11) . ? O2 C2 1.24(2) . ? N2 C102 1.394(14) . ? C2 C3 1.362(10) . ? Br3 C67 1.64(3) . ? Br3 Br13 1.99(2) . ? Br3 C66 2.17(3) . ? Br3 Br6 2.66(2) 11_667 ? O3 C3 1.421(12) . ? C3 C4 1.371(10) . ? C3 O4 1.405(13) . ? C4 O5 1.332(15) . ? C4 C5 1.393(9) . ? C4 O6 1.485(15) . ? Br5 C44 1.56(2) . ? Br5 Br7 2.35(2) 11_667 ? C5 C6 1.381(9) . ? C5 C7 1.545(10) . ? Br6 C44 1.79(2) . ? Br6 Br13 2.141(16) 12_547 ? Br6 Br3 2.66(2) 12_547 ? O7 C9 1.383(9) . ? C7 C8 1.523(9) . ? C7 C29 1.528(9) . ? Br8 C69 1.19(8) . ? Br8 Br7 1.24(3) . ? Br8 C64 1.49(7) . ? Br8 C68 2.13(6) . ? O8 C10 1.403(9) . ? C8 C9 1.384(10) . ? C8 C13 1.405(9) . ? O9 C11 1.40(2) . ? C9 C10 1.409(11) . ? O10 C11 1.43(2) . ? C10 C11 1.359(12) . ? O11 C16 1.419(10) . ? C11 C12 1.352(10) . ? O12 C17 1.425(13) . ? C12 C13 1.400(9) . ? C12 C14 1.524(10) . ? O13 C17 1.360(19) . ? O14 C18 1.344(18) . ? C14 C15 1.537(11) . ? C14 C53 1.547(12) . ? O15 C18 1.477(19) . ? C15 C20 1.361(10) . ? C15 C16 1.394(10) . ? O16 C23 1.408(9) . ? C16 C17 1.364(12) . ? O17 C24 1.403(9) . ? C17 C18 1.384(12) . ? O18 C25 1.383(9) . ? C18 C19 1.381(10) . ? C19 C20 1.407(10) . ? C19 C21 1.519(11) . ? C21 C37 1.514(10) . ? C21 C22 1.540(10) . ? C22 C27 1.382(9) . ? C22 C23 1.386(10) . ? C23 C24 1.348(11) . ? C24 C25 1.387(10) . ? C25 C26 1.374(9) . ? C26 C27 1.400(9) . ? C26 C28 1.545(9) . ? C28 C45 1.550(9) . ? C29 C30 1.528(10) . ? C30 C31 1.510(9) . ? C31 C32 1.521(10) . ? C32 C33 1.522(10) . ? C33 C34 1.538(11) . ? C34 C35 1.534(12) . ? C35 C36 1.499(13) . ? C37 C38 1.550(10) . ? C38 C39 1.502(11) . ? C39 C40 1.523(12) . ? C40 C41 1.470(13) . ? C41 C42 1.580(15) . ? C42 C43 1.513(16) . ? C43 C44 1.524(17) . ? C45 C46 1.547(10) . ? C46 C47 1.472(10) . ? C47 C48 1.541(10) . ? C48 C49 1.543(11) . ? C49 C50 1.491(11) . ? C50 C51 1.522(11) . ? C51 C52 1.498(11) . ? C53 C55 1.50(3) . ? C53 C54 1.60(3) . ? C54 C56 1.46(5) . ? C54 C65 1.46(5) . ? C55 C57 1.58(3) . ? C56 C58 1.61(5) . ? C57 C59 1.54(3) . ? C58 C65 1.31(5) . ? C58 C60 1.32(3) . ? C59 C61 1.45(3) . ? C60 C70 1.50(5) . ? C61 C62 1.55(4) . ? C62 C68 1.52(5) . ? C63 C64 0.89(9) . ? C63 C70 1.53(2) . ? C63 C66 1.54(8) . ? C63 C69 1.60(14) . ? C63 Br7 1.76(10) . ? C64 C66 0.72(7) . ? C64 C69 1.32(9) . ? C64 C68 1.38(6) . ? C64 C67 1.39(6) . ? C64 Br7 1.89(6) . ? C64 Br13 2.02(6) . ? C66 C67 1.10(4) . ? C66 C69 1.47(9) . ? C66 Br7 1.90(3) . ? C66 Br13 2.05(3) . ? C67 Br13 1.13(3) . ? C67 C68 1.78(6) . ? C67 C69 1.95(10) . ? C68 Br13 1.49(4) . ? C68 C69 1.73(9) . ? C69 Br7 1.89(9) . ? C69 Br13 2.25(9) . ? C101 C102 1.55(2) . ? Br7 Br5 2.35(2) 12_547 ? Br13 Br6 2.141(16) 11_667 ? 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 116.1(6) . . ? C6 C1 C28 124.0(6) . . ? C2 C1 C28 119.9(6) . . ? O2 C2 C3 104.5(10) . . ? O2 C2 C1 135.0(10) . . ? C3 C2 C1 120.4(6) . . ? O2 C2 O1 18.7(8) . . ? C3 C2 O1 123.0(6) . . ? C1 C2 O1 116.6(7) . . ? C67 Br3 Br13 34.5(13) . . ? C67 Br3 C66 29.6(14) . . ? Br13 Br3 C66 58.7(9) . . ? C67 Br3 Br6 76.9(16) . 11_667 ? Br13 Br3 Br6 52.5(6) . 11_667 ? C66 Br3 Br6 106.3(10) . 11_667 ? C2 C3 C4 121.8(6) . . ? C2 C3 O4 130.4(8) . . ? C4 C3 O4 107.8(7) . . ? C2 C3 O3 110.2(7) . . ? C4 C3 O3 127.9(8) . . ? O4 C3 O3 20.4(6) . . ? O5 C4 C3 110.1(7) . . ? O5 C4 C5 129.5(8) . . ? C3 C4 C5 120.2(7) . . ? O5 C4 O6 17.6(5) . . ? C3 C4 O6 127.5(7) . . ? C5 C4 O6 112.3(7) . . ? C44 Br5 Br7 175.3(8) . 11_667 ? C6 C5 C4 116.9(6) . . ? C6 C5 C7 121.9(6) . . ? C4 C5 C7 121.2(6) . . ? C44 Br6 Br13 169.0(8) . 12_547 ? C44 Br6 Br3 124.4(8) . 12_547 ? Br13 Br6 Br3 47.6(6) 12_547 12_547 ? C5 C6 C1 124.6(6) . . ? C8 C7 C29 112.7(6) . . ? C8 C7 C5 110.1(5) . . ? C29 C7 C5 112.9(6) . . ? C69 Br8 Br7 102(5) . . ? C69 Br8 C64 58(4) . . ? Br7 Br8 C64 87(3) . . ? C69 Br8 C68 54(5) . . ? Br7 Br8 C68 128(3) . . ? C64 Br8 C68 40(3) . . ? C9 C8 C13 116.8(6) . . ? C9 C8 C7 122.0(6) . . ? C13 C8 C7 121.2(6) . . ? O7 C9 C8 120.5(7) . . ? O7 C9 C10 119.2(7) . . ? C8 C9 C10 120.3(7) . . ? C11 C10 O8 122.2(7) . . ? C11 C10 C9 120.2(7) . . ? O8 C10 C9 117.6(8) . . ? C12 C11 C10 122.1(7) . . ? C12 C11 O9 129.2(9) . . ? C10 C11 O9 108.6(8) . . ? C12 C11 O10 113.8(8) . . ? C10 C11 O10 124.1(8) . . ? O9 C11 O10 15.7(9) . . ? C11 C12 C13 117.8(7) . . ? C11 C12 C14 121.1(6) . . ? C13 C12 C14 121.0(6) . . ? C12 C13 C8 122.7(7) . . ? C12 C14 C15 110.3(5) . . ? C12 C14 C53 114.3(7) . . ? C15 C14 C53 111.8(7) . . ? C20 C15 C16 117.3(7) . . ? C20 C15 C14 122.4(6) . . ? C16 C15 C14 120.3(7) . . ? C17 C16 C15 121.7(8) . . ? C17 C16 O11 119.0(7) . . ? C15 C16 O11 119.3(8) . . ? O13 C17 C16 133.5(11) . . ? O13 C17 C18 107.1(11) . . ? C16 C17 C18 119.3(7) . . ? O13 C17 O12 22.0(10) . . ? C16 C17 O12 112.0(9) . . ? C18 C17 O12 128.7(9) . . ? O14 C18 C19 130.1(10) . . ? O14 C18 C17 108.0(8) . . ? C19 C18 C17 121.9(8) . . ? O14 C18 O15 17.7(7) . . ? C19 C18 O15 112.4(9) . . ? C17 C18 O15 125.7(8) . . ? C18 C19 C20 116.3(8) . . ? C18 C19 C21 122.5(7) . . ? C20 C19 C21 121.3(6) . . ? C15 C20 C19 123.5(6) . . ? C37 C21 C19 114.3(6) . . ? C37 C21 C22 111.3(6) . . ? C19 C21 C22 110.6(6) . . ? C27 C22 C23 116.2(6) . . ? C27 C22 C21 121.6(6) . . ? C23 C22 C21 122.2(6) . . ? C24 C23 C22 121.9(7) . . ? C24 C23 O16 117.1(6) . . ? C22 C23 O16 121.0(7) . . ? C23 C24 C25 121.0(7) . . ? C23 C24 O17 121.5(7) . . ? C25 C24 O17 117.5(7) . . ? C26 C25 O18 122.3(6) . . ? C26 C25 C24 120.0(6) . . ? O18 C25 C24 117.7(6) . . ? C25 C26 C27 117.2(6) . . ? C25 C26 C28 121.4(6) . . ? C27 C26 C28 121.4(6) . . ? C22 C27 C26 123.6(6) . . ? C1 C28 C26 110.2(5) . . ? C1 C28 C45 114.0(6) . . ? C26 C28 C45 110.6(6) . . ? C30 C29 C7 113.5(6) . . ? C31 C30 C29 113.7(6) . . ? C30 C31 C32 115.0(6) . . ? C31 C32 C33 112.1(6) . . ? C32 C33 C34 114.6(7) . . ? C35 C34 C33 111.0(7) . . ? C36 C35 C34 112.8(8) . . ? C35 C36 Br2 113.2(8) . . ? C21 C37 C38 113.6(6) . . ? C39 C38 C37 114.2(7) . . ? C38 C39 C40 114.8(7) . . ? C41 C40 C39 115.7(8) . . ? C40 C41 C42 113.5(8) . . ? C43 C42 C41 116.2(10) . . ? C42 C43 C44 126.3(13) . . ? C43 C44 Br5 130.0(17) . . ? C43 C44 Br6 106.1(12) . . ? Br5 C44 