# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Parimal Paul' _publ_contact_author_email ppaul@csmcri.org _publ_section_title ; Cation-induced fluorescent excimer emission in calix[4]arene chemosensors bearing quinoline as fluoregenic unit: Experimental, molecular modeling and crystallographic studies ; loop_ _publ_author_name P.Paul S.Patra R.Gunupuru R.Lo S.Eringathodi B.Ganguly # Attachment '- CIF_revised_compounds 1 to 3.cif' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 775957' #TrackingRef '- CIF_revised_compounds 1 to 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H88 N6 O9' _chemical_formula_weight 1181.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 33.741(6) _cell_length_b 17.823(3) _cell_length_c 21.667(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13029(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7709 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 23.45 _exptl_crystal_description Plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5072 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9591 _exptl_absorpt_correction_T_max 0.9905 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'Omega-Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54952 _diffrn_reflns_av_R_equivalents 0.0883 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 24.00 _reflns_number_total 10218 _reflns_number_gt 8458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0862P)^2^+19.8491P] 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 10218 _refine_ls_number_parameters 810 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0899 _refine_ls_wR_factor_ref 0.2150 _refine_ls_wR_factor_gt 0.2024 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.21322(7) 1.07983(14) 0.25297(11) 0.0170(6) Uani 1 d . . . O2 O 0.29428(8) 1.20205(17) 0.22841(13) 0.0305(7) Uani 1 d . . . O3 O 0.17307(7) 1.05753(15) 0.13617(12) 0.0191(6) Uani 1 d . . . H3 H 0.1788 1.0205 0.1155 0.029 Uiso 1 calc R . . O4 O 0.19928(7) 0.92597(14) 0.09270(11) 0.0150(6) Uani 1 d . . . O5 O 0.29025(8) 0.93600(17) 0.01062(12) 0.0297(7) Uani 1 d . . . O6 O 0.22477(8) 0.93339(14) 0.22129(11) 0.0201(6) Uani 1 d . . . H6 H 0.2217 0.9756 0.2355 0.030 Uiso 1 calc R . . N1 N 0.25384(9) 1.13825(19) 0.16267(15) 0.0221(8) Uani 1 d . . . H1C H 0.2321 1.1163 0.1633 0.050 Uiso 1 d . . . N2 N 0.26141(11) 1.1435(2) -0.00468(16) 0.0323(9) Uani 1 d . . . N3 N 0.27392(9) 0.95028(18) 0.11192(14) 0.0194(7) Uani 1 d . . . H3C H 0.2584 0.9453 0.1375 0.050 Uiso 1 d . . . N4 N 0.35675(10) 0.9324(2) 0.21820(16) 0.0311(9) Uani 1 d . . . C1 C 0.18111(11) 1.0259(2) 0.34145(16) 0.0172(8) Uani 1 d . . . C2 C 0.14791(11) 1.0220(2) 0.37938(17) 0.0209(9) Uani 1 d . . . H2 H 0.1488 0.9912 0.4140 0.025 Uiso 1 calc R . . C3 C 0.11352(11) 1.0622(2) 0.36758(17) 0.0206(9) Uani 1 d . . . C4 C 0.11339(11) 1.1077(2) 0.31504(17) 0.0200(9) Uani 1 d . . . H4 H 0.0905 1.1348 0.3059 0.024 Uiso 1 calc R . . C5 C 0.14562(10) 1.1145(2) 0.27603(17) 0.0164(8) Uani 1 d . . . C6 C 0.17951(10) 1.0744(2) 0.29116(16) 0.0161(8) Uani 1 d . . . C7 C 0.14274(11) 1.1631(2) 0.21838(16) 0.0176(8) Uani 1 d . . . H7A H 0.1314 1.2113 0.2294 0.021 Uiso 1 calc R . . H7B H 0.1692 1.1719 0.2024 0.021 Uiso 1 calc R . . C8 C 0.11762(10) 1.12757(19) 0.16835(16) 0.0147(8) Uani 1 d . . . C9 C 0.07813(10) 1.1473(2) 0.16111(17) 0.0163(8) Uani 1 d . . . H9 H 0.0676 1.1836 0.1872 0.020 Uiso 1 calc R . . C10 C 0.05344(11) 1.1153(2) 0.11664(17) 0.0182(8) Uani 1 d . . . C11 C 0.07070(10) 1.0620(2) 0.07825(17) 0.0167(8) Uani 1 d . . . H11 H 0.0551 1.0398 0.0480 0.020 Uiso 1 calc R . . C12 C 0.11044(10) 1.04009(19) 0.08296(16) 0.0137(8) Uani 1 d . . . C13 C 0.13371(10) 1.0739(2) 0.12860(17) 0.0160(8) Uani 1 d . . . C14 C 0.12658(10) 0.9801(2) 0.04026(16) 0.0147(8) Uani 1 d . . . H14A H 0.1092 0.9754 0.0048 0.018 Uiso 1 calc R . . H14B H 0.1525 0.9954 0.0254 0.018 Uiso 1 calc R . . C15 C 0.13019(10) 0.9045(2) 0.07165(15) 0.0132(8) Uani 1 d . . . C16 C 0.09744(10) 0.8578(2) 0.07562(16) 0.0160(8) Uani 1 d . . . H16 H 0.0738 0.8730 0.0576 0.019 Uiso 1 calc R . . C17 C 0.09886(11) 0.7889(2) 0.10579(16) 0.0176(8) Uani 1 d . . . C18 C 0.13418(10) 0.7703(2) 0.13547(16) 0.0159(8) Uani 1 d . . . H18 H 0.1354 0.7257 0.1577 0.019 Uiso 1 calc R . . C19 C 0.16744(10) 0.8152(2) 0.13324(16) 0.0156(8) Uani 1 d . . . C20 C 0.16542(10) 0.8808(2) 0.09857(16) 0.0123(8) Uani 1 d . . . C21 C 0.20411(10) 0.7935(2) 0.17029(17) 0.0178(8) Uani 1 d . . . H21A H 0.2088 0.7402 0.1653 0.021 Uiso 1 calc R . . H21B H 0.2269 0.8199 0.1537 0.021 Uiso 1 calc R . . C22 C 0.20057(10) 0.8111(2) 0.23885(17) 0.0161(8) Uani 1 d . . . C23 C 0.18570(10) 0.7575(2) 0.27953(17) 0.0182(8) Uani 1 d . . . H23 H 0.1787 0.7106 0.2642 0.022 Uiso 1 calc R . . C24 C 0.18095(10) 0.7715(2) 0.34261(17) 0.0185(9) Uani 1 d . . . C25 C 0.19214(10) 0.8412(2) 0.36409(17) 0.0188(9) Uani 1 d . . . H25 H 0.1899 0.8511 0.4061 0.023 Uiso 1 calc R . . C26 C 0.20669(10) 0.8972(2) 0.32557(16) 0.0161(8) Uani 1 d . . . C27 C 0.21068(10) 0.8812(2) 0.26256(17) 0.0164(8) Uani 1 d . . . C28 C 0.21594(11) 0.9737(2) 0.35176(17) 0.0179(8) Uani 1 d . . . H28A H 0.2393 0.9940 0.3318 0.022 Uiso 1 calc R . . H28B H 0.2213 0.9695 0.3956 0.022 Uiso 1 calc R . . C29 C 0.07686(12) 1.0586(2) 0.4096(2) 0.0292(10) Uani 1 d . . . C30 C 0.07925(13) 0.9930(3) 0.4548(2) 0.0381(12) Uani 1 d . . . H30A H 0.0562 0.9930 0.4808 0.057 Uiso 1 calc R . . H30B H 0.1026 0.9980 0.4798 0.057 Uiso 1 calc R . . H30C H 0.0805 0.9467 0.4322 0.057 Uiso 1 calc R . . C31 C 0.03941(13) 1.0502(3) 0.3709(2) 0.0432(13) Uani 1 d . . . H31A H 0.0410 1.0050 0.3469 0.065 Uiso 1 calc R . . H31B H 0.0369 1.0926 0.3439 0.065 Uiso 1 calc R . . H31C H 0.0168 1.0477 0.3977 0.065 Uiso 1 calc R . . C32 C 0.07473(14) 1.1320(3) 0.4462(2) 0.0400(12) Uani 1 d . . . H32A H 0.0724 1.1735 0.4182 0.060 Uiso 1 calc R . . H32B H 0.0984 1.1376 0.4705 0.060 Uiso 1 calc R . . H32C H 0.0521 1.1309 0.4730 0.060 Uiso 1 calc R . . C33 C 0.01015(11) 1.1394(2) 0.11150(18) 0.0247(9) Uani 1 d . . . C34 C -0.01035(12) 1.1275(3) 0.1739(2) 0.0360(11) Uani 1 d . . . H34A H -0.0376 1.1427 0.1709 0.054 Uiso 1 calc R . . H34B H 0.0028 1.1569 0.2049 0.054 Uiso 1 calc R . . H34C H -0.0091 1.0754 0.1850 0.054 Uiso 1 calc R . . C35 C -0.01215(12) 1.0943(2) 0.0629(2) 0.0302(10) Uani 1 d . . . H35A H -0.0392 1.1111 0.0610 0.045 Uiso 1 calc R . . H35B H -0.0115 1.0421 0.0737 0.045 Uiso 1 calc R . . H35C H 0.0002 1.1013 0.0234 0.045 Uiso 1 calc R . . C36 C 0.00843(12) 1.2228(2) 0.0944(2) 0.0307(10) Uani 1 d . . . H36A H 0.0213 1.2304 0.0554 0.046 Uiso 1 calc R . . H36B H 0.0217 1.2517 0.1256 0.046 Uiso 1 calc R . . H36C H -0.0187 1.2384 0.0916 0.046 Uiso 1 calc R . . C37 C 0.06421(11) 0.7329(2) 0.10501(19) 0.0230(9) Uani 1 d . . . C38 C 0.05402(14) 0.7090(3) 0.1715(2) 0.0442(13) Uani 1 d . . . H38A H 0.0449 0.7518 0.1944 0.066 Uiso 1 calc R . . H38B H 0.0772 0.6887 0.1910 0.066 Uiso 1 calc R . . H38C H 0.0336 0.6715 0.1706 0.066 Uiso 1 calc R . . C39 C 0.02678(13) 0.7661(3) 0.0776(3) 0.0489(14) Uani 1 d . . . H39A H 0.0316 0.7803 0.0355 0.073 Uiso 1 calc R . . H39B H 0.0191 0.8095 0.1009 0.073 Uiso 1 calc R . . H39C H 0.0059 0.7294 0.0789 0.073 Uiso 1 calc R . . C40 C 0.07701(16) 0.6638(3) 0.0691(3) 0.0531(15) Uani 1 d . . . H40A H 0.0565 0.6265 0.0711 0.080 Uiso 1 calc R . . H40B H 0.1009 0.6440 0.0867 0.080 Uiso 1 calc R . . H40C H 0.0817 0.6772 0.0268 0.080 Uiso 1 calc R . . C41 C 0.16422(11) 0.7106(2) 0.38523(19) 0.0245(9) Uani 1 d . . . C42 C 0.12120(12) 0.6932(3) 0.3661(2) 0.0435(13) Uani 1 d . . . H42A H 0.1052 0.7374 0.3709 0.065 Uiso 1 calc R . . H42B H 0.1109 0.6538 0.3916 0.065 Uiso 1 calc R . . H42C H 0.1207 0.6775 0.3237 0.065 Uiso 1 calc R . . C43 C 0.16440(14) 0.7359(3) 0.45275(19) 0.0359(11) Uani 1 d . . . H43A H 0.1912 0.7441 0.4660 0.054 Uiso 1 calc R . . H43B H 0.1525 0.6978 0.4779 0.054 Uiso 1 calc R . . H43C H 0.1496 0.7817 0.4567 0.054 Uiso 1 calc R . . C44 C 0.18856(13) 0.6389(2) 0.3792(2) 0.0317(10) Uani 1 d . . . H44A H 0.1872 0.6211 0.3375 0.048 Uiso 1 calc R . . H44B H 0.1781 0.6014 0.4065 0.048 Uiso 1 calc R . . H44C H 0.2156 0.6491 0.3898 0.048 Uiso 1 calc R . . C45 C 0.24069(11) 1.1361(2) 0.27235(18) 0.0220(9) Uani 1 d . . . H45A H 0.2575 1.1162 0.3048 0.026 Uiso 1 calc R . . H45B H 0.2263 1.1788 0.2889 0.026 Uiso 1 calc R . . C46 C 0.26599(11) 1.1611(2) 0.21885(17) 0.0207(9) Uani 1 d . . . C47 C 0.27024(11) 1.1579(2) 0.10497(18) 0.0226(9) Uani 1 d . . . C48 C 0.25041(12) 1.1299(2) 0.05218(19) 0.0267(10) Uani 1 d . . . H48 H 0.2282 1.1001 0.0583 0.032 Uiso 1 calc R . . C49 C 0.29350(14) 1.1885(2) -0.0136(2) 0.0321(11) Uani 1 d . . . C50 C 0.30469(16) 1.2062(3) -0.0745(2) 0.0445(13) Uani 1 d . . . H50 H 0.2907 1.1856 -0.1075 0.053 Uiso 1 calc R . . C51 C 0.33541(18) 1.2526(3) -0.0856(2) 0.0552(16) Uani 1 d . . . H51 H 0.3424 1.2639 -0.1261 0.066 Uiso 1 calc R . . C52 C 0.35702(17) 1.2840(3) -0.0365(2) 0.0520(15) Uani 1 d . . . H52 H 0.3778 1.3168 -0.0446 0.062 Uiso 1 calc R . . C53 C 0.34752(15) 1.2665(3) 0.0231(2) 0.0421(12) Uani 1 d . . . H53 H 0.3624 1.2863 0.0554 0.051 Uiso 1 calc R . . C54 C 0.31537(13) 1.2186(2) 0.0361(2) 0.0295(10) Uani 1 d . . . C55 C 0.30337(12) 1.2015(2) 0.0970(2) 0.0289(10) Uani 1 d . . . H55 H 0.3176 1.2192 0.1308 0.035 Uiso 1 calc R . . C56 C 0.22372(10) 0.9115(2) 0.03990(17) 0.0190(9) Uani 1 d . . . H56A H 0.2136 0.9391 0.0047 0.023 Uiso 1 calc R . . H56B H 0.2228 0.8584 0.0300 0.023 Uiso 1 calc R . . C57 C 0.26592(11) 0.9344(2) 0.05186(17) 0.0204(9) Uani 1 d . . . C58 C 0.31181(10) 0.9645(2) 0.13636(17) 0.0186(8) Uani 1 d . . . C59 C 0.32211(12) 0.9282(2) 0.19156(18) 0.0247(9) Uani 1 d . . . H59 H 0.3028 0.8990 0.2106 0.030 Uiso 1 calc R . . C60 C 0.38448(11) 0.9785(2) 0.19137(19) 0.0251(9) Uani 1 d . . . C61 C 0.42217(12) 0.9837(3) 0.2190(2) 0.0366(11) Uani 1 d . . . H61 H 0.4278 0.9556 0.2541 0.044 Uiso 1 calc R . . C62 C 0.45023(13) 1.0290(3) 0.1949(2) 0.0439(13) Uani 1 d . . . H62 H 0.4750 1.0324 0.2136 0.053 Uiso 1 calc R . . C63 C 0.44213(13) 1.0711(3) 0.1417(2) 0.0455(13) Uani 1 d . . . H63 H 0.4617 1.1021 0.1254 0.055 Uiso 1 calc R . . C64 C 0.40621(13) 1.0674(3) 0.1137(2) 0.0359(11) Uani 1 d . . . H64 H 0.4012 1.0965 0.0789 0.043 Uiso 1 calc R . . C65 C 0.37636(11) 1.0194(2) 0.13701(18) 0.0232(9) Uani 1 d . . . C66 C 0.33915(11) 1.0104(2) 0.10894(18) 0.0220(9) Uani 1 d . . . H66 H 0.3332 1.0352 0.0723 0.026 Uiso 1 calc R . . N5 N 0.06513(9) 0.89811(19) 0.24901(15) 0.0240(8) Uani 1 d . . . O7 O 0.01127(10) 0.9266(2) 0.19063(17) 0.0526(10) Uani 1 d . . . C67 C 0.04396(15) 0.8498(3) 0.2908(2) 0.0429(12) Uani 1 d . . . H67A H 0.0440 0.8715 0.3314 0.064 Uiso 1 calc R . . H67B H 0.0566 0.8016 0.2921 0.064 Uiso 1 calc R . . H67C H 0.0171 0.8440 0.2768 0.064 Uiso 1 calc R . . C68 C 0.10756(12) 0.9056(3) 0.2571(2) 0.0370(11) Uani 1 d . . . H68A H 0.1179 0.9395 0.2266 0.056 Uiso 1 calc R . . H68B H 0.1199 0.8574 0.2524 0.056 Uiso 1 calc R . . H68C H 0.1130 0.9249 0.2975 0.056 Uiso 1 calc R . . C69 C 0.04623(12) 0.9332(3) 0.2029(2) 0.0305(10) Uani 1 d . . . H69 H 0.0611 0.9653 0.1783 0.037 Uiso 1 calc R . . N6 N 0.10898(14) 0.3991(3) 0.3298(2) 0.0564(13) Uani 1 d . . . O8 O 0.17377(13) 0.4402(3) 0.3183(2) 0.0769(13) Uani 1 d . . . C70 C 0.0993(3) 0.4549(4) 0.3741(3) 0.098(3) Uani 1 d . . . H70A H 0.1229 0.4704 0.3954 0.147 Uiso 1 calc R . . H70B H 0.0807 0.4348 0.4033 0.147 Uiso 1 calc R . . H70C H 0.0877 0.4974 0.3537 0.147 Uiso 1 calc R . . C71 C 0.07958(18) 0.3431(4) 0.3121(3) 0.0708(18) Uani 1 d . . . H71A H 0.0893 0.3148 0.2775 0.106 Uiso 1 calc R . . H71B H 0.0553 0.3677 0.3009 0.106 Uiso 1 calc R . . H71C H 0.0748 0.3099 0.3462 0.106 Uiso 1 calc R . . C72 C 0.14515(18) 0.3977(4) 0.3040(3) 0.0581(15) Uani 1 d . . . H72 H 0.1495 0.3626 0.2730 0.070 Uiso 1 calc R . . O9 O 0.20132(12) 0.4542(2) 0.44181(18) 0.0526(10) Uani 1 d . . . H9C H 0.2236(17) 0.413(3) 0.438(3) 0.069(18) Uiso 1 d . . . H9D H 0.2013(19) 0.437(4) 0.396(3) 0.09(2) Uiso 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 0.0193(13) 0.0179(14) 0.0139(13) -0.0031(11) -0.0007(10) -0.0065(10) O2 0.0264(15) 0.0383(18) 0.0269(16) -0.0063(14) 0.0027(12) -0.0147(14) O3 0.0170(13) 0.0201(15) 0.0202(15) -0.0076(12) -0.0035(11) 0.0002(11) O4 0.0167(13) 0.0191(14) 0.0092(13) -0.0014(11) 0.0014(10) -0.0025(10) O5 0.0232(14) 0.048(2) 0.0180(15) -0.0054(14) 0.0048(12) -0.0064(13) O6 0.0271(14) 0.0182(15) 0.0151(14) 0.0016(12) 0.0034(11) -0.0020(12) N1 0.0211(16) 0.0261(19) 0.0192(18) -0.0017(15) -0.0002(14) -0.0086(14) N2 0.046(2) 0.030(2) 0.021(2) 0.0005(17) 0.0008(16) -0.0029(17) N3 0.0192(16) 0.0283(19) 0.0108(16) 0.0013(14) 0.0035(13) -0.0034(14) N4 0.0295(19) 0.040(2) 0.0235(19) 0.0043(17) -0.0064(16) 0.0003(17) C1 0.0209(19) 0.022(2) 0.0087(18) -0.0057(16) -0.0016(15) -0.0052(16) C2 0.028(2) 0.022(2) 0.012(2) 0.0024(17) -0.0017(16) -0.0021(17) C3 0.025(2) 0.024(2) 0.013(2) -0.0043(18) -0.0010(16) 0.0004(17) C4 0.022(2) 0.019(2) 0.018(2) -0.0063(17) -0.0033(16) 0.0013(16) C5 0.0223(19) 0.0129(19) 0.0140(19) -0.0063(16) -0.0035(15) -0.0042(15) C6 0.0215(19) 0.015(2) 0.0118(19) -0.0032(16) -0.0005(15) -0.0073(16) C7 0.0219(19) 0.016(2) 0.015(2) 0.0009(16) 0.0005(15) 0.0003(16) C8 0.025(2) 0.0072(18) 0.0121(19) 0.0023(15) 0.0000(15) -0.0030(15) C9 0.025(2) 0.0113(19) 0.0123(19) 0.0025(16) 0.0013(16) 0.0043(15) C10 0.025(2) 0.017(2) 0.0125(19) 0.0055(16) -0.0016(16) 0.0007(16) C11 0.0193(19) 0.018(2) 0.0126(19) 0.0029(16) -0.0049(15) -0.0036(16) C12 0.0241(19) 0.0086(19) 0.0085(18) 0.0049(15) 0.0005(15) -0.0036(15) C13 0.0209(19) 0.013(2) 0.0141(19) 0.0032(16) -0.0011(15) -0.0027(15) C14 0.0165(18) 0.021(2) 0.0061(17) -0.0005(16) -0.0025(14) -0.0020(15) C15 0.0174(18) 0.0146(19) 0.0076(18) -0.0032(15) 0.0030(14) -0.0001(15) C16 0.0178(19) 0.019(2) 0.0111(19) -0.0026(16) -0.0022(15) 0.0027(16) C17 0.025(2) 0.019(2) 0.0087(18) -0.0051(16) 0.0024(15) -0.0010(16) C18 0.0237(19) 0.0101(19) 0.0140(19) 0.0000(16) 0.0007(16) 0.0017(15) C19 0.0208(19) 0.016(2) 0.0098(18) -0.0062(16) 0.0024(15) 0.0027(15) C20 0.0142(17) 0.015(2) 0.0081(18) -0.0067(15) 0.0019(14) -0.0016(15) C21 0.0178(18) 0.018(2) 0.017(2) -0.0007(17) -0.0003(15) 0.0027(16) C22 0.0097(17) 0.023(2) 0.015(2) 0.0028(17) -0.0015(14) 0.0048(15) C23 0.0140(18) 0.018(2) 0.023(2) 0.0026(17) -0.0051(15) 0.0037(15) C24 0.0157(18) 0.023(2) 0.017(2) 0.0101(17) -0.0007(15) 0.0038(16) C25 0.0192(19) 0.027(2) 0.0103(19) 0.0029(17) -0.0027(15) 0.0063(16) C26 0.0142(18) 0.022(2) 0.0122(19) 0.0061(17) -0.0016(14) 0.0043(15) C27 0.0125(17) 0.018(2) 0.018(2) 0.0057(17) -0.0016(15) 0.0013(15) C28 0.0204(19) 0.025(2) 0.0085(19) 0.0011(16) -0.0018(15) -0.0023(16) C29 0.026(2) 0.034(3) 0.027(2) 0.004(2) 0.0073(18) 0.0022(19) C30 0.037(3) 0.039(3) 0.038(3) 0.006(2) 0.021(2) 0.002(2) C31 0.026(2) 0.056(3) 0.047(3) 0.004(3) 0.010(2) -0.001(2) C32 0.052(3) 0.038(3) 0.030(3) -0.001(2) 0.018(2) 0.009(2) C33 0.022(2) 0.028(2) 0.024(2) -0.0026(19) -0.0030(17) 0.0069(17) C34 0.022(2) 0.050(3) 0.035(3) 0.002(2) -0.0002(19) 0.012(2) C35 0.024(2) 0.031(3) 0.036(3) -0.004(2) -0.0062(19) 0.0064(18) C36 0.032(2) 0.031(3) 0.029(2) 0.000(2) -0.0125(19) 0.0075(19) C37 0.022(2) 0.018(2) 0.029(2) -0.0032(18) 0.0008(17) -0.0063(16) C38 0.042(3) 0.054(3) 0.037(3) 0.006(2) -0.001(2) -0.023(2) C39 0.030(2) 0.041(3) 0.076(4) 0.020(3) -0.021(2) -0.019(2) C40 0.054(3) 0.042(3) 0.063(4) -0.019(3) 0.010(3) -0.025(3) C41 0.026(2) 0.023(2) 0.024(2) 0.0092(18) -0.0008(17) 0.0016(17) C42 0.027(2) 0.049(3) 0.054(3) 0.027(3) 0.003(2) -0.009(2) C43 0.049(3) 0.034(3) 0.025(2) 0.013(2) 0.012(2) 0.005(2) C44 0.043(3) 0.027(2) 0.025(2) 0.009(2) -0.001(2) -0.001(2) C45 0.024(2) 0.023(2) 0.019(2) -0.0058(18) -0.0044(16) -0.0062(17) C46 0.024(2) 0.022(2) 0.016(2) -0.0030(18) 0.0008(16) -0.0020(18) C47 0.026(2) 0.021(2) 0.022(2) -0.0019(18) 0.0050(17) -0.0007(17) C48 0.031(2) 0.025(2) 0.024(2) -0.0049(19) 0.0010(18) -0.0016(18) C49 0.051(3) 0.022(2) 0.024(2) -0.0052(19) 0.010(2) -0.002(2) C50 0.077(4) 0.029(3) 0.027(3) -0.003(2) 0.010(2) -0.006(3) C51 0.104(5) 0.033(3) 0.028(3) -0.001(2) 0.027(3) -0.014(3) C52 0.080(4) 0.033(3) 