# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_coden_Cambridge 440 _publ_contact_author_name 'Robertus J. M. Klein Gebbink' _publ_contact_author_address ; Metal-Mediated Synthesis Utrecht University Padualaan 8 Utrecht 3584CH NETHERLANDS ; _publ_contact_author_email R.J.M.KLEINGEBBINK@CHEM.UU.NL _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Ionic Core-Shell Dendrimers with a Poly-cationic Core: Structural Aspects and Host-Guest Binding Properties ; loop_ _publ_author_name _publ_author_address 'van de Coevering, Rob' ; Organic Chemistry and Catalysis Faculty of Science Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Bruijnincx, Pieter C. A.' ; Organic Chemistry and Catalysis Faculty of Science Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Lutz, Martin' ; Bijvoet Center for Biomolecular Research Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Spek, Anthony L.' ; Bijvoet Center for Biomolecular Research Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'van Koten, Gerard' ; Organic Chemistry and Catalysis Faculty of Science Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Klein Gebbink, Robertus J. M.' ; Organic Chemistry and Catalysis Faculty of Science Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; data_s2722a _database_code_depnum_ccdc_archive 'CCDC 644298' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H58 N2 O4 2+, 2(Br 1-)' _chemical_formula_sum 'C54 H58 Br2 N2 O4' _chemical_formula_weight 958.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 37.1517(5) _cell_length_b 37.1517(5) _cell_length_c 19.4231(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 23217.0(6) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 45264 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 23.26 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8964 _exptl_absorpt_coefficient_mu 1.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 33681 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 19.94 _reflns_number_total 4799 _reflns_number_gt 3558 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, SortAV' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1232P)^2^+47.8216P] 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 4799 _refine_ls_number_parameters 529 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1881 _refine_ls_wR_factor_gt 0.1749 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.006 _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 O1 O 0.06240(18) 0.18512(17) 0.1034(3) 0.0674(17) Uani 1 1 d . . . O2 O 0.16672(17) 0.14585(17) 0.1056(3) 0.0694(17) Uani 1 1 d . . . O3 O 0.40878(17) 0.25637(16) 0.0438(3) 0.0546(15) Uani 1 1 d . . . O4 O 0.51786(18) 0.39563(17) 0.0187(3) 0.0758(19) Uani 1 1 d D . . N1 N 0.20572(18) 0.28618(19) 0.2673(3) 0.0464(17) Uani 1 1 d . . . N2 N 0.39865(17) 0.36839(17) 0.2274(3) 0.0389(16) Uani 1 1 d . . . C1 C 0.2693(2) 0.3601(2) 0.2521(4) 0.043(2) Uani 1 1 d . . . C2 C 0.3069(2) 0.3636(2) 0.2731(4) 0.041(2) Uani 1 1 d . . . H2 H 0.3077 0.3477 0.3108 0.050 Uiso 1 1 calc R . . C3 C 0.3435(2) 0.3909(2) 0.2376(4) 0.0362(19) Uani 1 1 d . . . C4 C 0.3424(2) 0.4148(2) 0.1842(4) 0.0406(19) Uani 1 1 d . . . H4 H 0.3672 0.4338 0.1609 0.049 Uiso 1 1 calc R . . C5 C 0.3049(3) 0.4111(2) 0.1647(4) 0.054(2) Uani 1 1 d . . . H5 H 0.3041 0.4272 0.1274 0.064 Uiso 1 1 calc R . . C6 C 0.2681(2) 0.3840(2) 0.1990(4) 0.048(2) Uani 1 1 d . . . H6 H 0.2426 0.3821 0.1859 0.058 Uiso 1 1 calc R . . C7 C 0.2291(2) 0.3319(2) 0.2910(4) 0.048(2) Uani 1 1 d . . . H7A H 0.2102 0.3434 0.2861 0.057 Uiso 1 1 calc R . . H7B H 0.2357 0.3327 0.3406 0.057 Uiso 1 1 calc R . . C8 C 0.2296(3) 0.2652(2) 0.2869(4) 0.058(2) Uani 1 1 d . . . H8A H 0.2148 0.2364 0.2705 0.088 Uiso 1 1 calc R . . H8B H 0.2323 0.2655 0.3371 0.088 Uiso 1 1 calc R . . H8C H 0.2573 0.2800 0.2660 0.088 Uiso 1 1 calc R . . C9 C 0.1636(2) 0.2654(3) 0.3036(4) 0.068(3) Uani 1 1 d . . . H9A H 0.1483 0.2795 0.2908 0.102 Uiso 1 1 calc R . . H9B H 0.1679 0.2671 0.3536 0.102 Uiso 1 1 calc R . . H9C H 0.1477 0.2361 0.2898 0.102 Uiso 1 1 calc R . . C10 C 0.1980(2) 0.2841(2) 0.1894(3) 0.045(2) Uani 1 1 d . . . H10A H 0.1868 0.3026 0.1778 0.054 Uiso 1 1 calc R . . H10B H 0.2250 0.2949 0.1652 0.054 Uiso 1 1 calc R . . C11 C 0.1685(2) 0.2413(3) 0.1634(4) 0.049(2) Uani 1 1 d . . . C12 C 0.1283(3) 0.2302(3) 0.1484(4) 0.055(2) Uani 1 1 d . . . H12 H 0.1189 0.2493 0.1579 0.065 Uiso 1 1 calc R . . C13 C 0.1006(3) 0.1916(3) 0.1194(4) 0.055(2) Uani 1 1 d . . . C14 C 0.1144(3) 0.1631(3) 0.1076(4) 0.060(2) Uani 1 1 d . . . H14 H 0.0959 0.1361 0.0902 0.072 Uiso 1 1 calc R . . C15 C 0.1560(3) 0.1753(3) 0.1220(4) 0.054(2) Uani 1 1 d . . . C16 C 0.1830(3) 0.2135(3) 0.1487(4) 0.052(2) Uani 1 1 d . . . H16 H 0.2112 0.2213 0.1573 0.062 Uiso 1 1 calc R . . C17 C 0.0351(3) 0.1484(3) 0.0635(5) 0.074(3) Uani 1 1 d . . . H17A H 0.0518 0.1442 0.0282 0.088 Uiso 1 1 calc R . . H17B H 0.0146 0.1534 0.0391 0.088 Uiso 1 1 calc R . . C18 C 0.0127(3) 0.1104(4) 0.1045(7) 0.079(3) Uani 1 1 d . . . C19 C 0.0119(3) 0.1118(4) 0.1746(7) 0.097(3) Uani 1 1 d . . . H19 H 0.0270 0.1382 0.1963 0.117 Uiso 1 1 calc R . . C20 C -0.0106(5) 0.0757(5) 0.2176(9) 0.139(6) Uani 1 1 d . . . H20 H -0.0094 0.0775 0.2664 0.167 Uiso 1 1 calc R . . C21 C -0.0329(5) 0.0401(6) 0.1854(11) 0.132(6) Uani 1 1 d . . . H21 H -0.0497 0.0162 0.2126 0.159 Uiso 1 1 calc R . . C22 C -0.0336(4) 0.0351(5) 0.1160(13) 0.149(7) Uani 1 1 d . . . H22 H -0.0488 0.0083 0.0956 0.179 Uiso 1 1 calc R . . C23 C -0.0106(4) 0.0714(5) 0.0749(7) 0.111(4) Uani 1 1 d . . . H23 H -0.0113 0.0689 0.0262 0.133 Uiso 1 1 calc R . . C24 C 0.2085(3) 0.1564(3) 0.1218(5) 0.075(3) Uani 1 1 d . . . H24A H 0.2134 0.1615 0.1719 0.090 Uiso 1 1 calc R . . H24B H 0.2283 0.1821 0.0971 0.090 Uiso 1 1 calc R . . C25 C 0.2150(3) 0.1209(3) 0.1004(6) 0.067(3) Uani 1 1 d . . . C26 C 0.1970(3) 0.0828(3) 0.1350(6) 0.084(3) Uani 1 1 d . . . H26 H 0.1795 0.0784 0.1733 0.101 Uiso 1 1 calc R . . C27 C 0.2042(4) 0.0521(3) 0.1149(7) 0.086(3) Uani 1 1 d . . . H27 H 0.1924 0.0268 0.1398 0.103 Uiso 1 1 calc R . . C28 C 0.2288(4) 0.0579(4) 0.0575(7) 0.088(3) Uani 1 1 d . . . H28 H 0.2322 0.0357 0.0413 0.105 Uiso 1 1 calc R . . C29 C 0.2478(4) 0.0948(4) 0.0247(6) 0.093(3) Uani 1 1 d . . . H29 H 0.2666 0.0994 -0.0120 0.112 Uiso 1 1 calc R . . C30 C 0.2398(3) 0.1262(3) 0.0450(5) 0.080(3) Uani 1 1 d . . . H30 H 0.2518 0.1516 0.0200 0.096 Uiso 1 1 calc R . . C31 C 0.3850(2) 0.3976(2) 0.2614(4) 0.042(2) Uani 1 1 d . . . H31A H 0.3840 0.3937 0.3119 0.051 Uiso 1 1 calc R . . H31B H 0.4064 0.4268 0.2516 0.051 Uiso 1 1 calc R . . C32 C 0.3709(2) 0.3241(2) 0.2492(4) 0.044(2) Uani 1 1 d . . . H32A H 0.3426 0.3143 0.2326 0.067 Uiso 1 1 calc R . . H32B H 0.3707 0.3223 0.2996 0.067 Uiso 1 1 calc R . . H32C H 0.3812 0.3066 0.2297 0.067 Uiso 1 1 calc R . . C33 C 0.4421(2) 0.3833(2) 0.2535(4) 0.044(2) Uani 1 1 d . . . H33A H 0.4602 0.4124 0.2402 0.066 Uiso 1 1 calc R . . H33B H 0.4528 0.3662 0.2334 0.066 Uiso 1 1 calc R . . H33C H 0.4417 0.3809 0.3038 0.066 Uiso 1 1 calc R . . C34 C 0.3980(2) 0.3723(2) 0.1491(3) 0.0356(18) Uani 1 1 d . . . H34A H 0.3687 0.3577 0.1335 0.043 Uiso 1 1 calc R . . H34B H 0.4102 0.4020 0.1372 0.043 Uiso 1 1 calc R . . C35 C 0.4211(2) 0.3551(2) 0.1103(3) 0.0381(19) Uani 1 1 d . A . C36 C 0.4596(2) 0.3812(2) 0.0836(4) 0.046(2) Uani 1 1 d . . . H36 H 0.4726 0.4102 0.0925 0.055 Uiso 1 1 calc R A . C37 C 0.4805(3) 0.3658(3) 0.0433(4) 0.054(2) Uani 1 1 d . A . C38 C 0.4625(3) 0.3244(3) 0.0319(4) 0.053(2) Uani 1 1 d . . . H38 H 0.4766 0.3138 0.0053 0.064 Uiso 1 1 calc R A . C39 C 0.4236(3) 0.2973(3) 0.0588(4) 0.046(2) Uani 1 1 d . A . C40 C 0.4021(2) 0.3121(2) 0.0974(4) 