Br6 113.3(10) . . ? C46 C45 C28 114.3(6) . . ? C47 C46 C45 114.8(6) . . ? C46 C47 C48 111.8(6) . . ? C47 C48 C49 112.9(6) . . ? C50 C49 C48 113.8(7) . . ? C49 C50 C51 113.3(7) . . ? C52 C51 C50 113.7(7) . . ? C51 C52 Br1 113.2(6) . . ? C55 C53 C14 108.8(13) . . ? C55 C53 C54 19.7(12) . . ? C14 C53 C54 111.8(13) . . ? C56 C54 C65 51(2) . . ? C56 C54 C53 111(2) . . ? C65 C54 C53 120(3) . . ? C53 C55 C57 109(2) . . ? C54 C56 C58 110(3) . . ? C59 C57 C55 106.3(19) . . ? C65 C58 C60 144(3) . . ? C65 C58 C56 50(3) . . ? C60 C58 C56 105(2) . . ? C61 C59 C57 119(2) . . ? C58 C60 C70 118(3) . . ? C59 C61 C62 111(2) . . ? C68 C62 C61 122(3) . . ? C64 C63 C70 134(10) . . ? C64 C63 C66 15(5) . . ? C70 C63 C66 147(7) . . ? C64 C63 C69 56(8) . . ? C70 C63 C69 99(6) . . ? C66 C63 C69 56(4) . . ? C64 C63 Br7 84(8) . . ? C70 C63 Br7 124(7) . . ? C66 C63 Br7 70(3) . . ? C69 C63 Br7 68(5) . . ? C66 C64 C63 146(10) . . ? C66 C64 C69 87(8) . . ? C63 C64 C69 91(10) . . ? C66 C64 C68 129(8) . . ? C63 C64 C68 83(9) . . ? C69 C64 C68 80(5) . . ? C66 C64 C67 52(5) . . ? C63 C64 C67 162(10) . . ? C69 C64 C67 92(6) . . ? C68 C64 C67 80(4) . . ? C66 C64 Br8 112(8) . . ? C63 C64 Br8 46(8) . . ? C69 C64 Br8 50(4) . . ? C68 C64 Br8 96(5) . . ? C67 C64 Br8 141(5) . . ? C66 C64 Br7 80(6) . . ? C63 C64 Br7 68(8) . . ? C69 C64 Br7 70(4) . . ? C68 C64 Br7 136(5) . . ? C67 C64 Br7 130(5) . . ? Br8 C64 Br7 41(2) . . ? C66 C64 Br13 82(6) . . ? C63 C64 Br13 130(9) . . ? C69 C64 Br13 82(5) . . ? C68 C64 Br13 48(3) . . ? C67 C64 Br13 33(2) . . ? Br8 C64 Br13 126(4) . . ? Br7 C64 Br13 147(4) . . ? C58 C65 C54 131(4) . . ? C64 C66 C67 97(6) . . ? C64 C66 C69 64(6) . . ? C67 C66 C69 98(4) . . ? C64 C66 C63 19(7) . . ? C67 C66 C63 116(5) . . ? C69 C66 C63 64(5) . . ? C64 C66 Br7 78(6) . . ? C67 C66 Br7 164(3) . . ? C69 C66 Br7 67(4) . . ? C63 C66 Br7 60(4) . . ? C64 C66 Br13 77(6) . . ? C67 C66 Br13 24(2) . . ? C69 C66 Br13 78(3) . . ? C63 C66 Br13 96(4) . . ? Br7 C66 Br13 143.0(16) . . ? C64 C66 Br3 127(6) . . ? C67 C66 Br3 47(2) . . ? C69 C66 Br3 81(4) . . ? C63 C66 Br3 140(3) . . ? Br7 C66 Br3 124.1(15) . . ? Br13 C66 Br3 56.3(9) . . ? C66 C67 Br13 134(4) . . ? C66 C67 C64 31(3) . . ? Br13 C67 C64 106(4) . . ? C66 C67 Br3 103(3) . . ? Br13 C67 Br3 90(2) . . ? C64 C67 Br3 123(4) . . ? C66 C67 C68 80(3) . . ? Br13 C67 C68 56(2) . . ? C64 C67 C68 50(3) . . ? Br3 C67 C68 124(3) . . ? C66 C67 C69 48(3) . . ? Br13 C67 C69 90(3) . . ? C64 C67 C69 43(3) . . ? Br3 C67 C69 85(3) . . ? C68 C67 C69 55(3) . . ? C64 C68 Br13 89(4) . . ? C64 C68 C62 105(4) . . ? Br13 C68 C62 156(4) . . ? C64 C68 C69 49(4) . . ? Br13 C68 C69 88(4) . . ? C62 C68 C69 116(4) . . ? C64 C68 C67 50(3) . . ? Br13 C68 C67 39.2(16) . . ? C62 C68 C67 147(4) . . ? C69 C68 C67 67(4) . . ? C64 C68 Br8 44(3) . . ? Br13 C68 Br8 119(3) . . ? C62 C68 Br8 84(3) . . ? C69 C68 Br8 34(3) . . ? C67 C68 Br8 87(2) . . ? Br8 C69 C64 72(6) . . ? Br8 C69 C66 89(6) . . ? C64 C69 C66 29(4) . . ? Br8 C69 C63 43(5) . . ? C64 C69 C63 34(4) . . ? C66 C69 C63 60(5) . . ? Br8 C69 C68 91(6) . . ? C64 C69 C68 52(4) . . ? C66 C69 C68 73(4) . . ? C63 C69 C68 55(5) . . ? Br8 C69 Br7 40(3) . . ? C64 C69 Br7 69(5) . . ? C66 C69 Br7 68(3) . . ? C63 C69 Br7 60(5) . . ? C68 C69 Br7 114(5) . . ? Br8 C69 C67 117(7) . . ? C64 C69 C67 45(4) . . ? C66 C69 C67 34(2) . . ? C63 C69 C67 78(6) . . ? C68 C69 C67 57(3) . . ? Br7 C69 C67 102(4) . . ? Br8 C69 Br13 129(6) . . ? C64 C69 Br13 63(4) . . ? C66 C69 Br13 63(3) . . ? C63 C69 Br13 86(6) . . ? C68 C69 Br13 41(2) . . ? Br7 C69 Br13 129(4) . . ? C67 C69 Br13 30.1(16) . . ? C60 C70 C63 105(5) . . ? N2 C102 C101 142(7) . . ? Br8 Br7 C63 38(3) . . ? Br8 Br7 C64 52(3) . . ? C63 Br7 C64 28(3) . . ? Br8 Br7 C66 70(2) . . ? C63 Br7 C66 49(3) . . ? C64 Br7 C66 22(2) . . ? Br8 Br7 C69 38(3) . . ? C63 Br7 C69 52(4) . . ? C64 Br7 C69 41(3) . . ? C66 Br7 C69 46(3) . . ? Br8 Br7 Br5 168(2) . 12_547 ? C63 Br7 Br5 146(3) . 12_547 ? C64 Br7 Br5 138(2) . 12_547 ? C66 Br7 Br5 121.5(13) . 12_547 ? C69 Br7 Br5 152(3) . 12_547 ? C67 Br13 C68 84(3) . . ? C67 Br13 Br3 55.4(18) . . ? C68 Br13 Br3 119.1(19) . . ? C67 Br13 C64 41(2) . . ? C68 Br13 C64 43(2) . . ? Br3 Br13 C64 83(2) . . ? C67 Br13 C66 22.9(19) . . ? C68 Br13 C66 63.5(19) . . ? Br3 Br13 C66 64.9(11) . . ? C64 Br13 C66 20.3(19) . . ? C67 Br13 Br6 113(2) . 11_667 ? C68 Br13 Br6 160(2) . 11_667 ? Br3 Br13 Br6 79.9(8) . 11_667 ? C64 Br13 Br6 154(2) . 11_667 ? C66 Br13 Br6 135.2(11) . 11_667 ? C67 Br13 C69 60(3) . . ? C68 Br13 C69 50(3) . . ? Br3 Br13 C69 69(2) . . ? C64 Br13 C69 36(2) . . ? C66 Br13 C69 40(2) . . ? Br6 Br13 C69 146(2) 11_667 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.628 _refine_diff_density_min -2.032 _refine_diff_density_rms 0.233 #===END data_PgC4ClEthyleneglycol _database_code_depnum_ccdc_archive 'CCDC 604865' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C98 H122 Cl8 N4 O26' _chemical_formula_sum 'C98 H122 Cl8 N4 O26' _chemical_formula_weight 2055.60 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 12.663(4) _cell_length_b 19.072(7) _cell_length_c 21.232(7) _cell_angle_alpha 102.169(6) _cell_angle_beta 95.612(6) _cell_angle_gamma 92.779(6) _cell_volume 4976(3) _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 Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2164 _exptl_absorpt_coefficient_mu 0.