0.043(3) -0.006(2) 0.033(3) -0.018(3) C53 0.056(3) 0.034(3) 0.037(3) -0.011(2) 0.020(2) -0.010(2) C54 0.040(2) 0.018(2) 0.030(2) -0.0028(19) 0.014(2) 0.0010(19) C55 0.032(2) 0.027(2) 0.028(2) -0.010(2) 0.0056(19) -0.0041(19) C56 0.023(2) 0.025(2) 0.0087(18) -0.0039(17) 0.0035(15) -0.0012(17) C57 0.023(2) 0.025(2) 0.013(2) -0.0001(17) 0.0061(17) 0.0012(17) C58 0.0167(19) 0.019(2) 0.020(2) -0.0045(17) 0.0022(16) 0.0009(16) C59 0.027(2) 0.027(2) 0.020(2) 0.0031(19) 0.0000(17) -0.0032(18) C60 0.025(2) 0.027(2) 0.023(2) -0.0072(19) -0.0032(17) 0.0018(18) C61 0.026(2) 0.047(3) 0.036(3) -0.008(2) -0.012(2) 0.003(2) C62 0.025(2) 0.060(3) 0.046(3) -0.015(3) -0.011(2) -0.006(2) C63 0.028(2) 0.054(3) 0.054(3) -0.012(3) 0.005(2) -0.016(2) C64 0.035(3) 0.038(3) 0.035(3) -0.002(2) 0.004(2) -0.008(2) C65 0.022(2) 0.027(2) 0.021(2) -0.0083(18) 0.0012(17) -0.0004(17) C66 0.027(2) 0.020(2) 0.019(2) -0.0018(18) 0.0002(17) -0.0010(17) N5 0.0200(16) 0.029(2) 0.0231(18) 0.0023(16) 0.0013(14) 0.0039(14) O7 0.036(2) 0.070(3) 0.051(2) 0.005(2) -0.0047(17) 0.0065(18) C67 0.057(3) 0.035(3) 0.037(3) 0.011(2) 0.007(2) 0.003(2) C68 0.028(2) 0.041(3) 0.041(3) -0.012(2) -0.004(2) 0.007(2) C69 0.026(2) 0.037(3) 0.029(2) 0.004(2) 0.0042(19) 0.0017(19) N6 0.065(3) 0.051(3) 0.054(3) -0.011(2) -0.014(2) 0.029(2) O8 0.078(3) 0.068(3) 0.085(3) 0.002(3) -0.027(3) 0.001(2) C70 0.148(7) 0.085(6) 0.060(4) -0.026(4) -0.008(5) 0.057(5) C71 0.063(4) 0.071(4) 0.079(5) 0.017(4) -0.005(3) 0.024(3) C72 0.058(4) 0.059(4) 0.057(4) 0.000(3) -0.013(3) 0.019(3) O9 0.063(2) 0.049(2) 0.045(2) -0.0005(19) -0.0057(19) 0.0078(19) _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 C6 1.410(4) . ? O1 C45 1.429(4) . ? O2 C46 1.219(4) . ? O3 C13 1.369(4) . ? O3 H3 0.8200 . ? O4 C20 1.403(4) . ? O4 C56 1.433(4) . ? O5 C57 1.214(4) . ? O6 C27 1.375(4) . ? O6 H6 0.8200 . ? N1 C46 1.347(5) . ? N1 C47 1.411(5) . ? N1 H1C 0.832(3) . ? N2 C48 1.309(5) . ? N2 C49 1.361(6) . ? N3 C57 1.359(5) . ? N3 C58 1.407(5) . ? N3 H3C 0.768(3) . ? N4 C59 1.306(5) . ? N4 C60 1.373(5) . ? C1 C2 1.391(5) . ? C1 C6 1.392(5) . ? C1 C28 1.515(5) . ? C2 C3 1.387(5) . ? C2 H2 0.9300 . ? C3 C4 1.398(6) . ? C3 C29 1.538(5) . ? C4 C5 1.383(5) . ? C4 H4 0.9300 . ? C5 C6 1.387(5) . ? C5 C7 1.523(5) . ? C7 C8 1.515(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.387(5) . ? C8 C13 1.397(5) . ? C9 C10 1.396(5) . ? C9 H9 0.9300 . ? C10 C11 1.391(5) . ? C10 C33 1.527(5) . ? C11 C12 1.400(5) . ? C11 H11 0.9300 . ? C12 C13 1.399(5) . ? C12 C14 1.515(5) . ? C14 C15 1.514(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.386(5) . ? C15 C20 1.390(5) . ? C16 C17 1.392(5) . ? C16 H16 0.9300 . ? C17 C18 1.394(5) . ? C17 C37 1.537(5) . ? C18 C19 1.380(5) . ? C18 H18 0.9300 . ? C19 C20 1.391(5) . ? C19 C21 1.525(5) . ? C21 C22 1.523(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.393(5) . ? C22 C23 1.393(5) . ? C23 C24 1.399(5) . ? C23 H23 0.9300 . ? C24 C25 1.379(6) . ? C24 C41 1.533(5) . ? C25 C26 1.391(5) . ? C25 H25 0.9300 . ? C26 C27 1.401(5) . ? C26 C28 1.509(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C31 1.523(6) . ? C29 C30 1.527(6) . ? C29 C32 1.532(6) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C35 1.523(6) . ? C33 C36 1.532(6) . ? C33 C34 1.533(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C39 1.516(6) . ? C37 C40 1.520(6) . ? C37 C38 1.541(6) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C44 1.524(6) . ? C41 C43 1.531(6) . ? C41 C42 1.541(6) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.507(5) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C47 C55 1.372(6) . ? C47 C48 1.416(6) . ? C48 H48 0.9300 . ? C49 C50 1.409(6) . ? C49 C54 1.411(6) . ? C50 C51 1.348(7) . ? C50 H50 0.9300 . ? C51 C52 1.407(8) . ? C51 H51 0.9300 . ? C52 C53 1.367(7) . ? C52 H52 0.9300 . ? C53 C54 1.409(6) . ? C53 H53 0.9300 . ? C54 C55 1.414(6) . ? C55 H55 0.9300 . ? C56 C57 1.504(5) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C58 C66 1.368(5) . ? C58 C59 1.403(6) . ? C59 H59 0.9300 . ? C60 C61 1.409(6) . ? C60 C65 1.412(6) . ? C61 C62 1.350(7) . ? C61 H61 0.9300 . ? C62 C63 1.402(7) . ? C62 H62 0.9300 . ? C63 C64 1.357(6) . ? C63 H63 0.9300 . ? C64 C65 1.415(6) . ? C64 H64 0.9300 . ? C65 C66 1.404(5) . ? C66 H66 0.9300 . ? N5 C69 1.340(5) . ? N5 C67 1.440(5) . ? N5 C68 1.448(5) . ? O7 C69 1.215(5) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 H69 0.9300 . ? N6 C72 1.343(7) . ? N6 C70 1.421(7) . ? N6 C71 1.459(8) . ? O8 C72 1.266(7) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 H72 0.9300 . ? O9 H9C 1.05(6) . ? O9 H9D 1.03(7) . ? 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 O1 C45 113.5(3) . . ? C13 O3 H3 109.5 . . ? C20 O4 C56 115.9(3) . . ? C27 O6 H6 109.5 . . ? C46 N1 C47 127.3(3) . . ? C46 N1 H1C 113.4(3) . . ? C47 N1 H1C 118.4(3) . . ? C48 N2 C49 117.9(4) . . ? C57 N3 C58 125.4(3) . . ? C57 N3 H3C 122.1(3) . . ? C58 N3 H3C 111.7(3) . . ? C59 N4 C60 117.2(3) . . ? C2 C1 C6 117.5(3) . . ? C2 C1 C28 120.5(3) . . ? C6 C1 C28 121.8(3) . . ? C3 C2 C1 122.6(4) . . ? C3 C2 H2 118.7 . . ? C1 C2 H2 118.7 . . ? C2 C3 C4 116.9(3) . . ? C2 C3 C29 122.8(3) . . ? C4 C3 C29 120.3(3) . . ? C5 C4 C3 123.1(3) . . ? C5 C4 H4 118.5 . . ? C3 C4 H4 118.5 . . ? C4 C5 C6 117.3(3) . . ? C4 C5 C7 120.1(3) . . ? C6 C5 C7 122.6(3) . . ? C5 C6 C1 122.5(3) . . ? C5 C6 O1 119.4(3) . . ? C1 C6 O1 118.1(3) . . ? C8 C7 C5 112.6(3) . . ? C8 C7 H7A 109.1 . . ? C5 C7 H7A 109.1 . . ? C8 C7 H7B 109.1 . . ? C5 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C13 118.5(3) . . ? C9 C8 C7 120.8(3) . . ? C13 C8 C7 120.7(3) . . ? C8 C9 C10 123.2(3) . . ? C8 C9 H9 118.4 . . ? C10 C9 H9 118.4 . . ? C11 C10 C9 116.2(3) . . ? C11 C10 C33 123.3(3) . . ? C9 C10 C33 120.4(3) . . ? C10 C11 C12 123.2(3) . . ? C10 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C13 C12 C11 118.0(3) . . ? C13 C12 C14 122.3(3) . . ? C11 C12 C14 119.7(3) . . ? O3 C13 C8 116.7(3) . . ? O3 C13 C12 122.5(3) . . ? C8 C13 C12 120.8(3) . . ? C15 C14 C12 112.5(3) . . ? C15 C14 H14A 109.1 . . ? C12 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C12 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C20 118.3(3) . . ? C16 C15 C14 119.9(3) . . ? C20 C15 C14 121.8(3) . . ? C15 C16 C17 122.1(3) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C16 C17 C18 117.1(3) . . ? C16 C17 C37 122.8(3) . . ? C18 C17 C37 120.0(3) . . ? C19 C18 C17 122.7(3) . . ? C19 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? C18 C19 C20 117.9(3) . . ? C18 C19 C21 119.6(3) . . ? C20 C19 C21 122.5(3) . . ? C15 C20 C19 121.6(3) . . ? C15 C20 O4 118.9(3) . . ? C19 C20 O4 119.4(3) . . ? C22 C21 C19 113.4(3) . . ? C22 C21 H21A 108.9 . . ? C19 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? C19 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C27 C22 C23 118.0(3) . . ? C27 C22 C21 121.7(3) . . ? C23 C22 C21 120.3(3) . . ? C22 C23 C24 122.5(4) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C25 C24 C23 117.3(3) . . ? C25 C24 C41 122.4(3) . . ? C23 C24 C41 120.3(4) . . ? C24 C25 C26 122.7(3) . . ? C24 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C25 C26 C27 118.1(4) . . ? C25 C26 C28 119.7(3) . . ? C27 C26 C28 122.1(3) . . ? O6 C27 C22 116.8(3) . . ? O6 C27 C26 121.9(3) . . ? C22 C27 C26 121.3(3) . . ? C26 C28 C1 109.8(3) . . ? C26 C28 H28A 109.7 . . ? C1 C28 H28A 109.7 . . ? C26 C28 H28B 109.7 . . ? C1 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C31 C29 C30 108.7(4) . . ? C31 C29 C32 109.3(4) . . ? C30 C29 C32 108.9(4) . . ? C31 C29 C3 110.2(3) . . ? C30 C29 C3 111.7(3) . . ? C32 C29 C3 108.0(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C10 112.0(3) . . ? C35 C33 C36 109.0(3) . . ? C10 C33 C36 109.1(3) . . ? C35 C33 C34 108.3(4) . . ? C10 C33 C34 109.2(3) . . ? C36 C33 C34 109.3(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C40 110.6(4) . . ? C39 C37 C17 112.6(3) . . ? C40 C37 C17 108.4(3) . . ? C39 C37 C38 106.8(4) . . ? C40 C37 C38 108.5(4) . . ? C17 C37 C38 109.8(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C44 C41 C43 109.1(3) . . ? C44 C41 C24 110.1(3) . . ? C43 C41 C24 111.4(3) . . ? C44 C41 C42 108.4(4) . . ? C43 C41 C42 108.7(4) . . ? C24 C41 C42 109.1(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O1 C45 C46 110.4(3) . . ? O1 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? O1 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? O2 C46 N1 124.9(4) . . ? O2 C46 C45 119.3(3) . . ? N1 C46 C45 115.7(3) . . ? C55 C47 N1 124.8(4) . . ? C55 C47 C48 118.9(4) . . ? N1 C47 C48 116.3(3) . . ? N2 C48 C47 124.2(4) . . ? N2 C48 H48 117.9 . . ? C47 C48 H48 117.9 . . ? N2 C49 C50 118.5(4) . . ? N2 C49 C54 122.1(4) . . ? C50 C49 C54 119.3(4) . . ? C51 C50 C49 120.7(5) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C52 120.5(5) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C53 C52 C51 120.2(5) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C52 C53 C54 120.5(5) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C53 C54 C49 118.7(4) . . ? C53 C54 C55 122.5(4) . . ? C49 C54 C55 118.7(4) . . ? C47 C55 C54 118.2(4) . . ? C47 C55 H55 120.9 . . ? C54 C55 H55 120.9 . . ? O4 C56 C57 111.0(3) . . ? O4 C56 H56A 109.4 . . ? C57 C56 H56A 109.4 . . ? O4 C56 H56B 109.4 . . ? C57 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? O5 C57 N3 124.4(3) . . ? O5 C57 C56 121.3(3) . . ? N3 C57 C56 114.2(3) . . ? C66 C58 C59 118.6(3) . . ? C66 C58 N3 123.8(3) . . ? C59 C58 N3 117.6(3) . . ? N4 C59 C58 124.9(4) . . ? N4 C59 H59 117.6 . . ? C58 C59 H59 117.6 . . ? N4 C60 C61 118.3(4) . . ? N4 C60 C65 122.0(3) . . ? C61 C60 C65 119.7(4) . . ? C62 C61 C60 120.6(5) . . ? C62 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? C61 C62 C63 120.1(4) . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C64 C63 C62 121.1(4) . . ? C64 C63 H63 119.5 . . ? C62 C63 H63 119.5 . . ? C63 C64 C65 120.3(5) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? C66 C65 C60 118.4(4) . . ? C66 C65 C64 123.4(4) . . ? C60 C65 C64 118.2(4) . . ? C58 C66 C65 118.9(4) . . ? C58 C66 H66 120.6 . . ? C65 C66 H66 120.6 . . ? C69 N5 C67 120.8(4) . . ? C69 N5 C68 121.1(4) . . ? C67 N5 C68 118.0(4) . . ? N5 C67 H67A 109.5 . . ? N5 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N5 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N5 C68 H68A 109.5 . . ? N5 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? N5 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O7 C69 N5 125.4(4) . . ? O7 C69 H69 117.3 . . ? N5 C69 H69 117.3 . . ? C72 N6 C70 120.2(6) . . ? C72 N6 C71 119.7(5) . . ? C70 N6 C71 120.1(6) . . ? N6 C70 H70A 109.5 . . ? N6 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N6 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N6 C71 H71A 109.5 . . ? N6 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N6 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O8 C72 N6 125.4(6) . . ? O8 C72 H72 117.3 . . ? N6 C72 H72 117.3 . . ? H9C O9 H9D 74(4) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.654 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.098 #===END data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 775958' #TrackingRef '- CIF_revised_compounds 1 to 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H42 Cl6 N4 O6' _chemical_formula_weight 1031.60 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1151(18) _cell_length_b 12.632(2) _cell_length_c 20.705(4) _cell_angle_alpha 106.850(3) _cell_angle_beta 90.681(3) _cell_angle_gamma 103.566(3) _cell_volume 2452.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4740 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.94 _exptl_crystal_description BLOCKS _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7564 _exptl_absorpt_correction_T_max 0.9492 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17449 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8534 _reflns_number_gt 5934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.1240P)^2^+2.0889P] 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 8534 _refine_ls_number_parameters 645 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0880 _refine_ls_wR_factor_ref 0.2498 _refine_ls_wR_factor_gt 0.2291 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.5882(2) 0.2919(2) 0.12239(13) 0.0481(6) Uani 1 d . . . O2 O 0.3089(3) 0.1786(3) 0.07597(13) 0.0635(8) Uani 1 d . . . H2 H 0.2539 0.2042 0.1008 0.095 Uiso 1 calc R . . O3 O 0.1586(2) 0.2737(2) 0.17602(12) 0.0454(6) Uani 1 d . . . O4 O 0.4283(3) 0.4149(2) 0.20053(14) 0.0486(7) Uani 1 d . . . H4 H 0.4829 0.3865 0.1768 0.073 Uiso 1 calc R . . O5 O 0.7076(3) 0.1550(3) 0.22699(18) 0.0739(9) Uani 1 d . . . O6 O 0.0776(3) 0.1708(3) 0.31631(17) 0.0781(10) Uani 1 d . . . N1 N 0.4978(3) 0.1307(3) 0.17500(18) 0.0568(9) Uani 1 d . . . H1C H 0.4588 0.1470 0.1433 0.068 Uiso 1 calc R . . N2 N 0.1857(4) -0.0606(4) 0.1999(2) 0.0762(11) Uani 1 d . . . N3 N 0.2715(3) 0.2823(3) 0.29524(15) 0.0426(7) Uani 1 d . . . H3C H 0.3083 0.3103 0.2646 0.051 Uiso 1 calc R . . N4 N 0.5779(4) 0.4052(3) 0.41097(19) 0.0648(10) Uani 1 d . . . C1 C 0.6643(4) 0.4640(4) 0.0927(2) 0.0476(9) Uani 1 d . . . C2 C 0.6849(4) 0.5187(4) 0.0426(2) 0.0573(11) Uani 1 d . . . H2A H 0.7186 0.5976 0.0548 0.069 Uiso 1 calc R . . C3 C 0.6559(4) 0.4572(5) -0.0244(2) 0.0667(13) Uani 1 d . . . H3 H 0.6725 0.4944 -0.0573 0.080 Uiso 1 calc R . . C4 C 0.6026(5) 0.3415(5) -0.0434(2) 0.0697(13) Uani 1 d . . . H4A H 0.5824 0.3015 -0.0892 0.084 Uiso 1 calc R . . C5 C 0.5777(4) 0.2820(4) 0.0048(2) 0.0569(11) Uani 1 d . . . C6 C 0.6139(4) 0.3457(4) 0.07173(19) 0.0468(9) Uani 1 d . . . C7 C 0.5061(5) 0.1562(4) -0.0164(2) 0.0696(13) Uani 1 d . . . H7A H 0.5500 0.1157 -0.0537 0.084 Uiso 1 calc R . . H7B H 0.5147 0.1261 0.0211 0.084 Uiso 1 calc R . . C8 C 0.3563(5) 0.1351(4) -0.0380(2) 0.0626(12) Uani 1 d . . . C9 C 0.3087(6) 0.1024(4) -0.1063(2) 0.0761(15) Uani 1 d . . . H9 H 0.3690 0.0873 -0.1393 0.091 Uiso 1 calc R . . C10 C 0.1755(6) 0.0921(4) -0.1257(2) 0.0832(17) Uani 1 d . . . H10 H 0.1462 0.0694 -0.1714 0.100 Uiso 1 calc R . . C11 C 0.0852(5) 0.1149(4) -0.0781(2) 0.0762(15) Uani 1 d . . . H11 H -0.0043 0.1105 -0.0919 0.091 Uiso 1 calc R . . C12 C 0.1251(4) 0.1446(4) -0.0091(2) 0.0607(12) Uani 1 d . . . C13 C 0.2610(4) 0.1529(3) 0.00976(19) 0.0553(10) Uani 1 d . . . C14 C 0.0225(4) 0.1658(4) 0.0432(2) 0.0665(13) Uani 1 d . . . H14A H -0.0689 0.1338 0.0207 0.080 Uiso 1 calc R . . H14B H 0.0326 0.1259 0.0759 0.080 Uiso 1 calc R . . C15 C 0.0379(4) 0.2903(4) 0.0805(2) 0.0562(11) Uani 1 d . . . C16 C -0.0133(4) 0.3598(5) 0.0502(2) 0.0699(14) Uani 1 d . . . H16 H -0.0604 0.3277 0.0075 0.084 Uiso 1 calc R . . C17 C 0.0045(5) 0.4740(6) 0.0822(3) 0.0725(15) Uani 1 d . . . H17 H -0.0319 0.5184 0.0617 0.087 Uiso 1 calc R . . C18 C 0.0761(5) 0.5227(5) 0.1445(2) 0.0659(13) Uani 1 d . . . H18 H 0.0885 0.6006 0.1653 0.079 Uiso 1 calc R . . C19 C 0.1311(4) 0.4589(4) 0.1778(2) 0.0510(10) Uani 1 d . . . C20 C 0.1060(3) 0.3423(4) 0.1450(2) 0.0481(10) Uani 1 d . . . C21 C 0.2165(4) 0.5180(4) 0.2436(2) 0.0539(10) Uani 1 d . . . H21A H 0.2272 0.4617 0.2654 0.065 Uiso 1 calc R . . H21B H 0.1703 0.5697 0.2732 0.065 Uiso 1 calc R . . C22 C 0.3562(4) 0.5845(3) 0.23345(18) 0.0490(10) Uani 1 d . . . C23 C 0.3845(5) 0.7026(4) 0.2462(2) 0.0623(12) Uani 1 d . . . H23 H 0.3183 0.7410 0.2631 0.075 Uiso 1 calc R . . C24 C 0.5075(6) 0.7626(4) 0.2342(2) 0.0712(13) Uani 1 d . . . H24 H 0.5245 0.8412 0.2429 0.085 Uiso 1 calc R . . C25 C 0.6061(5) 0.7073(4) 0.2095(2) 0.0619(12) Uani 1 d . . . H25 H 0.6895 0.7495 0.2017 0.074 Uiso 1 calc R . . C26 C 0.5849(4) 0.5900(3) 0.19586(18) 0.0446(9) Uani 1 d . . . C27 C 0.4589(4) 0.5302(3) 0.20923(17) 0.0409(8) Uani 1 d . . . C28 C 0.6937(4) 0.5315(4) 0.1666(2) 0.0516(10) Uani 1 d . . . H28A H 0.7053 0.4804 0.1922 0.062 Uiso 1 calc R . . H28B H 0.7794 0.5887 0.1724 0.062 Uiso 1 calc R . . C29 C 0.6940(4) 0.2468(4) 0.1424(2) 0.0568(11) Uani 1 d . . . H29A H 0.7699 0.3086 0.1673 0.068 Uiso 1 calc R . . H29B H 0.7271 0.2012 0.1027 0.068 Uiso 1 calc R . . C30 C 0.6346(4) 0.1731(3) 0.1870(2) 0.0530(10) Uani 1 d . . . C31 C 0.4118(4) 0.0625(3) 0.2088(2) 