0.043(2) Uani 1 1 d . . . H40 H 0.3751 0.2935 0.1147 0.051 Uiso 1 1 calc R A . C41 C 0.3727(3) 0.2260(2) 0.0804(4) 0.057(2) Uani 1 1 d . . . H41A H 0.3480 0.2281 0.0672 0.068 Uiso 1 1 calc R . . H41B H 0.3769 0.2305 0.1307 0.068 Uiso 1 1 calc R . . C42 C 0.3664(2) 0.1842(2) 0.0614(4) 0.050(2) Uani 1 1 d . . . C43 C 0.3693(2) 0.1589(2) 0.1096(4) 0.049(2) Uani 1 1 d . . . H43 H 0.3745 0.1673 0.1564 0.059 Uiso 1 1 calc R . . C44 C 0.3647(3) 0.1203(3) 0.0894(5) 0.063(3) Uani 1 1 d . . . H44 H 0.3663 0.1026 0.1230 0.075 Uiso 1 1 calc R . . C45 C 0.3577(3) 0.1081(3) 0.0216(5) 0.065(3) Uani 1 1 d . . . H45 H 0.3550 0.0823 0.0078 0.078 Uiso 1 1 calc R . . C46 C 0.3548(3) 0.1340(3) -0.0255(5) 0.072(3) Uani 1 1 d . . . H46 H 0.3499 0.1258 -0.0725 0.086 Uiso 1 1 calc R . . C47 C 0.3587(3) 0.1711(3) -0.0069(4) 0.075(3) Uani 1 1 d . . . H47 H 0.3562 0.1881 -0.0408 0.090 Uiso 1 1 calc R . . C48A C 0.5311(6) 0.3803(4) -0.0434(9) 0.066(6) Uiso 0.487(14) 1 d PD A 1 H48A H 0.5097 0.3708 -0.0801 0.080 Uiso 0.487(14) 1 calc PR A 1 H48B H 0.5355 0.3570 -0.0306 0.080 Uiso 0.487(14) 1 calc PR A 1 C49A C 0.5720(8) 0.4178(6) -0.0681(13) 0.180(15) Uiso 0.487(14) 1 d PGD A 1 C50A C 0.5767(4) 0.4434(6) -0.1237(12) 0.210(17) Uiso 0.487(14) 1 d PG A 1 H50A H 0.5529 0.4416 -0.1453 0.251 Uiso 0.487(14) 1 calc PR A 1 C51A C 0.6162(5) 0.4717(4) -0.1476(8) 0.056(6) Uiso 0.487(14) 1 d PG A 1 H51A H 0.6194 0.4891 -0.1856 0.067 Uiso 0.487(14) 1 calc PR A 1 C52A C 0.6510(4) 0.4744(7) -0.1160(13) 0.220(19) Uiso 0.487(14) 1 d PG A 1 H52A H 0.6780 0.4937 -0.1324 0.264 Uiso 0.487(14) 1 calc PR A 1 C53A C 0.6463(9) 0.4488(11) -0.0604(15) 0.36(4) Uiso 0.487(14) 1 d PG A 1 H53A H 0.6701 0.4506 -0.0388 0.426 Uiso 0.487(14) 1 calc PR A 1 C54A C 0.6068(11) 0.4205(9) -0.0365(12) 0.32(3) Uiso 0.487(14) 1 d PG A 1 H54A H 0.6036 0.4031 0.0015 0.389 Uiso 0.487(14) 1 calc PR A 1 C48B C 0.5451(4) 0.3817(4) -0.0172(10) 0.060(6) Uiso 0.513(14) 1 d PD A 2 H48C H 0.5330 0.3688 -0.0622 0.072 Uiso 0.513(14) 1 calc PR A 2 H48D H 0.5480 0.3612 0.0114 0.072 Uiso 0.513(14) 1 calc PR A 2 C49B C 0.5874(3) 0.4213(3) -0.0270(7) 0.082(6) Uiso 0.513(14) 1 d PGD A 2 C50B C 0.5945(3) 0.4447(4) -0.0865(6) 0.092(7) Uiso 0.513(14) 1 d PG A 2 H50B H 0.5733 0.4362 -0.1202 0.110 Uiso 0.513(14) 1 calc PR A 2 C51B C 0.6327(4) 0.4804(4) -0.0967(6) 0.076(6) Uiso 0.513(14) 1 d PG A 2 H51B H 0.6376 0.4964 -0.1374 0.091 Uiso 0.513(14) 1 calc PR A 2 C52B C 0.6638(3) 0.4928(3) -0.0474(8) 0.094(7) Uiso 0.513(14) 1 d PG A 2 H52B H 0.6899 0.5172 -0.0544 0.113 Uiso 0.513(14) 1 calc PR A 2 C53B C 0.6567(4) 0.4694(4) 0.0122(7) 0.112(9) Uiso 0.513(14) 1 d PG A 2 H53B H 0.6779 0.4778 0.0459 0.134 Uiso 0.513(14) 1 calc PR A 2 C54B C 0.6185(4) 0.4337(4) 0.0224(6) 0.086(7) Uiso 0.513(14) 1 d PG A 2 H54B H 0.6136 0.4177 0.0631 0.103 Uiso 0.513(14) 1 calc PR A 2 Br1 Br 0.29158(2) 0.28481(3) 0.10300(4) 0.0530(4) Uani 1 1 d . . . Br2 Br 0.15156(2) 0.35278(3) 0.18935(4) 0.0550(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.048(4) 0.063(4) 0.085(4) -0.024(3) -0.019(3) 0.024(3) O2 0.054(4) 0.057(4) 0.097(5) -0.020(3) -0.018(3) 0.028(3) O3 0.065(4) 0.034(4) 0.057(4) -0.003(3) 0.014(3) 0.019(3) O4 0.066(4) 0.051(4) 0.102(5) 0.006(3) 0.039(4) 0.023(4) N1 0.039(4) 0.050(4) 0.040(4) 0.001(3) 0.005(3) 0.015(4) N2 0.039(4) 0.042(4) 0.036(4) -0.006(3) -0.007(3) 0.020(3) C1 0.028(5) 0.037(5) 0.051(5) -0.018(4) -0.004(4) 0.008(4) C2 0.044(5) 0.041(5) 0.035(4) -0.014(4) -0.001(4) 0.018(4) C3 0.037(5) 0.030(4) 0.039(5) -0.004(4) 0.001(4) 0.016(4) C4 0.039(5) 0.033(5) 0.048(5) 0.004(4) -0.001(4) 0.016(4) C5 0.054(6) 0.050(5) 0.055(5) 0.000(4) -0.008(5) 0.025(5) C6 0.036(5) 0.051(5) 0.058(6) -0.003(5) -0.006(4) 0.023(5) C7 0.039(5) 0.052(5) 0.045(5) -0.015(4) -0.003(4) 0.017(4) C8 0.057(6) 0.058(6) 0.047(5) 0.003(4) -0.004(4) 0.019(5) C9 0.046(6) 0.076(6) 0.054(6) -0.012(5) 0.011(5) 0.009(5) C10 0.039(5) 0.048(5) 0.041(5) -0.009(4) -0.001(4) 0.017(4) C11 0.040(6) 0.056(6) 0.047(5) -0.006(4) -0.002(4) 0.021(5) C12 0.049(6) 0.064(6) 0.058(5) -0.001(5) 0.002(5) 0.034(5) C13 0.039(6) 0.056(6) 0.064(6) -0.018(5) -0.017(5) 0.019(5) C14 0.051(6) 0.047(5) 0.073(6) -0.016(5) -0.009(5) 0.018(5) C15 0.045(6) 0.052(6) 0.069(6) -0.014(5) -0.003(5) 0.027(5) C16 0.047(5) 0.050(6) 0.055(5) -0.010(5) -0.011(4) 0.023(5) C17 0.047(6) 0.073(7) 0.091(7) -0.028(7) -0.023(6) 0.022(6) C18 0.052(6) 0.083(9) 0.099(9) -0.025(8) -0.016(6) 0.031(7) C19 0.079(8) 0.069(8) 0.125(11) -0.020(8) -0.010(8) 0.022(7) C20 0.128(12) 0.071(9) 0.159(13) 0.010(11) -0.020(10) 0.006(9) C21 0.100(12) 0.110(15) 0.200(18) 0.029(14) 0.022(13) 0.062(12) C22 0.074(10) 0.061(10) 0.29(2) -0.030(15) -0.028(14) 0.017(8) C23 0.085(9) 0.098(10) 0.149(12) -0.044(10) -0.025(9) 0.046(8) C24 0.055(6) 0.055(6) 0.121(8) -0.022(6) -0.010(6) 0.032(5) C25 0.053(6) 0.060(7) 0.081(7) -0.015(6) -0.018(6) 0.023(5) C26 0.063(7) 0.072(8) 0.105(8) -0.003(7) -0.003(6) 0.025(6) C27 0.102(9) 0.064(7) 0.115(10) -0.005(7) -0.027(8) 0.059(7) C28 0.096(9) 0.085(9) 0.110(10) -0.026(8) -0.040(8) 0.067(8) C29 0.125(10) 0.088(9) 0.097(8) 0.005(8) -0.013(7) 0.076(8) C30 0.108(9) 0.072(7) 0.080(8) 0.008(6) -0.007(7) 0.058(7) C31 0.042(5) 0.045(5) 0.037(4) -0.011(4) -0.003(4) 0.020(4) C32 0.053(5) 0.026(5) 0.044(5) 0.004(4) -0.009(4) 0.013(4) C33 0.037(5) 0.045(5) 0.046(5) -0.002(4) -0.006(4) 0.018(4) C34 0.040(5) 0.029(4) 0.035(4) 0.006(3) -0.003(4) 0.015(4) C35 0.042(5) 0.035(5) 0.033(4) 0.000(4) -0.007(4) 0.017(4) C36 0.050(6) 0.033(5) 0.048(5) -0.006(4) -0.007(4) 0.015(5) C37 0.055(6) 0.042(6) 0.061(6) 0.013(5) 0.019(5) 0.020(5) C38 0.063(6) 0.052(6) 0.049(5) 0.000(5) 0.013(5) 0.032(5) C39 0.054(6) 0.043(6) 0.043(5) -0.001(4) -0.003(4) 0.026(5) C40 0.039(5) 0.035(5) 0.043(5) -0.001(4) -0.005(4) 0.010(4) C41 0.075(7) 0.047(6) 0.052(5) 0.001(5) -0.002(5) 0.032(5) C42 0.063(6) 0.034(5) 0.051(6) 0.002(5) 0.004(4) 0.024(4) C43 0.057(6) 0.042(5) 0.044(5) -0.002(4) -0.003(4) 0.021(4) C44 0.067(6) 0.047(6) 0.075(7) 0.024(5) 0.005(5) 0.029(5) C45 0.080(7) 0.057(6) 0.053(6) -0.010(5) 0.003(5) 0.030(5) C46 0.104(8) 0.063(7) 0.048(6) -0.003(6) -0.011(5) 0.041(6) C47 0.128(9) 0.058(7) 0.046(6) -0.005(5) -0.010(6) 0.051(6) Br1 0.0482(6) 0.0658(6) 0.0395(5) -0.0013(4) -0.0003(4) 0.0242(5) Br2 0.0427(6) 0.0734(7) 0.0493(6) -0.0071(4) -0.0014(4) 0.0292(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 O1 C13 1.352(9) . ? O1 C17 1.451(10) . ? O2 C15 1.375(9) . ? O2 C24 1.432(9) . ? O3 C39 1.366(9) . ? O3 C41 1.437(9) . ? O4 C37 1.359(9) . ? O4 C48B 1.516(11) . ? O4 C48A 1.517(11) . ? N1 C8 1.492(10) . ? N1 C9 1.527(9) . ? N1 C10 1.536(9) . ? N1 C7 1.541(9) . ? N2 C32 1.503(8) . ? N2 C33 1.510(8) . ? N2 C34 1.528(8) . ? N2 C31 1.556(9) . ? C1 C6 1.377(10) . ? C1 C2 1.398(10) . ? C1 C7 1.529(10) . ? C2 C3 1.404(10) . ? C2 H2 0.9500 . ? C3 C4 1.381(10) . ? C3 C31 1.507(9) . ? C4 C5 1.382(10) . ? C4 H4 0.9500 . ? C5 C6 1.396(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.499(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.371(10) . ? C11 C16 1.411(11) . ? C12 C13 1.398(11) . ? C12 H12 0.9500 . ? C13 C14 1.408(11) . ? C14 C15 1.403(11) . ? C14 H14 0.9500 . ? C15 C16 1.368(11) . ? C16 H16 0.9500 . ? C17 C18 1.467(14) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.362(14) . ? C18 C23 1.387(15) . ? C19 C20 1.440(16) . ? C19 H19 0.9500 . ? C20 C21 1.315(19) . ? C20 H20 0.9500 . ? C21 C22 1.36(2) . ? C21 H21 0.9500 . ? C22 C23 1.43(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.515(12) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.365(13) . ? C25 C26 1.398(13) . ? C26 C27 1.349(13) . ? C26 H26 0.9500 . ? C27 C28 1.388(14) . ? C27 H27 0.9500 . ? C28 C29 