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9418 _exptl_absorpt_correction_T_max 0.9703 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _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 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35217 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.18 _reflns_number_total 21312 _reflns_number_gt 13666 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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. Crystals were weakly diffracting. ; _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^)+(0.0965P)^2^+4.7830P] 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 21312 _refine_ls_number_parameters 1286 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1118 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.2008 _refine_ls_wR_factor_gt 0.1740 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.123 _refine_ls_shift/su_mean 0.001 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 Cl1 Cl 0.15958(15) 0.25199(9) 0.49749(10) 0.0856(5) Uani 0.80 1 d P A 1 Cl1A Cl 0.1953(6) 0.2429(4) 0.5453(4) 0.0856(5) Uani 0.20 1 d PD B 2 Cl2 Cl 0.33388(10) 0.49844(7) 0.40253(5) 0.0637(3) Uani 1 1 d . . . Cl3 Cl 1.13339(12) 0.74104(7) 0.64274(7) 0.0666(4) Uani 0.90 1 d P C 2 Cl3A Cl 1.0917(11) 0.7311(6) 0.5878(7) 0.0666(4) Uani 0.10 1 d P C 1 Cl4 Cl 1.06934(11) 0.44824(8) 0.55127(6) 0.0709(4) Uani 1 1 d . . . Cl5 Cl 0.82734(9) 0.95910(7) 0.39382(5) 0.0562(3) Uani 1 1 d . . . Cl6 Cl 0.70693(13) 1.25718(7) 0.52612(7) 0.0854(5) Uani 1 1 d . . . Cl7 Cl 1.58364(16) 1.06904(10) 0.55391(7) 0.0706(5) Uani 0.85 1 d P D 2 Cl7A Cl 1.5379(10) 1.0581(8) 0.5675(7) 0.110(5) Uani 0.15 1 d P E 1 Cl8 Cl 1.62114(8) 0.81251(6) 0.64305(7) 0.0620(3) Uani 1 1 d . . . O1 O 0.74132(18) 0.37530(13) 0.90480(11) 0.0358(6) Uani 1 1 d . . . H1O H 0.7267 0.3404 0.9216 0.043 Uiso 1 1 calc R . . O2 O 0.52893(19) 0.35006(14) 0.92720(12) 0.0404(6) Uani 1 1 d . . . H2O H 0.5000 0.3835 0.9502 0.049 Uiso 1 1 calc R . . O3 O 0.36808(17) 0.36652(12) 0.84047(11) 0.0334(5) Uani 1 1 d . . . H3O H 0.3689 0.3500 0.8742 0.040 Uiso 1 1 calc R . . O4 O 0.20252(17) 0.42977(13) 0.78800(12) 0.0392(6) Uani 1 1 d . . . H4O H 0.2386 0.3939 0.7878 0.047 Uiso 1 1 calc R . . O5 O 0.13921(18) 0.56349(14) 0.82039(13) 0.0420(6) Uani 1 1 d . . . H5O H 0.1273 0.6072 0.8266 0.050 Uiso 1 1 calc R . . O6 O 0.23882(17) 0.67692(13) 0.78456(12) 0.0350(5) Uani 1 1 d . . . H6O H 0.2516 0.6926 0.8248 0.042 Uiso 1 1 calc R . . O7 O 0.40498(17) 0.77754(13) 0.82824(13) 0.0419(6) Uani 1 1 d . . . H7O H 0.3562 0.7563 0.8000 0.050 Uiso 1 1 calc R . . O8 O 0.57789(19) 0.83541(13) 0.91036(13) 0.0456(7) Uani 1 1 d . . . H8O H 0.5271 0.8598 0.9017 0.055 Uiso 1 1 calc R . . O9 O 0.77554(16) 0.78819(11) 0.89177(10) 0.0259(5) Uani 1 1 d . . . H9O H 0.7554 0.8095 0.9269 0.031 Uiso 1 1 calc R . . O10 O 0.95827(16) 0.70249(11) 0.91092(10) 0.0256(5) Uani 1 1 d . . . H10O H 0.9123 0.7327 0.9101 0.031 Uiso 1 1 calc R . . O11 O 1.01438(17) 0.59422(12) 0.96526(10) 0.0278(5) Uani 1 1 d . . . H11O H 1.0220 0.6389 0.9795 0.033 Uiso 1 1 calc R . . O12 O 0.94242(19) 0.45783(12) 0.91484(11) 0.0368(6) Uani 1 1 d . . . H12O H 0.8909 0.4315 0.9208 0.044 Uiso 1 1 calc R . . O13 O 1.21480(16) 0.86195(13) 0.87568(11) 0.0308(5) Uani 1 1 d . . . H13O H 1.1908 0.8283 0.8914 0.037 Uiso 1 1 calc R . . O14 O 0.99878(16) 0.84405(12) 0.89409(10) 0.0280(5) Uani 1 1 d . . . H14O H 1.0361 0.8649 0.9284 0.034 Uiso 1 1 calc R . . O15 O 0.84620(15) 0.87600(12) 0.80890(10) 0.0264(5) Uani 1 1 d . . . H15O H 0.8427 0.8597 0.8425 0.032 Uiso 1 1 calc R . . O16 O 0.69328(16) 0.96014(12) 0.77113(11) 0.0292(5) Uani 1 1 d . . . H16O H 0.7263 0.9227 0.7689 0.035 Uiso 1 1 calc R . . O17 O 0.64540(17) 1.09266(13) 0.82604(12) 0.0349(5) Uani 1 1 d . . . H17O H 0.6104 1.0530 0.8211 0.042 Uiso 1 1 calc R . . O18 O 0.76128(18) 1.21241(12) 0.81345(12) 0.0358(6) Uani 1 1 d . . . H18O H 0.7073 1.2082 0.8328 0.043 Uiso 1 1 calc R . . O19 O 0.94101(17) 1.29196(14) 0.87504(11) 0.0368(6) Uani 1 1 d . . . H19O H 0.8877 1.2694 0.8515 0.044 Uiso 1 1 calc R . . O20 O 1.11950(19) 1.31841(17) 0.95958(11) 0.0510(8) Uani 1 1 d . . . H20O H 1.0574 1.3304 0.9647 0.061 Uiso 1 1 calc R . . O21 O 1.30800(17) 1.27648(14) 0.92583(11) 0.0369(6) Uani 1 1 d . . . H21O H 1.2902 1.3007 0.9605 0.044 Uiso 1 1 calc R . . O22 O 1.46696(19) 1.18508(13) 0.92889(12) 0.0416(6) Uani 1 1 d . . . H22O H 1.4220 1.2161 0.9345 0.050 Uiso 1 1 calc R . . O23 O 1.49101(19) 1.06282(13) 0.97029(11) 0.0385(6) Uani 1 1 d . . . H23O H 1.5018 1.1060 0.9902 0.046 Uiso 1 1 calc R . . O24 O 1.41047(17) 0.93399(12) 0.89984(10) 0.0282(5) Uani 1 1 d . . . H24O H 1.3658 0.9000 0.8817 0.034 Uiso 1 1 calc R . . O25 O 1.3174(2) 0.75797(14) 1.06695(12) 0.0387(6) Uani 1 1 d . . . O26 O 1.1683(2) 0.73383(13) 0.90432(12) 0.0347(6) Uani 1 1 d . . . N1 N 0.6612(4) 0.6497(3) 0.9551(2) 0.0999(18) Uani 1 1 d . . . N2 N 0.5912(9) 0.4715(7) 1.0200(6) 0.112(4) Uiso 0.50 1 d PD F 2 N2B N 0.6264(8) 0.4423(6) 1.0384(5) 0.081(3) Uiso 0.50 1 d PD F 3 N3 N 1.1946(3) 1.13569(18) 0.98084(15) 0.0458(8) Uani 1 1 d . . . N4 N 0.8995(3) 1.0632(2) 0.99571(19) 0.0664(11) Uani 1 1 d . . . C1 C 0.5955(2) 0.40440(16) 0.75643(15) 0.0257(7) Uani 1 1 d . . . H1 H 0.6098 0.4162 0.7167 0.031 Uiso 1 1 calc R . . C2 C 0.6810(2) 0.39995(15) 0.80152(15) 0.0242(6) Uani 1 1 d . . . C3 C 0.6586(3) 0.38138(17) 0.85921(15) 0.0274(7) Uani 1 1 d . . . C4 C 0.5540(3) 0.37044(17) 0.87180(16) 0.0295(7) Uani 1 1 d . . . C5 C 0.4712(2) 0.37657(16) 0.82596(16) 0.0270(7) Uani 1 1 d . . . C6 C 0.4893(3) 0.39227(16) 0.76704(15) 0.0275(7) Uani 1 1 d . . . C7 C 0.3948(2) 0.39753(17) 0.71831(15) 0.0285(7) Uani 1 1 d . . . H7 H 0.3377 0.3619 0.7238 0.034 Uiso 1 1 calc R . . C8 C 0.4201(3) 0.3752(2) 0.64773(17) 0.0441(9) Uani 1 1 d . . . C9 C 0.3257(3) 0.3616(3) 0.6000(2) 0.0394(11) Uani 0.80 1 d P A 1 H9A H 0.2916 0.4074 0.6006 0.047 Uiso 0.80 1 calc PR A 1 H9B H 0.2743 0.3279 0.6129 0.047 Uiso 0.80 1 calc PR A 1 C9A C 0.4249(14) 0.3108(8) 0.6213(8) 0.030(4) Uani 0.20 1 d P B 2 H9A1 H 0.3720 0.2826 0.6391 0.035 Uiso 0.20 1 calc PR B 2 H9A2 H 0.4959 0.2966 0.6357 0.035 Uiso 0.20 1 calc PR B 2 C10 C 0.3501(5) 0.3302(4) 0.5309(3) 0.0565(16) Uani 0.80 1 d P A 1 H10A H 0.4020 0.3638 0.5183 0.068 Uiso 0.80 1 calc PR A 1 H10B H 0.3838 0.2844 0.5304 0.068 Uiso 0.80 1 calc PR A 1 C10A C 0.4069(14) 0.2849(11) 0.5444(9) 0.044(5) Uani 0.20 1 d PD B 2 H10C H 0.4574 0.3141 0.5259 0.053 Uiso 0.20 1 calc PR B 2 H10D H 0.4259 0.2344 0.5330 0.053 Uiso 0.20 1 calc PR B 2 C11 C 0.2535(4) 0.3166(3) 0.4815(3) 0.0578(15) Uani 0.80 1 d P A 1 H11A H 0.2758 0.2992 0.4378 0.069 Uiso 0.80 1 calc PR A 1 H11B H 0.2194 0.3622 0.4817 0.069 Uiso 0.80 1 calc PR A 1 C11A C 0.2956(14) 0.2890(14) 0.5112(9) 0.105(15) Uani 