0.0511(10) Uani 1 d . . . C32 C 0.2834(5) 0.0010(4) 0.1745(3) 0.0662(12) Uani 1 d . . . H32 H 0.2660 0.0040 0.1310 0.079 Uiso 1 calc R . . C33 C 0.2150(5) -0.0657(4) 0.2637(3) 0.0692(13) Uani 1 d . . . C34 C 0.1114(6) -0.1306(5) 0.2926(4) 0.0914(17) Uani 1 d . . . H34 H 0.0273 -0.1686 0.2684 0.110 Uiso 1 calc R . . C35 C 0.1361(8) -0.1367(6) 0.3558(4) 0.104(2) Uani 1 d . . . H35 H 0.0678 -0.1781 0.3749 0.125 Uiso 1 calc R . . C36 C 0.2620(8) -0.0820(6) 0.3924(3) 0.102(2) Uani 1 d . . . H36 H 0.2777 -0.0885 0.4353 0.122 Uiso 1 calc R . . C37 C 0.3625(6) -0.0189(5) 0.3658(3) 0.0822(15) Uani 1 d . . . H37 H 0.4459 0.0180 0.3910 0.099 Uiso 1 calc R . . C38 C 0.3415(5) -0.0090(4) 0.3009(2) 0.0595(11) Uani 1 d . . . C39 C 0.4408(5) 0.0561(3) 0.2715(2) 0.0569(11) Uani 1 d . . . H39 H 0.5258 0.0944 0.2948 0.068 Uiso 1 calc R . . C40 C 0.0693(4) 0.2188(4) 0.2166(2) 0.0552(11) Uani 1 d . . . H40A H 0.0296 0.1400 0.1904 0.066 Uiso 1 calc R . . H40B H -0.0046 0.2563 0.2274 0.066 Uiso 1 calc R . . C41 C 0.1402(4) 0.2215(3) 0.2806(2) 0.0482(9) Uani 1 d . . . C42 C 0.3550(4) 0.3048(3) 0.35483(18) 0.0419(8) Uani 1 d . . . C43 C 0.4874(4) 0.3754(4) 0.3597(2) 0.0558(11) Uani 1 d . . . H43 H 0.5121 0.4029 0.3233 0.067 Uiso 1 calc R . . C44 C 0.5421(4) 0.3659(4) 0.4650(2) 0.0548(10) Uani 1 d . . . C45 C 0.6394(5) 0.3963(5) 0.5213(2) 0.0730(13) Uani 1 d . . . H45 H 0.7254 0.4432 0.5215 0.088 Uiso 1 calc R . . C46 C 0.6071(6) 0.3568(5) 0.5748(3) 0.0864(16) Uani 1 d . . . H46 H 0.6705 0.3785 0.6121 0.104 Uiso 1 calc R . . C47 C 0.4812(7) 0.2850(6) 0.5746(3) 0.099(2) Uani 1 d . . . H47 H 0.4616 0.2568 0.6111 0.119 Uiso 1 calc R . . C48 C 0.3850(6) 0.2547(5) 0.5214(3) 0.0903(17) Uani 1 d . . . H48 H 0.2999 0.2077 0.5227 0.108 Uiso 1 calc R . . C49 C 0.4124(4) 0.2933(4) 0.4645(2) 0.0550(10) Uani 1 d . . . C50 C 0.3196(4) 0.2642(4) 0.4078(2) 0.0539(10) Uani 1 d . . . H50 H 0.2333 0.2168 0.4063 0.065 Uiso 1 calc R . . C51 C 0.8468(6) 0.0818(5) 0.3927(3) 0.0917(17) Uani 1 d . . . H51 H 0.8997 0.1127 0.3600 0.110 Uiso 1 calc R . . Cl1 Cl 0.7440(2) 0.17051(18) 0.42642(12) 0.1369(7) Uani 1 d . . . Cl2 Cl 0.9614(2) 0.0792(2) 0.45488(11) 0.1452(8) Uani 1 d . . . Cl3 Cl 0.7516(3) -0.0544(2) 0.34932(17) 0.1835(12) Uani 1 d . . . C52 C 0.8752(7) 0.5233(6) 0.3859(3) 0.124(3) Uani 1 d . . . H52 H 0.7908 0.4888 0.4028 0.149 Uiso 1 calc R A 1 Cl4 Cl 0.9811(6) 0.4122(4) 0.3765(3) 0.160(3) Uani 0.599(8) d P B 1 Cl5 Cl 0.8146(15) 0.6284(9) 0.3388(5) 0.135(4) Uani 0.36(2) d P B 1 Cl6 Cl 0.9602(12) 0.6273(8) 0.4565(4) 0.145(3) Uani 0.55(4) d P B 1 Cl4A Cl 0.8666(10) 0.4108(6) 0.3212(5) 0.180(5) Uani 0.401(8) d P B 2 Cl5A Cl 0.8672(7) 0.5521(16) 0.3172(4) 0.201(8) Uani 0.64(2) d P B 2 Cl6A Cl 1.002(3) 0.609(2) 0.4350(17) 0.206(8) Uani 0.45(4) d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0394(14) 0.0579(16) 0.0564(16) 0.0253(13) 0.0106(12) 0.0193(12) O2 0.0556(18) 0.091(2) 0.0428(16) 0.0142(15) 0.0024(13) 0.0236(16) O3 0.0308(13) 0.0625(17) 0.0473(14) 0.0263(13) 0.0020(11) 0.0076(11) O4 0.0457(15) 0.0407(15) 0.0640(17) 0.0209(13) 0.0191(13) 0.0124(11) O5 0.0535(18) 0.088(2) 0.096(2) 0.049(2) -0.0058(17) 0.0198(16) O6 0.0527(18) 0.111(3) 0.077(2) 0.062(2) -0.0018(16) -0.0090(17) N1 0.0443(19) 0.060(2) 0.075(2) 0.0338(19) 0.0017(17) 0.0132(16) N2 0.055(2) 0.074(3) 0.100(3) 0.033(2) 0.001(2) 0.008(2) N3 0.0386(17) 0.0510(19) 0.0438(17) 0.0242(14) 0.0037(13) 0.0095(14) N4 0.051(2) 0.079(3) 0.062(2) 0.025(2) -0.0070(18) 0.0045(18) C1 0.0291(18) 0.065(3) 0.056(2) 0.029(2) 0.0061(17) 0.0111(17) C2 0.035(2) 0.077(3) 0.068(3) 0.036(2) 0.0059(19) 0.011(2) C3 0.048(2) 0.101(4) 0.062(3) 0.043(3) 0.014(2) 0.017(3) C4 0.050(3) 0.107(4) 0.048(3) 0.020(3) 0.014(2) 0.017(3) C5 0.043(2) 0.078(3) 0.053(2) 0.019(2) 0.0187(19) 0.022(2) C6 0.0319(19) 0.069(3) 0.050(2) 0.027(2) 0.0153(17) 0.0219(18) C7 0.077(3) 0.071(3) 0.053(3) 0.002(2) 0.021(2) 0.025(3) C8 0.076(3) 0.046(2) 0.048(2) -0.0015(19) 0.012(2) -0.001(2) C9 0.104(4) 0.053(3) 0.048(3) -0.001(2) 0.017(3) -0.007(3) C10 0.100(4) 0.071(3) 0.047(3) 0.012(2) -0.010(3) -0.030(3) C11 0.066(3) 0.084(3) 0.052(3) 0.022(2) -0.021(2) -0.032(3) C12 0.056(3) 0.061(3) 0.049(2) 0.017(2) -0.007(2) -0.016(2) C13 0.062(3) 0.050(2) 0.040(2) 0.0064(18) -0.0055(19) -0.003(2) C14 0.038(2) 0.094(4) 0.056(3) 0.032(3) -0.0143(19) -0.018(2) C15 0.0271(19) 0.088(3) 0.054(2) 0.035(2) -0.0005(17) -0.0009(19) C16 0.029(2) 0.124(5) 0.064(3) 0.051(3) 0.0002(19) 0.006(2) C17 0.044(3) 0.124(5) 0.082(4) 0.067(4) 0.019(2) 0.039(3) C18 0.059(3) 0.095(4) 0.071(3) 0.047(3) 0.025(2) 0.044(3) C19 0.041(2) 0.077(3) 0.054(2) 0.035(2) 0.0219(18) 0.030(2) C20 0.0272(18) 0.077(3) 0.051(2) 0.036(2) 0.0099(16) 0.0139(18) C21 0.067(3) 0.064(3) 0.045(2) 0.022(2) 0.019(2) 0.035(2) C22 0.063(3) 0.053(2) 0.039(2) 0.0173(18) 0.0074(18) 0.024(2) C23 0.091(3) 0.051(3) 0.053(2) 0.016(2) 0.015(2) 0.031(2) C24 0.102(4) 0.039(2) 0.071(3) 0.016(2) 0.012(3) 0.017(3) C25 0.071(3) 0.049(3) 0.059(3) 0.019(2) -0.001(2) -0.001(2) C26 0.045(2) 0.046(2) 0.039(2) 0.0154(17) -0.0031(16) 0.0033(17) C27 0.050(2) 0.039(2) 0.0357(19) 0.0149(16) 0.0019(16) 0.0120(17) C28 0.034(2) 0.061(3) 0.059(2) 0.028(2) -0.0041(18) -0.0008(18) C29 0.039(2) 0.066(3) 0.075(3) 0.030(2) 0.007(2) 0.022(2) C30 0.048(2) 0.050(2) 0.066(3) 0.018(2) 0.004(2) 0.0216(19) C31 0.047(2) 0.040(2) 0.068(3) 0.0169(19) 0.003(2) 0.0142(18) C32 0.057(3) 0.061(3) 0.080(3) 0.026(2) -0.002(2) 0.008(2) C33 0.070(3) 0.055(3) 0.095(4) 0.030(3) 0.026(3) 0.028(2) C34 0.073(4) 0.085(4) 0.124(5) 0.041(4) 0.035(3) 0.021(3) C35 0.108(5) 0.097(5) 0.125(6) 0.051(4) 0.062(5) 0.034(4) C36 0.130(6) 0.107(5) 0.089(4) 0.048(4) 0.048(4) 0.045(5) C37 0.104(4) 0.076(3) 0.073(3) 0.027(3) 0.020(3) 0.028(3) C38 0.069(3) 0.044(2) 0.070(3) 0.018(2) 0.015(2) 0.022(2) C39 0.060(3) 0.047(2) 0.067(3) 0.018(2) 0.003(2) 0.017(2) C40 0.036(2) 0.077(3) 0.056(2) 0.035(2) 0.0027(18) 0.0002(19) C41 0.041(2) 0.059(2) 0.050(2) 0.0270(19) 0.0070(17) 0.0079(18) C42 0.042(2) 0.046(2) 0.042(2) 0.0166(17) 0.0034(16) 0.0146(17) C43 0.045(2) 0.074(3) 0.054(2) 0.032(2) 0.0033(19) 0.009(2) C44 0.056(3) 0.057(3) 0.050(2) 0.013(2) -0.0042(19) 0.017(2) C45 0.062(3) 0.086(4) 0.063(3) 0.015(3) -0.011(2) 0.013(3) C46 0.089(4) 0.109(4) 0.055(3) 0.019(3) -0.024(3) 0.022(3) C47 0.111(5) 0.123(5) 0.062(3) 0.047(3) -0.015(3) 0.004(4) C48 0.091(4) 0.112(4) 0.066(3) 0.048(3) -0.009(3) -0.004(3) C49 0.061(3) 0.055(3) 0.048(2) 0.0170(19) 0.000(2) 0.012(2) C50 0.051(2) 0.057(3) 0.052(2) 0.021(2) -0.0012(19) 0.0037(19) C51 0.076(4) 0.106(4) 0.082(4) 0.031(3) 0.016(3) -0.004(3) Cl1 0.1289(16) 0.1153(15) 0.1564(18) 0.0171(13) -0.0046(13) 0.0419(12) Cl2 0.1316(17) 0.202(2) 0.1149(15) 0.0465(15) 0.0110(12) 0.0667(16) Cl3 0.1290(18) 0.1102(16) 0.241(3) -0.0217(17) 0.0159(18) -0.0114(13) C52 0.095(5) 0.130(6) 0.091(4) 0.002(4) 0.027(4) -0.040(4) Cl4 0.200(5) 0.140(3) 0.145(4) 0.039(3) 0.056(4) 0.054(3) Cl5 0.137(7) 0.162(8) 0.108(5) 0.038(5) -0.017(4) 0.044(5) Cl6 0.144(6) 0.130(5) 0.113(4) -0.012(5) -0.021(4) 0.008(4) Cl4A 0.234(10) 0.136(5) 0.172(8) 0.019(5) 0.084(7) 0.082(5) Cl5A 0.134(4) 0.363(18) 0.111(4) 0.122(8) -0.021(3) 0.007(6) Cl6A 0.131(10) 0.259(13) 0.221(13) 0.141(10) -0.101(10) -0.044(8) _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 C6 1.403(4) . ? O1 C29 1.433(4) . ? O2 C13 1.368(5) . ? O2 H2 0.8200 . ? O3 C20 1.406(4) . ? O3 C40 1.437(4) . ? O4 C27 1.373(4) . ? O4 H4 0.8200 . ? O5 C30 1.208(5) . ? O6 C41 1.204(4) . ? N1 C30 1.352(5) . ? N1 C31 1.414(5) . ? N1 H1C 0.8600 . ? N2 C32 1.321(6) . ? N2 C33 1.373(7) . ? N3 C41 1.351(5) . ? N3 C42 1.405(5) . ? N3 H3C 0.8600 . ? N4 C43 1.301(5) . ? N4 C44 1.369(5) . ? C1 C6 1.394(6) . ? C1 C2 1.397(5) . ? C1 C28 1.507(6) . ? C2 C3 1.368(6) . ? C2 H2A 0.9300 . ? C3 C4 1.369(7) . ? C3 H3 0.9300 . ? C4 C5 1.405(6) . ? C4 H4A 0.9300 . ? C5 C6 1.381(6) . ? C5 C7 1.514(7) . ? C7 C8 1.514(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.396(6) . ? C8 C13 1.398(6) . ? C9 C10 1.367(8) . ? C9 H9 0.9300 . ? C10 C11 1.367(8) . ? C10 H10 0.9300 . ? C11 C12 1.395(6) . ? C11 H11 0.9300 . ? C12 C13 1.396(6) . ? C12 C14 1.520(6) . ? C14 C15 1.508(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.394(6) . ? C15 C16 1.399(6) . ? C16 C17 1.369(7) . ? C16 H16 0.9300 . ? C17 C18 1.369(7) . ? C17 H17 0.9300 . ? C18 C19 1.400(6) . ? C18 H18 0.9300 . ? C19 C20 1.391(6) . ? C19 C21 1.496(6) . ? C21 C22 1.516(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.395(6) . ? C22 C27 1.396(5) . ? C23 C24 1.362(7) . ? C23 H23 0.9300 . ? C24 C25 1.369(7) . ? C24 H24 0.9300 . ? C25 C26 1.389(6) . ? C25 H25 0.9300 . ? C26 C27 1.396(5) . ? C26 C28 1.505(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.526(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C31 C39 1.357(6) . ? C31 C32 1.407(6) . ? C32 H32 0.9300 . ? C33 C38 1.405(7) . ? C33 C34 1.424(7) . ? C34 C35 1.355(9) . ? C34 H34 0.9300 . ? C35 C36 1.390(9) . ? C35 H35 0.9300 . ? C36 C37 1.364(8) . ? C36 H36 0.9300 . ? C37 C38 1.402(7) . ? C37 H37 0.9300 . ? C38 C39 1.405(6) . ? C39 H39 0.9300 . ? C40 C41 1.488(5) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C42 C50 1.357(5) . ? C42 C43 1.409(5) . ? C43 H43 0.9300 . ? C44 C49 1.412(6) . ? C44 C45 1.418(6) . ? C45 C46 1.354(7) . ? C45 H45 0.9300 . ? C46 C47 1.379(8) . ? C46 H46 0.9300 . ? C47 C48 1.365(7) . ? C47 H47 0.9300 . ? C48 C49 1.406(6) . ? C48 H48 0.9300 . ? C49 C50 1.400(6) . ? C50 H50 0.9300 . ? C51 Cl1 1.713(7) . ? C51 Cl3 1.732(6) . ? C51 Cl2 1.736(6) . ? C51 H51 0.9800 . ? C52 Cl5A 1.573(9) . ? C52 Cl6A 1.586(14) . ? C52 Cl4A 1.630(9) . ? C52 Cl6 1.711(10) . ? C52 Cl4 1.926(10) . ? C52 Cl5 2.051(14) . ? C52 H52 0.9800 . ? Cl4A Cl5A 1.81(2) . ? 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 O1 C29 117.3(3) . . ? C13 O2 H2 109.5 . . ? C20 O3 C40 116.6(3) . . ? C27 O4 H4 109.5 . . ? C30 N1 C31 127.3(4) . . ? C30 N1 H1C 116.3 . . ? C31 N1 H1C 116.3 . . ? C32 N2 C33 116.6(4) . . ? C41 N3 C42 127.3(3) . . ? C41 N3 H3C 116.3 . . ? C42 N3 H3C 116.3 . . ? C43 N4 C44 117.9(4) . . ? C6 C1 C2 117.6(4) . . ? C6 C1 C28 121.6(3) . . ? C2 C1 C28 120.8(4) . . ? C3 C2 C1 120.5(4) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? C2 C3 C4 120.6(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 121.5(4) . . ? C3 C4 H4A 119.3 . . ? C5 C4 H4A 119.3 . . ? C6 C5 C4 116.5(4) . . ? C6 C5 C7 122.6(4) . . ? C4 C5 C7 120.8(4) . . ? C5 C6 C1 123.2(4) . . ? C5 C6 O1 119.3(4) . . ? C1 C6 O1 117.3(3) . . ? C8 C7 C5 111.9(4) . . ? C8 C7 H7A 109.2 . . ? C5 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C5 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C13 117.2(5) . . ? C9 C8 C7 121.5(4) . . ? C13 C8 C7 121.2(4) . . ? C10 C9 C8 121.6(5) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 120.3(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 121.1(5) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 117.8(4) . . ? C11 C12 C14 120.6(4) . . ? C13 C12 C14 121.6(4) . . ? O2 C13 C12 122.2(4) . . ? O2 C13 C8 116.0(4) . . ? C12 C13 C8 121.9(4) . . ? C15 C14 C12 113.8(3) . . ? C15 C14 H14A 108.8 . . ? C12 C14 H14A 108.8 . . ? C15 C14 H14B 108.8 . . ? C12 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C20 C15 C16 117.1(5) . . ? C20 C15 C14 122.5(4) . . ? C16 C15 C14 120.4(4) . . ? C17 C16 C15 121.3(4) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 120.0(4) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 122.1(5) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C20 C19 C18 116.3(4) . . ? C20 C19 C21 123.9(3) . . ? C18 C19 C21 119.7(4) . . ? C19 C20 C15 123.2(4) . . ? C19 C20 O3 118.9(3) . . ? C15 C20 O3 117.8(4) . . ? C19 C21 C22 111.7(3) . . ? C19 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? C19 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C27 117.8(4) . . ? C23 C22 C21 120.5(4) . . ? C27 C22 C21 121.6(3) . . ? C24 C23 C22 121.1(4) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 120.2(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 121.8(4) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C27 117.2(4) . . ? C25 C26 C28 120.4(4) . . ? C27 C26 C28 122.3(3) . . ? O4 C27 C22 115.5(3) . . ? O4 C27 C26 122.5(3) . . ? C22 C27 C26 121.9(3) . . ? C26 C28 C1 114.4(3) . . ? C26 C28 H28A 108.7 . . ? C1 C28 H28A 108.7 . . ? C26 C28 H28B 108.7 . . ? C1 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? O1 C29 C30 108.0(3) . . ? O1 C29 H29A 110.1 . . ? C30 C29 H29A 110.1 . . ? O1 C29 H29B 110.1 . . ? C30 C29 H29B 110.1 . . ? H29A C29 H29B 108.4 . . ? O5 C30 N1 125.9(4) . . ? O5 C30 C29 120.8(4) . . ? N1 C30 C29 113.3(4) . . ? C39 C31 C32 118.5(4) . . ? C39 C31 N1 125.6(4) . . ? C32 C31 N1 115.8(4) . . ? N2 C32 C31 124.7(5) . . ? N2 C32 H32 117.7 . . ? C31 C32 H32 117.7 . . ? N2 C33 C38 122.6(4) . . ? N2 C33 C34 118.0(5) . . ? C38 C33 C34 119.4(5) . . ? C35 C34 C33 119.6(6) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 121.0(6) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C37 C36 C35 120.4(6) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C38 120.8(6) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C37 C38 C33 118.7(5) . . ? C37 C38 C39 123.1(5) . . ? C33 C38 C39 118.1(4) . . ? C31 C39 C38 119.5(4) . . ? C31 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? O3 C40 C41 112.9(3) . . ? O3 C40 H40A 109.0 . . ? C41 C40 H40A 109.0 . . ? O3 C40 H40B 109.0 . . ? C41 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? O6 C41 N3 124.1(4) . . ? O6 C41 C40 118.7(3) . . ? N3 C41 C40 117.2(3) . . ? C50 C42 N3 125.8(3) . . ? C50 C42 C43 117.3(3) . . ? N3 C42 C43 116.8(3) . . ? N4 C43 C42 125.1(4) . . ? N4 C43 H43 117.4 . . ? C42 C43 H43 117.4 . . ? N4 C44 C49 121.2(4) . . ? N4 C44 C45 119.0(4) . . ? C49 C44 C45 119.8(4) . . ? C46 C45 C44 120.0(5) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.7(5) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C48 C47 C46 120.7(5) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C47 C48 C49 121.2(5) . . ? C47 C48 H48 119.4 . . ? C49 C48 H48 119.4 . . ? C50 C49 C48 124.2(4) . . ? C50 C49 C44 118.2(4) . . ? C48 C49 C44 117.6(4) . . ? C42 C50 C49 120.3(4) . . ? C42 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? Cl1 C51 Cl3 111.4(3) . . ? Cl1 C51 Cl2 110.9(3) . . ? Cl3 C51 Cl2 111.4(4) . . ? Cl1 C51 H51 107.6 . . ? Cl3 C51 H51 107.6 . . ? Cl2 C51 H51 107.6 . . ? Cl5A C52 Cl6A 110.8(9) . . ? Cl5A C52 Cl4A 68.7(9) . . ? Cl6A C52 Cl4A 131.0(18) . . ? Cl5A C52 Cl6 119.3(8) . . ? Cl6A C52 Cl6 22.2(15) . . ? Cl4A C52 Cl6 151.8(8) . . ? Cl5A C52 Cl4 108.8(8) . . ? Cl6A C52 Cl4 84.8(14) . . ? Cl4A C52 Cl4 53.2(4) . . ? Cl6 C52 Cl4 100.5(6) . . ? Cl5A C52 Cl5 35.2(5) . . ? Cl6A C52 Cl5 101.6(7) . . ? Cl4A C52 Cl5 100.3(6) . . ? Cl6 C52 Cl5 97.5(6) . . ? Cl4 C52 Cl5 143.5(6) . . ? Cl5A C52 H52 119.2 . . ? Cl6A C52 H52 122.5 . . ? Cl4A C52 H52 93.8 . . ? Cl6 C52 H52 103.2 . . ? Cl4 C52 H52 103.2 . . ? Cl5 C52 H52 103.2 . . ? C52 Cl4A Cl5A 54.1(5) . . ? C52 Cl5A Cl4A 57.1(6) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.772 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.065 #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 775959' #TrackingRef '- CIF_revised_compounds 1 to 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H52 N4 O6' _chemical_formula_weight 877.