1.346(14) . ? C28 H28 0.9500 . ? C29 C30 1.398(13) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.504(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.368(10) . ? C35 C40 1.409(10) . ? C36 C37 1.409(11) . ? C36 H36 0.9500 . ? C37 C38 1.353(11) . ? C38 C39 1.386(11) . ? C38 H38 0.9500 . ? C39 C40 1.391(10) . ? C40 H40 0.9500 . ? C41 C42 1.497(10) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.369(10) . ? C42 C47 1.395(11) . ? C43 C44 1.410(11) . ? C43 H43 0.9500 . ? C44 C45 1.374(11) . ? C44 H44 0.9500 . ? C45 C46 1.372(12) . ? C45 H45 0.9500 . ? C46 C47 1.359(12) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48A C49A 1.536(13) . ? C48A H48A 0.9900 . ? C48A H48B 0.9900 . ? C49A C50A 1.3900 . ? C49A C54A 1.3900 . ? C50A C51A 1.3900 . ? C50A H50A 0.9500 . ? C51A C52A 1.3900 . ? C51A H51A 0.9500 . ? C52A C53A 1.3900 . ? C52A H52A 0.9500 . ? C53A C54A 1.3900 . ? C53A H53A 0.9500 . ? C54A H54A 0.9500 . ? C48B C49B 1.536(13) . ? C48B H48C 0.9900 . ? C48B H48D 0.9900 . ? C49B C50B 1.3900 . ? C49B C54B 1.3900 . ? C50B C51B 1.3900 . ? C50B H50B 0.9500 . ? C51B C52B 1.3900 . ? C51B H51B 0.9500 . ? C52B C53B 1.3900 . ? C52B H52B 0.9500 . ? C53B C54B 1.3900 . ? C53B H53B 0.9500 . ? C54B H54B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 O1 C17 118.0(6) . . ? C15 O2 C24 115.9(6) . . ? C39 O3 C41 117.8(6) . . ? C37 O4 C48B 117.8(7) . . ? C37 O4 C48A 111.4(7) . . ? C48B O4 C48A 27.1(9) . . ? C8 N1 C9 110.1(6) . . ? C8 N1 C10 111.7(6) . . ? C9 N1 C10 108.2(6) . . ? C8 N1 C7 110.2(6) . . ? C9 N1 C7 106.9(6) . . ? C10 N1 C7 109.7(5) . . ? C32 N2 C33 109.3(5) . . ? C32 N2 C34 110.5(5) . . ? C33 N2 C34 111.3(5) . . ? C32 N2 C31 111.2(5) . . ? C33 N2 C31 105.3(5) . . ? C34 N2 C31 109.3(5) . . ? C6 C1 C2 120.8(7) . . ? C6 C1 C7 118.4(7) . . ? C2 C1 C7 120.6(7) . . ? C1 C2 C3 119.1(7) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 120.2(7) . . ? C4 C3 C31 118.8(7) . . ? C2 C3 C31 120.7(7) . . ? C5 C4 C3 119.7(7) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.1(7) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 119.1(7) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C1 C7 N1 115.3(6) . . ? C1 C7 H7A 108.5 . . ? N1 C7 H7A 108.5 . . ? C1 C7 H7B 108.5 . . ? N1 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N1 113.8(6) . . ? C11 C10 H10A 108.8 . . ? N1 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? N1 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C16 119.8(7) . . ? C12 C11 C10 119.9(8) . . ? C16 C11 C10 120.1(7) . . ? C11 C12 C13 121.7(8) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? O1 C13 C12 116.3(8) . . ? O1 C13 C14 125.0(7) . . ? C12 C13 C14 118.7(7) . . ? C15 C14 C13 118.8(7) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C16 C15 O2 124.0(7) . . ? C16 C15 C14 121.9(8) . . ? O2 C15 C14 114.1(7) . . ? C15 C16 C11 119.0(8) . . ? C15 C16 H16 120.5 . . ? C11 C16 H16 120.5 . . ? O1 C17 C18 114.0(8) . . ? O1 C17 H17A 108.7 . . ? C18 C17 H17A 108.7 . . ? O1 C17 H17B 108.7 . . ? C18 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C19 C18 C23 116.1(12) . . ? C19 C18 C17 121.3(10) . . ? C23 C18 C17 122.6(12) . . ? C18 C19 C20 123.9(12) . . ? C18 C19 H19 118.1 . . ? C20 C19 H19 118.1 . . ? C21 C20 C19 116.2(15) . . ? C21 C20 H20 121.9 . . ? C19 C20 H20 121.9 . . ? C20 C21 C22 124.7(18) . . ? C20 C21 H21 117.7 . . ? C22 C21 H21 117.7 . . ? C21 C22 C23 117.6(15) . . ? C21 C22 H22 121.2 . . ? C23 C22 H22 121.2 . . ? C18 C23 C22 121.5(14) . . ? C18 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? O2 C24 C25 109.0(7) . . ? O2 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? O2 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C30 C25 C26 118.2(9) . . ? C30 C25 C24 118.7(10) . . ? C26 C25 C24 123.1(10) . . ? C27 C26 C25 121.3(11) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C28 119.5(11) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C29 C28 C27 120.6(10) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 119.5(11) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C25 C30 C29 120.7(10) . . ? C25 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C3 C31 N2 114.6(5) . . ? C3 C31 H31A 108.6 . . ? N2 C31 H31A 108.6 . . ? C3 C31 H31B 108.6 . . ? N2 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? N2 C32 H32A 109.5 . . ? N2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 N2 114.9(5) . . ? C35 C34 H34A 108.6 . . ? N2 C34 H34A 108.6 . . ? C35 C34 H34B 108.6 . . ? N2 C34 H34B 108.6 . . ? H34A C34 H34B 107.5 . . ? C36 C35 C40 119.4(7) . . ? C36 C35 C34 120.3(7) . . ? C40 C35 C34 120.2(7) . . ? C35 C36 C37 121.0(7) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C38 C37 O4 126.4(8) . . ? C38 C37 C36 119.5(7) . . ? O4 C37 C36 114.2(7) . . ? C37 C38 C39 120.5(8) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? O3 C39 C38 114.9(7) . . ? O3 C39 C40 124.3(7) . . ? C38 C39 C40 120.8(7) . . ? C39 C40 C35 118.8(7) . . ? C39 C40 H40 120.6 . . ? C35 C40 H40 120.6 . . ? O3 C41 C42 107.0(6) . . ? O3 C41 H41A 110.3 . . ? C42 C41 H41A 110.3 . . ? O3 C41 H41B 110.3 . . ? C42 C41 H41B 110.3 . . ? H41A C41 H41B 108.6 . . ? C43 C42 C47 118.8(7) . . ? C43 C42 C41 121.4(7) . . ? C47 C42 C41 119.8(7) . . ? C42 C43 C44 119.9(7) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C45 C44 C43 120.6(8) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C46 C45 C44 118.4(8) . . ? C46 C45 H45 120.8 . . ? C44 C45 H45 120.8 . . ? C47 C46 C45 121.9(8) . . ? C47 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? C46 C47 C42 120.5(8) . . ? C46 C47 H47 119.8 . . ? C42 C47 H47 119.8 . . ? O4 C48A C49A 105.5(8) . . ? O4 C48A H48A 110.6 . . ? C49A C48A H48A 110.6 . . ? O4 C48A H48B 110.6 . . ? C49A C48A H48B 110.6 . . ? H48A C48A H48B 108.8 . . ? C50A C49A C54A 120.0 . . ? C50A C49A C48A 126(2) . . ? C54A C49A C48A 113(2) . . ? C49A C50A C51A 120.0 . . ? C49A C50A H50A 120.0 . . ? C51A C50A H50A 120.0 . . ? C50A C51A C52A 120.0 . . ? C50A C51A H51A 120.0 . . ? C52A C51A H51A 120.0 . . ? C51A C52A C53A 120.0 . . ? C51A C52A H52A 120.0 . . ? C53A C52A H52A 120.0 . . ? C52A C53A C54A 120.0 . . ? C52A C53A H53A 120.0 . . ? C54A C53A H53A 120.0 . . ? C53A C54A C49A 120.0 . . ? C53A C54A H54A 120.0 . . ? C49A C54A H54A 120.0 . . ? O4 C48B C49B 105.5(8) . . ? O4 C48B H48C 110.6 . . ? C49B C48B H48C 110.7 . . ? O4 C48B H48D 110.7 . . ? C49B C48B H48D 110.6 . . ? H48C C48B H48D 108.8 . . ? C50B C49B C54B 120.0 . . ? C50B C49B C48B 119.1(12) . . ? C54B C49B C48B 120.9(12) . . ? C51B C50B C49B 120.0 . . ? C51B C50B H50B 120.0 . . ? C49B C50B H50B 120.0 . . ? C50B C51B C52B 120.0 . . ? C50B C51B H51B 120.0 . . ? C52B C51B H51B 120.0 . . ? C51B C52B C53B 120.0 . . ? C51B C52B H52B 120.0 . . ? C53B C52B H52B 120.0 . . ? C52B C53B C54B 120.0 . . ? C52B C53B H53B 120.0 . . ? C54B C53B H53B 120.0 . . ? C53B C54B C49B 120.0 . . ? C53B C54B H54B 120.0 . . ? C49B C54B H54B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -2.2(10) . . . . ? C7 C1 C2 C3 -177.9(6) . . . . ? C1 C2 C3 C4 2.0(10) . . . . ? C1 C2 C3 C31 175.9(6) . . . . ? C2 C3 C4 C5 -1.5(10) . . . . ? C31 C3 C4 C5 -175.5(6) . . . . ? C3 C4 C5 C6 1.2(11) . . . . ? C2 C1 C6 C5 1.9(11) . . . . ? C7 C1 C6 C5 177.6(6) . . . . ? C4 C5 C6 C1 -1.4(11) . . . . ? C6 C1 C7 N1 97.4(8) . . . . ? C2 C1 C7 N1 -86.8(8) . . . . ? C8 N1 C7 C1 69.6(8) . . . . ? C9 N1 C7 C1 -170.8(7) . . . . ? C10 N1 C7 C1 -53.8(8) . . . . ? C8 N1 C10 C11 68.7(8) . . . . ? C9 N1 C10 C11 -52.6(8) . . . . ? C7 N1 C10 C11 -168.8(6) . . . . ? N1 C10 C11 C12 102.5(8) . . . . ? N1 C10 C11 C16 -83.0(8) . . . . ? C16 C11 C12 C13 0.8(12) . . . . ? C10 C11 C12 C13 175.4(7) . . . . ? C17 O1 C13 C12 170.3(8) . . . . ? C17 