0.20 1 d PD B 2 H11C H 0.2932 0.2673 0.4644 0.126 Uiso 0.20 1 calc PR B 2 H11D H 0.2799 0.3401 0.5157 0.126 Uiso 0.20 1 calc PR B 2 C12 C 0.3993(2) 0.53083(18) 0.71758(15) 0.0275(7) Uani 1 1 d . A . H12 H 0.4601 0.5239 0.6947 0.033 Uiso 1 1 calc R . . C13 C 0.3501(2) 0.47154(17) 0.73494(15) 0.0261(7) Uani 1 1 d . . . C14 C 0.2621(2) 0.48335(18) 0.76902(16) 0.0300(7) Uani 1 1 d . A . C15 C 0.2258(2) 0.55164(19) 0.78587(16) 0.0313(7) Uani 1 1 d . . . C16 C 0.2762(2) 0.60931(18) 0.76792(16) 0.0299(7) Uani 1 1 d . A . C17 C 0.3632(2) 0.59963(18) 0.73239(15) 0.0263(7) Uani 1 1 d . . . C18 C 0.4178(2) 0.66302(18) 0.71094(15) 0.0280(7) Uani 1 1 d . A . H18 H 0.3652 0.7005 0.7112 0.034 Uiso 1 1 calc R . . C19 C 0.4471(3) 0.64133(19) 0.64158(15) 0.0308(7) Uani 1 1 d . . . H19A H 0.4825 0.6836 0.6301 0.037 Uiso 1 1 calc R A . H19B H 0.4986 0.6037 0.6398 0.037 Uiso 1 1 calc R . . C20 C 0.3513(3) 0.6130(2) 0.59137(16) 0.0367(8) Uani 1 1 d . A . H20A H 0.3065 0.5780 0.6075 0.044 Uiso 1 1 calc R . . H20B H 0.3078 0.6534 0.5856 0.044 Uiso 1 1 calc R . . C21 C 0.3853(3) 0.5768(2) 0.52641(17) 0.0416(9) Uani 1 1 d . . . H21A H 0.4272 0.6124 0.5093 0.050 Uiso 1 1 calc R A . H21B H 0.4318 0.5379 0.5326 0.050 Uiso 1 1 calc R . . C22 C 0.2916(3) 0.5457(2) 0.47785(17) 0.0449(9) Uani 1 1 d . A . H22A H 0.2474 0.5849 0.4695 0.054 Uiso 1 1 calc R . . H22B H 0.2473 0.5121 0.4959 0.054 Uiso 1 1 calc R . . C23 C 0.6164(2) 0.67485(16) 0.75228(14) 0.0237(6) Uani 1 1 d . A . H23 H 0.6265 0.6384 0.7157 0.028 Uiso 1 1 calc R . . C24 C 0.5136(2) 0.69675(16) 0.75986(15) 0.0249(6) Uani 1 1 d . . . C25 C 0.5005(2) 0.74990(17) 0.81410(17) 0.0290(7) Uani 1 1 d . A . C26 C 0.5874(2) 0.78122(17) 0.85753(16) 0.0285(7) Uani 1 1 d . . . C27 C 0.6879(2) 0.75727(16) 0.84928(14) 0.0225(6) Uani 1 1 d . A . C28 C 0.7047(2) 0.70421(15) 0.79613(14) 0.0205(6) Uani 1 1 d . . . C29 C 0.8172(2) 0.68116(16) 0.78752(13) 0.0201(6) Uani 1 1 d . A . H29 H 0.8667 0.7239 0.8087 0.024 Uiso 1 1 calc R . . C30 C 0.8379(2) 0.66251(18) 0.71627(14) 0.0273(7) Uani 1 1 d . . . H30A H 0.7998 0.6156 0.6953 0.033 Uiso 1 1 calc R A . H30B H 0.8083 0.6992 0.6942 0.033 Uiso 1 1 calc R . . C31 C 0.9547(3) 0.6586(2) 0.70697(17) 0.0387(8) Uani 1 1 d . A . H31A H 0.9845 0.6212 0.7281 0.046 Uiso 1 1 calc R . . H31B H 0.9934 0.7052 0.7282 0.046 Uiso 1 1 calc R . . C32 C 0.9718(3) 0.6410(2) 0.63542(19) 0.0515(10) Uani 1 1 d . . . H32A H 0.9425 0.5911 0.6164 0.062 Uiso 1 1 calc R A . H32B H 0.9305 0.6733 0.6132 0.062 Uiso 1 1 calc R . . C33 C 1.0844(4) 0.6477(3) 0.6216(2) 0.0601(12) Uani 1 1 d . C . C34 C 0.8066(2) 0.55049(16) 0.79783(14) 0.0215(6) Uani 1 1 d . A . H34 H 0.7572 0.5407 0.7599 0.026 Uiso 1 1 calc R . . C35 C 0.8450(2) 0.62144(15) 0.82299(13) 0.0187(6) Uani 1 1 d . . . C36 C 0.9136(2) 0.63486(16) 0.88057(14) 0.0211(6) Uani 1 1 d . A . C37 C 0.9436(2) 0.57883(16) 0.90986(13) 0.0212(6) Uani 1 1 d . . . C38 C 0.9054(2) 0.50855(16) 0.88230(14) 0.0234(6) Uani 1 1 d . A . C39 C 0.8362(2) 0.49282(16) 0.82505(14) 0.0222(6) Uani 1 1 d . . . C40 C 0.7971(2) 0.41542(16) 0.79116(15) 0.0254(6) Uani 1 1 d . A . H40 H 0.8406 0.3827 0.8123 0.030 Uiso 1 1 calc R . . C41 C 0.8163(3) 0.40038(18) 0.71982(15) 0.0295(7) Uani 1 1 d . . . H41A H 0.7897 0.3503 0.6992 0.035 Uiso 1 1 calc R A . H41B H 0.7750 0.4328 0.6978 0.035 Uiso 1 1 calc R . . C42 C 0.9330(3) 0.4107(2) 0.71006(16) 0.0351(8) Uani 1 1 d . A . H42A H 0.9711 0.3698 0.7205 0.042 Uiso 1 1 calc R . . H42B H 0.9651 0.4552 0.7401 0.042 Uiso 1 1 calc R . . C43 C 0.9467(3) 0.4159(2) 0.64023(17) 0.0444(9) Uani 1 1 d . . . H43A H 0.9171 0.3705 0.6105 0.053 Uiso 1 1 calc R A . H43B H 0.9055 0.4554 0.6292 0.053 Uiso 1 1 calc R . . C44 C 1.0603(3) 0.4294(3) 0.6299(2) 0.0560(11) Uani 1 1 d . A . H44A H 1.0995 0.3866 0.6338 0.067 Uiso 1 1 calc R . . H44B H 1.0935 0.4706 0.6636 0.067 Uiso 1 1 calc R . . C45 C 1.0845(2) 0.92451(16) 0.73878(14) 0.0212(6) Uani 1 1 d . . . H45 H 1.1031 0.9440 0.7034 0.025 Uiso 1 1 calc R . . C46 C 1.1661(2) 0.90745(15) 0.78076(14) 0.0204(6) Uani 1 1 d . . . C47 C 1.1367(2) 0.87975(16) 0.83289(14) 0.0235(6) Uani 1 1 d . . . C48 C 1.0304(2) 0.87089(16) 0.84272(14) 0.0224(6) Uani 1 1 d . . . C49 C 0.9514(2) 0.88681(15) 0.79924(14) 0.0206(6) Uani 1 1 d . . . C50 C 0.9764(2) 0.91423(15) 0.74625(13) 0.0198(6) Uani 1 1 d . . . C51 C 0.8880(2) 0.93363(16) 0.70024(14) 0.0213(6) Uani 1 1 d . . . H51 H 0.8263 0.8978 0.6969 0.026 Uiso 1 1 calc R . . C52 C 0.9191(2) 0.92859(18) 0.63187(14) 0.0255(7) Uani 1 1 d . . . H52A H 0.9771 0.9658 0.6334 0.031 Uiso 1 1 calc R . . H52B H 0.9470 0.8811 0.6169 0.031 Uiso 1 1 calc R . . C53 C 0.8279(2) 0.93824(19) 0.58288(14) 0.0285(7) Uani 1 1 d . . . H53A H 0.7759 0.8960 0.5746 0.034 Uiso 1 1 calc R . . H53B H 0.7910 0.9813 0.6011 0.034 Uiso 1 1 calc R . . C54 C 0.8675(3) 0.9467(2) 0.51955(15) 0.0317(7) Uani 1 1 d . . . H54A H 0.9116 0.9926 0.5269 0.038 Uiso 1 1 calc R . . H54B H 0.9132 0.9071 0.5048 0.038 Uiso 1 1 calc R . . C55 C 0.7779(3) 0.9459(2) 0.46751(16) 0.0430(9) Uani 1 1 d . . . H55A H 0.7308 0.9844 0.4827 0.052 Uiso 1 1 calc R . . H55B H 0.7353 0.8993 0.4588 0.052 Uiso 1 1 calc R . . C56 C 0.9076(2) 1.07056(17) 0.72443(14) 0.0227(6) Uani 1 1 d . . . H56 H 0.9693 1.0661 0.7022 0.027 Uiso 1 1 calc R . . C57 C 0.8510(2) 1.00785(16) 0.72965(13) 0.0204(6) Uani 1 1 d . . . C58 C 0.7613(2) 1.01592(17) 0.76336(14) 0.0239(6) Uani 1 1 d . . . C59 C 0.7321(2) 1.08368(18) 0.79122(15) 0.0260(7) Uani 1 1 d . . . C60 C 0.7900(2) 1.14477(17) 0.78499(15) 0.0266(7) Uani 1 1 d . . . C61 C 0.8785(2) 1.13920(17) 0.75002(14) 0.0237(6) Uani 1 1 d . . . C62 C 0.9413(2) 1.20626(17) 0.74138(15) 0.0247(6) Uani 1 1 d . . . H62 H 0.8947 1.2471 0.7515 0.030 Uiso 1 1 calc R . . C63 C 0.9661(3) 1.20088(18) 0.67124(15) 0.0299(7) Uani 1 1 d . . . H63A H 1.0094 1.2447 0.6688 0.036 Uiso 1 1 calc R . . H63B H 1.0090 1.1591 0.6587 0.036 Uiso 1 1 calc R . . C64 C 0.8668(3) 1.1926(2) 0.62347(16) 0.0341(8) Uani 1 1 d . . . H64A H 0.8206 1.2317 0.6385 0.041 Uiso 1 1 calc R . . H64B H 0.8271 1.1464 0.6229 0.041 Uiso 1 