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 28.539(4) _cell_length_b 17.712(2) _cell_length_c 36.055(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 18225(4) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7115 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 21.12 _exptl_crystal_description Blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7424 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9564 _exptl_absorpt_correction_T_max 0.9901 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 87742 _diffrn_reflns_av_R_equivalents 0.1199 _diffrn_reflns_av_sigmaI/netI 0.0917 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16038 _reflns_number_gt 11556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0348P)^2^+30.7075P] 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 16038 _refine_ls_number_parameters 1193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1350 _refine_ls_R_factor_gt 0.0967 _refine_ls_wR_factor_ref 0.1797 _refine_ls_wR_factor_gt 0.1662 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.186 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.25997(9) 0.19062(14) 0.19363(7) 0.0190(6) Uani 1 d . . . O2 O 0.16398(11) 0.12610(16) 0.15911(8) 0.0299(7) Uani 1 d . . . O3 O 0.35999(10) 0.26884(15) 0.10700(7) 0.0210(6) Uani 1 d . . . O4 O 0.38008(9) 0.37277(14) 0.20871(7) 0.0196(6) Uani 1 d . . . O5 O 0.32750(12) 0.52329(17) 0.25780(10) 0.0433(9) Uani 1 d . . . O6 O 0.41133(9) 0.15321(14) 0.22090(7) 0.0191(6) Uani 1 d . . . N1 N 0.15902(12) 0.24052(18) 0.18784(9) 0.0217(8) Uani 1 d . . . H1C H 0.1707 0.2669 0.2056 0.026 Uiso 1 calc R . . N2 N 0.07002(19) 0.3811(2) 0.16654(13) 0.0613(15) Uani 1 d . . . N3 N 0.30546(12) 0.40317(18) 0.24382(9) 0.0236(8) Uani 1 d . . . H3C H 0.3154 0.3623 0.2337 0.028 Uiso 1 calc R . . N4 N 0.18668(12) 0.33402(19) 0.25229(10) 0.0258(8) Uani 1 d . . . C1 C 0.29053(14) 0.1429(2) 0.17330(11) 0.0170(9) Uani 1 d . . . C2 C 0.31881(14) 0.0931(2) 0.19345(11) 0.0173(9) Uani 1 d . . . C3 C 0.34767(14) 0.0451(2) 0.17266(11) 0.0205(9) Uani 1 d . . . H3 H 0.3661 0.0098 0.1850 0.025 Uiso 1 calc R . . C4 C 0.34952(15) 0.0488(2) 0.13461(12) 0.0258(10) Uani 1 d . . . H4 H 0.3684 0.0156 0.1214 0.031 Uiso 1 calc R . . C5 C 0.32275(15) 0.1026(2) 0.11609(11) 0.0228(10) Uani 1 d . . . H5 H 0.3249 0.1063 0.0904 0.027 Uiso 1 calc R . . C6 C 0.29288(14) 0.1510(2) 0.13517(11) 0.0186(9) Uani 1 d . . . C7 C 0.26561(15) 0.2119(2) 0.11465(11) 0.0229(10) Uani 1 d . . . H7A H 0.2701 0.2052 0.0882 0.028 Uiso 1 calc R . . H7B H 0.2325 0.2056 0.1198 0.028 Uiso 1 calc R . . C8 C 0.27991(15) 0.2918(2) 0.12510(10) 0.0191(9) Uani 1 d . . . C9 C 0.24671(15) 0.3432(2) 0.13833(11) 0.0242(10) Uani 1 d . . . H9 H 0.2156 0.3284 0.1404 0.029 Uiso 1 calc R . . C10 C 0.25952(16) 0.4161(2) 0.14851(11) 0.0269(11) Uani 1 d . . . H10 H 0.2369 0.4502 0.1566 0.032 Uiso 1 calc R . . C11 C 0.30588(15) 0.4378(2) 0.14660(11) 0.0227(10) Uani 1 d . . . H11 H 0.3144 0.4861 0.1540 0.027 Uiso 1 calc R . . C12 C 0.34008(15) 0.3882(2) 0.13367(11) 0.0193(9) Uani 1 d . . . C13 C 0.32592(14) 0.3165(2) 0.12188(10) 0.0186(9) Uani 1 d . . . C14 C 0.39127(15) 0.4118(2) 0.13181(12) 0.0237(10) Uani 1 d . . . H14A H 0.4008 0.4114 0.1060 0.028 Uiso 1 calc R . . H14B H 0.3935 0.4636 0.1404 0.028 Uiso 1 calc R . . C15 C 0.42644(14) 0.3650(2) 0.15361(11) 0.0201(9) Uani 1 d . . . C16 C 0.46678(15) 0.3390(2) 0.13612(12) 0.0276(11) Uani 1 d . . . H16 H 0.4713 0.3492 0.1111 0.033 Uiso 1 calc R . . C17 C 0.50030(15) 0.2983(2) 0.15537(13) 0.0294(11) Uani 1 d . . . H17 H 0.5274 0.2819 0.1435 0.035 Uiso 1 calc R . . C18 C 0.49309(15) 0.2823(2) 0.19233(12) 0.0268(10) Uani 1 d . . . H18 H 0.5153 0.2540 0.2051 0.032 Uiso 1 calc R . . C19 C 0.45325(14) 0.3074(2) 0.21106(11) 0.0201(9) Uani 1 d . . . C20 C 0.42073(13) 0.3490(2) 0.19089(11) 0.0175(9) Uani 1 d . . . C21 C 0.44648(15) 0.2884(2) 0.25183(11) 0.0240(10) Uani 1 d . . . H21A H 0.4705 0.2525 0.2589 0.029 Uiso 1 calc R . . H21B H 0.4518 0.3340 0.2661 0.029 Uiso 1 calc R . . C22 C 0.39952(15) 0.2562(2) 0.26316(11) 0.0208(9) Uani 1 d . . . C23 C 0.37244(16) 0.2893(2) 0.29059(11) 0.0241(10) Uani 1 d . . . H23 H 0.3837 0.3317 0.3029 0.029 Uiso 1 calc R . . C24 C 0.32911(15) 0.2606(2) 0.29993(11) 0.0261(10) Uani 1 d . . . H24 H 0.3113 0.2835 0.3184 0.031 Uiso 1 calc R . . C25 C 0.31222(15) 0.1971(2) 0.28155(11) 0.0218(10) Uani 1 d . . . H25 H 0.2828 0.1783 0.2876 0.026 Uiso 1 calc R . . C26 C 0.33849(14) 0.1613(2) 0.25426(10) 0.0188(9) Uani 1 d . . . C27 C 0.38260(15) 0.1895(2) 0.24640(10) 0.0186(9) Uani 1 d . . . C28 C 0.31971(15) 0.0906(2) 0.23505(11) 0.0208(9) Uani 1 d . . . H28A H 0.3387 0.0479 0.2426 0.025 Uiso 1 calc R . . H28B H 0.2881 0.0815 0.2438 0.025 Uiso 1 calc R . . C29 C 0.21877(13) 0.1539(2) 0.20758(11) 0.0203(9) Uani 1 d . . . H29A H 0.2122 0.1716 0.2325 0.024 Uiso 1 calc R . . H29B H 0.2240 0.0998 0.2087 0.024 Uiso 1 calc R . . C30 C 0.17767(14) 0.1703(2) 0.18287(11) 0.0201(9) Uani 1 d . . . C31 C 0.12283(14) 0.2748(2) 0.16718(11) 0.0210(9) Uani 1 d . . . C32 C 0.10468(15) 0.2477(2) 0.13480(12) 0.0242(10) Uani 1 d . . . H32 H 0.1173 0.2048 0.1238 0.029 Uiso 1 calc R . . C33 C 0.06634(15) 0.2856(2) 0.11817(11) 0.0230(10) Uani 1 d . . . C34 C 0.04274(16) 0.2578(3) 0.08703(12) 0.0302(11) Uani 1 d . . . H34 H 0.0538 0.2146 0.0753 0.036 Uiso 1 calc R . . C35 C 0.00367(17) 0.2933(3) 0.07369(12) 0.0348(12) Uani 1 d . . . H35 H -0.0125 0.2730 0.0537 0.042 Uiso 1 calc R . . C36 C -0.0119(2) 0.3603(3) 0.09021(14) 0.0487(15) Uani 1 d . . . H36 H -0.0378 0.3854 0.0806 0.058 Uiso 1 calc R . . C37 C 0.0108(2) 0.3888(3) 0.12020(16) 0.069(2) Uani 1 d . . . H37 H 0.0000 0.4331 0.1311 0.083 Uiso 1 calc R . . C38 C 0.05011(19) 0.3525(3) 0.13502(13) 0.0379(13) Uani 1 d . . . C39 C 0.1049(2) 0.3436(3) 0.18139(15) 0.0483(15) Uani 1 d . . . H39 H 0.1188 0.3635 0.2026 0.058 Uiso 1 calc R . . C40 C 0.36357(15) 0.2751(2) 0.06723(11) 0.0237(10) Uani 1 d . . . H40A H 0.3668 0.3277 0.0602 0.028 Uiso 1 calc R . . H40B H 0.3355 0.2552 0.0556 0.028 Uiso 1 calc R . . C41 C 0.40583(15) 0.2311(2) 0.05453(11) 0.0256(10) Uani 1 d . . . H41A H 0.4015 0.1781 0.0604 0.031 Uiso 1 calc R . . H41B H 0.4334 0.2489 0.0676 0.031 Uiso 1 calc R . . C42 C 0.41338(16) 0.2398(3) 0.01290(12) 0.0310(11) Uani 1 d . . . H42A H 0.3869 0.2195 -0.0001 0.046 Uiso 1 calc R . . H42B H 0.4412 0.2131 0.0057 0.046 Uiso 1 calc R . . H42C H 0.4168 0.2924 0.0069 0.046 Uiso 1 calc R . . C43 C 0.38118(15) 0.4464(2) 0.22464(13) 0.0277(11) Uani 1 d . . . H43A H 0.3862 0.4837 0.2054 0.033 Uiso 1 calc R . . H43B H 0.4068 0.4499 0.2422 0.033 Uiso 1 calc R . . C44 C 0.33544(15) 0.4615(2) 0.24405(12) 0.0260(10) Uani 1 d . . . C45 C 0.25999(14) 0.4010(2) 0.25808(11) 0.0192(9) Uani 1 d . . . C46 C 0.24134(15) 0.4492(2) 0.28388(11) 0.0207(9) Uani 1 d . . . H46 H 0.2600 0.4859 0.2950 0.025 Uiso 1 calc R . . C47 C 0.19390(14) 0.4426(2) 0.29342(10) 0.0182(9) Uani 1 d . . . C48 C 0.17104(16) 0.4936(2) 0.31751(11) 0.0255(10) Uani 1 d . . . H48 H 0.1883 0.5317 0.3289 0.031 Uiso 1 calc R . . C49 C 0.12445(17) 0.4880(2) 0.32439(12) 0.0290(11) Uani 1 d . . . H49 H 0.1101 0.5231 0.3398 0.035 Uiso 1 calc R . . C50 C 0.09788(17) 0.4304(3) 0.30860(12) 0.0322(11) Uani 1 d . . . H50 H 0.0661 0.4265 0.3139 0.039 Uiso 1 calc R . . C51 C 0.11884(15) 0.3790(2) 0.28515(12) 0.0271(10) Uani 1 d . . . H51 H 0.1010 0.3407 0.2746 0.033 Uiso 1 calc R . . C52 C 0.16674(15) 0.3840(2) 0.27712(10) 0.0201(9) Uani 1 d . . . C53 C 0.23055(15) 0.3432(2) 0.24378(12) 0.0242(10) Uani 1 d . . . H53 H 0.2437 0.3093 0.2270 0.029 Uiso 1 calc R . . C54 C 0.43895(15) 0.0935(2) 0.23744(12) 0.0262(10) Uani 1 d . . . H54A H 0.4186 0.0534 0.2462 0.031 Uiso 1 calc R . . H54B H 0.4564 0.1130 0.2584 0.031 Uiso 1 calc R . . C55 C 0.47211(15) 0.0635(2) 0.20851(12) 0.0289(11) Uani 1 d . . . H55A H 0.4926 0.1038 0.2002 0.035 Uiso 1 calc R . . H55B H 0.4544 0.0457 0.1873 0.035 Uiso 1 calc R . . C56 C 0.50136(17) -0.0008(3) 0.22416(14) 0.0407(13) Uani 1 d . . . H56A H 0.5179 0.0164 0.2457 0.061 Uiso 1 calc R . . H56B H 0.5234 -0.0174 0.2058 0.061 Uiso 1 calc R . . H56C H 0.4812 -0.0420 0.2308 0.061 Uiso 1 calc R . . O7 O 0.74790(9) 0.20515(14) 0.05149(7) 0.0197(6) Uani 1 d . . . O8 O 0.83924(10) 0.28813(16) 0.08421(8) 0.0315(8) Uani 1 d . . . O9 O 0.59929(10) 0.22432(15) 0.02577(7) 0.0217(7) Uani 1 d . . . O10 O 0.62797(9) 0.01746(14) 0.04415(7) 0.0198(6) Uani 1 d . . . O11 O 0.67790(10) -0.11539(15) -0.01761(8) 0.0263(7) Uani 1 d . . . O12 O 0.64442(10) 0.14164(15) 0.14107(7) 0.0221(7) Uani 1 d . . . N5 N 0.85293(12) 0.16860(18) 0.06323(9) 0.0203(8) Uani 1 d . . . H5C H 0.8432 0.1360 0.0473 0.024 Uiso 1 calc R . . N6 N 0.94621(13) 0.0433(2) 0.09468(10) 0.0295(9) Uani 1 d . . . N7 N 0.70381(12) -0.00658(18) 0.00935(9) 0.0216(8) Uani 1 d . . . H7C H 0.6949 0.0301 0.0233 0.026 Uiso 1 calc R . . N8 N 0.82443(12) 0.05630(18) 0.00820(9) 0.0215(8) Uani 1 d . . . C57 C 0.71541(14) 0.2561(2) 0.06661(11) 0.0171(9) Uani 1 d . . . C58 C 0.71033(15) 0.2585(2) 0.10488(10) 0.0201(9) Uani 1 d . . . C59 C 0.67915(15) 0.3120(2) 0.11938(12) 0.0257(10) Uani 1 d . . . H59 H 0.6748 0.3150 0.1449 0.031 Uiso 1 calc R . . C60 C 0.65471(16) 0.3607(2) 0.09615(13) 0.0300(11) Uani 1 d . . . H60 H 0.6353 0.3976 0.1062 0.036 Uiso 1 calc R . . C61 C 0.65919(15) 0.3540(2) 0.05831(12) 0.0245(10) Uani 1 d . . . H61 H 0.6424 0.3864 0.0429 0.029 Uiso 1 calc R . . C62 C 0.68835(14) 0.2997(2) 0.04255(11) 0.0180(9) Uani 1 d . . . C63 C 0.68845(15) 0.2876(2) 0.00086(11) 0.0217(10) Uani 1 d . . . H63A H 0.6714 0.3290 -0.0105 0.026 Uiso 1 calc R . . H63B H 0.7206 0.2906 -0.0077 0.026 Uiso 1 calc R . . C64 C 0.66763(15) 0.2143(2) -0.01318(11) 0.0225(10) Uani 1 d . . . C65 C 0.69054(16) 0.1747(2) -0.04148(11) 0.0265(10) Uani 1 d . . . H65 H 0.7195 0.1919 -0.0498 0.032 Uiso 1 calc R . . C66 C 0.67143(16) 0.1107(2) -0.05741(12) 0.0283(11) Uani 1 d . . . H66 H 0.6871 0.0857 -0.0764 0.034 Uiso 1 calc R . . C67 C 0.62861(16) 0.0845(2) -0.04471(11) 0.0278(11) Uani 1 d . . . H67 H 0.6155 0.0418 -0.0556 0.033 Uiso 1 calc R . . C68 C 0.60478(15) 0.1204(2) -0.01612(11) 0.0210(10) Uani 1 d . . . C69 C 0.62421(15) 0.1871(2) -0.00191(10) 0.0210(10) Uani 1 d . . . C70 C 0.55798(15) 0.0907(2) -0.00274(11) 0.0245(10) Uani 1 d . . . H70A H 0.5339 0.1259 -0.0105 0.029 Uiso 1 calc R . . H70B H 0.5519 0.0432 -0.0152 0.029 Uiso 1 calc R . . C71 C 0.55281(15) 0.0780(2) 0.03855(11) 0.0217(10) Uani 1 d . . . C72 C 0.51280(15) 0.1051(2) 0.05663(12) 0.0264(10) Uani 1 d . . . H72 H 0.4896 0.1290 0.0428 0.032 Uiso 1 calc R . . C73 C 0.50674(16) 0.0973(2) 0.09437(13) 0.0310(11) Uani 1 d . . . H73 H 0.4797 0.1152 0.1057 0.037 Uiso 1 calc R . . C74 C 0.54141(15) 0.0624(2) 0.11520(12) 0.0256(10) Uani 1 d . . . H74 H 0.5378 0.0585 0.1408 0.031 Uiso 1 calc R . . C75 C 0.58130(14) 0.0333(2) 0.09870(11) 0.0185(9) Uani 1 d . . . C76 C 0.58615(14) 0.0422(2) 0.06044(11) 0.0176(9) Uani 1 d . . . C77 C 0.61775(15) -0.0081(2) 0.12165(11) 0.0246(10) Uani 1 d . . . H77A H 0.6082 -0.0058 0.1474 0.029 Uiso 1 calc R . . H77B H 0.6173 -0.0608 0.1144 0.029 Uiso 1 calc R . . C78 C 0.66734(15) 0.0194(2) 0.11919(11) 0.0229(10) Uani 1 d . . . C79 C 0.70348(16) -0.0289(2) 0.10774(11) 0.0259(10) Uani 1 d . . . H79 H 0.6967 -0.0790 0.1022 0.031 Uiso 1 calc R . . C80 C 0.74865(17) -0.0035(3) 0.10460(12) 0.0318(11) Uani 1 d . . . H80 H 0.7723 -0.0368 0.0977 0.038 Uiso 1 calc R . . C81 C 0.75955(16) 0.0717(2) 0.11161(11) 0.0282(11) Uani 1 d . . . H81 H 0.7901 0.0887 0.1084 0.034 Uiso 1 calc R . . C82 C 0.72478(15) 0.1219(2) 0.12340(11) 0.0221(10) Uani 1 d . . . C83 C 0.67962(15) 0.0938(2) 0.12805(10) 0.0215(10) Uani 1 d . . . C84 C 0.73641(16) 0.2046(2) 0.13015(11) 0.0259(10) Uani 1 d . . . H84A H 0.7291 0.2169 0.1557 0.031 Uiso 1 calc R . . H84B H 0.7698 0.2119 0.1267 0.031 Uiso 1 calc R . . C85 C 0.78932(14) 0.2399(2) 0.03637(11) 0.0222(10) Uani 1 d . . . H85A H 0.7828 0.2923 0.0306 0.027 Uiso 1 calc R . . H85B H 0.7980 0.2146 0.0135 0.027 Uiso 1 calc R . . C86 C 0.82965(15) 0.2353(2) 0.06369(11) 0.0208(10) Uani 1 d . . . C87 C 0.89105(14) 0.1458(2) 0.08540(11) 0.0187(9) Uani 1 d . . . C88 C 0.91049(14) 0.1875(2) 0.11326(11) 0.0217(10) Uani 1 d . . . H88 H 0.8983 0.2344 0.1197 0.026 Uiso 1 calc R . . C89 C 0.94996(14) 0.1572(2) 0.13222(11) 0.0207(9) Uani 1 d . . . C90 C 0.97328(15) 0.1982(3) 0.16061(11) 0.0283(11) Uani 1 d . . . H90 H 0.9624 0.2455 0.1677 0.034 Uiso 1 calc R . . C91 C 1.01192(15) 0.1674(3) 0.17756(12) 0.0291(11) Uani 1 d . . . H91 H 1.0274 0.1946 0.1959 0.035 Uiso 1 calc R . . C92 C 1.02845(17) 0.0953(3) 0.16753(13) 0.0360(12) Uani 1 d . . . H92 H 1.0544 0.0750 0.1795 0.043 Uiso 1 calc R . . C93 C 1.00660(16) 0.0552(3) 0.14039(12) 0.0326(11) Uani 1 d . . . H93 H 1.0179 0.0078 0.1338 0.039 Uiso 1 calc R . . C94 C 0.96705(15) 0.0850(2) 0.12221(12) 0.0257(10) Uani 1 d . . . C95 C 0.91025(16) 0.0731(2) 0.07780(12) 0.0264(10) Uani 1 d . . . H95 H 0.8960 0.0445 0.0593 0.032 Uiso 1 calc R . . C96 C 0.56893(15) 0.2827(2) 0.01181(12) 0.0256(10) Uani 1 d . . . H96A H 0.5481 0.2619 -0.0069 0.031 Uiso 1 calc R . . H96B H 0.5875 0.3222 0.0004 0.031 Uiso 1 calc R . . C97 C 0.54058(16) 0.3151(3) 0.04323(12) 0.0296(11) Uani 1 d . . . H97A H 0.5614 0.3302 0.0632 0.035 Uiso 1 calc R . . H97B H 0.5194 0.2769 0.0527 0.035 Uiso 1 calc R . . C98 C 0.51253(17) 0.3831(3) 0.03009(14) 0.0391(13) Uani 1 d . . . H98A H 0.5336 0.4234 0.0238 0.059 Uiso 1 calc R . . H98B H 0.4919 0.3994 0.0495 0.059 Uiso 1 calc R . . H98C H 0.4945 0.3695 0.0087 0.059 Uiso 1 calc R . . C99 C 0.62680(14) -0.0523(2) 0.02438(11) 0.0211(9) Uani 1 d . . . H99A H 0.6005 -0.0526 0.0073 0.025 Uiso 1 calc R . . H99B H 0.6229 -0.0939 0.0416 0.025 Uiso 1 calc R . . C100 C 0.67168(15) -0.0615(2) 0.00329(10) 0.0179(9) Uani 1 d . . . C101 C 0.74988(15) -0.0018(2) -0.00423(10) 0.0193(9) Uani 1 d . . . C102 C 0.76718(15) -0.0396(2) -0.03443(11) 0.0205(9) Uani 1 d . . . H102 H 0.7478 -0.0694 -0.0491 0.025 Uiso 1 calc R . . C103 C 0.81547(15) -0.0320(2) -0.04257(10) 0.0188(9) Uani 1 d . . . C104 C 0.83745(16) -0.0713(2) -0.07231(10) 0.0207(10) Uani 1 d . . . H104 H 0.8194 -0.1002 -0.0884 0.025 Uiso 1 calc R . . C105 C 0.88477(16) -0.0669(2) -0.07742(11) 0.0234(10) Uani 1 d . . . H105 H 0.8987 -0.0932 -0.0968 0.028 Uiso 1 calc R . . C106 C 0.91272(15) -0.0230(2) -0.05363(11) 0.0230(10) Uani 1 d . . . H106 H 0.9450 -0.0218 -0.0569 0.028 Uiso 1 calc R . . C107 C 0.89256(15) 0.0180(2) -0.02569(11) 0.0218(10) Uani 1 d . . . H107 H 0.9110 0.0481 -0.0104 0.026 Uiso 1 calc R . . C108 C 0.84387(14) 0.0145(2) -0.02016(10) 0.0173(9) Uani 1 d . . . C109 C 0.77990(15) 0.0477(2) 0.01513(11) 0.0238(10) Uani 1 d . . . H109 H 0.7670 0.0763 0.0342 0.029 Uiso 1 calc R . . C110 C 0.64305(18) 0.1463(4) 0.18054(13) 0.0500(15) Uani 1 d . . . H10E H 0.6548 0.0993 0.1908 0.060 Uiso 1 calc R . . H10D H 0.6640 0.1863 0.1885 0.060 Uiso 1 calc R . . C111 C 0.5995(2) 0.1599(5) 0.19499(15) 0.095(3) Uani 1 d . . . H11E H 0.5789 0.1200 0.1864 0.114 Uiso 1 calc R . . H11D H 0.5882 0.2067 0.1842 0.114 Uiso 1 calc R . . C112 C 0.59389(17) 0.1659(3) 0.23674(12) 0.0367(12) Uani 1 d . . . H12F H 0.6113 0.1262 0.2485 0.055 Uiso 1 calc R . . H12E H 0.5613 0.1613 0.2431 0.055 Uiso 1 calc R . . H12D H 0.6054 0.2139 0.2450 0.055 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0168(15) 0.0197(15) 0.0205(15) -0.0011(11) 0.0049(13) -0.0007(12) O2 0.0336(19) 0.0278(17) 0.0284(17) -0.0126(14) -0.0098(15) 0.0094(14) O3 0.0229(16) 0.0214(15) 0.0188(15) 0.0049(12) 0.0034(13) 0.0018(13) O4 0.0171(15) 0.0189(15) 0.0228(15) -0.0010(12) 0.0018(13) -0.0022(12) O5 0.039(2) 0.0294(19) 0.062(2) -0.0193(17) 0.0111(18) -0.0090(16) O6 0.0183(15) 0.0228(15) 0.0163(15) 0.0020(12) 0.0006(13) 0.0016(12) N1 0.022(2) 0.0179(18) 0.025(2) -0.0060(15) -0.0036(16) -0.0015(15) N2 0.089(4) 0.037(3) 0.058(3) -0.019(2) -0.032(3) 0.035(3) N3 0.022(2) 0.0161(18) 0.033(2) -0.0040(15) 0.0008(17) 0.0003(15) N4 0.021(2) 0.0235(19) 0.033(2) -0.0060(16) 0.0017(18) -0.0009(16) C1 0.016(2) 0.011(2) 0.024(2) -0.0028(17) 0.0003(18) -0.0032(17) C2 0.018(2) 0.016(2) 0.018(2) 0.0013(16) -0.0025(18) -0.0051(18) C3 0.021(2) 0.015(2) 0.025(2) 0.0048(17) -0.0039(19) -0.0017(18) C4 0.018(2) 0.022(2) 0.038(3) -0.008(2) 0.001(2) -0.0026(19) C5 0.028(3) 0.022(2) 0.019(2) -0.0051(18) -0.001(2) -0.008(2) C6 0.021(2) 0.020(2) 0.015(2) -0.0015(17) -0.0025(18) -0.0053(18) C7 0.022(2) 0.024(2) 0.023(2) 0.0006(18) -0.001(2) -0.0050(19) C8 0.025(2) 0.020(2) 0.012(2) 0.0074(17) -0.0049(18) 0.0007(19) C9 0.016(2) 0.030(2) 0.027(2) 0.0097(19) 0.001(2) 0.003(2) C10 0.031(3) 0.024(2) 0.026(2) 0.0055(19) 0.001(2) 0.011(2) C11 0.032(3) 0.016(2) 0.020(2) 0.0035(17) -0.005(2) 0.0033(19) C12 0.026(2) 0.017(2) 0.015(2) 0.0049(16) -0.0010(19) 0.0008(18) C13 0.022(2) 0.022(2) 0.012(2) 0.0058(16) 0.0004(18) 0.0037(19) C14 0.033(3) 0.017(2) 0.021(2) 0.0046(17) -0.003(2) -0.0058(19) C15 0.017(2) 0.021(2) 0.022(2) -0.0003(18) -0.0009(19) -0.0087(18) C16 0.026(3) 0.031(3) 