O1 C13 C14 -8.1(12) . . . . ? C11 C12 C13 O1 -176.5(7) . . . . ? C11 C12 C13 C14 2.0(12) . . . . ? O1 C13 C14 C15 175.2(8) . . . . ? C12 C13 C14 C15 -3.2(13) . . . . ? C24 O2 C15 C16 3.4(12) . . . . ? C24 O2 C15 C14 -177.8(8) . . . . ? C13 C14 C15 C16 1.7(13) . . . . ? C13 C14 C15 O2 -177.1(7) . . . . ? O2 C15 C16 C11 179.8(7) . . . . ? C14 C15 C16 C11 1.1(12) . . . . ? C12 C11 C16 C15 -2.4(12) . . . . ? C10 C11 C16 C15 -176.9(7) . . . . ? C13 O1 C17 C18 82.6(10) . . . . ? O1 C17 C18 C19 12.2(13) . . . . ? O1 C17 C18 C23 -171.5(9) . . . . ? C23 C18 C19 C20 1.5(17) . . . . ? C17 C18 C19 C20 178.0(10) . . . . ? C18 C19 C20 C21 -3(2) . . . . ? C19 C20 C21 C22 5(2) . . . . ? C20 C21 C22 C23 -4(3) . . . . ? C19 C18 C23 C22 -0.8(16) . . . . ? C17 C18 C23 C22 -177.3(11) . . . . ? C21 C22 C23 C18 2(2) . . . . ? C15 O2 C24 C25 -179.9(8) . . . . ? O2 C24 C25 C30 109.0(9) . . . . ? O2 C24 C25 C26 -71.3(11) . . . . ? C30 C25 C26 C27 0.7(14) . . . . ? C24 C25 C26 C27 -179.0(9) . . . . ? C25 C26 C27 C28 -2.1(15) . . . . ? C26 C27 C28 C29 4.5(16) . . . . ? C27 C28 C29 C30 -5.6(16) . . . . ? C26 C25 C30 C29 -1.7(14) . . . . ? C24 C25 C30 C29 178.0(9) . . . . ? C28 C29 C30 C25 4.2(15) . . . . ? C4 C3 C31 N2 -94.1(8) . . . . ? C2 C3 C31 N2 92.0(8) . . . . ? C32 N2 C31 C3 -67.0(7) . . . . ? C33 N2 C31 C3 174.8(6) . . . . ? C34 N2 C31 C3 55.2(7) . . . . ? C32 N2 C34 C35 -73.2(7) . . . . ? C33 N2 C34 C35 48.4(8) . . . . ? C31 N2 C34 C35 164.2(6) . . . . ? N2 C34 C35 C36 -102.6(7) . . . . ? N2 C34 C35 C40 81.3(8) . . . . ? C40 C35 C36 C37 0.3(11) . . . . ? C34 C35 C36 C37 -175.8(6) . . . . ? C48B O4 C37 C38 -8.7(15) . . . . ? C48A O4 C37 C38 20.4(14) . . . . ? C48B O4 C37 C36 172.0(11) . . . . ? C48A O4 C37 C36 -158.9(11) . . . . ? C35 C36 C37 C38 -1.4(12) . . . . ? C35 C36 C37 O4 178.0(7) . . . . ? O4 C37 C38 C39 -178.4(8) . . . . ? C36 C37 C38 C39 0.9(12) . . . . ? C41 O3 C39 C38 168.3(7) . . . . ? C41 O3 C39 C40 -12.3(10) . . . . ? C37 C38 C39 O3 -179.9(7) . . . . ? C37 C38 C39 C40 0.7(12) . . . . ? O3 C39 C40 C35 178.9(6) . . . . ? C38 C39 C40 C35 -1.7(10) . . . . ? C36 C35 C40 C39 1.2(10) . . . . ? C34 C35 C40 C39 177.4(6) . . . . ? C39 O3 C41 C42 -172.7(6) . . . . ? O3 C41 C42 C43 116.3(8) . . . . ? O3 C41 C42 C47 -61.7(10) . . . . ? C47 C42 C43 C44 0.1(12) . . . . ? C41 C42 C43 C44 -177.8(7) . . . . ? C42 C43 C44 C45 0.9(12) . . . . ? C43 C44 C45 C46 -1.1(13) . . . . ? C44 C45 C46 C47 0.3(15) . . . . ? C45 C46 C47 C42 0.7(15) . . . . ? C43 C42 C47 C46 -0.9(14) . . . . ? C41 C42 C47 C46 177.1(9) . . . . ? C37 O4 C48A C49A 176.5(16) . . . . ? C48B O4 C48A C49A -74.0(17) . . . . ? O4 C48A C49A C50A -101.7(15) . . . . ? O4 C48A C49A C54A 88.9(15) . . . . ? C54A C49A C50A C51A 0.0 . . . . ? C48A C49A C50A C51A -168.8(15) . . . . ? C49A C50A C51A C52A 0.0 . . . . ? C50A C51A C52A C53A 0.0 . . . . ? C51A C52A C53A C54A 0.0 . . . . ? C52A C53A C54A C49A 0.0 . . . . ? C50A C49A C54A C53A 0.0 . . . . ? C48A C49A C54A C53A 170.2(14) . . . . ? C37 O4 C48B C49B -170.0(10) . . . . ? C48A O4 C48B C49B 107(2) . . . . ? O4 C48B C49B C50B -89.3(13) . . . . ? O4 C48B C49B C54B 91.3(13) . . . . ? C54B C49B C50B C51B 0.0 . . . . ? C48B C49B C50B C51B -179.3(10) . . . . ? C49B C50B C51B C52B 0.0 . . . . ? C50B C51B C52B C53B 0.0 . . . . ? C51B C52B C53B C54B 0.0 . . . . ? C52B C53B C54B C49B 0.0 . . . . ? C50B C49B C54B C53B 0.0 . . . . ? C48B C49B C54B C53B 179.3(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 19.94 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.865 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.083 #===END data_s2331b _database_code_depnum_ccdc_archive 'CCDC 644299' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H32 N O2, C14 H14 N3 O3 S, 2.5(C6 H6)' _chemical_formula_sum 'C59 H61 N4 O5 S' _chemical_formula_weight 938.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9322(2) _cell_length_b 13.9718(2) _cell_length_c 19.3040(4) _cell_angle_alpha 100.3272(10) _cell_angle_beta 92.3451(8) _cell_angle_gamma 103.8291(9) _cell_volume 2549.18(8) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 998 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 34970 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.52 _reflns_number_total 11536 _reflns_number_gt 8939 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'DENZO 1.11.0' _computing_data_reduction 'DENZO 1.11.0' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0507P)^2^+0.6051P] 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 11536 _refine_ls_number_parameters 808 _refine_ls_number_restraints 123 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 1.25181(3) 0.55604(3) 0.376312(17) 0.03089(9) Uani 1 1 d . . . O11 O 1.26955(11) 0.46151(9) 0.39189(6) 0.0463(3) Uani 1 1 d . B . O21 O 1.38042(10) 0.62039(9) 0.36198(6) 0.0498(3) Uani 1 1 d . B . O31 O 1.17732(11) 0.60534(9) 0.42829(5) 0.0458(3) Uani 1 1 d . B . N31 N 0.39063(13) 0.37044(10) -0.12810(6) 0.0388(3) Uani 1 1 d . . . C131 C 0.25311(16) 0.30495(12) -0.12940(9) 0.0439(4) Uani 1 1 d . B . H13A H 0.2613 0.2386 -0.1228 0.066 Uiso 1 1 calc R . . H13B H 0.2012 0.2983 -0.1750 0.066 Uiso 1 1 calc R . . H13C H 0.2037 0.3336 -0.0913 0.066 Uiso 1 1 calc R . . C141 C 0.41271(17) 0.43556(13) -0.17954(8) 0.0434(4) Uani 1 1 d . B . H14A H 0.5062 0.4408 -0.1955 0.065 Uiso 0.50 1 calc PR A 5 H14B H 0.4037 0.5025 -0.1578 0.065 Uiso 0.50 1 calc PR A 5 H14C H 0.3431 0.4073 -0.2201 0.065 Uiso 0.50 1 calc PR A 5 H14D H 0.4605 0.4067 -0.2183 0.065 Uiso 0.50 1 calc PR A 6 H14E H 0.4698 0.5021 -0.1568 0.065 Uiso 0.50 1 calc PR A 6 H14F H 0.3227 0.4419 -0.1983 0.065 Uiso 0.50 1 calc PR A 6 N11 N 0.8859(2) 0.47897(16) 0.10790(12) 0.0303(6) Uani 0.673(4) 1 d PD B 1 N21 N 0.7751(2) 0.40988(16) 0.10094(13) 0.0312(5) Uani 0.673(4) 1 d PD B 1 C11 C 0.9688(3) 0.4885(3) 0.17239(15) 0.0245(6) Uani 0.673(4) 1 d PD B 1 C21 C 0.9363(4) 0.4280(3) 0.2219(2) 0.0284(7) Uani 0.673(4) 1 d PD B 1 H21 H 0.8548 0.3742 0.2140 0.034 Uiso 0.673(4) 1 calc PR B 1 C31 C 1.0243(7) 0.4471(5) 0.2831(3) 0.0317(11) Uani 0.673(4) 1 d PD B 1 H31 H 1.0028 0.4056 0.3171 0.038 Uiso 0.673(4) 1 calc PR B 1 C41 C 1.1420(6) 0.5252(5) 0.2953(3) 0.0211(12) Uani 0.673(4) 1 d PD B 1 C51 C 1.1763(5) 0.5851(4) 0.2449(3) 0.0230(8) Uani 0.673(4) 1 d PD B 1 H51 H 1.2584 0.6384 0.2526 0.028 Uiso 0.673(4) 1 calc PR B 1 C61 C 1.0886(4) 0.5657(3) 0.18338(19) 0.0281(7) Uani 0.673(4) 1 d PD B 1 H61 H 1.1113 0.6059 0.1486 0.034 Uiso 0.673(4) 1 calc PR B 1 C71 C 0.6862(4) 0.4006(3) 0.0398(2) 0.0297(9) Uani 0.673(4) 1 d PD B 1 C81 C 0.5584(5) 0.3314(4) 0.0345(3) 0.0320(9) Uani 0.673(4) 1 d PD B 1 H81 H 0.5388 0.2914 0.0695 0.038 Uiso 0.673(4) 1 calc PR B 1 C91 C 0.4589(6) 0.3193(5) -0.0207(4) 0.0299(9) Uani 0.673(4) 1 d PD B 1 H91 H 0.3724 0.2711 -0.0230 0.036 Uiso 0.673(4) 1 calc PR B 1 C101 C 0.4835(11) 0.3763(10) -0.0727(6) 0.0298(15) Uani 0.673(4) 1 d PD B 1 C111 C 0.6151(9) 0.4471(8) -0.0672(4) 0.0380(14) Uani 0.673(4) 1 d PD B 1 H111 H 0.6347 0.4875 -0.1020 0.046 Uiso 0.673(4) 1 calc PR B 1 C121 C 0.7145(6) 0.4581(5) -0.0126(3) 0.0336(10) Uani 0.673(4) 1 d PD B 1 H121 H 0.8022 0.5048 -0.0104 0.040 Uiso 0.673(4) 1 calc PR B 1 N12 N 0.8178(4) 0.4172(3) 0.1343(2) 0.0286(11) Uani 0.327(4) 1 d PD B 2 N22 N 0.8374(5) 0.4563(4) 0.0803(2) 0.0298(11) Uani 0.327(4) 1 d PD B 2 C12 C 0.9330(6) 0.4539(5) 0.1874(3) 0.0211(12) Uani 0.327(4) 1 d PD B 2 C22 C 1.0422(7) 0.5347(6) 0.1872(4) 0.0259(15) Uani 0.327(4) 1 d PD B 2 H22 H 1.0484 0.5704 0.1494 0.031 Uiso 0.327(4) 1 calc PR B 2 C32 C 1.1436(11) 0.5632(9) 0.2435(7) 0.034(2) Uani 0.327(4) 1 d PD B 2 H32 H 1.2197 0.6190 0.2430 0.040 Uiso 0.327(4) 1 calc PR B 2 C42 C 1.1409(13) 