1 calc R . . C65 C 0.8901(4) 1.1943(2) 0.55491(18) 0.0521(11) Uani 1 1 d . . . H65A H 0.9295 1.2407 0.5557 0.062 Uiso 1 1 calc R . . H65B H 0.9370 1.1555 0.5403 0.062 Uiso 1 1 calc R . . C66 C 0.7927(4) 1.1856(3) 0.5060(2) 0.0630(13) Uani 1 1 d . . . H66A H 0.7531 1.1391 0.5043 0.076 Uiso 1 1 calc R . . H66B H 0.8152 1.1849 0.4625 0.076 Uiso 1 1 calc R . . C67 C 1.1400(2) 1.20035(16) 0.77609(15) 0.0249(6) Uani 1 1 d . . . H67 H 1.1458 1.1726 0.7340 0.030 Uiso 1 1 calc R . . C68 C 1.0402(2) 1.22411(17) 0.79085(15) 0.0239(6) Uani 1 1 d . . . C69 C 1.0323(2) 1.26409(18) 0.85316(15) 0.0272(7) Uani 1 1 d . . . C70 C 1.1216(2) 1.27989(19) 0.89821(15) 0.0299(7) Uani 1 1 d . . . C71 C 1.2194(2) 1.25629(18) 0.88157(15) 0.0275(7) Uani 1 1 d . . . C72 C 1.2310(2) 1.21587(16) 0.82075(15) 0.0244(6) Uani 1 1 d . . . C73 C 1.3403(2) 1.18992(17) 0.80603(15) 0.0259(7) Uani 1 1 d . . . H73 H 1.3944 1.2277 0.8318 0.031 Uiso 1 1 calc R . . C74 C 1.3579(3) 1.18276(19) 0.73457(16) 0.0312(7) Uani 1 1 d . . . H74A H 1.3114 1.1418 0.7080 0.037 Uiso 1 1 calc R . . H74B H 1.3369 1.2269 0.7205 0.037 Uiso 1 1 calc R . . C75 C 1.4718(3) 1.1711(3) 0.7223(2) 0.0448(10) Uani 1 1 d . . . C76 C 1.4762(4) 1.1348(4) 0.6495(2) 0.0548(9) Uani 0.85 1 d P D 2 H76A H 1.4330 1.0883 0.6392 0.066 Uiso 0.85 1 calc PR D 2 H76B H 1.4443 1.1659 0.6220 0.066 Uiso 0.85 1 calc PR D 2 C76A C 1.526(2) 1.1696(15) 0.6669(14) 0.0548(9) Uani 0.15 1 d PD E 1 H76C H 1.5995 1.1918 0.6779 0.066 Uiso 0.15 1 calc PR E 1 H76D H 1.4868 1.1922 0.6345 0.066 Uiso 0.15 1 calc PR E 1 C77 C 1.5856(4) 1.1221(3) 0.6340(2) 0.0548(9) Uani 0.85 1 d P D 2 H77A H 1.6216 1.0970 0.6655 0.066 Uiso 0.85 1 calc PR D 2 H77B H 1.6262 1.1688 0.6375 0.066 Uiso 0.85 1 calc PR D 2 C77A C 1.522(2) 1.0859(14) 0.6447(13) 0.0548(9) Uani 0.15 1 d PD E 1 H77C H 1.4527 1.0652 0.6528 0.066 Uiso 0.15 1 calc PR E 1 H77D H 1.5785 1.0676 0.6713 0.066 Uiso 0.15 1 calc PR E 1 C78 C 1.3161(2) 1.05388(16) 0.79452(13) 0.0211(6) Uani 1 1 d . . . H78 H 1.2735 1.0519 0.7547 0.025 Uiso 1 1 calc R . . C79 C 1.3594(2) 1.12108(17) 0.83002(14) 0.0229(6) Uani 1 1 d . . . C80 C 1.4193(2) 1.12207(17) 0.88917(15) 0.0277(7) Uani 1 1 d . . . C81 C 1.4345(2) 1.05942(18) 0.91087(14) 0.0272(7) Uani 1 1 d . . . C82 C 1.3916(2) 0.99335(17) 0.87389(14) 0.0229(6) Uani 1 1 d . . . C83 C 1.3319(2) 0.98989(16) 0.81418(13) 0.0200(6) Uani 1 1 d . . . C84 C 1.2837(2) 0.91785(16) 0.77268(14) 0.0210(6) Uani 1 1 d . . . H84 H 1.3199 0.8796 0.7904 0.025 Uiso 1 1 calc R . . C85 C 1.3063(2) 0.90763(17) 0.70187(14) 0.0243(6) Uani 1 1 d . . . H85A H 1.2677 0.8626 0.6764 0.029 Uiso 1 1 calc R . . H85B H 1.2789 0.9480 0.6840 0.029 Uiso 1 1 calc R . . C86 C 1.4246(2) 0.9042(2) 0.69425(15) 0.0318(7) Uani 1 1 d . . . H86A H 1.4624 0.9508 0.7166 0.038 Uiso 1 1 calc R . . H86B H 1.4534 0.8665 0.7154 0.038 Uiso 1 1 calc R . . C87 C 1.4463(3) 0.8881(2) 0.62423(17) 0.0444(10) Uani 1 1 d . . . H87A H 1.4156 0.9252 0.6031 0.053 Uiso 1 1 calc R . . H87B H 1.4091 0.8411 0.6023 0.053 Uiso 1 1 calc R . . C88 C 1.5626(3) 0.8857(3) 0.61444(19) 0.0483(10) Uani 1 1 d . . . H88A H 1.6010 0.9316 0.6379 0.058 Uiso 1 1 calc R . . H88B H 1.5703 0.8803 0.5677 0.058 Uiso 1 1 calc R . . C89 C 0.5481(4) 0.5680(3) 0.8634(2) 0.0600(12) Uani 1 1 d . . . H89A H 0.4732 0.5684 0.8715 0.090 Uiso 1 1 calc R . . H89B H 0.5709 0.5190 0.8587 0.090 Uiso 1 1 calc R . . H89C H 0.5565 0.5849 0.8235 0.090 Uiso 1 1 calc R . . C90 C 0.6071(4) 0.6111(3) 0.9127(2) 0.0633(13) Uani 1 1 d . . . C91 C 0.7786(7) 0.5350(5) 1.0409(4) 0.0389(19) Uiso 0.50 1 d P F 1 H91A H 0.8358 0.5083 1.0214 0.058 Uiso 0.50 1 calc PR F 1 H91B H 0.8021 0.5568 1.0864 0.058 Uiso 0.50 1 calc PR F 1 H91C H 0.7608 0.5729 1.0176 0.058 Uiso 0.50 1 calc PR F 1 C91A C 0.7847(19) 0.5058(14) 1.0251(12) 0.070(6) Uiso 0.25 1 d P F 2 H91D H 0.7805 0.5326 0.9904 0.105 Uiso 0.25 1 calc PR F 2 H91E H 0.8213 0.4619 1.0115 0.105 Uiso 0.25 1 calc PR F 2 H91F H 0.8242 0.5357 1.0643 0.105 Uiso 0.25 1 calc PR F 2 C91B C 0.832(2) 0.5136(17) 1.0601(16) 0.096(8) Uiso 0.25 1 d P F 3 H91G H 0.8467 0.5263 1.1075 0.144 Uiso 0.25 1 calc PR F 3 H91H H 0.8535 0.5549 1.0422 0.144 Uiso 0.25 1 calc PR F 3 H91I H 0.8733 0.4728 1.0431 0.144 Uiso 0.25 1 calc PR F 3 C92 C 0.6903(6) 0.4889(4) 1.0369(3) 0.100(2) Uiso 1 1 d D . . C93 C 1.0695(3) 1.0754(2) 0.87817(16) 0.0382(8) Uani 1 1 d . . . H93A H 1.0620 1.0234 0.8755 0.057 Uiso 1 1 calc R . . H93B H 1.0997 1.0847 0.8397 0.057 Uiso 1 1 calc R . . H93C H 0.9995 1.0950 0.8804 0.057 Uiso 1 1 calc R . . C94 C 1.1396(3) 1.10966(19) 0.93596(16) 0.0337(8) Uani 1 1 d . . . C95 C 0.7246(3) 0.9925(2) 0.9435(2) 0.0547(11) Uani 1 1 d . . . H95A H 0.6679 1.0257 0.9441 0.082 Uiso 1 1 calc R . . H95B H 0.7068 0.9559 0.9677 0.082 Uiso 1 1 calc R . . H95C H 0.7320 0.9691 0.8985 0.082 Uiso 1 1 calc R . . C96 C 0.8226(3) 1.0315(2) 0.97267(18) 0.0420(9) Uani 1 1 d . . . C97 C 1.2356(3) 0.7154(2) 0.95667(18) 0.0437(9) Uani 1 1 d . . . H97A H 1.3049 0.7020 0.9416 0.052 Uiso 1 1 calc R . . H97B H 1.2018 0.6733 0.9694 0.052 Uiso 1 1 calc R . . C98 C 1.2533(3) 0.7768(2) 1.01398(18) 0.0440(9) Uani 1 1 d . . . H98A H 1.2891 0.8183 1.0016 0.053 Uiso 1 1 calc R . . H98B H 1.1838 0.7912 1.0281 0.053 Uiso 1 1 calc R . . H250 H 1.382(3) 0.770(2) 1.0640(18) 0.037(11) Uiso 1 1 d . . . H260 H 1.105(5) 0.723(3) 0.906(3) 0.11(2) Uiso 1 1 d . . . H75B H 1.513(3) 1.2115(18) 0.7388(15) 0.016(8) Uiso 1 1 d . G 2 H75A H 1.502(3) 1.139(2) 0.7523(19) 0.045(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0887(12) 0.0583(9) 0.0921(13) -0.0014(9) -0.0244(10) -0.0228(8) Cl1A 0.0887(12) 0.0583(9) 0.0921(13) -0.0014(9) -0.0244(10) -0.0228(8) Cl2 0.0664(7) 0.0798(8) 0.0367(5) -0.0003(5) -0.0085(5) 0.0083(6) Cl3 0.0776(9) 0.0504(7) 0.0722(9) 0.0100(6) 0.0280(7) -0.0167(6) Cl3A 0.0776(9) 0.0504(7) 0.0722(9) 0.0100(6) 0.0280(7) -0.0167(6) Cl4 0.0848(9) 0.0856(9) 0.0473(6) 0.0204(6) 0.0237(6) -0.0039(7) Cl5 0.0602(6) 0.0834(8) 0.0298(5) 0.0270(5) -0.0004(4) -0.0038(6) Cl6 0.1077(11) 0.0671(8) 0.0766(8) 0.0228(7) -0.0378(8) 0.0248(8) Cl7 0.0767(12) 