0.026(2) -0.001(2) 0.003(2) -0.010(2) C17 0.016(2) 0.033(3) 0.039(3) 0.002(2) 0.005(2) -0.004(2) C18 0.017(2) 0.026(2) 0.037(3) 0.005(2) -0.002(2) -0.0047(19) C19 0.013(2) 0.021(2) 0.026(2) -0.0012(18) -0.0025(19) -0.0041(18) C20 0.010(2) 0.022(2) 0.020(2) 0.0002(17) -0.0001(18) -0.0083(18) C21 0.022(2) 0.027(2) 0.023(2) -0.0038(19) -0.005(2) 0.0002(19) C22 0.023(2) 0.022(2) 0.017(2) 0.0078(17) -0.0016(19) 0.0028(19) C23 0.035(3) 0.021(2) 0.016(2) -0.0012(18) -0.002(2) 0.003(2) C24 0.030(3) 0.030(2) 0.019(2) -0.0008(19) 0.002(2) 0.005(2) C25 0.022(2) 0.028(2) 0.016(2) 0.0066(18) 0.0045(19) -0.0022(19) C26 0.019(2) 0.024(2) 0.013(2) 0.0047(17) -0.0018(18) 0.0019(18) C27 0.026(2) 0.023(2) 0.0071(19) 0.0024(16) -0.0029(18) 0.0042(19) C28 0.018(2) 0.022(2) 0.022(2) 0.0050(17) 0.0022(19) -0.0012(18) C29 0.018(2) 0.024(2) 0.019(2) 0.0007(18) 0.0045(19) -0.0014(18) C30 0.022(2) 0.016(2) 0.022(2) 0.0019(18) 0.0015(19) 0.0003(18) C31 0.019(2) 0.019(2) 0.025(2) 0.0016(18) -0.0007(19) -0.0018(18) C32 0.024(2) 0.022(2) 0.026(2) -0.0003(19) 0.004(2) 0.0072(19) C33 0.025(2) 0.022(2) 0.023(2) 0.0043(18) 0.006(2) 0.0016(19) C34 0.038(3) 0.034(3) 0.019(2) 0.002(2) 0.003(2) 0.008(2) C35 0.031(3) 0.052(3) 0.021(2) 0.010(2) 0.001(2) 0.008(2) C36 0.055(4) 0.060(4) 0.031(3) 0.003(3) -0.006(3) 0.033(3) C37 0.096(5) 0.059(4) 0.052(4) -0.014(3) -0.027(4) 0.054(4) C38 0.054(3) 0.028(3) 0.032(3) 0.001(2) -0.006(3) 0.013(2) C39 0.065(4) 0.026(3) 0.054(4) -0.011(2) -0.020(3) 0.012(3) C40 0.028(3) 0.022(2) 0.021(2) 0.0041(18) -0.002(2) 0.0023(19) C41 0.020(2) 0.032(3) 0.025(2) 0.0027(19) -0.001(2) 0.000(2) C42 0.029(3) 0.036(3) 0.028(3) 0.000(2) 0.002(2) -0.001(2) C43 0.024(2) 0.021(2) 0.039(3) -0.008(2) 0.001(2) -0.006(2) C44 0.028(3) 0.023(2) 0.027(2) -0.0022(19) -0.004(2) -0.005(2) C45 0.019(2) 0.017(2) 0.022(2) 0.0018(17) 0.0025(19) 0.0001(18) C46 0.028(3) 0.018(2) 0.016(2) 0.0027(17) -0.0062(19) -0.0004(19) C47 0.025(2) 0.021(2) 0.009(2) 0.0078(16) -0.0039(18) 0.0007(18) C48 0.039(3) 0.026(2) 0.012(2) -0.0005(17) 0.001(2) 0.001(2) C49 0.039(3) 0.025(2) 0.023(2) 0.0030(19) 0.007(2) 0.006(2) C50 0.029(3) 0.035(3) 0.033(3) 0.003(2) 0.009(2) 0.006(2) C51 0.022(2) 0.027(2) 0.032(3) 0.003(2) 0.000(2) -0.002(2) C52 0.028(3) 0.021(2) 0.012(2) 0.0045(17) -0.0020(19) -0.0005(19) C53 0.026(3) 0.018(2) 0.028(2) -0.0098(18) 0.002(2) -0.0015(19) C54 0.028(3) 0.027(2) 0.023(2) 0.0017(19) -0.007(2) 0.004(2) C55 0.022(2) 0.030(3) 0.035(3) -0.003(2) -0.004(2) 0.002(2) C56 0.035(3) 0.046(3) 0.041(3) -0.001(2) -0.001(3) 0.018(2) O7 0.0182(15) 0.0188(14) 0.0221(15) -0.0014(12) -0.0003(13) -0.0005(12) O8 0.0316(18) 0.0202(16) 0.0426(19) -0.0129(14) -0.0109(16) 0.0060(14) O9 0.0253(17) 0.0275(16) 0.0124(14) -0.0003(12) -0.0005(13) 0.0007(13) O10 0.0166(15) 0.0208(15) 0.0221(15) -0.0042(12) 0.0007(13) -0.0005(12) O11 0.0295(18) 0.0231(16) 0.0262(16) -0.0071(13) 0.0039(14) -0.0050(14) O12 0.0294(17) 0.0257(16) 0.0113(15) -0.0001(12) -0.0021(13) 0.0017(14) N5 0.021(2) 0.0181(18) 0.0215(19) -0.0083(14) -0.0012(16) -0.0013(15) N6 0.036(2) 0.029(2) 0.024(2) -0.0033(17) 0.0011(19) 0.0083(18) N7 0.023(2) 0.0192(18) 0.0227(19) -0.0068(15) 0.0027(16) -0.0002(16) N8 0.022(2) 0.0236(19) 0.0185(19) -0.0063(15) 0.0039(16) -0.0028(16) C57 0.016(2) 0.015(2) 0.020(2) -0.0028(17) -0.0004(18) -0.0034(17) C58 0.026(2) 0.023(2) 0.011(2) 0.0003(17) -0.0007(18) -0.0084(19) C59 0.034(3) 0.026(2) 0.018(2) -0.0112(18) 0.007(2) -0.013(2) C60 0.029(3) 0.023(2) 0.037(3) -0.012(2) 0.001(2) -0.002(2) C61 0.023(2) 0.015(2) 0.036(3) -0.0016(18) -0.003(2) -0.0006(19) C62 0.018(2) 0.015(2) 0.021(2) 0.0032(17) 0.0016(18) -0.0031(17) C63 0.019(2) 0.025(2) 0.021(2) 0.0074(18) -0.0017(19) -0.0037(19) C64 0.028(3) 0.024(2) 0.015(2) 0.0066(18) -0.002(2) -0.001(2) C65 0.033(3) 0.029(2) 0.017(2) 0.0063(19) 0.004(2) 0.000(2) C66 0.035(3) 0.029(3) 0.020(2) -0.0013(19) 0.003(2) 0.004(2) C67 0.039(3) 0.027(2) 0.017(2) -0.0017(19) -0.006(2) -0.003(2) C68 0.025(2) 0.027(2) 0.012(2) 0.0027(18) -0.0054(19) 0.0010(19) C69 0.029(3) 0.026(2) 0.007(2) 0.0027(17) -0.0039(19) 0.005(2) C70 0.029(3) 0.019(2) 0.026(2) 0.0036(18) -0.007(2) -0.0029(19) C71 0.018(2) 0.021(2) 0.026(2) 0.0014(18) -0.002(2) -0.0044(18) C72 0.020(2) 0.026(2) 0.034(3) 0.007(2) -0.001(2) 0.0009(19) C73 0.022(3) 0.033(3) 0.038(3) -0.003(2) 0.013(2) -0.002(2) C74 0.028(3) 0.022(2) 0.027(2) -0.0072(19) 0.010(2) -0.006(2) C75 0.021(2) 0.015(2) 0.019(2) 0.0002(16) 0.0008(19) -0.0084(18) C76 0.017(2) 0.018(2) 0.019(2) 0.0001(17) 0.0037(18) -0.0058(18) C77 0.036(3) 0.020(2) 0.018(2) 0.0023(17) 0.001(2) -0.003(2) C78 0.030(3) 0.025(2) 0.014(2) 0.0079(17) -0.0069(19) 0.001(2) C79 0.036(3) 0.021(2) 0.020(2) 0.0020(18) -0.006(2) 0.004(2) C80 0.031(3) 0.031(3) 0.033(3) 0.006(2) -0.001(2) 0.011(2) C81 0.022(3) 0.037(3) 0.026(2) 0.012(2) -0.004(2) -0.002(2) C82 0.028(3) 0.027(2) 0.011(2) 0.0087(17) -0.0064(19) 0.001(2) C83 0.029(3) 0.026(2) 0.009(2) 0.0057(17) -0.0045(19) 0.000(2) C84 0.029(3) 0.032(3) 0.017(2) 0.0045(19) -0.002(2) -0.008(2) C85 0.019(2) 0.025(2) 0.022(2) 0.0004(18) 0.0021(19) -0.0001(19) C86 0.023(2) 0.016(2) 0.024(2) -0.0011(18) 0.0069(19) -0.0015(18) C87 0.020(2) 0.021(2) 0.016(2) 0.0021(17) 0.0028(18) -0.0017(18) C88 0.021(2) 0.025(2) 0.019(2) -0.0017(18) 0.0045(19) 0.0010(19) C89 0.016(2) 0.029(2) 0.017(2) 0.0029(18) 0.0041(18) -0.0009(19) C90 0.020(2) 0.043(3) 0.022(2) 0.001(2) 0.004(2) -0.001(2) C91 0.021(3) 0.049(3) 0.017(2) 0.000(2) 0.000(2) 0.002(2) C92 0.028(3) 0.051(3) 0.029(3) 0.008(2) -0.002(2) 0.010(2) C93 0.033(3) 0.041(3) 0.024(3) 0.009(2) 0.000(2) 0.013(2) C94 0.025(3) 0.027(2) 0.025(2) 0.0042(19) 0.008(2) 0.004(2) C95 0.032(3) 0.025(2) 0.022(2) -0.0009(19) 0.000(2) 0.001(2) C96 0.023(2) 0.030(2) 0.024(2) 0.0013(19) -0.004(2) 0.002(2) C97 0.023(2) 0.037(3) 0.029(3) -0.003(2) 0.008(2) -0.001(2) C98 0.040(3) 0.036(3) 0.041(3) 0.001(2) 0.010(3) 0.002(2) C99 0.020(2) 0.021(2) 0.022(2) -0.0014(18) 0.0030(19) -0.0009(18) C100 0.025(2) 0.018(2) 0.010(2) -0.0002(17) 0.0012(18) -0.0025(19) C101 0.024(2) 0.019(2) 0.015(2) -0.0006(17) -0.0020(19) 0.0008(18) C102 0.026(2) 0.021(2) 0.015(2) -0.0021(17) -0.0027(19) -0.0035(19) C103 0.027(2) 0.015(2) 0.014(2) 0.0044(16) -0.0013(19) -0.0011(18) C104 0.036(3) 0.016(2) 0.010(2) -0.0013(16) 0.0039(19) -0.0027(19) C105 0.036(3) 0.016(2) 0.018(2) -0.0003(17) 0.007(2) 0.001(2) C106 0.024(2) 0.023(2) 0.022(2) 0.0055(18) 0.004(2) 0.0019(19) C107 0.027(3) 0.021(2) 0.017(2) 0.0037(17) -0.0013(19) -0.0040(19) C108 0.028(2) 0.013(2) 0.011(2) 0.0033(16) -0.0026(18) 0.0009(18) C109 0.028(3) 0.019(2) 0.024(2) -0.0068(18) 0.006(2) 0.0031(19) C110 0.035(3) 0.091(4) 0.024(3) 0.013(3) -0.001(2) -0.006(3) C111 0.036(4) 0.214(9) 0.036(3) -0.049(5) -0.006(3) 0.049(5) C112 0.027(3) 0.053(3) 0.030(3) -0.011(2) -0.006(2) 0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.419(4) . ? O1 C29 1.435(4) . ? O2 C30 1.225(5) . ? O3 C13 1.395(5) . ? O3 C40 1.442(5) . ? O4 C20 1.391(5) . ? O4 C43 1.425(5) . ? O5 C44 1.222(5) . ? O6 C27 1.390(5) . ? O6 C54 1.447(5) . ? N1 C30 1.364(5) . ? N1 C31 1.411(5) . ? N1 H1C 0.8600 . ? N2 C39 1.310(6) . ? N2 C38 1.368(6) . ? N3 C44 1.342(5) . ? N3 C45 1.396(5) . ? N3 H3C 0.8600 . ? N4 C53 1.299(5) . ? N4 C52 1.382(5) . ? C1 C6 1.384(5) . ? C1 C2 1.399(5) . ? C2 C3 1.401(5) . ? C2 C28 1.501(5) . ? C3 C4 1.374(6) . ? C3 H3 0.9300 . ? C4 C5 1.392(6) . ? C4 H4 0.9300 . ? C5 C6 1.391(6) . ? C5 H5 0.9300 . ? C6 C7 1.523(5) . ? C7 C8 1.519(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.389(6) . ? C8 C9 1.398(6) . ? C9 C10 1.392(6) . ? C9 H9 0.9300 . ? C10 C11 1.379(6) . ? C10 H10 0.9300 . ? C11 C12 1.394(6) . ? C11 H11 0.9300 . ? C12 C13 1.398(5) . ? C12 C14 1.521(6) . ? C14 C15 1.521(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.383(5) . ? C15 C16 1.391(6) . ? C16 C17 1.385(6) . ? C16 H16 0.9300 . ? C17 C18 1.378(6) . ? C17 H17 0.9300 . ? C18 C19 1.395(6) . ? C18 H18 0.9300 . ? C19 C20 1.391(5) . ? C19 C21 1.520(6) . ? C21 C22 1.513(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.386(6) . ? C22 C27 1.411(6) . ? C23 C24 1.379(6) . ? C23 H23 0.9300 . ? C24 C25 1.391(6) . ? C24 H24 0.9300 . ? C25 C26 1.390(5) . ? C25 H25 0.9300 . ? C26 C27 1.384(6) . ? C26 C28 1.528(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.501(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C31 C32 1.364(6) . ? C31 C39 1.418(6) . ? C32 C33 1.417(6) . ? C32 H32 0.9300 . ? C33 C34 1.399(6) . ? C33 C38 1.409(6) . ? C34 C35 1.368(6) . ? C34 H34 0.9300 . ? C35 C36 1.400(7) . ? C35 H35 0.9300 . ? C36 C37 1.356(7) . ? C36 H36 0.9300 . ? C37 C38 1.400(7) . ? C37 H37 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.507(6) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.524(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.505(6) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C45 C46 1.370(5) . ? C45 C53 1.421(5) . ? C46 C47 1.402(6) . ? C46 H46 0.9300 . ? C47 C48 1.413(6) . ? C47 C52 1.422(5) . ? C48 C49 1.356(6) . ? C48 H48 0.9300 . ? C49 C50 1.394(6) . ? C49 H49 0.9300 . ? C50 C51 1.378(6) . ? C50 H50 0.9300 . ? C51 C52 1.400(6) . ? C51 H51 0.9300 . ? C53 H53 0.9300 . ? C54 C55 1.505(6) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.521(6) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? O7 C57 1.403(5) . ? O7 C85 1.440(5) . ? O8 C86 1.224(5) . ? O9 C69 1.392(5) . ? O9 C96 1.440(5) . ? O10 C76 1.400(5) . ? O10 C99 1.427(4) . ? O11 C100 1.229(4) . ? O12 C83 1.396(5) . ? O12 C110 1.426(5) . ? N5 C86 1.356(5) . ? N5 C87 1.409(5) . ? N5 H5C 0.8600 . ? N6 C95 1.304(5) . ? N6 C94 1.373(5) . ? N7 C100 1.354(5) . ? N7 C101 1.405(5) . ? N7 H7C 0.8600 . ? N8 C109 1.304(5) . ? N8 C108 1.379(5) . ? C57 C58 1.388(5) . ? C57 C62 1.395(5) . ? C58 C59 1.401(6) . ? C58 C84 1.515(6) . ? C59 C60 1.390(6) . ? C59 H59 0.9300 . ? C60 C61 1.375(6) . ? C60 H60 0.9300 . ? C61 C62 1.394(6) . ? C61 H61 0.9300 . ? C62 C63 1.518(5) . ? C63 C64 1.516(5) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C69 1.390(6) . ? C64 C65 1.400(6) . ? C65 C66 1.382(6) . ? C65 H65 0.9300 . ? C66 C67 1.385(6) . ? C66 H66 0.9300 . ? C67 C68 1.389(6) . ? C67 H67 0.9300 . ? C68 C69 1.402(6) . ? C68 C70 1.514(6) . ? C70 C71 1.513(6) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C76 1.390(6) . ? C71 C72 1.400(6) . ? C72 C73 1.379(6) . ? C72 H72 0.9300 . ? C73 C74 1.387(6) . ? C73 H73 0.9300 . ? C74 C75 1.384(6) . ? C74 H74 0.9300 . ? C75 C76 1.395(5) . ? C75 C77 1.519(6) . ? C77 C78 1.499(6) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 C83 1.400(6) . ? C78 C79 1.402(6) . ? C79 C80 1.370(6) . ? C79 H79 0.9300 . ? C80 C81 1.391(6) . ? C80 H80 0.9300 . ? C81 C82 1.398(6) . ? C81 H81 0.9300 . ? C82 C83 1.391(6) . ? C82 C84 1.521(6) . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C85 C86 1.517(6) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C87 C88 1.364(5) . ? C87 C95 1.427(6) . ? C88 C89 1.422(6) . ? C88 H88 0.9300 . ? C89 C94 1.416(6) . ? C89 C90 1.420(6) . ? C90 C91 1.373(6) . ? C90 H90 0.9300 . ? C91 C92 1.409(6) . ? C91 H91 0.9300 . ? C92 C93 1.360(6) . ? C92 H92 0.9300 . ? C93 C94 1.408(6) . ? C93 H93 0.9300 . ? C95 H95 0.9300 . ? C96 C97 1.506(6) . ? C96 H96A 0.9700 . ? C96 H96B 0.9700 . ? C97 C98 1.522(6) . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? C99 C100 1.498(5) . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C101 C102 1.370(5) . ? C101 C109 1.411(6) . ? C102 C103 1.416(6) . ? C102 H102 0.9300 . ? C103 C108 1.410(5) . ? C103 C104 1.424(5) . ? C104 C105 1.365(6) . ? C104 H104 0.9300 . ? C105 C106 1.406(6) . ? C105 H105 0.9300 . ? C106 C107 1.369(6) . ? C106 H106 0.9300 . ? C107 C108 1.405(6) . ? C107 H107 0.9300 . ? C109 H109 0.9300 . ? C110 C111 1.368(7) . ? C110 H10E 0.9700 . ? C110 H10D 0.9700 . ? C111 C112 1.518(7) . ? C111 H11E 0.9700 . ? C111 H11D 0.9700 . ? C112 H12F 0.9600 . ? C112 H12E 0.9600 . ? C112 H12D 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 C29 114.5(3) . . ? C13 O3 C40 112.6(3) . . ? C20 O4 C43 116.4(3) . . ? C27 O6 C54 112.8(3) . . ? C30 N1 C31 127.5(3) . . ? C30 N1 H1C 116.3 . . ? C31 N1 H1C 116.3 . . ? C39 N2 C38 117.9(4) . . ? C44 N3 C45 127.7(4) . . ? C44 N3 H3C 116.1 . . ? C45 N3 H3C 116.1 . . ? C53 N4 C52 118.0(4) . . ? C6 C1 C2 123.6(4) . . ? C6 C1 O1 118.8(3) . . ? C2 C1 O1 117.5(3) . . ? C1 C2 C3 116.3(4) . . ? C1 C2 C28 123.2(4) . . ? C3 C2 C28 120.5(4) . . ? C4 C3 C2 121.9(4) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 121.4(4) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C1 C6 C5 117.2(4) . . ? C1 C6 C7 122.1(4) . . ? C5 C6 C7 120.7(4) . . ? C8 C7 C6 113.7(3) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C13 C8 C9 117.6(4) . . ? C13 C8 C7 121.8(4) . . ? C9 C8 C7 120.6(4) . . ? C10 C9 C8 121.1(4) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 119.8(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 120.9(4) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C13 118.1(4) . . ? C11 C12 C14 120.9(4) . . ? C13 C12 C14 120.9(4) . . ? C8 C13 O3 120.0(3) . . ? C8 C13 C12 122.3(4) . . ? O3 C13 C12 117.7(4) . . ? C15 C14 C12 117.4(3) . . ? C15 C14 H14A 107.9 . . ? C12 C14 H14A 107.9 . . ? C15 C14 H14B 107.9 . . ? C12 C14 H14B 107.9 . . ? H14A C14 H14B 107.2 . . ? C20 C15 C16 118.1(4) . . ? C20 C15 C14 122.4(4) . . ? C16 C15 C14 119.5(4) . . ? C17 C16 C15 121.1(4) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C18 C17 C16 119.3(4) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 121.6(4) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C20 C19 C18 117.4(4) . . ? C20 C19 C21 122.6(4) . . ? C18 C19 C21 120.1(4) . . ? C15 C20 C19 122.6(4) . . ? C15 C20 O4 119.0(4) . . ? C19 C20 O4 118.4(3) . . ? C22 C21 C19 117.2(3) . . ? C22 C21 H21A 108.0 . . ? C19 C21 H21A 108.0 . . ? C22 C21 H21B 108.0 . . ? C19 C21 H21B 108.0 . . ? H21A C21 H21B 107.2 . . ? C23 C22 C27 118.0(4) . . ? C23 C22 C21 121.8(4) . . ? C27 C22 C21 120.2(4) . . ? C24 C23 C22 121.2(4) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 119.5(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 121.3(4) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C27 C26 C25 118.0(4) . . ? C27 C26 C28 121.5(4) . . ? C25 C26 C28 120.4(4) . . ? C26 C27 O6 120.3(3) . . ? C26 C27 C22 121.7(4) . . ? O6 C27 C22 118.0(4) . . ? C2 C28 C26 115.8(3) . . ? C2 C28 H28A 108.3 . . ? C26 C28 H28A 108.3 . . ? C2 C28 H28B 108.3 . . ? C26 C28 H28B 108.3 . . ? H28A C28 H28B 107.4 . . ? O1 C29 C30 110.1(3) . . ? O1 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? O1 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? O2 C30 N1 123.4(4) . . ? O2 C30 C29 122.7(4) . . ? N1 C30 C29 113.8(3) . . ? C32 C31 N1 125.3(4) . . ? C32 C31 C39 118.3(4) . . ? N1 C31 C39 116.3(4) . . ? C31 C32 C33 119.2(4) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C38 118.9(4) . . ? C34 C33 C32 123.0(4) . . ? C38 C33 C32 118.0(4) . . ? C35 C34 C33 120.9(4) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 119.9(5) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 120.2(5) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 121.1(5) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? N2 C38 C37 118.7(5) . . ? N2 C38 C33 122.2(4) . . ? C37 C38 C33 119.0(5) . . ? N2 C39 C31 124.2(5) . . ? N2 C39 H39 117.9 . . ? C31 C39 H39 117.9 . . ? O3 C40 C41 108.6(3) . . ? O3 C40 H40A 110.0 . . ? C41 C40 H40A 110.0 . . ? O3 C40 H40B 110.0 . . ? C41 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? C40 C41 C42 111.1(4) . . ? C40 C41 H41A 109.4 . . ? C42 C41 H41A 109.4 . . ? C40 C41 H41B 109.4 . . ? C42 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O4 C43 C44 109.4(3) . . ? O4 C43 H43A 109.8 . . ? C44 C43 H43A 109.8 . . ? O4 C43 H43B 109.8 . . ? C44 C43 H43B 109.8 . . ? H43A C43 H43B 108.2 . . ? O5 C44 N3 125.0(4) . . ? O5 C44 C43 120.6(4) . . ? N3 C44 C43 114.4(4) . . ? C46 C45 N3 126.4(4) . . ? C46 C45 C53 117.7(4) . . ? N3 C45 C53 115.9(4) . . ? C45 C46 C47 119.3(4) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? C46 C47 C48 122.9(4) . . ? C46 C47 C52 119.1(4) . . ? C48 C47 C52 118.0(4) . . ? C49 C48 C47 121.2(4) . . ? C49 C48 H48 119.4 . . ? C47 C48 H48 119.4 . . ? C48 C49 C50 120.8(4) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C51 C50 C49 119.9(4) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C50 C51 C52 120.6(4) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? N4 C52 C51 119.7(4) . . ? N4 C52 C47 120.7(4) . . ? C51 C52 C47 119.6(4) . . ? N4 C53 C45 125.1(4) . . ? N4 C53 H53 117.5 . . ? C45 C53 H53 117.5 . . ? O6 C54 C55 108.3(3) . . ? O6 C54 H54A 110.0 . . ? C55 C54 H54A 110.0 . . ? O6 C54 H54B 110.0 . . ? C55 C54 H54B 110.0 . . ? H54A C54 H54B 108.4 . . ? C54 C55 C56 110.6(4) . . ? C54 C55 H55A 109.5 . . ? C56 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 108.1 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C57 O7 C85 114.5(3) . . ? C69 O9 C96 113.4(3) . . ? C76 O10 C99 117.4(3) . . ? C83 O12 C110 113.0(3) . . ? C86 N5 C87 128.4(3) . . ? C86 N5 H5C 115.8 . . ? C87 N5 H5C 115.8 . . ? C95 N6 C94 117.5(4) . . ? C100 N7 C101 128.3(3) . . ? C100 N7 H7C 115.8 . . ? C101 N7 H7C 115.8 . . ? C109 N8 C108 118.1(3) . . ? C58 C57 C62 122.9(4) . . ? C58 C57 O7 118.4(3) . . ? C62 C57 O7 118.7(3) . . ? C57 C58 C59 117.3(4) . . ? C57 C58 C84 121.8(4) . . ? C59 C58 C84 120.9(4) . . ? C60 C59 C58 120.9(4) . . ? C60 C59 H59 119.6 . . ? C58 C59 H59 119.6 . . ? C61 C60 C59 119.9(4) . . ? C61 C60 H60 120.1 . . ? C59 C60 H60 120.1 . . ? C60 C61 C62 121.3(4) . . ? C60 C61 H61 119.4 . . ? C62 C61 H61 119.4 . . ? C61 C62 C57 117.4(4) . . ? C61 C62 C63 120.1(4) . . ? C57 C62 C63 122.5(4) . . ? C64 C63 C62 116.8(3) . . ? C64 C63 H63A 108.1 . . ? C62 C63 H63A 108.1 . . ? C64 C63 H63B 108.1 . . ? C62 C63 H63B 108.1 . . ? H63A C63 H63B 107.3 . . ? C69 C64 C65 117.1(4) . . ? C69 C64 C63 123.3(4) . . ? C65 C64 C63 119.3(4) . . ? C66 C65 C64 122.0(4) . . ? C66 C65 H65 119.0 . . ? C64 C65 H65 119.0 . . ? C65 C66 C67 119.1(4) . . ? C65 C66 H66 120.5 . . ? C67 C66 H66 120.5 . . ? C66 C67 C68 121.6(4) . . ? C66 C67 H67 119.2 . . ? C68 C67 H67 119.2 . . ? C67 C68 C69 117.6(4) . . ? C67 C68 C70 120.6(4) . . ? C69 C68 C70 121.7(4) . . ? C64 C69 O9 120.0(4) . . ? C64 C69 C68 122.5(4) . . ? O9 C69 C68 117.3(4) . . ? C71 C70 C68 116.8(3) . . ? C71 C70 H70A 108.1 . . ? C68 C70 H70A 108.1 . . ? C71 C70 H70B 108.1 . . ? C68 C70 H70B 108.1 . . ? H70A C70 H70B 107.3 . . ? C76 C71 C72 116.8(4) . . ? C76 C71 C70 124.0(4) . . ? C72 C71 C70 119.2(4) . . ? C73 C72 C71 121.9(4) . . ? C73 C72 H72 119.1 . . ? C71 C72 H72 119.1 . . ? C72 C73 C74 119.3(4) . . ? C72 C73 H73 120.3 . . ? C74 C73 H73 120.3 . . ? C75 C74 C73 121.3(4) . . ? C75 C74 H74 119.3 . . ? C73 C74 H74 119.3 . . ? C74 C75 C76 117.7(4) . . ? C74 C75 C77 120.6(4) . . ? C76 C75 C77 121.7(4) . . ? C71 C76 C75 123.0(4) . . ? C71 C76 O10 119.2(3) . . ? C75 C76 O10 117.7(4) . . ? C78 C77 C75 117.2(3) . . ? C78 C77 H77A 108.0 . . ? C75 C77 H77A 108.0 . . ? C78 C77 H77B 108.0 . . ? C75 C77 H77B 108.0 . . ? H77A C77 H77B 107.2 . . ? C83 C78 C79 117.2(4) . . ? C83 C78 C77 121.9(4) . . ? C79 C78 C77 120.9(4) . . ? C80 C79 C78 121.0(4) . . ? C80 C79 H79 119.5 . . ? C78 C79 H79 119.5 . . ? C79 C80 C81 120.7(4) . . ? C79 C80 H80 119.6 . . ? C81 C80 H80 119.6 . . ? C80 C81 C82 120.3(4) . . ? C80 C81 H81 119.8 . . ? C82 C81 H81 119.8 . . ? C83 C82 C81 117.8(4) . . ? C83 C82 C84 121.8(4) . . ? C81 C82 C84 120.3(4) . . ? C82 C83 O12 119.3(4) . . ? C82 C83 C78 122.7(4) . . ? O12 C83 C78 117.9(4) . . ? C58 C84 C82 113.8(3) . . ? C58 C84 H84A 108.8 . . ? C82 C84 H84A 108.8 . . ? C58 C84 H84B 108.8 . . ? C82 C84 H84B 108.8 . . ? H84A C84 H84B 107.7 . . ? O7 C85 C86 110.8(3) . . ? O7 C85 H85A 109.5 . . ? C86 C85 H85A 109.5 . . ? O7 C85 H85B 109.5 . . ? C86 C85 H85B 109.5 . . ? H85A C85 H85B 108.1 . . ? O8 C86 N5 124.3(4) . . ? O8 C86 C85 121.4(4) . . ? N5 C86 C85 114.2(3) . . ? C88 C87 N5 125.3(4) . . ? C88 C87 C95 118.3(4) . . ? N5 C87 C95 116.5(4) . . ? C87 C88 C89 118.2(4) . . ? C87 C88 H88 120.9 . . ? C89 C88 H88 120.9 . . ? C94 C89 C90 118.9(4) . . ? C94 C89 C88 119.4(4) . . ? C90 C89 C88 121.7(4) . . ? C91 C90 C89 119.6(4) . . ? C91 C90 H90 120.2 . . ? C89 C90 H90 120.2 . . ? C90 C91 C92 120.9(4) . . ? C90 C91 H91 119.5 . . ? C92 C91 H91 119.5 . . ? C93 C92 C91 120.3(4) . . ? C93 C92 H92 119.9 . . ? C91 C92 H92 119.9 . . ? C92 C93 C94 120.5(4) . . ? C92 C93 H93 119.8 . . ? C94 C93 H93 119.8 . . ? N6 C94 C93 118.9(4) . . ? N6 C94 C89 121.4(4) . . ? C93 C94 C89 119.7(4) . . ? N6 C95 C87 125.3(4) . . ? N6 C95 H95 117.4 . . ? C87 C95 H95 117.4 . . ? O9 C96 C97 109.5(3) . . ? O9 C96 H96A 109.8 . . ? C97 C96 H96A 109.8 . . ? O9 C96 H96B 109.8 . . ? C97 C96 H96B 109.8 . . ? H96A C96 H96B 108.2 . . ? C96 C97 C98 110.5(4) . . ? C96 C97 H97A 109.6 . . ? C98 C97 H97A 109.6 . . ? C96 C97 H97B 109.6 . . ? C98 C97 H97B 109.6 . . ? H97A C97 H97B 108.1 . . ? C97 C98 H98A 109.5 . . ? C97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? O10 C99 C100 109.1(3) . . ? O10 C99 H99A 109.9 . . ? C100 C99 H99A 109.9 . . ? O10 C99 H99B 109.9 . . ? C100 C99 H99B 109.9 . . ? H99A C99 H99B 108.3 . . ? O11 C100 N7 124.0(4) . . ? O11 C100 C99 121.3(4) . . ? N7 C100 C99 114.8(3) . . ? C102 C101 N7 125.8(4) . . ? C102 C101 C109 118.6(4) . . ? N7 C101 C109 115.6(3) . . ? C101 C102 C103 118.0(4) . . ? C101 C102 H102 121.0 . . ? C103 C102 H102 121.0 . . ? C108 C103 C102 119.8(4) . . ? C108 C103 C104 117.6(4) . . ? C102 C103 C104 122.6(4) . . ? C105 C104 C103 120.6(4) . . ? C105 C104 H104 119.7 . . ? C103 C104 H104 119.7 . . ? C104 C105 C106 120.7(4) . . ? C104 C105 H105 119.7 . . ? C106 C105 H105 119.7 . . ? C107 C106 C105 120.3(4) . . ? C107 C106 H106 119.9 . . ? C105 C106 H106 119.9 . . ? C106 C107 C108 119.8(4) . . ? C106 C107 H107 120.1 . . ? C108 C107 H107 120.1 . . ? N8 C108 C107 118.6(4) . . ? N8 C108 C103 120.5(4) . . ? C107 C108 C103 120.9(4) . . ? N8 C109 C101 124.7(4) . . ? N8 C109 H109 117.6 . . ? C101 C109 H109 117.6 . . ? C111 C110 O12 114.5(4) . . ? C111 C110 H10E 108.6 . . ? O12 C110 H10E 108.6 . . ? C111 C110 H10D 108.6 . . ? O12 C110 H10D 108.6 . . ? H10E C110 H10D 107.6 . . ? C110 C111 C112 119.1(5) . . ? C110 C111 H11E 107.5 . . ? C112 C111 H11E 107.5 . . ? C110 C111 H11D 107.5 . . ? C112 C111 H11D 107.5 . . ? H11E C111 H11D 107.0 . . ? C111 C112 H12F 109.5 . . ? C111 C112 H12E 109.5 . . ? H12F C112 H12E 109.5 . . ? C111 C112 H12D 109.5 . . ? H12F C112 H12D 109.5 . . ? H12E C112 H12D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.417 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.061 data_Hgcomplex2 _database_code_depnum_ccdc_archive 'CCDC 860244' #TrackingRef 'Hgcomplex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H44 Cl4 Hg2 N4 O7' _chemical_formula_weight 1367.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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 15.4628(9) _cell_length_b 24.0204(16) _cell_length_c 13.4669(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.6380(10) _cell_angle_gamma 90.00 _cell_volume 4860.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4413 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 21.67 _exptl_crystal_description PLATES _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 6.586 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.2198 _exptl_absorpt_correction_T_max 0.5054 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'Omega-Phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24328 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10494 _reflns_number_gt 6537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.1235P)^2^+1.4383P] 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 10494 _refine_ls_number_parameters 612 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.2121 _refine_ls_wR_factor_gt 0.1847 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.65256(3) 0.851753(17) 0.76424(4) 0.05738(17) Uani 1 d . . . Hg2 Hg 0.41742(3) 0.51948(2) 0.57859(4) 0.0682(2) Uani 1 d . . . Cl1 Cl 0.3327(3) 0.43769(15) 0.5660(3) 0.0887(11) Uani 1 d . . . Cl2 Cl 0.57921(19) 0.48225(11) 0.6319(2) 0.0632(7) Uani 1 d . . . Cl3 Cl 0.7905(2) 0.82291(14) 0.8576(3) 0.0731(9) Uani 1 d . . . Cl4 Cl 0.5453(3) 0.89106(17) 0.6362(3) 0.0880(11) Uani 1 d . . . O1 O 0.8230(4) 0.6526(3) 0.9093(5) 0.0463(16) Uani 1 d . . . H1C H 0.8334 0.6628 0.8552 0.069 Uiso 1 calc R . . O2 O 0.7298(4) 0.5488(2) 0.9061(5) 0.0420(15) Uani 1 d . . . O3 O 0.7902(5) 0.5610(2) 0.7319(5) 0.0495(17) Uani 1 d . . . H3C H 0.7551 0.5495 0.7642 0.074 Uiso 1 calc R . . O4 O 0.8378(4) 0.6753(3) 0.7097(5) 0.0422(15) Uani 1 d . . . O5 O 0.4996(5) 0.5657(3) 0.8746(8) 0.073(2) Uani 1 d . . . O6 O 0.6787(4) 0.7723(3) 0.5965(6) 0.0527(17) Uani 1 d . . . N1 N 0.6109(5) 0.6292(3) 0.8830(6) 0.0426(18) Uani 1 d . . . H1A H 0.6674 0.6320 0.8897 0.051 Uiso 1 calc R . . N2 N 0.5705(6) 0.7772(3) 0.8393(6) 0.0470(19) Uani 1 d . . . N3 N 0.6657(5) 0.6799(3) 0.6260(6) 0.0405(18) Uani 1 d . . . H3A H 0.6965 0.6501 0.6423 0.049 Uiso 1 calc R . . N4 N 0.4550(6) 0.6076(4) 0.5931(7) 0.053(2) Uani 1 d . . . C1 C 0.9589(6) 0.7051(4) 0.9759(8) 0.044(2) Uani 1 d . . . C2 C 1.0228(6) 0.7191(4) 1.0619(9) 0.050(3) Uani 1 d . . . H2 H 1.0670 0.7441 1.0555 0.060 Uiso 1 calc R . . C3 C 1.0241(7) 0.6974(4) 1.1582(10) 0.058(3) Uani 1 d . . . H3 H 1.0674 0.7082 1.2153 0.070 Uiso 1 calc R . . C4 C 0.9579(7) 0.6586(4) 1.1665(9) 0.052(3) Uani 1 d . . . H4 H 0.9594 0.6427 1.2299 0.062 Uiso 1 calc R . . C5 C 0.8915(6) 0.6433(4) 1.0844(8) 0.042(2) Uani 1 d . . . C6 C 0.8921(6) 0.6672(4) 0.9882(8) 0.043(2) Uani 1 d . . . C7 C 0.8246(6) 0.5991(4) 1.0949(7) 0.0361(19) Uani 1 d . . . H7A H 0.7661 0.6101 1.0558 0.043 Uiso 1 calc R . . H7B H 0.8223 0.5961 1.1660 0.043 Uiso 1 calc R . . C8 C 0.8489(6) 0.5425(4) 1.0569(7) 0.038(2) Uani 1 d . . . C9 C 0.9208(7) 0.5142(4) 1.1121(8) 0.045(2) Uani 1 d . . . H9 H 0.9528 0.5290 1.1736 0.054 Uiso 1 calc R . . C10 C 0.9473(6) 0.4633(4) 1.0780(8) 0.044(2) Uani 1 d . . . H10 H 0.9950 0.4436 1.1175 0.053 Uiso 1 calc R . . C11 C 0.9018(6) 0.4432(4) 0.9857(8) 0.045(2) Uani 1 d . . . H11 H 0.9203 0.4099 0.9619 0.054 Uiso 1 calc R . . C12 C 0.8289(6) 0.4706(4) 0.9262(8) 0.041(2) Uani 1 d . . . C13 C 0.8032(5) 0.5204(3) 0.9649(7) 0.0354(19) Uani 1 d . . . C14 C 0.7825(7) 0.4482(4) 0.8212(7) 0.046(2) Uani 1 d . . . H14A H 0.7780 0.4080 0.8261 0.056 Uiso 1 calc R . . H14B H 0.7223 0.4629 0.8036 0.056 Uiso 1 calc R . . C15 C 0.8264(6) 0.4614(4) 0.7346(7) 0.040(2) Uani 1 d . . . C16 C 0.8650(7) 0.4197(4) 0.6900(8) 0.053(3) Uani 1 d . . . H16 H 0.8638 0.3836 0.7145 0.063 Uiso 1 calc R . . C17 C 0.9057(8) 0.4292(5) 0.6100(10) 0.065(3) Uani 1 d . . . H17 H 0.9298 0.3999 0.5804 0.078 Uiso 1 calc R . . C18 C 0.9096(7) 0.4833(5) 0.5751(9) 0.059(3) Uani 1 d . . . H18 H 0.9369 0.4903 0.5218 0.070 Uiso 1 calc R . . C19 C 0.8726(7) 0.5276(4) 0.6196(8) 0.050(2) Uani 1 d . . . C20 C 0.8296(6) 0.5166(4) 0.6953(8) 0.042(2) Uani 1 d . . . C21 C 0.8830(7) 0.5871(5) 0.5850(8) 0.051(3) Uani 1 d . . . H21A H 0.9010 0.5863 0.5207 0.062 Uiso 1 calc R . . H21B H 0.8259 0.6058 0.5734 0.062 Uiso 1 calc R . . C22 C 0.9503(7) 0.6194(4) 0.6619(8) 0.047(2) Uani 1 d . . . C23 C 1.0414(7) 0.6066(5) 0.6771(8) 0.054(3) Uani 1 d . . . H23 H 1.0593 0.5799 0.6361 0.065 Uiso 1 calc R . . C24 C 1.1047(7) 0.6331(5) 0.7520(10) 0.058(3) Uani 1 d . . . H24 H 1.1647 0.6245 0.7603 0.069 Uiso 1 calc R . . C25 C 1.0789(7) 0.6724(4) 0.8147(8) 0.049(2) Uani 1 d . . . H25 H 1.1217 0.6893 0.8660 0.059 Uiso 1 calc R . . C26 C 0.9902(6) 0.6868(4) 0.8018(8) 0.042(2) Uani 1 d . . . C27 C 0.9296(6) 0.6603(4) 0.7240(9) 0.046(2) Uani 1 d . . . C28 C 0.9624(6) 0.7281(4) 0.8716(9) 0.049(2) Uani 1 d . . . H28A H 0.9040 0.7423 0.8385 0.059 Uiso 1 calc R . . H28B H 1.0036 0.7592 0.8814 0.059 Uiso 1 calc R . . C29 C 0.6454(6) 0.5309(4) 0.9196(9) 0.050(3) Uani 1 d . . . H29A H 0.6504 0.5211 0.9906 0.060 Uiso 1 calc R . . H29B H 0.6262 0.4982 0.8781 0.060 Uiso 1 calc R . . C30 C 0.5774(7) 0.5769(4) 0.8889(8) 0.050(2) Uani 1 d . . . C31 C 0.5608(7) 0.6787(4) 0.8667(8) 0.047(2) Uani 1 d . . . C32 C 0.6076(6) 0.7272(4) 0.8541(7) 0.040(2) Uani 1 d . . . H32 H 0.6680 0.7241 0.8563 0.047 Uiso 1 calc R . . C33 C 0.4802(6) 0.7822(4) 0.8370(7) 0.045(2) Uani 1 d . . . C34 C 0.4415(7) 0.8347(4) 0.8310(8) 0.050(2) Uani 1 d . . . H34 H 0.4756 0.8664 0.8288 0.060 Uiso 1 calc R . . C35 C 0.3514(8) 0.8395(5) 0.8283(9) 0.061(3) Uani 1 d . . . H35 H 0.3255 0.8746 0.8258 0.074 Uiso 1 calc R . . C36 C 0.2994(7) 0.7920(5) 0.8293(8) 0.054(3) Uani 1 d . . . H36 H 0.2386 0.7956 0.8243 0.065 Uiso 1 calc R . . C37 C 0.3372(7) 0.7407(4) 0.8375(8) 0.050(2) Uani 1 d . . . H37 H 0.3020 0.7095 0.8387 0.060 Uiso 1 calc R . . C38 C 0.4297(6) 0.7340(4) 0.8443(7) 0.046(2) Uani 1 d . . . C39 C 0.4724(6) 0.6816(4) 0.8583(7) 0.045(2) Uani 1 d . . . H39 H 0.4397 0.6494 0.8615 0.054 Uiso 1 calc R . . C40 C 0.8107(6) 0.7212(4) 0.6407(8) 0.047(2) Uani 1 d . . . H40A H 0.8288 0.7144 0.5775 0.057 Uiso 1 calc R . . H40B H 0.8395 0.7551 0.6710 0.057 Uiso 1 calc R . . C41 C 0.7133(6) 0.7280(4) 0.6191(7) 0.039(2) Uani 1 d . . . C42 C 0.5727(6) 0.6741(4) 0.6094(7) 0.039(2) Uani 1 d . . . C43 C 0.5400(6) 0.6210(4) 0.6060(7) 0.047(2) Uani 1 d . . . H43 H 0.5808 0.5920 0.6133 0.056 Uiso 1 calc R . . C44 C 0.3953(7) 0.6515(5) 0.5879(8) 0.052(3) Uani 1 d . . . C45 C 0.3036(7) 0.6386(6) 0.5748(10) 0.064(3) Uani 1 d . . . H45 H 0.2841 0.6019 0.5694 0.077 Uiso 1 calc R . . C46 C 0.2438(8) 0.6823(6) 0.5702(11) 0.076(4) Uani 1 d . . . H46 H 0.1840 0.6744 0.5646 0.091 Uiso 1 calc R . . C47 C 0.2715(9) 0.7385(7) 0.5738(10) 0.078(4) Uani 1 d . . . H47 H 0.2301 0.7670 0.5682 0.094 Uiso 1 calc R . . C48 C 0.3618(7) 0.7507(5) 0.5858(8) 0.052(3) Uani 1 d . . . H48 H 0.3811 0.7875 0.5914 0.063 Uiso 1 calc R . . C49 C 0.4234(6) 0.7070(4) 0.5895(7) 0.045(2) Uani 1 d . . . C50 C 0.5155(6) 0.7177(4) 0.6008(7) 0.043(2) Uani 1 d . . . H50 H 0.5364 0.7541 0.6022 0.052 Uiso 1 calc R . . C51 C 0.2788(13) 0.5074(11) 0.7678(19) 0.161(10) Uani 1 d . . . H51A H 0.3074 0.4769 0.8086 0.241 Uiso 1 calc R . . H51B H 0.2427 0.4935 0.7047 0.241 Uiso 1 calc R . . H51C H 0.2419 0.5271 0.8043 0.241 Uiso 1 calc R . . O7 O 0.3481(12) 0.5463(8) 0.7455(14) 0.171(6) Uiso 1 d . . . H7 H 0.3546 0.5727 0.7852 0.257 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0581(3) 0.0434(3) 0.0671(3) 0.00063(19) 0.0078(2) 0.00436(18) Hg2 0.0573(3) 0.0576(3) 0.0820(4) 0.0120(2) 0.0010(3) -0.0235(2) Cl1 0.084(2) 0.077(2) 0.093(2) 0.0251(19) -0.0025(19) -0.0386(18) Cl2 0.0571(17) 0.0485(15) 0.0710(19) 0.0095(13) -0.0113(14) -0.0066(12) Cl3 0.0592(18) 0.075(2) 0.082(2) -0.0125(16) 0.0104(16) 0.0196(15) Cl4 0.097(3) 0.090(3) 0.070(2) 0.0225(19) 0.0062(19) 0.024(2) O1 0.040(4) 0.047(4) 0.050(4) -0.002(3) 0.008(3) -0.011(3) O2 0.037(4) 0.033(3) 0.053(4) 0.007(3) 0.006(3) 0.006(3) O3 0.068(5) 0.027(3) 0.057(4) 0.007(3) 0.022(4) 0.004(3) O4 0.032(3) 0.039(4) 0.052(4) 0.014(3) 0.004(3) 0.000(3) O5 0.033(4) 0.056(5) 0.122(7) -0.007(5) 0.003(4) 0.003(3) O6 0.043(4) 0.032(4) 0.080(5) 0.004(3) 0.008(4) -0.002(3) N1 0.033(4) 0.035(4) 0.054(5) 0.002(4) -0.002(4) 0.003(3) N2 0.051(5) 0.039(5) 0.050(5) 0.005(4) 0.011(4) 0.012(4) N3 0.025(4) 0.031(4) 0.061(5) 0.001(3) 0.001(4) -0.001(3) N4 0.045(5) 0.052(5) 0.062(6) 0.006(4) 0.010(4) -0.014(4) C1 0.028(5) 0.027(4) 0.072(7) -0.005(4) 0.003(5) 0.006(3) C2 0.032(5) 0.038(5) 0.082(8) -0.006(5) 0.019(5) -0.004(4) C3 0.039(6) 0.043(6) 0.085(9) -0.021(6) 0.000(6) 0.002(4) C4 0.043(6) 0.048(6) 0.059(7) -0.006(5) 0.001(5) 0.013(5) C5 0.039(5) 0.036(5) 0.052(6) -0.005(4) 0.010(5) 0.011(4) C6 0.030(5) 0.031(5) 0.068(7) -0.009(4) 0.009(5) 0.001(4) C7 0.037(5) 0.035(5) 0.036(5) -0.004(4) 0.008(4) 0.002(4) C8 0.036(5) 0.035(5) 0.043(5) 0.001(4) 0.013(4) 0.000(4) C9 0.048(6) 0.041(5) 0.046(6) -0.004(4) 0.011(5) -0.002(4) C10 0.031(5) 0.042(5) 0.054(6) 0.004(4) 0.000(5) 0.005(4) C11 0.043(6) 0.032(5) 0.057(6) -0.004(4) 0.005(5) 0.003(4) C12 0.034(5) 0.032(5) 0.055(6) 0.000(4) 0.006(5) 0.001(4) C13 0.027(4) 0.030(4) 0.047(5) 0.008(4) 0.004(4) 0.005(3) C14 0.049(6) 0.038(5) 0.047(6) -0.002(4) -0.001(5) -0.002(4) C15 0.040(5) 0.030(5) 0.045(5) -0.005(4) -0.002(4) 0.002(4) C16 0.052(6) 0.037(5) 0.064(7) -0.015(5) 0.003(6) 0.003(4) C17 0.049(7) 