0.5160(11) 0.2998(6) 0.035(4) Uani 0.327(4) 1 d PD B 2 C52 C 1.0251(12) 0.4338(9) 0.2988(5) 0.0201(17) Uani 0.327(4) 1 d PD B 2 H52 H 1.0177 0.3990 0.3370 0.024 Uiso 0.327(4) 1 calc PR B 2 C62 C 0.9225(7) 0.4032(6) 0.2431(4) 0.0286(15) Uani 0.327(4) 1 d PD B 2 H62 H 0.8453 0.3478 0.2431 0.034 Uiso 0.327(4) 1 calc PR B 2 C72 C 0.7231(7) 0.4271(7) 0.0284(4) 0.0259(17) Uani 0.327(4) 1 d PD B 2 C82 C 0.7390(11) 0.4766(11) -0.0277(6) 0.033(2) Uani 0.327(4) 1 d PD B 2 H82 H 0.8251 0.5226 -0.0307 0.039 Uiso 0.327(4) 1 calc PR B 2 C92 C 0.6312(14) 0.4600(13) -0.0797(7) 0.026(2) Uani 0.327(4) 1 d PD B 2 H92 H 0.6451 0.4937 -0.1184 0.031 Uiso 0.327(4) 1 calc PR B 2 C102 C 0.505(2) 0.396(2) -0.0762(12) 0.024(3) Uani 0.327(4) 1 d PD B 2 C112 C 0.4907(13) 0.3429(10) -0.0189(8) 0.037(3) Uani 0.327(4) 1 d PD B 2 H112 H 0.4057 0.2955 -0.0162 0.045 Uiso 0.327(4) 1 calc PR B 2 C122 C 0.5981(9) 0.3600(7) 0.0321(5) 0.0303(18) Uani 0.327(4) 1 d PD B 2 H122 H 0.5864 0.3253 0.0704 0.036 Uiso 0.327(4) 1 calc PR B 2 O13 O 0.44543(9) 0.23686(7) 0.21084(5) 0.0319(2) Uani 1 1 d . . . O23 O 0.81005(10) 0.19494(7) 0.35523(5) 0.0360(2) Uani 1 1 d . . . N3 N 0.71159(10) 0.57969(7) 0.42869(5) 0.0203(2) Uani 1 1 d . . . C13 C 0.53265(12) 0.27398(9) 0.27188(7) 0.0254(3) Uani 1 1 d . . . C23 C 0.62792(13) 0.21961(10) 0.28432(7) 0.0293(3) Uani 1 1 d . . . H23 H 0.6324 0.1616 0.2511 0.035 Uiso 1 1 calc R . . C33 C 0.71693(13) 0.25116(10) 0.34606(7) 0.0284(3) Uani 1 1 d . . . C43 C 0.70996(12) 0.33554(9) 0.39552(7) 0.0254(3) Uani 1 1 d . . . H43 H 0.7679 0.3549 0.4386 0.030 Uiso 1 1 calc R . . C53 C 0.61688(12) 0.39064(9) 0.38058(6) 0.0222(2) Uani 1 1 d . . . C63 C 0.52680(12) 0.36027(9) 0.31928(6) 0.0234(3) Uani 1 1 d . . . H63 H 0.4624 0.3978 0.3099 0.028 Uiso 1 1 calc R . . C73 C 0.34665(13) 0.29167(10) 0.19744(7) 0.0291(3) Uani 1 1 d . . . H73A H 0.3955 0.3617 0.1956 0.035 Uiso 1 1 calc R . . H73B H 0.2843 0.2935 0.2361 0.035 Uiso 1 1 calc R . . C83 C 0.26224(13) 0.24229(10) 0.12815(7) 0.0303(3) Uani 1 1 d . . . C93 C 0.17238(14) 0.29249(12) 0.10169(8) 0.0381(3) Uani 1 1 d . . . H93 H 0.1659 0.3558 0.1273 0.046 Uiso 1 1 calc R . . C103 C 0.09239(16) 0.25037(14) 0.03816(9) 0.0487(4) Uani 1 1 d . . . H103 H 0.0310 0.2847 0.0203 0.058 Uiso 1 1 calc R . . C113 C 0.10193(17) 0.15852(15) 0.00086(9) 0.0523(4) Uani 1 1 d . . . H113 H 0.0473 0.1300 -0.0428 0.063 Uiso 1 1 calc R . . C123 C 0.19003(17) 0.10814(13) 0.02652(8) 0.0467(4) Uani 1 1 d . . . H123 H 0.1957 0.0448 0.0008 0.056 Uiso 1 1 calc R . . C133 C 0.27113(15) 0.15017(11) 0.09044(8) 0.0361(3) Uani 1 1 d . . . H133 H 0.3324 0.1156 0.1081 0.043 Uiso 1 1 calc R . . C143 C 0.90881(14) 0.23439(11) 0.41629(7) 0.0344(3) Uani 1 1 d . . . H14G H 0.8610 0.2272 0.4598 0.041 Uiso 1 1 calc R . . H14H H 0.9507 0.3067 0.4183 0.041 Uiso 1 1 calc R . . C153 C 1.02032(13) 0.17861(10) 0.41219(7) 0.0282(3) Uani 1 1 d . . . C163 C 1.04031(14) 0.12481(10) 0.46372(8) 0.0326(3) Uani 1 1 d . . . H163 H 0.9771 0.1178 0.4992 0.039 Uiso 1 1 calc R . . C173 C 1.15123(16) 0.08135(10) 0.46405(8) 0.0382(3) Uani 1 1 d . . . H173 H 1.1638 0.0443 0.4995 0.046 Uiso 1 1 calc R . . C183 C 1.24307(15) 0.09150(11) 0.41340(9) 0.0428(4) Uani 1 1 d . . . H183 H 1.3197 0.0618 0.4140 0.051 Uiso 1 1 calc R . . C193 C 1.22491(16) 0.14485(11) 0.36127(9) 0.0450(4) Uani 1 1 d . . . H193 H 1.2889 0.1519 0.3261 0.054 Uiso 1 1 calc R . . C203 C 1.11284(16) 0.18784(11) 0.36072(8) 0.0384(3) Uani 1 1 d . . . H203 H 1.0995 0.2239 0.3248 0.046 Uiso 1 1 calc R . . C213 C 0.60684(12) 0.48152(9) 0.43303(6) 0.0215(2) Uani 1 1 d . . . H21A H 0.6190 0.4679 0.4812 0.026 Uiso 1 1 calc R . . H21B H 0.5119 0.4911 0.4265 0.026 Uiso 1 1 calc R . . C223 C 0.85581(12) 0.57631(10) 0.45172(7) 0.0258(3) Uani 1 1 d . . . H22A H 0.8849 0.5254 0.4180 0.039 Uiso 1 1 calc R . . H22B H 0.8571 0.5591 0.4988 0.039 Uiso 1 1 calc R . . H22C H 0.9199 0.6422 0.4535 0.039 Uiso 1 1 calc R . . C233 C 0.67014(13) 0.66089(9) 0.47870(6) 0.0242(3) Uani 1 1 d . . . H23A H 0.5765 0.6644 0.4632 0.036 Uiso 1 1 calc R . . H23B H 0.7363 0.7255 0.4792 0.036 Uiso 1 1 calc R . . H23C H 0.6705 0.6458 0.5263 0.036 Uiso 1 1 calc R . . C243 C 0.70297(12) 0.59749(9) 0.35340(6) 0.0232(3) Uani 1 1 d . . . H24A H 0.7341 0.5441 0.3221 0.028 Uiso 1 1 calc R . . H24B H 0.6044 0.5912 0.3380 0.028 Uiso 1 1 calc R . . C253 C 0.78822(13) 0.69805(9) 0.34361(6) 0.0239(3) Uani 1 1 d . . . C263 C 0.72541(15) 0.77643(10) 0.34258(7) 0.0325(3) Uani 1 1 d . . . H263 H 0.6294 0.7670 0.3497 0.039 Uiso 1 1 calc R . . C273 C 0.80145(17) 0.86838(11) 0.33128(8) 0.0411(4) Uani 1 1 d . . . H273 H 0.7576 0.9217 0.3309 0.049 Uiso 1 1 calc R . . C283 C 0.94013(17) 0.88257(11) 0.32057(8) 0.0419(4) Uani 1 1 d . . . H283 H 0.9923 0.9459 0.3133 0.050 Uiso 1 1 calc R . . C293 C 1.00362(16) 0.80480(12) 0.32031(9) 0.0442(4) Uani 1 1 d . . . H293 H 1.0994 0.8145 0.3126 0.053 Uiso 1 1 calc R . . C303 C 0.92775(14) 0.71255(11) 0.33135(8) 0.0342(3) Uani 1 1 d . . . H303 H 0.9715 0.6589 0.3305 0.041 Uiso 1 1 calc R . . C14 C 0.4957(2) 0.06401(19) 0.56097(11) 0.0679(6) Uani 1 1 d . . . H14 H 0.4930 0.1090 0.6038 0.081 Uiso 1 1 calc R . . C24 C 0.4147(2) -0.03266(19) 0.55002(12) 0.0646(6) Uani 1 1 d . . . H24 H 0.3562 -0.0540 0.5849 0.078 Uiso 1 1 calc R . . C34 C 0.5817(2) 0.09744(17) 0.51044(13) 0.0664(6) Uani 1 1 d . . . H34 H 0.6369 0.1647 0.5184 0.080 Uiso 1 1 calc R . . C15 C 0.8638(2) 0.11828(15) 0.14857(11) 0.0612(5) Uani 1 1 d . . . H15 H 0.9557 0.1595 0.1608 0.073 Uiso 1 1 calc R . . C25 C 0.7733(2) 0.14603(14) 0.10573(10) 0.0549(5) Uani 1 1 d . . . H25 H 0.8017 0.2067 0.0885 0.066 Uiso 1 1 calc R . . C35 C 0.6411(2) 0.08582(15) 0.08772(11) 0.0575(5) Uani 1 1 d . . . H35 H 0.5779 0.1040 0.0573 0.069 Uiso 1 1 calc R . . C45 C 0.6005(2) -0.00135(15) 0.11398(12) 0.0644(5) Uani 1 1 d . . . H45 H 0.5088 -0.0429 0.1021 0.077 Uiso 1 1 calc R . . C55 C 0.6915(2) -0.02784(15) 0.15683(12) 0.0653(6) Uani 1 1 d . . . H55 H 0.6631 -0.0879 0.1748 0.078 Uiso 1 1 calc R . . C65 C 0.8229(2) 0.03112(17) 0.17411(11) 0.0661(5) Uani 1 1 d . . . H65 H 0.8863 0.0121 0.2038 0.079 Uiso 1 1 calc R . . C16 C 0.3206(13) 0.9363(7) 0.2444(6) 0.071(4) Uani 0.458(12) 1 d PDU C 3 H16 H 0.3311 0.9855 0.2865 0.085 Uiso 0.458(12) 1 calc PR C 3 C26 C 0.3881(10) 0.8609(8) 0.2412(5) 0.065(3) Uani 0.458(12) 1 d PDU C 3 H26 H 0.4445 0.8581 0.2813 0.078 Uiso 0.458(12) 1 calc PR C 3 C36 C 0.3753(7) 0.7891(5) 0.1804(5) 0.0501(16) Uani 0.458(12) 1 d PDU C 3 H36 H 0.4216 0.7365 0.1775 0.060 Uiso 0.458(12) 1 calc PR C 3 C46 C 0.2922(8) 0.7976(6) 0.1245(4) 0.057(2) Uani 0.458(12) 1 d PDU C 3 H46 H 0.2811 0.7483 0.0824 0.068 Uiso 0.458(12) 1 calc PR C 3 C56 C 0.2260(7) 0.8700(10) 0.1250(6) 0.093(5) Uani 0.458(12) 1 d PDU C 3 H56 H 0.1718 0.8733 0.0842 0.112 Uiso 0.458(12) 1 calc PR C 3 C66 C 0.2385(10) 0.9409(8) 0.1873(6) 0.073(3) Uani 0.458(12) 1 d PDU C 3 H66 H 0.1900 0.9922 0.1900 0.088 Uiso 0.458(12) 1 calc PR C 3 C17 C 0.3482(9) 0.9375(6) 0.2486(3) 0.047(2) Uani 0.542(12) 1 d PDU C 4 H17 H 0.3912 0.9775 0.2927 0.056 Uiso 0.542(12) 1 calc PR C 4 C27 C 0.3748(8) 0.8454(6) 0.2253(4) 0.056(2) Uani 0.542(12) 1 d PDU C 4 H27 H 0.4359 0.8215 0.2531 0.067 Uiso 0.542(12) 1 calc PR C 4 C37 C 0.3123(11) 0.7880(4) 0.1613(4) 0.069(2) Uani 0.542(12) 1 d PDU C 4 H37 H 0.3296 0.7243 0.1445 0.083 Uiso 0.542(12) 1 calc PR C 4 C47 C 0.2246(13) 0.8246(5) 0.1223(4) 0.098(4) Uani 0.542(12) 1 d PDU C 4 H47 H 0.1811 0.7847 0.0783 0.117 Uiso 0.542(12) 1 calc PR C 4 C57 C 0.1979(8) 0.9137(5) 0.1437(4) 0.079(2) Uani 0.542(12) 1 d PDU C 4 H57 H 0.1377 0.9373 0.1151 0.094 Uiso 0.542(12) 1 calc PR C 4 C67 C 0.2599(7) 0.9716(5) 0.2085(4) 0.0524(16) Uani 0.542(12) 