0.0857(12) 0.0452(8) -0.0037(7) 0.0175(8) 0.0217(10) Cl7A 0.084(8) 0.124(10) 0.127(11) 0.004(7) 0.092(8) 0.005(7) Cl8 0.0409(6) 0.0390(6) 0.1025(9) -0.0031(6) 0.0317(6) 0.0016(4) O1 0.0313(12) 0.0406(14) 0.0421(14) 0.0212(11) 0.0069(10) 0.0091(11) O2 0.0396(14) 0.0472(16) 0.0461(15) 0.0263(12) 0.0200(11) 0.0161(12) O3 0.0274(12) 0.0356(13) 0.0442(14) 0.0212(11) 0.0104(10) 0.0025(10) O4 0.0247(12) 0.0392(14) 0.0606(16) 0.0245(12) 0.0097(11) -0.0003(10) O5 0.0305(13) 0.0424(15) 0.0586(16) 0.0159(13) 0.0189(12) 0.0077(11) O6 0.0289(12) 0.0331(13) 0.0422(14) 0.0060(11) 0.0040(10) 0.0027(10) O7 0.0195(11) 0.0320(14) 0.0664(17) -0.0057(12) 0.0006(11) 0.0053(10) O8 0.0281(13) 0.0346(14) 0.0619(17) -0.0184(12) 0.0070(12) 0.0059(11) O9 0.0218(11) 0.0265(12) 0.0259(11) -0.0014(9) 0.0020(8) -0.0015(9) O10 0.0280(11) 0.0186(11) 0.0285(11) 0.0040(9) -0.0037(9) 0.0030(9) O11 0.0333(12) 0.0223(11) 0.0253(11) 0.0036(9) -0.0049(9) 0.0018(9) O12 0.0446(14) 0.0232(12) 0.0424(14) 0.0142(10) -0.0108(11) 0.0018(10) O13 0.0203(11) 0.0402(14) 0.0398(13) 0.0271(11) 0.0012(9) 0.0038(9) O14 0.0233(11) 0.0346(13) 0.0322(12) 0.0211(10) 0.0040(9) -0.0002(9) O15 0.0180(10) 0.0340(13) 0.0328(12) 0.0183(10) 0.0051(9) 0.0027(9) O16 0.0240(11) 0.0274(12) 0.0393(13) 0.0120(10) 0.0090(9) 0.0023(9) O17 0.0238(11) 0.0327(13) 0.0527(15) 0.0129(11) 0.0169(10) 0.0061(10) O18 0.0265(12) 0.0285(13) 0.0556(15) 0.0086(11) 0.0177(11) 0.0089(10) O19 0.0203(11) 0.0549(16) 0.0341(13) 0.0039(11) 0.0054(9) 0.0128(11) O20 0.0275(13) 0.091(2) 0.0289(13) -0.0037(13) 0.0049(10) 0.0141(14) O21 0.0241(12) 0.0516(16) 0.0343(13) 0.0085(11) 0.0006(10) 0.0042(11) O22 0.0413(14) 0.0263(13) 0.0474(15) -0.0037(11) -0.0211(11) 0.0092(11) O23 0.0478(15) 0.0341(14) 0.0271(12) 0.0000(10) -0.0154(10) 0.0085(11) O24 0.0287(11) 0.0295(12) 0.0270(11) 0.0107(9) -0.0056(9) 0.0044(9) O25 0.0373(15) 0.0406(15) 0.0405(14) 0.0160(12) -0.0003(11) 0.0045(12) O26 0.0285(13) 0.0352(14) 0.0434(14) 0.0179(11) -0.0022(11) 0.0010(11) N1 0.093(4) 0.137(5) 0.053(3) -0.005(3) -0.001(3) -0.022(3) N3 0.056(2) 0.046(2) 0.0326(17) 0.0050(14) 0.0005(15) 0.0006(16) N4 0.064(3) 0.069(3) 0.057(2) -0.003(2) 0.010(2) -0.011(2) C1 0.0309(17) 0.0176(15) 0.0284(16) 0.0034(12) 0.0071(13) -0.0017(12) C2 0.0257(16) 0.0136(14) 0.0326(16) 0.0022(12) 0.0055(13) 0.0023(12) C3 0.0315(17) 0.0215(16) 0.0312(17) 0.0083(13) 0.0056(13) 0.0070(13) C4 0.0306(17) 0.0254(17) 0.0369(18) 0.0127(14) 0.0103(14) 0.0063(13) C5 0.0261(16) 0.0182(15) 0.0395(18) 0.0088(13) 0.0113(13) 0.0016(12) C6 0.0299(17) 0.0186(15) 0.0328(17) 0.0031(13) 0.0042(13) -0.0004(12) C7 0.0242(16) 0.0272(17) 0.0313(17) 0.0025(13) 0.0030(13) -0.0092(13) C8 0.044(2) 0.049(2) 0.0314(19) -0.0040(17) 0.0047(16) -0.0145(18) C9 0.028(2) 0.049(3) 0.036(2) 0.001(2) -0.0015(18) 0.000(2) C9A 0.050(10) 0.011(7) 0.039(9) 0.013(7) 0.036(8) 0.019(7) C10 0.042(3) 0.086(5) 0.033(3) -0.005(3) 0.003(2) 0.006(3) C10A 0.050(11) 0.039(11) 0.038(10) -0.006(8) 0.002(8) 0.026(9) C11 0.057(3) 0.067(4) 0.042(3) -0.003(3) 0.001(3) 0.008(3) C11A 0.14(3) 0.16(3) 0.012(10) -0.012(14) -0.025(13) 0.12(3) C12 0.0218(15) 0.0329(18) 0.0273(16) 0.0069(13) 0.0005(12) -0.0013(13) C13 0.0217(15) 0.0284(17) 0.0270(16) 0.0070(13) -0.0027(12) -0.0040(13) C14 0.0219(16) 0.0350(19) 0.0348(17) 0.0138(15) 0.0005(13) -0.0038(13) C15 0.0188(15) 0.041(2) 0.0360(18) 0.0134(15) 0.0037(13) 0.0013(14) C16 0.0224(16) 0.0326(18) 0.0342(17) 0.0090(14) -0.0024(13) 0.0002(13) C17 0.0187(15) 0.0332(18) 0.0273(16) 0.0114(13) -0.0041(12) -0.0046(13) C18 0.0207(15) 0.0305(18) 0.0344(17) 0.0131(14) -0.0012(13) -0.0018(13) C19 0.0267(16) 0.0365(19) 0.0299(17) 0.0132(14) -0.0020(13) -0.0051(14) C20 0.0303(18) 0.047(2) 0.0327(18) 0.0145(16) -0.0044(14) -0.0038(16) C21 0.037(2) 0.054(2) 0.0331(19) 0.0126(17) -0.0023(15) -0.0032(17) C22 0.043(2) 0.053(2) 0.035(2) 0.0079(17) -0.0059(16) -0.0052(18) C23 0.0253(15) 0.0234(16) 0.0235(15) 0.0077(12) 0.0020(12) 0.0024(12) C24 0.0196(15) 0.0236(16) 0.0325(16) 0.0116(13) -0.0021(12) -0.0014(12) C25 0.0195(15) 0.0228(16) 0.0455(19) 0.0077(14) 0.0047(13) 0.0050(12) C26 0.0262(16) 0.0209(16) 0.0361(17) 0.0000(13) 0.0049(13) 0.0018(13) C27 0.0197(14) 0.0211(15) 0.0271(15) 0.0068(12) 0.0018(12) -0.0012(12) C28 0.0224(15) 0.0178(15) 0.0241(15) 0.0099(12) 0.0037(11) 0.0021(11) C29 0.0205(14) 0.0203(15) 0.0209(14) 0.0070(11) 0.0032(11) 0.0009(11) C30 0.0302(17) 0.0311(18) 0.0234(15) 0.0117(13) 0.0041(12) 0.0024(13) C31 0.0291(18) 0.047(2) 0.041(2) 0.0084(17) 0.0151(15) 0.0022(16) C32 0.055(3) 0.053(3) 0.043(2) -0.0011(19) 0.0193(19) -0.003(2) C33 0.053(3) 0.056(3) 0.067(3) 0.000(2) 0.024(2) -0.011(2) C34 0.0194(14) 0.0225(16) 0.0226(14) 0.0052(12) 0.0023(11) 0.0015(12) C35 0.0188(14) 0.0178(14) 0.0213(14) 0.0064(11) 0.0058(11) 0.0043(11) C36 0.0208(14) 0.0201(15) 0.0221(14) 0.0024(12) 0.0057(11) 0.0024(12) C37 0.0201(14) 0.0253(16) 0.0193(14) 0.0069(12) 0.0025(11) 0.0047(12) C38 0.0254(15) 0.0206(15) 0.0265(15) 0.0077(12) 0.0059(12) 0.0073(12) C39 0.0216(15) 0.0193(15) 0.0271(15) 0.0051(12) 0.0076(12) 0.0036(12) C40 0.0261(16) 0.0178(15) 0.0317(16) 0.0042(12) 0.0039(13) -0.0002(12) C41 0.0304(17) 0.0246(17) 0.0315(17) 0.0010(13) 0.0052(13) 0.0026(13) C42 0.0320(18) 0.037(2) 0.0344(18) 0.0011(15) 0.0082(14) 0.0032(15) C43 0.043(2) 0.053(2) 0.0332(19) 0.0009(17) 0.0096(16) -0.0055(18) C44 0.049(2) 0.079(3) 0.044(2) 0.020(2) 0.0151(19) 0.004(2) C45 0.0237(15) 0.0212(15) 0.0196(14) 0.0057(11) 0.0053(11) 0.0000(12) C46 0.0206(14) 0.0181(15) 0.0232(14) 0.0042(11) 0.0046(11) 0.0043(11) C47 0.0217(15) 0.0239(16) 0.0273(15) 0.0106(12) 0.0018(12) 0.0058(12) C48 0.0220(15) 0.0225(15) 0.0258(15) 0.0107(12) 0.0058(12) 0.0029(12) C49 0.0156(13) 0.0182(15) 0.0288(15) 0.0057(12) 0.0043(11) 0.0010(11) C50 0.0197(14) 0.0188(15) 0.0198(14) 0.0018(11) 0.0016(11) 0.0017(11) C51 0.0145(13) 0.0256(16) 0.0238(15) 0.0063(12) 0.0008(11) -0.0001(11) C52 0.0212(15) 0.0322(18) 0.0224(15) 0.0050(13) 0.0011(12) 0.0027(13) C53 0.0233(16) 0.0392(19) 0.0229(15) 0.0069(14) 0.0023(12) 0.0023(14) C54 0.0287(17) 0.044(2) 