0.062(8) 0.081(8) -0.025(6) 0.007(6) 0.004(5) C18 0.044(6) 0.069(8) 0.063(7) -0.013(6) 0.014(6) -0.002(5) C19 0.047(6) 0.049(6) 0.054(6) -0.005(5) 0.013(5) -0.002(4) C20 0.042(5) 0.034(5) 0.048(6) -0.002(4) 0.007(5) 0.002(4) C21 0.041(6) 0.061(7) 0.054(6) -0.009(5) 0.015(5) -0.008(5) C22 0.046(6) 0.042(6) 0.052(6) 0.007(4) 0.010(5) -0.003(4) C23 0.052(7) 0.052(6) 0.062(7) 0.009(5) 0.021(6) 0.002(5) C24 0.038(6) 0.057(7) 0.082(8) 0.007(6) 0.021(6) 0.000(5) C25 0.038(5) 0.046(6) 0.059(7) 0.007(5) 0.003(5) -0.007(4) C26 0.028(5) 0.034(5) 0.062(6) 0.004(4) 0.007(5) -0.008(4) C27 0.033(5) 0.034(5) 0.074(7) 0.020(5) 0.018(5) 0.003(4) C28 0.033(5) 0.034(5) 0.079(7) 0.002(5) 0.011(5) -0.004(4) C29 0.039(5) 0.031(5) 0.076(7) 0.008(5) 0.007(5) -0.006(4) C30 0.037(6) 0.049(6) 0.060(7) -0.002(5) 0.007(5) 0.004(4) C31 0.050(6) 0.035(5) 0.058(6) -0.005(4) 0.020(5) 0.009(4) C32 0.034(5) 0.046(5) 0.038(5) -0.008(4) 0.005(4) 0.002(4) C33 0.044(6) 0.049(6) 0.041(5) 0.001(4) 0.008(5) 0.009(4) C34 0.057(7) 0.038(5) 0.053(6) 0.003(4) 0.013(5) 0.009(5) C35 0.062(7) 0.053(7) 0.062(7) -0.004(5) 0.000(6) 0.034(6) C36 0.044(6) 0.068(7) 0.044(6) 0.008(5) -0.004(5) 0.021(5) C37 0.041(6) 0.052(6) 0.057(6) 0.002(5) 0.011(5) 0.017(4) C38 0.042(6) 0.054(6) 0.037(5) 0.003(4) -0.002(4) 0.006(4) C39 0.039(5) 0.050(6) 0.043(5) 0.009(4) 0.002(4) 0.009(4) C40 0.043(6) 0.035(5) 0.063(7) 0.011(5) 0.010(5) -0.003(4) C41 0.032(5) 0.035(5) 0.046(5) 0.002(4) 0.004(4) -0.003(4) C42 0.032(5) 0.041(5) 0.042(5) 0.000(4) 0.003(4) 0.000(4) C43 0.033(5) 0.056(6) 0.045(6) 0.005(5) -0.003(4) -0.008(4) C44 0.040(6) 0.064(7) 0.051(6) 0.008(5) 0.007(5) 0.004(5) C45 0.039(6) 0.078(8) 0.076(8) 0.019(6) 0.013(6) -0.006(5) C46 0.038(6) 0.103(11) 0.087(10) 0.026(8) 0.016(6) 0.003(6) C47 0.060(8) 0.101(11) 0.080(9) 0.002(8) 0.029(7) 0.014(7) C48 0.044(6) 0.063(7) 0.046(6) 0.001(5) 0.003(5) 0.008(5) C49 0.039(5) 0.051(6) 0.044(6) 0.000(4) 0.009(5) 0.002(4) C50 0.045(6) 0.043(5) 0.038(5) -0.004(4) 0.003(4) -0.008(4) C51 0.098(14) 0.22(3) 0.19(2) 0.05(2) 0.092(16) 0.005(15) _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 Hg1 Cl4 2.296(3) . ? Hg1 Cl3 2.312(3) . ? Hg1 N2 2.538(8) . ? Hg2 N4 2.190(9) . ? Hg2 Cl1 2.346(3) . ? Hg2 Cl2 2.594(3) . ? Hg2 Cl2 2.847(3) 3_666 ? Cl2 Hg2 2.847(3) 3_666 ? O1 C6 1.363(12) . ? O1 H1C 0.8200 . ? O2 C13 1.400(10) . ? O2 C29 1.426(11) . ? O3 C20 1.376(11) . ? O3 H3C 0.8200 . ? O4 C27 1.432(11) . ? O4 C40 1.440(11) . ? O5 C30 1.204(12) . ? O6 C41 1.198(11) . ? N1 C30 1.367(13) . ? N1 C31 1.407(12) . ? N1 H1A 0.8600 . ? N2 C32 1.326(12) . ? N2 C33 1.395(12) . ? N3 C41 1.385(11) . ? N3 C42 1.408(11) . ? N3 H3A 0.8600 . ? N4 C43 1.325(12) . ? N4 C44 1.393(14) . ? C1 C2 1.375(14) . ? C1 C6 1.415(13) . ? C1 C28 1.523(15) . ? C2 C3 1.394(16) . ? C2 H2 0.9300 . ? C3 C4 1.407(15) . ? C3 H3 0.9300 . ? C4 C5 1.370(15) . ? C4 H4 0.9300 . ? C5 C6 1.419(14) . ? C5 C7 1.511(13) . ? C7 C8 1.531(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.363(13) . ? C8 C13 1.379(13) . ? C9 C10 1.401(13) . ? C9 H9 0.9300 . ? C10 C11 1.364(14) . ? C10 H10 0.9300 . ? C11 C12 1.385(13) . ? C11 H11 0.9300 . ? C12 C13 1.400(12) . ? C12 C14 1.525(13) . ? C14 C15 1.515(14) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.375(13) . ? C15 C20 1.431(13) . ? C16 C17 1.389(17) . ? C16 H16 0.9300 . ? C17 C18 1.388(17) . ? C17 H17 0.9300 . ? C18 C19 1.409(15) . ? C18 H18 0.9300 . ? C19 C20 1.368(14) . ? C19 C21 1.522(15) . ? C21 C22 1.500(14) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.377(14) . ? C22 C23 1.408(14) . ? C23 C24 1.385(16) . ? C23 H23 0.9300 . ? C24 C25 1.386(16) . ? C24 H24 0.9300 . ? C25 C26 1.385(13) . ? C25 H25 0.9300 . ? C26 C27 1.385(15) . ? C26 C28 1.497(14) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.513(14) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C31 C39 1.347(13) . ? C31 C32 1.403(13) . ? C32 H32 0.9300 . ? C33 C34 1.389(14) . ? C33 C38 1.414(14) . ? C34 C35 1.391(15) . ? C34 H34 0.9300 . ? C35 C36 1.398(17) . ? C35 H35 0.9300 . ? C36 C37 1.357(14) . ? C36 H36 0.9300 . ? C37 C38 1.421(13) . ? C37 H37 0.9300 . ? C38 C39 1.413(14) . ? C39 H39 0.9300 . ? C40 C41 1.475(13) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C42 C50 1.359(13) . ? C42 C43 1.369(13) . ? C43 H43 0.9300 . ? C44 C49 1.400(15) . ? C44 C45 1.420(15) . ? C45 C46 1.391(18) . ? C45 H45 0.9300 . ? C46 C47 1.41(2) . ? C46 H46 0.9300 . ? C47 C48 1.399(16) . ? C47 H47 0.9300 . ? C48 C49 1.411(14) . ? C48 H48 0.9300 . ? C49 C50 1.420(13) . ? C50 H50 0.9300 . ? C51 O7 1.50(2) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? O7 H7 0.8200 . ? 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 Cl4 Hg1 Cl3 160.47(14) . . ? Cl4 Hg1 N2 104.4(2) . . ? Cl3 Hg1 N2 93.2(2) . . ? N4 Hg2 Cl1 161.3(3) . . ? N4 Hg2 Cl2 95.2(2) . . ? Cl1 Hg2 Cl2 102.54(12) . . ? N4 Hg2 Cl2 92.1(2) . 3_666 ? Cl1 Hg2 Cl2 93.26(11) . 3_666 ? Cl2 Hg2 Cl2 91.58(9) . 3_666 ? Hg2 Cl2 Hg2 88.42(8) . 3_666 ? C6 O1 H1C 109.5 . . ? C13 O2 C29 115.2(7) . . ? C20 O3 H3C 109.5 . . ? C27 O4 C40 114.0(6) . . ? C30 N1 C31 125.6(8) . . ? C30 N1 H1A 117.2 . . ? C31 N1 H1A 117.2 . . ? C32 N2 C33 118.5(8) . . ? C32 N2 Hg1 117.4(6) . . ? C33 N2 Hg1 121.4(6) . . ? C41 N3 C42 127.7(8) . . ? C41 N3 H3A 116.2 . . ? C42 N3 H3A 116.2 . . ? C43 N4 C44 116.6(9) . . ? C43 N4 Hg2 118.7(7) . . ? C44 N4 Hg2 124.7(7) . . ? C2 C1 C6 117.3(10) . . ? C2 C1 C28 120.9(9) . . ? C6 C1 C28 121.8(9) . . ? C1 C2 C3 122.8(9) . . ? C1 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? C2 C3 C4 118.1(10) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 122.3(11) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 117.6(9) . . ? C4 C5 C7 120.8(9) . . ? C6 C5 C7 121.4(9) . . ? O1 C6 C1 122.3(9) . . ? O1 C6 C5 115.8(8) . . ? C1 C6 C5 121.9(9) . . ? C5 C7 C8 111.4(7) . . ? C5 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? C5 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C13 118.4(8) . . ? C9 C8 C7 119.6(8) . . ? C13 C8 C7 121.8(8) . . ? C8 C9 C10 121.4(9) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C11 C10 C9 118.7(9) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C12 122.3(9) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C11 C12 C13 117.0(9) . . ? C11 C12 C14 120.7(8) . . ? C13 C12 C14 122.3(8) . . ? C8 C13 O2 119.7(8) . . ? C8 C13 C12 122.2(8) . . ? O2 C13 C12 118.0(8) . . ? C15 C14 C12 116.1(8) . . ? C15 C14 H14A 108.3 . . ? C12 C14 H14A 108.3 . . ? C15 C14 H14B 108.3 . . ? C12 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C16 C15 C20 117.2(9) . . ? C16 C15 C14 120.1(9) . . ? C20 C15 C14 122.7(8) . . ? C15 C16 C17 122.8(10) . . ? C15 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? C18 C17 C16 118.7(10) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 120.6(10) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 119.2(10) . . ? C20 C19 C21 121.0(9) . . ? C18 C19 C21 119.8(9) . . ? C19 C20 O3 116.7(8) . . ? C19 C20 C15 121.4(9) . . ? O3 C20 C15 121.9(8) . . ? C22 C21 C19 112.3(9) . . ? C22 C21 H21A 109.1 . . ? C19 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? C19 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? C27 C22 C23 115.8(10) . . ? C27 C22 C21 124.4(9) . . ? C23 C22 C21 119.7(9) . . ? C24 C23 C22 121.1(10) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 120.1(10) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.8(10) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 117.0(9) . . ? C25 C26 C28 120.6(9) . . ? C27 C26 C28 122.3(8) . . ? C22 C27 C26 125.0(9) . . ? C22 C27 O4 117.6(9) . . ? C26 C27 O4 117.4(9) . . ? C26 C28 C1 114.6(8) . . ? C26 C28 H28A 108.6 . . ? C1 C28 H28A 108.6 . . ? C26 C28 H28B 108.6 . . ? C1 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? O2 C29 C30 110.1(8) . . ? O2 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? O2 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.2 . . ? O5 C30 N1 125.1(9) . . ? O5 C30 C29 118.9(10) . . ? N1 C30 C29 115.9(8) . . ? C39 C31 C32 119.3(9) . . ? C39 C31 N1 124.6(9) . . ? C32 C31 N1 116.1(8) . . ? N2 C32 C31 123.6(9) . . ? N2 C32 H32 118.2 . . ? C31 C32 H32 118.2 . . ? C34 C33 N2 119.7(9) . . ? C34 C33 C38 120.7(9) . . ? N2 C33 C38 119.6(9) . . ? C33 C34 C35 119.5(10) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 120.5(9) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 120.2(10) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 121.1(11) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C39 C38 C33 119.4(9) . . ? C39 C38 C37 122.8(10) . . ? C33 C38 C37 117.8(9) . . ? C31 C39 C38 119.4(10) . . ? C31 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? O4 C40 C41 109.9(7) . . ? O4 C40 H40A 109.7 . . ? C41 C40 H40A 109.7 . . ? O4 C40 H40B 109.7 . . ? C41 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? O6 C41 N3 123.1(8) . . ? O6 C41 C40 121.5(8) . . ? N3 C41 C40 115.4(8) . . ? C50 C42 C43 119.2(9) . . ? C50 C42 N3 123.8(9) . . ? C43 C42 N3 117.0(8) . . ? N4 C43 C42 125.4(10) . . ? N4 C43 H43 117.3 . . ? C42 C43 H43 117.3 . . ? N4 C44 C49 121.4(9) . . ? N4 C44 C45 118.1(10) . . ? C49 C44 C45 120.4(10) . . ? C46 C45 C44 118.4(12) . . ? C46 C45 H45 120.8 . . ? C44 C45 H45 120.8 . . ? C45 C46 C47 121.7(11) . . ? C45 C46 H46 119.1 . . ? C47 C46 H46 119.1 . . ? C48 C47 C46 119.4(12) . . ? C48 C47 H47 120.3 . . ? C46 C47 H47 120.3 . . ? C47 C48 C49 119.6(11) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C44 C49 C48 120.2(9) . . ? C44 C49 C50 118.4(9) . . ? C48 C49 C50 121.3(10) . . ? C42 C50 C49 119.0(9) . . ? C42 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? O7 C51 H51A 109.5 . . ? O7 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O7 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C51 O7 H7 109.5 . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 4.394 _refine_diff_density_min -1.236 _refine_diff_density_rms 0.187 # Attachment 'Hgcomplex3.cif' data_Hgcomplex3 _database_code_depnum_ccdc_archive 'CCDC 860245' #TrackingRef 'Hgcomplex3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H53 Cl5 Hg N4 O7' _chemical_formula_weight 1283.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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 15.618(4) _cell_length_b 17.009(4) _cell_length_c 19.256(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.062(4) _cell_angle_gamma 90.00 _cell_volume 5095(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6336 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.38 _exptl_crystal_description Plates _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 3.343 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.3961 _exptl_absorpt_correction_T_max 0.8779 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24080 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.1326 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11449 _reflns_number_gt 7677 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0463P)^2^+455.0399P] 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 SHELXL _refine_ls_extinction_coef 0.00094(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11449 _refine_ls_number_parameters 668 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1703 _refine_ls_R_factor_gt 0.1255 _refine_ls_wR_factor_ref 0.3127 _refine_ls_wR_factor_gt 0.2909 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.58912(5) 0.57865(4) 0.32510(4) 0.0165(2) Uani 1 1 d . . . Cl1 Cl 0.7072(3) 0.4902(3) 0.3376(3) 0.0251(10) Uani 1 1 d . . . Cl2 Cl 0.4427(3) 0.5533(3) 0.3159(3) 0.0260(10) Uani 1 1 d . . . N1 N 0.8611(10) 0.7068(9) 0.2071(8) 0.018(3) Uani 1 1 d . . . H1 H 0.8875 0.7097 0.2481 0.022 Uiso 1 1 calc R . . N2 N 0.6432(10) 0.6635(8) 0.2437(7) 0.016(3) Uani 1 1 d . . . N3 N 0.8413(10) 0.7507(8) 0.4598(7) 0.016(3) Uani 1 1 d . . . H3C H 0.8694 0.7614 0.4991 0.019 Uiso 1 1 calc R . . N4 N 0.6309(11) 0.6736(9) 0.4117(7) 0.018(3) Uani 1 1 d . . . O1 O 1.0254(9) 0.7141(8) 0.2404(7) 0.022(3) Uani 1 1 d . . . O2 O 0.8778(10) 0.6907(9) 0.0953(8) 0.033(4) Uani 1 1 d . . . O3 O 1.1852(9) 0.6096(8) 0.4252(7) 0.025(3) Uani 1 1 d . . . O4 O 0.9996(8) 0.7690(7) 0.4803(6) 0.019(3) Uani 1 1 d . . . O5 O 0.8482(8) 0.7281(8) 0.3442(6) 0.020(3) Uani 1 1 d . . . O6 O 1.1716(9) 0.9132(7) 0.3670(7) 0.021(3) Uani 1 1 d . . . C1 C 1.1522(14) 0.7918(11) 0.2503(10) 0.025(4) Uani 1 1 d . . . C2 C 1.2388(15) 0.7980(13) 0.2608(10) 0.030(5) Uani 1 1 d . . . H2 H 1.2658 0.8459 0.2551 0.036 Uiso 1 1 calc R . . C3 C 1.2858(15) 0.7323(14) 0.2801(12) 0.034(5) Uani 1 1 d . . . H3 H 1.3453 0.7359 0.2868 0.041 Uiso 1 1 calc R . . C4 C 1.2470(13) 0.6620(12) 0.2896(10) 0.025(4) Uani 1 1 d . . . H4 H 1.2799 0.6185 0.3044 0.030 Uiso 1 1 calc R . . C5 C 1.1607(14) 0.6553(11) 0.2775(11) 0.025(4) Uani 1 1 d . . . C6 C 1.1134(13) 0.7212(13) 0.2545(10) 0.025(4) Uani 1 1 d . . . C7 C 1.1189(12) 0.5786(11) 0.2861(9) 0.020(4) Uani 1 1 d . . . H7A H 1.1629 0.5383 0.2914 0.024 Uiso 1 1 calc R . . H7B H 1.0824 0.5670 0.2439 0.024 Uiso 1 1 calc R . . C8 C 1.0657(12) 0.5746(11) 0.3470(10) 0.020(4) Uani 1 1 d . . . C9 C 0.9805(13) 0.5543(10) 0.3395(10) 0.022(4) Uani 1 1 d . . . H9 H 0.9556 0.5388 0.2960 0.027 Uiso 1 1 calc R . . C10 C 0.9329(15) 0.5565(11) 0.3935(11) 0.027(5) Uani 1 1 d . . . H10 H 0.8753 0.5427 0.3855 0.033 Uiso 1 1 calc R . . C11 C 0.9626(14) 0.5777(11) 0.4608(11) 0.029(5) Uani 1 1 d . . . H11 H 0.9277 0.5792 0.4974 0.034 Uiso 1 1 calc R . . C12 C 1.0511(14) 0.5969(10) 0.4684(10) 0.023(4) Uani 1 1 d . . . C13 C 1.1008(14) 0.5918(9) 0.4141(10) 0.024(4) Uani 1 1 d . . . C14 C 1.0845(13) 0.6320(10) 0.5367(9) 0.021(4) Uani 1 1 d . . . H14A H 1.0372 0.6350 0.5661 0.025 Uiso 1 1 calc R . . H14B H 1.1267 0.5961 0.5591 0.025 Uiso 1 1 calc R . . C15 C 1.1242(14) 0.7104(11) 0.5351(10) 0.024(4) Uani 1 1 d . . . C16 C 1.2057(15) 0.7203(12) 0.5686(10) 0.029(5) Uani 1 1 d . . . H16 H 1.2347 0.6770 0.5886 0.034 Uiso 1 1 calc R . . C17 C 1.2451(16) 0.7940(13) 0.5727(12) 0.035(5) Uani 1 1 d . . . H17 H 1.2998 0.8005 0.5952 0.042 Uiso 1 1 calc R . . C18 C 1.2001(15) 0.8578(14) 0.5421(9) 0.030(5) Uani 1 1 d . . . H18 H 1.2253 0.9073 0.5461 0.035 Uiso 1 1 calc R . . C19 C 1.1221(14) 0.8514(12) 0.5071(11) 0.028(5) Uani 1 1 d . . . C20 C 1.0846(12) 0.7766(11) 0.5041(9) 0.019(4) Uani 1 1 d . . . C21 C 1.0735(14) 0.9217(11) 0.4818(11) 0.030(5) Uani 1 1 d . . . H21A H 1.0283 0.9304 0.5124 0.036 Uiso 1 1 calc R . . H21B H 1.1120 0.9664 0.4870 0.036 Uiso 1 1 calc R . . C22 C 1.0341(14) 0.9216(11) 0.4102(10) 0.027(4) Uani 1 1 d . . . C23 C 0.9444(14) 0.9280(11) 0.3937(10) 0.027(4) Uani 1 1 d . . . H23 H 0.9082 0.9400 0.4280 0.032 Uiso 1 1 calc R . . C24 C 0.9125(15) 0.9164(11) 0.3273(11) 0.028(4) Uani 1 1 d . . . H24 H 0.8536 0.9220 0.3165 0.034 Uiso 1 1 calc R . . C25 C 0.9605(12) 0.8974(10) 0.2767(11) 0.022(4) Uani 1 1 d . . . H25 H 0.9341 0.8866 0.2326 0.026 Uiso 1 1 calc R . . C26 C 1.0481(13) 0.8933(10) 0.2877(10) 0.022(4) Uani 1 1 d . . . C27 C 1.0845(12) 0.9098(9) 0.3547(10) 0.019(4) Uani 1 1 d . . . C28 C 1.1021(13) 0.8662(12) 0.2300(10) 0.024(4) Uani 1 1 d . . . H28A H 1.0647 0.8565 0.1879 0.029 Uiso 1 1 calc R . . H28B H 1.1419 0.9076 0.2200 0.029 Uiso 1 1 calc R . . C29 C 1.0038(13) 0.6984(13) 0.1704(9) 0.027(4) Uani 1 1 d . . . H29A H 1.0269 0.6477 0.1585 0.032 Uiso 1 1 calc R . . H29B H 1.0287 0.7381 0.1421 0.032 Uiso 1 1 calc R . . C30 C 0.9072(14) 0.6981(12) 0.1554(11) 0.028(5) Uani 1 1 d . . . C31 C 0.7715(12) 0.7119(11) 0.2017(8) 0.019(4) Uani 1 1 d . . . C32 C 0.7272(14) 0.7676(11) 0.1645(10) 0.025(4) Uani 1 1 d . . . H32 H 0.7557 0.8036 0.1383 0.030 Uiso 1 1 calc R . . C33 C 0.6402(14) 0.7709(11) 0.1655(9) 0.022(4) Uani 1 1 d . . . C34 C 0.5903(14) 0.8302(12) 0.1289(12) 0.028(5) Uani 1 1 d . . . H34 H 0.6165 0.8658 0.1008 0.034 Uiso 1 1 calc R . . C35 C 0.5070(16) 0.8347(14) 0.1349(13) 0.040(6) Uani 1 1 d . . . H35 H 0.4755 0.8752 0.1125 0.048 Uiso 1 1 calc R . . C36 C 0.4646(13) 0.7796(11) 0.1746(10) 0.023(4) Uani 1 1 d . . . H36 H 0.4055 0.7832 0.1773 0.028 Uiso 1 1 calc R . . C37 C 0.5095(13) 0.7222(11) 0.2084(9) 0.022(4) Uani 1 1 d . . . H37 H 0.4816 0.6853 0.2340 0.026 Uiso 1 1 calc R . . C38 C 0.5963(13) 