1 d PDU C 4 H67 H 0.2409 1.0349 0.2249 0.063 Uiso 0.542(12) 1 calc PR C 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.02036(16) 0.0512(2) 0.02461(17) 0.00976(15) -0.00112(12) 0.01457(14) O11 0.0473(6) 0.0675(8) 0.0389(6) 0.0248(5) 0.0024(5) 0.0326(6) O21 0.0205(5) 0.0716(8) 0.0537(7) 0.0163(6) -0.0052(5) 0.0030(5) O31 0.0359(6) 0.0768(8) 0.0273(5) -0.0010(5) -0.0040(4) 0.0287(6) N31 0.0410(7) 0.0470(7) 0.0253(6) 0.0088(5) -0.0088(5) 0.0056(6) C131 0.0446(9) 0.0450(9) 0.0379(8) 0.0065(7) -0.0091(7) 0.0066(7) C141 0.0491(9) 0.0546(10) 0.0265(7) 0.0102(7) -0.0047(6) 0.0125(8) N11 0.0301(12) 0.0327(12) 0.0264(12) 0.0053(9) -0.0013(9) 0.0054(9) N21 0.0290(11) 0.0335(11) 0.0302(13) 0.0080(10) -0.0034(9) 0.0060(9) C11 0.0259(17) 0.0255(18) 0.0237(14) 0.0082(12) 0.0037(12) 0.0069(14) C21 0.0265(13) 0.026(2) 0.032(2) 0.0107(13) 0.0015(15) 0.0022(13) C31 0.0335(18) 0.040(2) 0.029(2) 0.0205(14) 0.0061(15) 0.0129(15) C41 0.018(2) 0.030(2) 0.0149(19) 0.0011(15) -0.0075(14) 0.0090(15) C51 0.019(2) 0.029(2) 0.0225(13) 0.0117(13) 0.0013(12) 0.0026(15) C61 0.0263(18) 0.039(2) 0.0217(13) 0.0145(12) 0.0044(12) 0.0075(14) C71 0.031(2) 0.033(2) 0.0253(15) 0.0098(13) -0.0004(16) 0.0057(17) C81 0.031(2) 0.031(2) 0.0321(15) 0.0147(15) -0.0022(16) 0.0007(16) C91 0.029(2) 0.030(3) 0.0268(15) 0.0083(16) -0.0058(14) 0.0004(17) C101 0.031(2) 0.026(5) 0.027(3) 0.002(2) -0.004(2) 0.002(2) C111 0.050(3) 0.037(3) 0.027(2) 0.0140(16) 0.0046(18) 0.0065(19) C121 0.033(2) 0.033(3) 0.030(2) 0.0048(16) -0.0016(17) -0.0004(15) N12 0.027(2) 0.032(2) 0.025(2) 0.0086(18) -0.0048(17) 0.0047(17) N22 0.029(3) 0.027(2) 0.030(3) 0.002(2) -0.001(2) 0.003(2) C12 0.023(3) 0.021(3) 0.021(3) 0.012(2) 0.003(2) 0.004(2) C22 0.027(4) 0.031(5) 0.024(3) 0.018(3) 0.008(3) 0.006(3) C32 0.017(4) 0.027(5) 0.048(4) 0.006(3) 0.006(3) -0.009(3) C42 0.029(6) 0.048(6) 0.049(7) 0.032(4) 0.027(4) 0.028(4) C52 0.016(2) 0.021(3) 0.022(4) 0.008(3) -0.004(3) 0.001(2) C62 0.026(3) 0.025(4) 0.032(4) 0.011(2) -0.003(3) -0.002(2) C72 0.028(4) 0.029(4) 0.018(3) 0.005(3) -0.005(3) 0.001(3) C82 0.035(4) 0.028(4) 0.033(5) 0.008(3) -0.002(3) 0.001(3) C92 0.028(4) 0.027(4) 0.016(4) 0.004(3) -0.008(3) -0.002(3) C102 0.035(7) 0.018(7) 0.017(3) 0.011(3) -0.002(4) -0.002(4) C112 0.031(5) 0.026(5) 0.045(4) 0.007(4) -0.002(4) -0.011(3) C122 0.031(6) 0.033(5) 0.024(3) 0.015(3) 0.000(3) -0.004(4) O13 0.0264(5) 0.0335(5) 0.0309(5) -0.0077(4) -0.0103(4) 0.0109(4) O23 0.0318(5) 0.0360(5) 0.0379(5) -0.0085(4) -0.0121(4) 0.0182(4) N3 0.0163(5) 0.0249(5) 0.0185(5) 0.0015(4) -0.0003(4) 0.0049(4) C13 0.0185(6) 0.0290(7) 0.0250(6) 0.0003(5) -0.0023(5) 0.0030(5) C23 0.0246(6) 0.0277(7) 0.0312(7) -0.0064(5) -0.0024(5) 0.0078(5) C33 0.0229(6) 0.0296(7) 0.0319(7) -0.0002(5) -0.0027(5) 0.0105(5) C43 0.0206(6) 0.0288(6) 0.0244(6) -0.0001(5) -0.0020(5) 0.0060(5) C53 0.0184(6) 0.0247(6) 0.0223(6) 0.0035(5) 0.0035(5) 0.0036(5) C63 0.0176(6) 0.0261(6) 0.0253(6) 0.0030(5) 0.0006(5) 0.0049(5) C73 0.0263(6) 0.0312(7) 0.0288(7) 0.0019(5) -0.0031(5) 0.0090(5) C83 0.0229(6) 0.0382(8) 0.0275(7) 0.0057(6) -0.0009(5) 0.0041(5) C93 0.0279(7) 0.0483(9) 0.0393(8) 0.0115(7) -0.0005(6) 0.0101(6) C103 0.0310(8) 0.0729(12) 0.0438(9) 0.0191(9) -0.0068(7) 0.0124(8) C113 0.0366(9) 0.0782(13) 0.0331(8) 0.0053(8) -0.0128(7) 0.0036(8) C123 0.0410(9) 0.0531(10) 0.0352(8) -0.0053(7) -0.0053(7) 0.0028(7) C133 0.0311(7) 0.0408(8) 0.0322(7) 0.0007(6) -0.0041(6) 0.0067(6) C143 0.0294(7) 0.0389(8) 0.0325(7) -0.0048(6) -0.0078(6) 0.0146(6) C153 0.0234(6) 0.0277(7) 0.0310(7) 0.0003(5) -0.0039(5) 0.0069(5) C163 0.0315(7) 0.0270(7) 0.0351(7) 0.0035(6) -0.0037(6) 0.0021(5) C173 0.0419(8) 0.0256(7) 0.0440(9) 0.0033(6) -0.0145(7) 0.0081(6) C183 0.0311(8) 0.0274(7) 0.0675(11) -0.0024(7) -0.0098(7) 0.0135(6) C193 0.0397(8) 0.0359(8) 0.0603(10) 0.0047(7) 0.0191(8) 0.0127(7) C203 0.0471(9) 0.0334(8) 0.0410(8) 0.0119(6) 0.0091(7) 0.0176(7) C213 0.0163(5) 0.0261(6) 0.0212(6) 0.0031(5) 0.0023(4) 0.0043(5) C223 0.0157(6) 0.0324(7) 0.0282(6) 0.0051(5) -0.0023(5) 0.0049(5) C233 0.0229(6) 0.0262(6) 0.0214(6) -0.0007(5) 0.0006(5) 0.0065(5) C243 0.0213(6) 0.0293(6) 0.0177(6) 0.0031(5) -0.0003(5) 0.0049(5) C253 0.0232(6) 0.0276(6) 0.0193(6) 0.0024(5) -0.0004(5) 0.0051(5) C263 0.0320(7) 0.0362(8) 0.0334(7) 0.0101(6) 0.0057(6) 0.0132(6) C273 0.0539(10) 0.0337(8) 0.0409(8) 0.0116(7) 0.0091(7) 0.0170(7) C283 0.0495(9) 0.0319(8) 0.0381(8) 0.0114(6) -0.0016(7) -0.0040(7) C293 0.0270(7) 0.0521(10) 0.0546(10) 0.0242(8) 0.0055(7) 0.0014(7) C303 0.0273(7) 0.0381(8) 0.0418(8) 0.0152(6) 0.0087(6) 0.0106(6) C14 0.0631(13) 0.1032(18) 0.0536(11) 0.0066(11) -0.0012(10) 0.0597(13) C24 0.0540(11) 0.0900(16) 0.0702(14) 0.0367(12) 0.0175(10) 0.0399(12) C34 0.0482(11) 0.0744(14) 0.0905(16) 0.0265(12) 0.0028(11) 0.0347(10) C15 0.0505(11) 0.0653(12) 0.0640(12) 0.0160(10) 0.0083(9) 0.0045(9) C25 0.0581(11) 0.0442(10) 0.0658(12) 0.0167(9) 0.0196(9) 0.0127(8) C35 0.0523(11) 0.0635(12) 0.0623(12) 0.0114(9) 0.0157(9) 0.0243(9) C45 0.0552(11) 0.0494(11) 0.0805(14) 0.0015(10) 0.0230(11) 0.0031(9) C55 0.0797(15) 0.0457(11) 0.0807(15) 0.0215(10) 0.0394(12) 0.0234(10) C65 0.0688(13) 0.0794(14) 0.0639(13) 0.0303(11) 0.0212(10) 0.0307(12) C16 0.088(7) 0.047(5) 0.084(8) 0.008(5) 0.045(5) 0.028(4) C26 0.095(6) 0.071(5) 0.032(3) 0.004(3) 0.022(3) 0.031(4) C36 0.067(4) 0.039(2) 0.053(4) 0.018(3) 0.016(3) 0.023(3) C46 0.056(3) 0.043(3) 0.062(4) 0.011(3) -0.001(3) -0.008(3) C56 0.036(3) 0.138(15) 0.125(8) 0.080(9) 0.014(4) 0.019(5) C66 0.060(5) 0.058(6) 0.113(10) 0.017(6) 0.030(6) 0.033(5) C17 0.045(2) 0.063(5) 0.034(3) 0.011(3) 0.000(2) 0.014(2) C27 0.074(4) 0.056(4) 0.054(5) 0.028(3) 0.030(3) 0.033(3) C37 0.122(7) 0.041(2) 0.061(4) 0.023(3) 0.034(5) 0.039(4) C47 0.133(8) 0.055(5) 0.079(4) 0.007(3) -0.053(5) -0.010(4) C57 0.079(4) 0.050(3) 0.085(4) 0.001(3) -0.047(4) -0.009(3) C67 0.065(3) 0.038(3) 0.048(3) 0.003(2) -0.012(2) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O31 1.4440(10) . ? S1 O21 1.4442(11) . ? S1 O11 1.4544(11) . ? S1 C42 1.727(9) . ? S1 C41 1.792(3) . ? N31 C101 1.362(6) . ? N31 C102 1.417(11) . ? N31 C131 1.447(2) . ? N31 C141 1.4519(19) . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C141 H14D 0.9800 . ? C141 H14E 0.9800 . ? C141 H14F 0.9800 . ? N11 N21 1.263(3) . ? N11 C11 1.431(3) . ? N21 C71 1.413(4) . ? C11 C61 1.382(3) . ? C11 C21 1.384(4) . ? C21 C31 1.386(6) . ? C21 H21 0.9500 . ? C31 C41 1.374(8) . ? C31 H31 0.9500 . ? C41 C51 1.395(8) . ? C51 C61 1.389(6) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C71 C81 1.387(4) . ? C71 C121 1.397(5) . ? C81 C91 1.381(7) . ? C81 H81 0.9500 . ? C91 C101 1.384(8) . ? C91 H91 0.9500 . ? C101 C111 1.425(8) . ? C111 C121 1.376(8) . ? C111 H111 0.9500 . ? C121 H121 0.9500 . ? N12 N22 1.263(6) . ? N12 C12 1.434(6) . ? N22 C72 1.414(6) . ? C12 C22 1.367(6) . ? C12 C62 1.384(6) . ? C22 C32 1.385(10) . ? C22 H22 0.9500 . ? C32 C42 1.366(13) . ? C32 H32 0.9500 . ? C42 C52 1.414(13) . ? C52 C62 1.385(9) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? C72 C122 1.378(6) . ? C72 C82 1.380(7) . ? C82 C92 1.385(11) . ? C82 H82 0.9500 . ? C92 C102 1.368(13) . ? C92 H92 0.9500 . ? C102 C112 1.430(13) . ? C112 C122 1.369(12) . ? C112 H112 0.9500 . ? C122 H122 0.9500 . ? O13 C13 1.3750(14) . ? O13 C73 1.4231(15) . ? O23 C33 1.3739(15) . ? O23 C143 1.4386(15) . ? N3 C223 1.4965(14) . ? N3 C233 1.5006(15) . ? N3 C243 1.5202(15) . ? N3 C213 1.5287(15) . ? C13 C23 1.3859(18) . ? C13 C63 1.3915(17) . ? C23 C33 1.3912(18) . ? C23 H23 0.9500 . ? C33 C43 1.3953(17) . ? C43 C53 1.3886(17) . ? C43 H43 0.9500 . ? C53 C63 1.3903(16) . ? C53 C213 1.5017(16) . ? C63 H63 0.9500 . ? C73 C83 