0.0231(16) 0.0102(14) 0.0003(13) -0.0008(15) C55 0.041(2) 0.068(3) 0.0225(17) 0.0151(17) 0.0009(15) 0.0050(19) C56 0.0152(14) 0.0307(17) 0.0236(15) 0.0096(13) 0.0003(11) 0.0034(12) C57 0.0180(14) 0.0247(16) 0.0190(14) 0.0072(12) -0.0017(11) 0.0028(11) C58 0.0183(14) 0.0299(17) 0.0246(15) 0.0098(13) -0.0001(11) 0.0011(12) C59 0.0180(14) 0.0345(18) 0.0289(16) 0.0111(14) 0.0063(12) 0.0072(13) C60 0.0225(15) 0.0258(17) 0.0324(17) 0.0074(13) 0.0024(13) 0.0068(13) C61 0.0198(15) 0.0289(17) 0.0241(15) 0.0106(13) -0.0008(11) 0.0037(12) C62 0.0231(15) 0.0249(16) 0.0296(16) 0.0114(13) 0.0058(12) 0.0065(12) C63 0.0338(18) 0.0280(17) 0.0317(17) 0.0137(14) 0.0050(14) 0.0049(14) C64 0.0382(19) 0.036(2) 0.0308(17) 0.0126(15) 0.0011(14) 0.0089(15) C65 0.070(3) 0.056(3) 0.033(2) 0.0160(19) 0.0039(19) 0.012(2) C66 0.089(3) 0.064(3) 0.034(2) 0.013(2) -0.009(2) 0.009(3) C67 0.0238(15) 0.0196(15) 0.0321(16) 0.0066(13) 0.0054(12) -0.0002(12) C68 0.0201(15) 0.0257(16) 0.0293(16) 0.0132(13) 0.0028(12) 0.0019(12) C69 0.0199(15) 0.0339(18) 0.0323(17) 0.0143(14) 0.0075(12) 0.0062(13) C70 0.0255(16) 0.0379(19) 0.0277(16) 0.0083(14) 0.0065(13) 0.0040(14) C71 0.0190(15) 0.0329(18) 0.0341(17) 0.0147(14) 0.0039(12) 0.0018(13) C72 0.0193(15) 0.0231(16) 0.0349(17) 0.0130(13) 0.0084(12) 0.0020(12) C73 0.0194(15) 0.0234(16) 0.0358(17) 0.0073(13) 0.0046(12) 0.0035(12) C74 0.0314(17) 0.0288(18) 0.0391(19) 0.0152(14) 0.0107(14) 0.0105(14) C75 0.034(2) 0.061(3) 0.047(2) 0.021(2) 0.0171(17) 0.015(2) C76 0.040(2) 0.081(3) 0.0413(18) 0.0046(18) 0.0085(15) 0.0111(18) C76A 0.040(2) 0.081(3) 0.0413(18) 0.0046(18) 0.0085(15) 0.0111(18) C77 0.040(2) 0.081(3) 0.0413(18) 0.0046(18) 0.0085(15) 0.0111(18) C77A 0.040(2) 0.081(3) 0.0413(18) 0.0046(18) 0.0085(15) 0.0111(18) C78 0.0184(14) 0.0275(16) 0.0182(14) 0.0064(12) 0.0015(11) 0.0030(12) C79 0.0152(14) 0.0278(17) 0.0280(15) 0.0095(13) 0.0043(11) 0.0057(12) C80 0.0212(15) 0.0273(17) 0.0310(17) -0.0007(13) -0.0017(12) 0.0049(13) C81 0.0239(16) 0.0346(18) 0.0221(15) 0.0049(13) -0.0027(12) 0.0100(13) C82 0.0203(14) 0.0271(16) 0.0238(15) 0.0096(12) 0.0035(11) 0.0071(12) C83 0.0162(13) 0.0253(16) 0.0206(14) 0.0077(12) 0.0044(11) 0.0054(11) C84 0.0185(14) 0.0230(15) 0.0228(14) 0.0068(12) 0.0042(11) 0.0036(12) C85 0.0185(14) 0.0282(17) 0.0244(15) 0.0025(12) 0.0018(11) -0.0019(12) C86 0.0218(16) 0.044(2) 0.0295(17) 0.0046(15) 0.0074(13) 0.0029(14) C87 0.0266(18) 0.075(3) 0.0283(18) 0.0015(18) 0.0096(14) 0.0015(18) C88 0.034(2) 0.072(3) 0.039(2) 0.009(2) 0.0160(16) -0.0013(19) C89 0.065(3) 0.052(3) 0.065(3) 0.017(2) 0.010(2) 0.002(2) C90 0.062(3) 0.083(4) 0.043(3) 0.011(2) 0.009(2) 0.000(3) C93 0.046(2) 0.037(2) 0.0294(18) 0.0045(15) 0.0035(15) -0.0007(16) C94 0.046(2) 0.0300(18) 0.0267(17) 0.0078(14) 0.0081(15) 0.0059(16) C95 0.055(3) 0.050(3) 0.059(3) 0.015(2) -0.005(2) 0.007(2) C96 0.051(2) 0.039(2) 0.036(2) 0.0055(17) 0.0130(18) 0.0066(19) C97 0.049(2) 0.039(2) 0.044(2) 0.0147(17) -0.0065(17) 0.0071(17) C98 0.049(2) 0.039(2) 0.046(2) 0.0160(17) -0.0032(18) 0.0109(18) _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 Cl1 C11 1.777(6) . ? Cl1A C11A 1.804(19) . ? Cl2 C22 1.806(4) . ? Cl3 C33 1.805(5) . ? Cl3A C33 1.880(13) . ? Cl4 C44 1.793(4) . ? Cl5 C55 1.802(4) . ? Cl6 C66 1.793(5) . ? Cl7 C77 1.784(5) . ? Cl7A C77A 1.65(3) . ? Cl8 C88 1.799(5) . ? O1 C3 1.381(4) . ? O2 C4 1.374(4) . ? O3 C5 1.384(4) . ? O4 C14 1.391(4) . ? O5 C15 1.379(4) . ? O6 C16 1.383(4) . ? O7 C25 1.378(4) . ? O8 C26 1.375(4) . ? O9 C27 1.382(3) . ? O10 C36 1.381(4) . ? O11 C37 1.377(3) . ? O12 C38 1.377(4) . ? O13 C47 1.380(3) . ? O14 C48 1.383(3) . ? O15 C49 1.380(3) . ? O16 C58 1.384(4) . ? O17 C59 1.380(4) . ? O18 C60 1.386(4) . ? O19 C69 1.377(4) . ? O20 C70 1.358(4) . ? O21 C71 1.375(4) . ? O22 C80 1.386(4) . ? O23 C81 1.376(3) . ? O24 C82 1.381(4) . ? O25 C98 1.439(4) . ? O26 C97 1.447(4) . ? N1 C90 1.172(6) . ? N2 C92 1.279(11) . ? N2B C92 1.181(10) . ? N3 C94 1.130(4) . ? N4 C96 1.131(5) . ? C1 C2 1.391(4) . ? C1 C6 1.401(4) . ? C2 C3 1.395(4) . ? C2 C40 1.531(4) . ? C3 C4 1.392(4) . ? C4 C5 1.386(5) . ? C5 C6 1.384(4) . ? C6 C7 1.526(4) . ? C7 C13 1.531(5) . ? C7 C8 1.539(5) . ? C8 C9A 1.247(15) . ? C8 C9 1.464(5) . ? C9 C10 1.531(7) . ? C9A C10A 1.59(2) . ? C10 C11 1.507(7) . ? C10A C11A 1.526(17) . ? C12 C13 1.399(4) . ? C12 C17 1.393(5) . ? C13 C14 1.388(4) . ? C14 C15 1.389(5) . ? C15 C16 1.385(5) . ? C16 C17 1.393(4) . ? C17 C18 1.536(4) . ? C18 C19 1.530(5) . ? C18 C24 1.536(4) . ? C19 C20 1.530(4) . ? C20 C21 1.520(5) . ? C21 C22 1.503(5) . ? C23 C24 1.400(4) . ? C23 C28 1.395(4) . ? C24 C25 1.394(5) . ? C25 C26 1.387(4) . ? C26 C27 1.387(4) . ? C27 C28 1.389(4) . ? C28 C29 1.528(4) . ? C29 C30 1.531(4) . ? C29 C35 1.529(4) . ? C30 C31 1.515(4) . ? C31 C32 1.524(5) . ? C32 C33 1.489(6) . ? C34 C35 1.391(4) . ? C34 C39 1.397(4) . ? C35 C36 1.398(4) . ? C36 C37 1.395(4) . ? C37 C38 1.387(4) . ? C38 C39 1.395(4) . ? C39 C40 1.534(4) . ? C40 C41 1.527(4) . ? C41 C42 1.521(5) . ? C42 C43 1.532(5) . ? C43 C44 1.495(5) . ? C45 C46 1.393(4) . ? C45 C50 1.403(4) . ? C46 C47 1.396(4) . ? C46 C84 1.524(4) . ? C47 C48 1.390(4) . ? C48 C49 1.383(4) . ? C49 C50 1.393(4) . ? C50 C51 1.524(4) . ? C51 C52 1.526(4) . ? C51 C57 1.537(4) . ? C52 C53 1.522(4) . ? C53 C54 1.517(4) . ? C54 C55 1.502(4) . ? C56 C57 1.394(4) . ? C56 C61 1.389(4) . ? C57 C58 1.398(4) . ? C58 C59 1.387(4) . ? C59 C60 1.383(4) . ? C60 C61 1.400(4) . ? C61 C62 1.526(4) . ? C62 C68 1.529(4) . ? C62 C63 1.535(4) . ? C63 C64 1.516(4) . ? C64 C65 1.520(5) . ? C65 C66 1.511(6) . ? C67 C72 1.396(4) . ? C67 C68 1.404(4) . ? C68 C69 1.397(4) . ? C69 C70 1.385(4) . ? C70 C71 1.390(4) . ? C71 C72 1.383(5) . ? C72 C73 1.532(4) . ? C73 C79 1.526(4) . ? C73 C74 1.534(4) . ? C74 C75 1.509(5) . ? C75 C76A 1.41(3) . ? C75 C76 1.561(6) . ? C76 C77 1.476(6) . ? C76A C77A 1.564(19) . ? C78 C83 1.388(4) . ? C78 C79 1.398(4) . ? C79 C80 1.399(4) . ? C80 C81 1.383(5) . ? C81 C82 1.390(5) . ? C82 C83 1.398(4) . ? C83 C84 1.530(4) . ? C84 C85 1.532(4) . ? C85 C86 1.526(4) . ? C86 C87 1.508(5) . ? C87 C88 1.509(5) . ? C89 C90 1.325(7) . ? C91 C92 1.373(11) . ? C91A C92 1.28(2) . ? C91B C92 1.83(3) . ? C93 C94 1.454(5) . ? C95 C96 1.429(6) . ? C97 C98 1.491(6) . ? 