0.7178(11) 0.2053(11) 0.023(4) Uani 1 1 d . . . C39 C 0.7275(12) 0.6610(12) 0.2423(10) 0.021(4) Uani 1 1 d . . . H39 H 0.7586 0.6238 0.2695 0.026 Uiso 1 1 calc R . . C40 C 1.2369(12) 0.5594(10) 0.4478(9) 0.017(4) Uiso 1 1 d . . . H40A H 1.2398 0.5204 0.4114 0.021 Uiso 1 1 calc R . . H40B H 1.2118 0.5335 0.4861 0.021 Uiso 1 1 calc R . . C41 C 1.3247(15) 0.5788(14) 0.4725(12) 0.036(5) Uani 1 1 d . . . H41A H 1.3225 0.6119 0.5132 0.043 Uiso 1 1 calc R . . H41B H 1.3479 0.6107 0.4368 0.043 Uiso 1 1 calc R . . C42 C 1.3883(17) 0.5148(15) 0.4913(11) 0.040(6) Uani 1 1 d . . . H42A H 1.4372 0.5364 0.5184 0.060 Uiso 1 1 calc R . . H42B H 1.4064 0.4917 0.4495 0.060 Uiso 1 1 calc R . . H42C H 1.3620 0.4753 0.5180 0.060 Uiso 1 1 calc R . . C43 C 0.9772(11) 0.7512(10) 0.4123(9) 0.013(3) Uiso 1 1 d . . . H43A H 1.0048 0.7026 0.4001 0.016 Uiso 1 1 calc R . . H43B H 0.9959 0.7927 0.3826 0.016 Uiso 1 1 calc R . . C44 C 0.8831(12) 0.7425(10) 0.4019(9) 0.018(4) Uani 1 1 d . . . C45 C 0.7530(12) 0.7419(11) 0.4557(9) 0.017(4) Uiso 1 1 d . . . C46 C 0.7044(12) 0.7911(11) 0.4943(9) 0.017(4) Uiso 1 1 d . . . H46 H 0.7306 0.8298 0.5229 0.020 Uiso 1 1 calc R . . C47 C 0.6172(14) 0.7814(10) 0.4894(9) 0.023(4) Uani 1 1 d . . . C48 C 0.5630(15) 0.8309(13) 0.5233(10) 0.029(5) Uani 1 1 d . . . H48 H 0.5866 0.8700 0.5529 0.035 Uiso 1 1 calc R . . C49 C 0.4782(14) 0.8228(13) 0.5140(10) 0.029(5) Uani 1 1 d . . . H49 H 0.4432 0.8564 0.5369 0.035 Uiso 1 1 calc R . . C50 C 0.4398(16) 0.7628(13) 0.4689(13) 0.036(5) Uani 1 1 d . . . H50 H 0.3804 0.7574 0.4622 0.043 Uiso 1 1 calc R . . C51 C 0.4922(13) 0.7144(11) 0.4366(10) 0.024(4) Uani 1 1 d . . . H51 H 0.4687 0.6744 0.4080 0.029 Uiso 1 1 calc R . . C52 C 0.5814(13) 0.7242(11) 0.4457(9) 0.020(4) Uani 1 1 d . . . C53 C 0.7130(12) 0.6822(11) 0.4191(9) 0.020(4) Uani 1 1 d . . . H53 H 0.7468 0.6456 0.3982 0.024 Uiso 1 1 calc R . . C54 C 1.2031(14) 0.9907(12) 0.3561(13) 0.032(5) Uani 1 1 d . . . H54A H 1.1816 1.0264 0.3898 0.038 Uiso 1 1 calc R . . H54B H 1.1824 1.0087 0.3098 0.038 Uiso 1 1 calc R . . C55 C 1.2981(16) 0.9913(15) 0.3634(16) 0.048(7) Uani 1 1 d . . . H55A H 1.3192 1.0431 0.3526 0.058 Uiso 1 1 calc R . . H55B H 1.3200 0.9538 0.3315 0.058 Uiso 1 1 calc R . . C56 C 1.3282(19) 0.9696(15) 0.4377(12) 0.051(8) Uani 1 1 d . . . H56A H 1.2972 1.0000 0.4692 0.076 Uiso 1 1 calc R . . H56B H 1.3886 0.9803 0.4462 0.076 Uiso 1 1 calc R . . H56C H 1.3180 0.9147 0.4450 0.076 Uiso 1 1 calc R . . C57 C 0.602(2) 0.9317(15) 0.3179(12) 0.057(9) Uani 1 1 d . . . H57 H 0.5988 0.9563 0.2717 0.068 Uiso 1 1 calc R A 1 Cl4 Cl 0.6797(4) 0.8577(4) 0.3246(3) 0.0430(14) Uani 1 1 d . B . Cl5 Cl 0.5009(10) 0.8875(10) 0.3332(9) 0.071(4) Uani 0.71 1 d P B 1 Cl6 Cl 0.6157(16) 1.0006(12) 0.3817(12) 0.102(8) Uani 0.57 1 d P B 1 Cl5A Cl 0.526(3) 0.926(3) 0.3556(19) 0.079(11) Uani 0.29 1 d P B 2 Cl6A Cl 0.671(2) 1.0161(12) 0.3486(16) 0.102(11) Uani 0.43 1 d P B 2 O100 O 0.5885(7) 0.5782(7) 0.1847(6) 0.016(2) 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 Hg1 0.0238(4) 0.0124(3) 0.0138(3) -0.0007(3) 0.0038(2) -0.0009(3) Cl1 0.030(3) 0.015(2) 0.030(2) -0.0025(18) 0.006(2) 0.0049(18) Cl2 0.019(2) 0.027(2) 0.033(3) -0.007(2) 0.0047(19) -0.0054(19) N1 0.018(8) 0.020(8) 0.016(7) 0.002(6) 0.001(6) -0.008(6) N2 0.025(8) 0.011(7) 0.013(7) -0.002(6) 0.008(6) -0.003(6) N3 0.027(8) 0.017(7) 0.003(6) 0.002(5) 0.003(6) -0.002(6) N4 0.031(9) 0.017(7) 0.007(7) -0.002(6) 0.006(6) -0.003(7) O1 0.024(7) 0.024(7) 0.018(6) -0.006(5) 0.003(5) -0.002(6) O2 0.036(9) 0.038(9) 0.027(8) 0.000(7) 0.011(7) -0.008(7) O3 0.026(8) 0.024(7) 0.025(7) -0.004(6) 0.003(6) -0.006(6) O4 0.024(7) 0.019(6) 0.016(6) 0.005(5) 0.010(5) 0.001(5) O5 0.025(7) 0.027(7) 0.007(6) 0.001(5) 0.000(5) -0.004(6) O6 0.027(7) 0.015(6) 0.023(6) -0.003(5) 0.007(5) -0.010(6) C1 0.044(13) 0.010(8) 0.021(10) -0.007(7) 0.002(9) 0.003(8) C2 0.042(13) 0.027(11) 0.021(10) 0.000(8) 0.006(9) 0.003(10) C3 0.029(12) 0.036(12) 0.040(13) 0.008(10) 0.011(10) 0.000(10) C4 0.025(11) 0.026(10) 0.027(10) -0.009(8) 0.012(8) 0.011(8) C5 0.033(12) 0.012(9) 0.030(11) -0.006(8) 0.005(9) -0.007(8) C6 0.025(11) 0.034(11) 0.017(9) -0.001(8) 0.010(8) 0.000(9) C7 0.031(10) 0.012(8) 0.017(8) -0.010(7) 0.000(7) 0.009(8) C8 0.022(9) 0.012(8) 0.027(9) -0.008(8) 0.005(7) 0.005(8) C9 0.034(11) 0.006(8) 0.027(10) -0.008(7) 0.006(8) 0.006(7) C10 0.041(13) 0.011(9) 0.030(11) 0.004(7) 0.000(9) 0.011(8) C11 0.038(12) 0.004(7) 0.041(11) 0.010(8) -0.013(9) 0.003(8) C12 0.042(12) 0.011(9) 0.017(9) 0.008(7) 0.005(8) -0.009(8) C13 0.045(13) 0.002(8) 0.028(10) 0.003(7) 0.011(9) 0.004(7) C14 0.032(11) 0.014(8) 0.018(9) 0.006(7) 0.015(8) 0.002(8) C15 0.037(12) 0.019(9) 0.020(9) 0.008(7) 0.017(8) -0.004(8) C16 0.047(14) 0.022(10) 0.016(9) 0.005(8) -0.002(9) 0.004(9) C17 0.037(13) 0.029(11) 0.037(12) -0.007(10) -0.006(10) -0.012(10) C18 0.043(13) 0.041(12) 0.006(8) -0.011(8) 0.009(8) -0.006(10) C19 0.034(12) 0.022(10) 0.028(11) -0.005(8) 0.007(9) -0.003(9) C20 0.022(10) 0.022(9) 0.013(8) -0.006(7) 0.004(7) 0.004(8) C21 0.042(12) 0.004(7) 0.047(12) -0.006(9) 0.016(10) -0.002(9) C22 0.047(12) 0.009(8) 0.023(9) -0.007(8) -0.006(9) 0.002(9) C23 0.043(12) 0.012(9) 0.026(10) -0.003(8) -0.001(9) 0.009(9) C24 0.044(12) 0.006(8) 0.035(11) -0.003(8) 0.004(9) 0.003(9) C25 0.022(10) 0.013(8) 0.030(10) 0.004(7) 0.003(8) -0.011(7) C26 0.024(10) 0.010(8) 0.032(11) 0.014(7) 0.007(8) 0.000(7) C27 0.025(10) 0.004(8) 0.029(9) 0.005(7) 0.008(8) 0.002(7) C28 0.024(10) 0.025(10) 0.022(10) 0.005(8) -0.002(8) -0.002(8) C29 0.029(11) 0.040(12) 0.012(9) 0.002(8) 0.006(8) 0.008(9) C30 0.036(12) 0.021(10) 0.026(11) 0.000(8) -0.005(9) -0.006(9) C31 0.026(10) 0.025(10) 0.005(7) 0.002(7) 0.004(7) -0.002(8) C32 0.039(12) 0.017(9) 0.017(9) 0.010(7) -0.002(8) -0.003(8) C33 0.040(12) 0.018(9) 0.007(8) 0.005(7) 0.000(8) -0.002(8) C34 0.029(12) 0.019(10) 0.038(12) 0.001(9) 0.007(9) 0.009(8) C35 0.041(14) 0.034(13) 0.046(14) 0.015(11) 0.007(11) 0.014(11) C36 0.020(10) 0.025(10) 0.028(10) 0.012(8) 0.023(8) 0.007(8) C37 0.033(11) 0.025(10) 0.009(8) 0.004(7) 0.014(7) -0.005(8) C38 0.027(11) 0.012(9) 0.031(11) -0.004(8) 0.007(8) -0.011(8) C39 0.021(10) 0.028(10) 0.015(9) -0.001(8) 0.001(7) -0.003(8) C41 0.040(13) 0.035(12) 0.037(12) -0.009(11) 0.019(10) -0.011(11) C42 0.054(16) 0.046(14) 0.019(11) -0.014(10) 0.004(10) 0.006(12) C44 0.026(10) 0.012(8) 0.018(9) -0.007(7) 0.007(7) -0.005(7) C47 0.052(13) 0.014(9) 0.006(8) 0.004(6) 0.011(8) 0.000(8) C48 0.046(14) 0.029(11) 0.014(9) -0.007(8) 0.010(9) -0.004(10) C49 0.034(12) 0.031(11) 0.024(10) -0.007(9) 0.016(9) 0.006(9) C50 0.041(14) 0.022(11) 0.047(14) -0.007(10) 0.024(11) -0.003(10) C51 0.033(11) 0.019(9) 0.019(9) -0.001(7) 0.000(8) 0.009(8) C52 0.033(11) 0.017(9) 0.012(8) 0.002(7) 0.010(8) -0.001(8) C53 0.019(10) 0.025(10) 0.015(9) -0.004(7) 0.002(7) -0.005(8) C54 0.037(13) 0.014(9) 0.045(13) 0.007(9) 0.004(10) -0.013(9) C55 0.032(13) 0.032(13) 0.08(2) 0.003(13) 0.011(13) -0.022(11) C56 0.08(2) 0.041(14) 0.030(13) 0.015(11) -0.025(13) -0.024(13) C57 0.12(3) 0.037(14) 0.016(11) -0.010(10) 0.001(13) 0.015(16) Cl4 0.049(4) 0.042(3) 0.037(3) 0.008(3) 0.002(3) -0.003(3) Cl5 0.058(9) 0.077(10) 0.079(10) -0.001(8) 0.009(7) 0.018(7) Cl6 0.124(18) 0.064(12) 0.114(17) -0.072(12) -0.007(13) -0.002(11) Cl5A 0.07(2) 0.10(3) 0.06(2) 0.03(2) 0.042(19) 0.01(2) Cl6A 0.15(3) 0.037(10) 0.10(2) -0.029(12) -0.079(19) 0.021(14) O100 0.015(6) 0.004(5) 0.028(7) -0.001(5) -0.007(5) -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 Hg1 Cl2 2.319(5) . ? Hg1 N2 2.342(14) . ? Hg1 N4 2.372(14) . ? Hg1 Cl1 2.375(5) . ? N1 C30 1.29(3) . ? N1 C31 1.40(2) . ? N1 H1 0.8600 . ? N2 C39 1.32(2) . ? N2 C38 1.36(3) . ? N3 C44 1.35(2) . ? N3 C45 1.38(2) . ? N3 H3C 0.8600 . ? N4 C53 1.29(2) . ? N4 C52 1.36(2) . ? O1 C6 1.38(2) . ? O1 C29 1.39(2) . ? O2 C30 1.21(2) . ? O3 C40 1.23(2) . ? O3 C13 1.35(3) . ? O4 C43 1.36(2) . ? O4 C20 1.37(2) . ? O5 C44 1.22(2) . ? O6 C27 1.36(2) . ? O6 C54 1.43(2) . ? C1 C6 1.35(3) . ? C1 C2 1.35(3) . ? C1 C28 1.52(3) . ? C2 C3 1.37(3) . ? C2 H2 0.9300 . ? C3 C4 1.36(3) . ? C3 H3 0.9300 . ? C4 C5 1.35(3) . ? C4 H4 0.9300 . ? C5 C6 1.39(3) . ? C5 C7 1.47(3) . ? C7 C8 1.50(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.37(3) . ? C8 C13 1.39(3) . ? C9 C10 1.33(3) . ? C9 H9 0.9300 . ? C10 C11 1.38(3) . ? C10 H10 0.9300 . ? C11 C12 1.42(3) . ? C11 H11 0.9300 . ? C12 C13 1.36(3) . ? C12 C14 1.50(3) . ? C14 C15 1.47(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.39(3) . ? C15 C20 1.39(3) . ? C16 C17 1.40(3) . ? C16 H16 0.9300 . ? C17 C18 1.39(3) . ? C17 H17 0.9300 . ? C18 C19 1.34(3) . ? C18 H18 0.9300 . ? C19 C20 1.40(3) . ? C19 C21 1.48(3) . ? C21 C22 1.46(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.40(3) . ? C22 C23 1.41(3) . ? C23 C24 1.35(3) . ? C23 H23 0.9300 . ? C24 C25 1.32(3) . ? C24 H24 0.9300 . ? C25 C26 1.37(3) . ? C25 H25 0.9300 . ? C26 C27 1.39(3) . ? C26 C28 1.52(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.51(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C31 C32 1.34(3) . ? C31 C39 1.39(3) . ? C32 C33 1.36(3) . ? C32 H32 0.9300 . ? C33 C38 1.40(3) . ? C33 C34 1.42(3) . ? C34 C35 1.32(3) . ? C34 H34 0.9300 . ? C35 C36 1.41(3) . ? C35 H35 0.9300 . ? C36 C37 1.34(3) . ? C36 H36 0.9300 . ? C37 C38 1.36(3) . ? C37 H37 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.45(3) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.50(3) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.47(2) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C45 C53 1.36(2) . ? C45 C46 1.39(3) . ? C46 C47 1.37(3) . ? C46 H46 0.9300 . ? C47 C52 1.37(3) . ? C47 C48 1.40(3) . ? C48 C49 1.33(3) . ? C48 H48 0.9300 . ? C49 C50 1.44(3) . ? C49 H49 0.9300 . ? C50 C51 1.35(3) . ? C50 H50 0.9300 . ? C51 C52 1.40(3) . ? C51 H51 0.9300 . ? C53 H53 0.9300 . ? C54 C55 1.48(3) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.51(4) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 Cl5A 1.45(5) . ? C57 Cl6 1.70(3) . ? C57 Cl4 1.75(3) . ? C57 Cl5 1.80(4) . ? C57 Cl6A 1.86(4) . ? C57 H57 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Hg1 N2 118.3(4) . . ? Cl2 Hg1 N4 112.9(4) . . ? N2 Hg1 N4 87.6(5) . . ? Cl2 Hg1 Cl1 129.93(17) . . ? N2 Hg1 Cl1 97.8(4) . . ? N4 Hg1 Cl1 101.4(4) . . ? C30 N1 C31 125.1(17) . . ? C30 N1 H1 117.5 . . ? C31 N1 H1 117.5 . . ? C39 N2 C38 120.1(16) . . ? C39 N2 Hg1 114.4(12) . . ? C38 N2 Hg1 125.1(12) . . ? C44 N3 C45 119.6(15) . . ? C44 N3 H3C 120.2 . . ? C45 N3 H3C 120.2 . . ? C53 N4 C52 118.6(16) . . ? C53 N4 Hg1 111.4(12) . . ? C52 N4 Hg1 129.4(13) . . ? C6 O1 C29 111.1(15) . . ? C40 O3 C13 120.2(15) . . ? C43 O4 C20 120.1(14) . . ? C27 O6 C54 111.5(15) . . ? C6 C1 C2 120.5(19) . . ? C6 C1 C28 122(2) . . ? C2 C1 C28 117.3(18) . . ? C1 C2 C3 119(2) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 121(2) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 120(2) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 118.7(18) . . ? C4 C5 C7 120.0(18) . . ? C6 C5 C7 121.3(19) . . ? C1 C6 O1 120.6(19) . . ? C1 C6 C5 120.4(19) . . ? O1 C6 C5 118.8(18) . . ? C5 C7 C8 114.2(15) . . ? C5 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? C5 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C13 116.7(18) . . ? C9 C8 C7 122.0(17) . . ? C13 C8 C7 121.3(17) . . ? C10 C9 C8 121(2) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 125(2) . . ? C9 C10 H10 117.5 . . ? C11 C10 H10 117.5 . . ? C10 C11 C12 114(2) . . ? C10 C11 H11 123.2 . . ? C12 C11 H11 123.2 . . ? C13 C12 C11 121.6(19) . . ? C13 C12 C14 121.6(19) . . ? C11 C12 C14 116.4(18) . . ? O3 C13 C12 118.7(18) . . ? O3 C13 C8 119.5(17) . . ? C12 C13 C8 122(2) . . ? C15 C14 C12 117.2(15) . . ? C15 C14 H14A 108.0 . . ? C12 C14 H14A 108.0 . . ? C15 C14 H14B 108.0 . . ? C12 C14 H14B 108.0 . . ? H14A C14 H14B 107.2 . . ? C16 C15 C20 117.1(18) . . ? C16 C15 C14 118.1(18) . . ? C20 C15 C14 124.7(19) . . ? C15 C16 C17 121.2(19) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 118(2) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C19 C18 C17 123(2) . . ? C19 C18 H18 118.3 . . ? C17 C18 H18 118.3 . . ? C18 C19 C20 117(2) . . ? C18 C19 C21 121(2) . . ? C20 C19 C21 121.4(19) . . ? O4 C20 C15 116.5(17) . . ? O4 C20 C19 119.3(17) . . ? C15 C20 C19 123.3(19) . . ? C22 C21 C19 118.3(17) . . ? C22 C21 H21A 107.7 . . ? C19 C21 H21A 107.7 . . ? C22 C21 H21B 107.7 . . ? C19 C21 H21B 107.7 . . ? H21A C21 H21B 107.1 . . ? C27 C22 C23 117.0(17) . . ? C27 C22 C21 120.3(19) . . ? C23 C22 C21 122.6(19) . . ? C24 C23 C22 119(2) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C25 C24 C23 123(2) . . ? C25 C24 H24 118.3 . . ? C23 C24 H24 118.3 . . ? C24 C25 C26 122(2) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C25 C26 C27 117.0(19) . . ? C25 C26 C28 120.8(19) . . ? C27 C26 C28 122.0(18) . . ? O6 C27 C26 119.3(17) . . ? O6 C27 C22 118.9(17) . . ? C26 C27 C22 121.8(18) . . ? C1 C28 C26 111.6(16) . . ? C1 C28 H28A 109.3 . . ? C26 C28 H28A 109.3 . . ? C1 C28 H28B 109.3 . . ? C26 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? O1 C29 C30 109.8(16) . . ? O1 C29 H29A 109.7 . . ? C30 C29 H29A 109.7 . . ? O1 C29 H29B 109.7 . . ? C30 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? O2 C30 N1 124(2) . . ? O2 C30 C29 118(2) . . ? N1 C30 C29 118.0(17) . . ? C32 C31 C39 118.9(19) . . ? C32 C31 N1 123.3(17) . . ? C39 C31 N1 117.5(17) . . ? C31 C32 C33 119.3(18) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C32 C33 C38 121.1(18) . . ? C32 C33 C34 121.7(18) . . ? C38 C33 C34 117(2) . . ? C35 C34 C33 120(2) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 122(2) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C37 C36 C35 119.8(19) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C36 C37 C38 120.0(17) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? N2 C38 C37 120.3(17) . . ? N2 C38 C33 118.1(18) . . ? C37 C38 C33 121.6(19) . . ? N2 C39 C31 122.4(18) . . ? N2 C39 H39 118.8 . . ? C31 C39 H39 118.8 . . ? O3 C40 C41 122.1(18) . . ? O3 C40 H40A 106.8 . . ? C41 C40 H40A 106.8 . . ? O3 C40 H40B 106.8 . . ? C41 C40 H40B 106.8 . . ? H40A C40 H40B 106.6 . . ? C40 C41 C42 120(2) . . ? C40 C41 H41A 107.3 . . ? C42 C41 H41A 107.3 . . ? C40 C41 H41B 107.3 . . ? C42 C41 H41B 107.3 . . ? H41A C41 H41B 106.9 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O4 C43 C44 108.7(14) . . ? O4 C43 H43A 109.9 . . ? C44 C43 H43A 109.9 . . ? O4 C43 H43B 109.9 . . ? C44 C43 H43B 109.9 . . ? H43A C43 H43B 108.3 . . ? O5 C44 N3 124.4(18) . . ? O5 C44 C43 120.3(16) . . ? N3 C44 C43 115.3(16) . . ? C53 C45 N3 121.4(17) . . ? C53 C45 C46 118.8(17) . . ? N3 C45 C46 119.5(16) . . ? C47 C46 C45 118.5(17) . . ? C47 C46 H46 120.7 . . ? C45 C46 H46 120.7 . . ? C46 C47 C52 118.5(18) . . ? C46 C47 C48 122.4(19) . . ? C52 C47 C48 119(2) . . ? C49 C48 C47 121(2) . . ? C49 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? C48 C49 C50 121.0(19) . . ? C48 C49 H49 119.5 . . ? C50 C49 H49 119.5 . . ? C51 C50 C49 118(2) . . ? C51 C50 H50 120.8 . . ? C49 C50 H50 120.8 . . ? C50 C51 C52 120(2) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? N4 C52 C47 121.6(19) . . ? N4 C52 C51 117.8(17) . . ? C47 C52 C51 120.5(18) . . ? N4 C53 C45 123.4(18) . . ? N4 C53 H53 118.3 . . ? C45 C53 H53 118.3 . . ? O6 C54 C55 110.4(18) . . ? O6 C54 H54A 109.6 . . ? C55 C54 H54A 109.6 . . ? O6 C54 H54B 109.6 . . ? C55 C54 H54B 109.6 . . ? H54A C54 H54B 108.1 . . ? C54 C55 C56 108(2) . . ? C54 C55 H55A 110.0 . . ? C56 C55 H55A 110.0 . . ? C54 C55 H55B 110.0 . . ? C56 C55 H55B 110.0 . . ? H55A C55 H55B 108.4 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? Cl5A C57 Cl6 75(2) . . ? Cl5A C57 Cl4 121(2) . . ? Cl6 C57 Cl4 113.6(19) . . ? Cl5A C57 Cl5 28.0(19) . . ? Cl6 C57 Cl5 103.1(18) . . ? Cl4 C57 Cl5 107.6(15) . . ? Cl5A C57 Cl6A 112(3) . . ? Cl6 C57 Cl6A 37.2(13) . . ? Cl4 C57 Cl6A 98.9(19) . . ? Cl5 C57 Cl6A 140(2) . . ? Cl5A C57 H57 120.4 . . ? Cl6 C57 H57 110.7 . . ? Cl4 C57 H57 110.7 . . ? Cl5 C57 H57 110.7 . . ? Cl6A C57 H57 86.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 9.875 _refine_diff_density_min -9.143 _refine_diff_density_rms 0.345