1.5063(18) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C83 C133 1.385(2) . ? C83 C93 1.3928(19) . ? C93 C103 1.385(2) . ? C93 H93 0.9500 . ? C103 C113 1.381(3) . ? C103 H103 0.9500 . ? C113 C123 1.375(2) . ? C113 H113 0.9500 . ? C123 C133 1.396(2) . ? C123 H123 0.9500 . ? C133 H133 0.9500 . ? C143 C153 1.4959(17) . ? C143 H14G 0.9900 . ? C143 H14H 0.9900 . ? C153 C203 1.383(2) . ? C153 C163 1.3846(19) . ? C163 C173 1.380(2) . ? C163 H163 0.9500 . ? C173 C183 1.367(2) . ? C173 H173 0.9500 . ? C183 C193 1.385(2) . ? C183 H183 0.9500 . ? C193 C203 1.386(2) . ? C193 H193 0.9500 . ? C203 H203 0.9500 . ? C213 H21A 0.9900 . ? C213 H21B 0.9900 . ? C223 H22A 0.9800 . ? C223 H22B 0.9800 . ? C223 H22C 0.9800 . ? C233 H23A 0.9800 . ? C233 H23B 0.9800 . ? C233 H23C 0.9800 . ? C243 C253 1.5054(17) . ? C243 H24A 0.9900 . ? C243 H24B 0.9900 . ? C253 C263 1.3865(18) . ? C253 C303 1.3882(18) . ? C263 C273 1.385(2) . ? C263 H263 0.9500 . ? C273 C283 1.374(2) . ? C273 H273 0.9500 . ? C283 C293 1.380(2) . ? C283 H283 0.9500 . ? C293 C303 1.386(2) . ? C293 H293 0.9500 . ? C303 H303 0.9500 . ? C14 C24 1.371(3) . ? C14 C34 1.393(3) . ? C14 H14 0.9500 . ? C24 C34 1.350(3) 2_656 ? C24 H24 0.9500 . ? C34 C24 1.350(3) 2_656 ? C34 H34 0.9500 . ? C15 C25 1.365(3) . ? C15 C65 1.373(3) . ? C15 H15 0.9500 . ? C25 C35 1.372(3) . ? C25 H25 0.9500 . ? C35 C45 1.381(3) . ? C35 H35 0.9500 . ? C45 C55 1.359(3) . ? C45 H45 0.9500 . ? C55 C65 1.358(3) . ? C55 H55 0.9500 . ? C65 H65 0.9500 . ? C16 C66 1.363(7) . ? C16 C26 1.372(7) . ? C16 H16 0.9500 . ? C26 C36 1.380(7) . ? C26 H26 0.9500 . ? C36 C46 1.371(8) . ? C36 H36 0.9500 . ? C46 C56 1.331(11) . ? C46 H46 0.9500 . ? C56 C66 1.396(9) . ? C56 H56 0.9500 . ? C66 H66 0.9500 . ? C17 C67 1.369(6) . ? C17 C27 1.376(6) . ? C17 H17 0.9500 . ? C27 C37 1.377(7) . ? C27 H27 0.9500 . ? C37 C47 1.373(8) . ? C37 H37 0.9500 . ? C47 C57 1.331(12) . ? C47 H47 0.9500 . ? C57 C67 1.391(6) . ? C57 H57 0.9500 . ? C67 H67 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O31 S1 O21 113.85(8) . . ? O31 S1 O11 112.35(7) . . ? O21 S1 O11 112.62(7) . . ? O31 S1 C42 106.0(5) . . ? O21 S1 C42 109.2(5) . . ? O11 S1 C42 101.9(5) . . ? O31 S1 C41 105.4(2) . . ? O21 S1 C41 105.3(2) . . ? O11 S1 C41 106.5(2) . . ? C42 S1 C41 5.0(7) . . ? C101 N31 C102 13.1(10) . . ? C101 N31 C131 117.1(4) . . ? C102 N31 C131 129.8(7) . . ? C101 N31 C141 124.6(4) . . ? C102 N31 C141 111.4(6) . . ? C131 N31 C141 117.68(12) . . ? N31 C131 H13A 109.5 . . ? N31 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? N31 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? N31 C141 H14A 109.5 . . ? N31 C141 H14B 109.5 . . ? N31 C141 H14C 109.5 . . ? N31 C141 H14D 109.5 . . ? N31 C141 H14E 109.5 . . ? N31 C141 H14F 109.5 . . ? N21 N11 C11 112.7(3) . . ? N11 N21 C71 114.9(3) . . ? C61 C11 C21 120.3(3) . . ? C61 C11 N11 114.6(3) . . ? C21 C11 N11 125.1(3) . . ? C11 C21 C31 119.1(3) . . ? C11 C21 H21 120.4 . . ? C31 C21 H21 120.4 . . ? C41 C31 C21 121.0(4) . . ? C41 C31 H31 119.5 . . ? C21 C31 H31 119.5 . . ? C31 C41 C51 119.9(3) . . ? C31 C41 S1 121.9(5) . . ? C51 C41 S1 118.2(4) . . ? C61 C51 C41 119.1(4) . . ? C61 C51 H51 120.4 . . ? C41 C51 H51 120.4 . . ? C11 C61 C51 120.4(3) . . ? C11 C61 H61 119.8 . . ? C51 C61 H61 119.8 . . ? C81 C71 C121 118.8(3) . . ? C81 C71 N21 115.8(4) . . ? C121 C71 N21 125.4(4) . . ? C91 C81 C71 121.5(4) . . ? C91 C81 H81 119.3 . . ? C71 C81 H81 119.3 . . ? C81 C91 C101 120.9(5) . . ? C81 C91 H91 119.6 . . ? C101 C91 H91 119.5 . . ? N31 C101 C91 124.7(7) . . ? N31 C101 C111 117.8(7) . . ? C91 C101 C111 117.5(4) . . ? C121 C111 C101 121.4(5) . . ? C121 C111 H111 119.3 . . ? C101 C111 H111 119.3 . . ? C111 C121 C71 120.0(4) . . ? C111 C121 H121 120.0 . . ? C71 C121 H121 120.0 . . ? N22 N12 C12 112.8(5) . . ? N12 N22 C72 114.8(6) . . ? C22 C12 C62 120.9(5) . . ? C22 C12 N12 125.0(6) . . ? C62 C12 N12 114.1(5) . . ? C12 C22 C32 118.2(6) . . ? C12 C22 H22 120.9 . . ? C32 C22 H22 120.9 . . ? C42 C32 C22 124.1(8) . . ? C42 C32 H32 117.9 . . ? C22 C32 H32 117.9 . . ? C32 C42 C52 116.1(7) . . ? C32 C42 S1 126.5(9) . . ? C52 C42 S1 116.9(8) . . ? C62 C52 C42 121.2(7) . . ? C62 C52 H52 119.4 . . ? C42 C52 H52 119.4 . . ? C12 C62 C52 119.5(6) . . ? C12 C62 H62 120.2 . . ? C52 C62 H62 120.2 . . ? C122 C72 C82 119.2(6) . . ? C122 C72 N22 125.6(7) . . ? C82 C72 N22 115.1(7) . . ? C72 C82 C92 120.9(8) . . ? C72 C82 H82 119.6 . . ? C92 C82 H82 119.5 . . ? C102 C92 C82 121.0(9) . . ? C102 C92 H92 119.5 . . ? C82 C92 H92 119.5 . . ? C92 C102 N31 125.3(12) . . ? C92 C102 C112 117.7(8) . . ? N31 C102 C112 116.8(11) . . ? C122 C112 C102 120.7(8) . . ? C122 C112 H112 119.7 . . ? C102 C112 H112 119.7 . . ? C112 C122 C72 120.5(8) . . ? C112 C122 H122 119.7 . . ? C72 C122 H122 119.7 . . ? C13 O13 C73 116.58(9) . . ? C33 O23 C143 115.21(10) . . ? C223 N3 C233 109.20(9) . . ? C223 N3 C243 110.92(9) . . ? C233 N3 C243 110.70(9) . . ? C223 N3 C213 110.63(9) . . ? C233 N3 C213 106.12(9) . . ? C243 N3 C213 109.16(9) . . ? O13 C13 C23 115.91(11) . . ? O13 C13 C63 122.97(11) . . ? C23 C13 C63 121.12(11) . . ? C13 C23 C33 119.08(11) . . ? C13 C23 H23 120.5 . . ? C33 C23 H23 120.5 . . ? O23 C33 C23 116.51(11) . . ? O23 C33 C43 122.62(11) . . ? C23 C33 C43 120.87(11) . . ? C53 C43 C33 118.82(11) . . ? C53 C43 H43 120.6 . . ? C33 C43 H43 120.6 . . ? C43 C53 C63 121.15(11) . . ? C43 C53 C213 119.91(11) . . ? C63 C53 C213 118.85(10) . . ? C53 C63 C13 118.87(11) . . ? C53 C63 H63 120.6 . . ? C13 C63 H63 120.6 . . ? O13 C73 C83 109.65(10) . . ? O13 C73 H73A 109.7 . . ? C83 C73 H73A 109.7 . . ? O13 C73 H73B 109.7 . . ? C83 C73 H73B 109.7 . . ? H73A C73 H73B 108.2 . . ? C133 C83 C93 119.51(13) . . ? C133 C83 C73 122.65(12) . . ? C93 C83 C73 117.84(13) . . ? C103 C93 C83 120.15(15) . . ? C103 C93 H93 119.9 . . ? C83 C93 H93 119.9 . . ? C113 C103 C93 119.98(15) . . ? C113 C103 H103 120.0 . . ? C93 C103 H103 120.0 . . ? C123 C113 C103 120.40(15) . . ? C123 C113 H113 119.8 . . ? C103 C113 H113 119.8 . . ? C113 C123 C133 119.96(16) . . ? C113 C123 H123 120.0 . . ? C133 C123 H123 120.0 . . ? C83 C133 C123 120.00(14) . . ? C83 C133 H133 120.0 . . ? C123 C133 H133 120.0 . . ? O23 C143 C153 109.62(10) . . ? O23 C143 H14G 109.7 . . ? C153 C143 H14G 109.7 . . ? O23 C143 H14H 109.7 . . ? C153 C143 H14H 109.7 . . ? H14G C143 H14H 108.2 . . ? C203 C153 C163 119.06(12) . . ? C203 C153 C143 120.31(13) . . ? C163 C153 C143 120.35(13) . . ? C173 C163 C153 120.60(14) . . ? C173 C163 H163 119.7 . . ? C153 C163 H163 119.7 . . ? C183 C173 C163 120.07(14) . . ? C183 C173 H173 120.0 . . ? C163 C173 H173 120.0 . . ? C173 C183 C193 120.30(13) . . ? C173 C183 H183 119.9 . . ? C193 C183 H183 119.9 . . ? C183 C193 C203 119.56(15) . . ? C183 C193 H193 120.2 . . ? C203 C193 H193 120.2 . . ? C153 C203 C193 120.41(14) . . ? C153 C203 H203 119.8 . . ? C193 C203 H203 119.8 . . ? C53 C213 N3 115.73(9) . . ? C53 C213 H21A 108.3 . . ? N3 C213 H21A 108.3 . . ? C53 C213 H21B 108.3 . . ? N3 C213 H21B 108.3 . . ? H21A C213 H21B 107.4 . . ? N3 C223 H22A 109.5 . . ? N3 C223 H22B 109.5 . . ? H22A C223 H22B 109.5 . . ? N3 C223 H22C 109.5 . . ? H22A C223 H22C 109.5 . . ? H22B C223 H22C 109.5 . . ? N3 C233 H23A 109.5 . . ? N3 C233 H23B 109.5 . . ? H23A C233 H23B 109.5 . . ? N3 C233 H23C 109.5 . . ? H23A C233 H23C 109.5 . . ? H23B C233 H23C 109.5 . . ? C253 C243 N3 114.64(10) . . ? C253 C243 H24A 108.6 . . ? N3 C243 H24A 108.6 . . ? C253 C243 H24B 108.6 . . ? N3 C243 H24B 108.6 . . ? H24A C243 H24B 107.6 . . ? C263 C253 C303 118.83(12) . . ? C263 C253 C243 119.88(11) . . ? C303 C253 C243 121.17(12) . . ? C273 C263 C253 120.56(13) . . ? C273 C263 H263 119.7 . . ? C253 C263 