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 123.0(3) . . ? C1 C2 C3 117.7(3) . . ? C1 C2 C40 123.3(3) . . ? C3 C2 C40 119.0(3) . . ? O1 C3 C4 119.8(3) . . ? O1 C3 C2 119.5(3) . . ? C4 C3 C2 120.7(3) . . ? O2 C4 C5 118.0(3) . . ? O2 C4 C3 122.3(3) . . ? C5 C4 C3 119.6(3) . . ? C6 C5 O3 120.0(3) . . ? C6 C5 C4 121.8(3) . . ? O3 C5 C4 118.1(3) . . ? C5 C6 C1 117.1(3) . . ? C5 C6 C7 119.3(3) . . ? C1 C6 C7 123.6(3) . . ? C6 C7 C13 110.6(2) . . ? C6 C7 C8 112.4(3) . . ? C13 C7 C8 114.1(3) . . ? C9A C8 C9 77.6(9) . . ? C9A C8 C7 121.1(7) . . ? C9 C8 C7 113.8(3) . . ? C8 C9 C10 113.5(4) . . ? C8 C9A C10A 120.7(13) . . ? C11 C10 C9 113.8(4) . . ? C11A C10A C9A 117.3(15) . . ? C10 C11 Cl1 111.8(4) . . ? C10A C11A Cl1A 111.9(14) . . ? C13 C12 C17 122.9(3) . . ? C14 C13 C12 117.3(3) . . ? C14 C13 C7 122.2(3) . . ? C12 C13 C7 120.4(3) . . ? C15 C14 C13 121.1(3) . . ? C15 C14 O4 114.6(3) . . ? C13 C14 O4 124.3(3) . . ? O5 C15 C16 118.7(3) . . ? O5 C15 C14 121.1(3) . . ? C16 C15 C14 120.2(3) . . ? O6 C16 C15 119.7(3) . . ? O6 C16 C17 119.7(3) . . ? C15 C16 C17 120.6(3) . . ? C16 C17 C12 117.7(3) . . ? C16 C17 C18 120.9(3) . . ? C12 C17 C18 121.4(3) . . ? C19 C18 C17 111.7(3) . . ? C19 C18 C24 112.7(3) . . ? C17 C18 C24 110.6(2) . . ? C20 C19 C18 113.5(3) . . ? C21 C20 C19 111.7(3) . . ? C22 C21 C20 111.9(3) . . ? C21 C22 Cl2 111.2(3) . . ? C24 C23 C28 122.8(3) . . ? C25 C24 C23 117.6(3) . . ? C25 C24 C18 120.8(3) . . ? C23 C24 C18 121.6(3) . . ? O7 C25 C26 114.6(3) . . ? O7 C25 C24 124.7(3) . . ? C26 C25 C24 120.6(3) . . ? O8 C26 C25 122.2(3) . . ? O8 C26 C27 117.6(3) . . ? C25 C26 C27 120.2(3) . . ? O9 C27 C26 121.0(3) . . ? O9 C27 C28 117.8(3) . . ? C26 C27 C28 121.1(3) . . ? C27 C28 C23 117.5(3) . . ? C27 C28 C29 119.5(3) . . ? C23 C28 C29 123.0(3) . . ? C28 C29 C30 112.6(2) . . ? C28 C29 C35 112.1(2) . . ? C30 C29 C35 112.5(2) . . ? C31 C30 C29 113.5(3) . . ? C30 C31 C32 111.7(3) . . ? C33 C32 C31 115.3(4) . . ? C32 C33 Cl3 109.7(3) . . ? C32 C33 Cl3A 103.6(5) . . ? Cl3 C33 Cl3A 38.1(4) . . ? C35 C34 C39 123.9(3) . . ? C34 C35 C36 116.9(3) . . ? C34 C35 C29 121.3(3) . . ? C36 C35 C29 121.8(3) . . ? O10 C36 C37 115.9(3) . . ? O10 C36 C35 123.2(3) . . ? C37 C36 C35 120.9(3) . . ? O11 C37 C38 120.7(3) . . ? O11 C37 C36 118.9(3) . . ? C38 C37 C36 120.4(3) . . ? O12 C38 C37 115.1(3) . . ? O12 C38 C39 124.3(3) . . ? C37 C38 C39 120.6(3) . . ? C34 C39 C38 117.3(3) . . ? C34 C39 C40 120.6(3) . . ? C38 C39 C40 122.1(3) . . ? C41 C40 C2 113.4(3) . . ? C41 C40 C39 110.8(2) . . ? C2 C40 C39 110.6(2) . . ? C42 C41 C40 113.0(3) . . ? C41 C42 C43 111.6(3) . . ? C44 C43 C42 112.8(3) . . ? C43 C44 Cl4 110.6(3) . . ? C46 C45 C50 123.2(3) . . ? C45 C46 C47 117.3(3) . . ? C45 C46 C84 123.5(3) . . ? C47 C46 C84 119.2(3) . . ? O13 C47 C48 119.7(3) . . ? O13 C47 C46 119.3(3) . . ? C48 C47 C46 121.0(3) . . ? C47 C48 C49 120.2(3) . . ? C47 C48 O14 122.4(3) . . ? C49 C48 O14 117.3(2) . . ? O15 C49 C48 119.4(3) . . ? O15 C49 C50 119.5(2) . . ? C48 C49 C50 121.0(3) . . ? C49 C50 C45 117.3(3) . . ? C49 C50 C51 120.0(2) . . ? C45 C50 C51 122.6(3) . . ? C50 C51 C52 112.8(2) . . ? C50 C51 C57 109.7(2) . . ? C52 C51 C57 112.6(2) . . ? C53 C52 C51 113.9(2) . . ? C54 C53 C52 111.3(3) . . ? C55 C54 C53 112.2(3) . . ? C54 C55 Cl5 111.1(3) . . ? C57 C56 C61 123.5(3) . . ? C56 C57 C58 117.1(3) . . ? C56 C57 C51 120.7(3) . . ? C58 C57 C51 122.2(3) . . ? O16 C58 C59 114.0(3) . . ? O16 C58 C57 125.2(3) . . ? C59 C58 C57 120.8(3) . . ? O17 C59 C60 117.8(3) . . ? O17 C59 C58 121.7(3) . . ? C60 C59 C58 120.5(3) . . ? C59 C60 O18 120.4(3) . . ? C59 C60 C61 120.5(3) . . ? O18 C60 C61 119.0(3) . . ? C56 C61 C60 117.5(3) . . ? C56 C61 C62 121.6(3) . . ? C60 C61 C62 121.0(3) . . ? C61 C62 C68 110.5(2) . . ? C61 C62 C63 112.4(3) . . ? C68 C62 C63 113.2(2) . . ? C64 C63 C62 112.9(3) . . ? C63 C64 C65 113.4(3) . . ? C66 C65 C64 114.7(4) . . ? C65 C66 Cl6 111.6(3) . . ? C72 C67 C68 122.7(3) . . ? C69 C68 C67 118.2(3) . . ? C69 C68 C62 119.8(3) . . ? C67 C68 C62 122.0(3) . . ? O19 C69 C70 114.6(3) . . ? O19 C69 C68 125.4(3) . . ? C70 C69 C68 120.0(3) . . ? O20 C70 C69 123.0(3) . . ? O20 C70 C71 116.7(3) . . ? C69 C70 C71 120.2(3) . . ? O21 C71 C72 118.9(3) . . ? O21 C71 C70 119.1(3) . . ? C72 C71 C70 121.9(3) . . ? C71 C72 C67 117.0(3) . . ? C71 C72 C73 119.3(3) . . ? C67 C72 C73 123.7(3) . . ? C79 C73 C72 110.6(2) . . ? C79 C73 C74 112.7(3) . . ? C72 C73 C74 112.8(3) . . ? C75 C74 C73 112.9(3) . . ? C76A C75 C74 132.3(13) . . ? C76A C75 C76 34.2(12) . . ? C74 C75 C76 109.7(4) . . ? C77 C76 C75 112.6(4) . . ? C75 C76A C77A 96(2) . . ? C76 C77 Cl7 110.2(4) . . ? C76A C77A Cl7A 113(2) . . ? C83 C78 C79 123.7(3) . . ? C80 C79 C78 116.5(3) . . ? C80 C79 C73 121.8(3) . . ? C78 C79 C73 121.7(3) . . ? C81 C80 O22 116.5(3) . . ? C81 C80 C79 121.2(3) . . ? O22 C80 C79 122.3(3) . . ? O23 C81 C80 119.5(3) . . ? O23 C81 C82 119.7(3) . . ? C80 C81 C82 120.8(3) . . ? O24 C82 C81 116.5(3) . . ? O24 C82 C83 123.7(3) . . ? C81 C82 C83 119.9(3) . . ? C78 C83 C82 117.9(3) . . ? C78 C83 C84 121.2(2) . . ? C82 C83 C84 120.9(3) . . ? C83 C84 C46 110.6(2) . . ? C83 C84 C85 112.4(2) . . ? C46 C84 C85 113.7(2) . . ? C86 C85 C84 112.6(2) . . ? C87 C86 C85 112.6(3) . . ? C86 C87 C88 114.4(3) . . ? C87 C88 Cl8 111.7(3) . . ? N1 C90 C89 178.1(6) . . ? N2B C92 N2 40.9(7) . . ? N2B C92 C91A 146.9(15) . . ? N2 C92 C91A 152.6(14) . . ? N2B C92 C91 168.5(10) . . ? N2 C92 C91 150.6(10) . . ? C91A C92 C91 25.8(12) . . ? N2B C92 C91B 139.4(12) . . ? N2 C92 C91B 179.3(13) . . ? C91A C92 C91B 26.7(15) . . ? C91 C92 C91B 29.1(10) . . ? N3 C94 C93 179.3(4) . . ? N4 C96 C95 179.0(5) . . ? O26 C97 C98 111.1(3) . . ? O25 C98 C97 111.4(3) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.18 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.951 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.073 #===END