H263 119.7 . . ? C283 C273 C263 120.14(14) . . ? C283 C273 H273 119.9 . . ? C263 C273 H273 119.9 . . ? C273 C283 C293 119.99(14) . . ? C273 C283 H283 120.0 . . ? C293 C283 H283 120.0 . . ? C283 C293 C303 120.03(14) . . ? C283 C293 H293 120.0 . . ? C303 C293 H293 120.0 . . ? C293 C303 C253 120.41(13) . . ? C293 C303 H303 119.8 . . ? C253 C303 H303 119.8 . . ? C24 C14 C34 121.2(2) . . ? C24 C14 H14 119.4 . . ? C34 C14 H14 119.4 . . ? C34 C24 C14 119.9(2) 2_656 . ? C34 C24 H24 120.0 2_656 . ? C14 C24 H24 120.0 . . ? C24 C34 C14 118.9(2) 2_656 . ? C24 C34 H34 120.6 2_656 . ? C14 C34 H34 120.6 . . ? C25 C15 C65 120.40(19) . . ? C25 C15 H15 119.8 . . ? C65 C15 H15 119.8 . . ? C15 C25 C35 119.59(18) . . ? C15 C25 H25 120.2 . . ? C35 C25 H25 120.2 . . ? C25 C35 C45 119.63(19) . . ? C25 C35 H35 120.2 . . ? C45 C35 H35 120.2 . . ? C55 C45 C35 120.14(19) . . ? C55 C45 H45 119.9 . . ? C35 C45 H45 119.9 . . ? C65 C55 C45 120.30(19) . . ? C65 C55 H55 119.9 . . ? C45 C55 H55 119.9 . . ? C55 C65 C15 119.9(2) . . ? C55 C65 H65 120.0 . . ? C15 C65 H65 120.0 . . ? C66 C16 C26 120.2(7) . . ? C66 C16 H16 119.9 . . ? C26 C16 H16 119.9 . . ? C16 C26 C36 121.0(7) . . ? C16 C26 H26 119.5 . . ? C36 C26 H26 119.5 . . ? C46 C36 C26 116.5(6) . . ? C46 C36 H36 121.8 . . ? C26 C36 H36 121.8 . . ? C56 C46 C36 124.6(7) . . ? C56 C46 H46 117.7 . . ? C36 C46 H46 117.7 . . ? C46 C56 C66 118.0(7) . . ? C46 C56 H56 121.0 . . ? C66 C56 H56 121.0 . . ? C16 C66 C56 119.8(6) . . ? C16 C66 H66 120.1 . . ? C56 C66 H66 120.1 . . ? C67 C17 C27 120.1(6) . . ? C67 C17 H17 120.0 . . ? C27 C17 H17 120.0 . . ? C37 C27 C17 119.6(5) . . ? C37 C27 H27 120.2 . . ? C17 C27 H27 120.2 . . ? C47 C37 C27 118.9(5) . . ? C47 C37 H37 120.6 . . ? C27 C37 H37 120.6 . . ? C57 C47 C37 122.6(6) . . ? C57 C47 H47 118.7 . . ? C37 C47 H47 118.7 . . ? C47 C57 C67 118.8(7) . . ? C47 C57 H57 120.6 . . ? C67 C57 H57 120.6 . . ? C17 C67 C57 120.1(6) . . ? C17 C67 H67 119.9 . . ? C57 C67 H67 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 N11 N21 C71 177.0(3) . . . . ? N21 N11 C11 C61 -177.7(3) . . . . ? N21 N11 C11 C21 1.8(4) . . . . ? C61 C11 C21 C31 1.1(6) . . . . ? N11 C11 C21 C31 -178.4(5) . . . . ? C11 C21 C31 C41 0.4(10) . . . . ? C21 C31 C41 C51 -1.5(11) . . . . ? C21 C31 C41 S1 176.2(5) . . . . ? O31 S1 C41 C31 -75.0(7) . . . . ? O21 S1 C41 C31 164.4(6) . . . . ? O11 S1 C41 C31 44.6(7) . . . . ? C42 S1 C41 C31 22(8) . . . . ? O31 S1 C41 C51 102.8(5) . . . . ? O21 S1 C41 C51 -17.8(6) . . . . ? O11 S1 C41 C51 -137.6(5) . . . . ? C42 S1 C41 C51 -160(9) . . . . ? C31 C41 C51 C61 1.2(10) . . . . ? S1 C41 C51 C61 -176.7(5) . . . . ? C21 C11 C61 C51 -1.5(6) . . . . ? N11 C11 C61 C51 178.1(4) . . . . ? C41 C51 C61 C11 0.3(9) . . . . ? N11 N21 C71 C81 -174.3(4) . . . . ? N11 N21 C71 C121 2.5(7) . . . . ? C121 C71 C81 C91 -0.8(9) . . . . ? N21 C71 C81 C91 176.3(6) . . . . ? C71 C81 C91 C101 -0.2(14) . . . . ? C102 N31 C101 C91 172(11) . . . . ? C131 N31 C101 C91 4.7(18) . . . . ? C141 N31 C101 C91 175.1(10) . . . . ? C102 N31 C101 C111 -7(8) . . . . ? C131 N31 C101 C111 -174.5(10) . . . . ? C141 N31 C101 C111 -4.1(18) . . . . ? C81 C91 C101 N31 -178.8(11) . . . . ? C81 C91 C101 C111 0(2) . . . . ? N31 C101 C111 C121 179.6(10) . . . . ? C91 C101 C111 C121 0(2) . . . . ? C101 C111 C121 C71 -1.2(16) . . . . ? C81 C71 C121 C111 1.4(11) . . . . ? N21 C71 C121 C111 -175.3(7) . . . . ? C12 N12 N22 C72 -176.2(6) . . . . ? N22 N12 C12 C22 11.2(8) . . . . ? N22 N12 C12 C62 -172.1(6) . . . . ? C62 C12 C22 C32 1.3(13) . . . . ? N12 C12 C22 C32 177.9(9) . . . . ? C12 C22 C32 C42 -1(2) . . . . ? C22 C32 C42 C52 -1(2) . . . . ? C22 C32 C42 S1 -171.8(11) . . . . ? O31 S1 C42 C32 99.0(14) . . . . ? O21 S1 C42 C32 -24.0(16) . . . . ? O11 S1 C42 C32 -143.3(14) . . . . ? C41 S1 C42 C32 15(7) . . . . ? O31 S1 C42 C52 -72.1(12) . . . . ? O21 S1 C42 C52 164.9(11) . . . . ? O11 S1 C42 C52 45.5(13) . . . . ? C41 S1 C42 C52 -156(9) . . . . ? C32 C42 C52 C62 1(2) . . . . ? S1 C42 C52 C62 173.0(11) . . . . ? C22 C12 C62 C52 -1.0(14) . . . . ? N12 C12 C62 C52 -177.9(9) . . . . ? C42 C52 C62 C12 -0.1(19) . . . . ? N12 N22 C72 C122 -1.4(12) . . . . ? N12 N22 C72 C82 174.3(10) . . . . ? C122 C72 C82 C92 0(2) . . . . ? N22 C72 C82 C92 -175.6(14) . . . . ? C72 C82 C92 C102 1(3) . . . . ? C82 C92 C102 N31 -177(2) . . . . ? C82 C92 C102 C112 -3(4) . . . . ? C101 N31 C102 C92 166(12) . . . . ? C131 N31 C102 C92 -179(2) . . . . ? C141 N31 C102 C92 -11(4) . . . . ? C101 N31 C102 C112 -8(7) . . . . ? C131 N31 C102 C112 7(4) . . . . ? C141 N31 C102 C112 175(2) . . . . ? C92 C102 C112 C122 3(4) . . . . ? N31 C102 C112 C122 177.5(18) . . . . ? C102 C112 C122 C72 -1(3) . . . . ? C82 C72 C122 C112 -0.4(19) . . . . ? N22 C72 C122 C112 175.2(12) . . . . ? C73 O13 C13 C23 179.78(12) . . . . ? C73 O13 C13 C63 0.24(18) . . . . ? O13 C13 C23 C33 -178.22(12) . . . . ? C63 C13 C23 C33 1.3(2) . . . . ? C143 O23 C33 C23 174.67(12) . . . . ? C143 O23 C33 C43 -5.52(19) . . . . ? C13 C23 C33 O23 -179.38(12) . . . . ? C13 C23 C33 C43 0.8(2) . . . . ? O23 C33 C43 C53 177.17(12) . . . . ? C23 C33 C43 C53 -3.0(2) . . . . ? C33 C43 C53 C63 3.18(19) . . . . ? C33 C43 C53 C213 179.74(11) . . . . ? C43 C53 C63 C13 -1.11(18) . . . . ? C213 C53 C63 C13 -177.70(11) . . . . ? O13 C13 C63 C53 178.33(11) . . . . ? C23 C13 C63 C53 -1.19(19) . . . . ? C13 O13 C73 C83 178.77(11) . . . . ? O13 C73 C83 C133 7.99(18) . . . . ? O13 C73 C83 C93 -171.89(12) . . . . ? C133 C83 C93 C103 0.1(2) . . . . ? C73 C83 C93 C103 179.99(13) . . . . ? C83 C93 C103 C113 -0.2(2) . . . . ? C93 C103 C113 C123 0.3(3) . . . . ? C103 C113 C123 C133 -0.4(3) . . . . ? C93 C83 C133 C123 -0.2(2) . . . . ? C73 C83 C133 C123 179.91(13) . . . . ? C113 C123 C133 C83 0.4(2) . . . . ? C33 O23 C143 C153 -168.66(12) . . . . ? O23 C143 C153 C203 67.44(17) . . . . ? O23 C143 C153 C163 -118.65(14) . . . . ? C203 C153 C163 C173 0.3(2) . . . . ? C143 C153 C163 C173 -173.68(12) . . . . ? C153 C163 C173 C183 0.3(2) . . . . ? C163 C173 C183 C193 -0.4(2) . . . . ? C173 C183 C193 C203 -0.1(2) . . . . ? C163 C153 C203 C193 -0.8(2) . . . . ? C143 C153 C203 C193 173.21(13) . . . . ? C183 C193 C203 C153 0.7(2) . . . . ? C43 C53 C213 N3 85.22(14) . . . . ? C63 C53 C213 N3 -98.14(13) . . . . ? C223 N3 C213 C53 -68.88(12) . . . . ? C233 N3 C213 C53 172.78(10) . . . . ? C243 N3 C213 C53 53.44(12) . . . . ? C223 N3 C243 C253 -65.00(13) . . . . ? C233 N3 C243 C253 56.39(13) . . . . ? C213 N3 C243 C253 172.85(10) . . . . ? N3 C243 C253 C263 -97.80(13) . . . . ? N3 C243 C253 C303 86.05(14) . . . . ? C303 C253 C263 C273 -1.6(2) . . . . ? C243 C253 C263 C273 -177.85(12) . . . . ? C253 C263 C273 C283 0.4(2) . . . . ? C263 C273 C283 C293 0.7(2) . . . . ? C273 C283 C293 C303 -0.5(2) . . . . ? C283 C293 C303 C253 -0.8(2) . . . . ? C263 C253 C303 C293 1.8(2) . . . . ? C243 C253 C303 C293 178.02(13) . . . . ? C34 C14 C24 C34 0.4(3) . . . 2_656 ? C24 C14 C34 C24 -0.4(3) . . . 2_656 ? C65 C15 C25 C35 -0.6(3) . . . . ? C15 C25 C35 C45 1.0(3) . . . . ? C25 C35 C45 C55 -0.7(3) . . . . ? C35 C45 C55 C65 0.0(3) . . . . ? C45 C55 C65 C15 0.4(3) . . . . ? C25 C15 C65 C55 -0.1(3) . . . . ? C66 C16 C26 C36 0.5(3) . . . . ? C16 C26 C36 C46 -0.1(3) . . . . ? C26 C36 C46 C56 0.8(6) . . . . ? C36 C46 C56 C66 -1.8(7) . . . . ? C26 C16 C66 C56 -1.5(6) . . . . ? C46 C56 C66 C16 2.2(7) . . . . ? C67 C17 C27 C37 0.1(3) . . . . ? C17 C27 C37 C47 0.0(3) . . . . ? C27 C37 C47 C57 0.4(6) . . . . ? C37 C47 C57 C67 -0.9(8) . . . . ? C27 C17 C67 C57 -0.7(6) . . . . ? C47 C57 C67 C17 1.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.232 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.037 #===END