# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_u130614mas1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C95 H74 Cl15 N3 O3' _chemical_formula_weight 1837.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 22.2423(5) _cell_length_b 9.3087(2) _cell_length_c 22.5200(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.449(2) _cell_angle_gamma 90.00 _cell_volume 4534.83(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 7900 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 65.78 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 4.570 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3410 _exptl_absorpt_correction_T_max 0.8037 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 30648 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 67.87 _reflns_number_total 12985 _reflns_number_gt 10255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.1887P)^2^+1.2384P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 12985 _refine_ls_number_parameters 1142 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.2640 _refine_ls_wR_factor_gt 0.2403 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.030 _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 C85A C -0.2544(3) 0.9663(13) 0.2540(3) 0.067(3) Uani 0.81(2) 1 d PD A 1 H85A H -0.2794 0.9392 0.2833 0.080 Uiso 0.81(2) 1 calc PR A 1 H85B H -0.2551 0.8848 0.2256 0.080 Uiso 0.81(2) 1 calc PR A 1 C86A C -0.2823(5) 1.0953(18) 0.2188(6) 0.118(5) Uani 0.81(2) 1 d PD A 1 H86A H -0.2577 1.1235 0.1892 0.141 Uiso 0.81(2) 1 calc PR A 1 H86B H -0.2829 1.1769 0.2468 0.141 Uiso 0.81(2) 1 calc PR A 1 C87A C -0.3508(6) 1.055(3) 0.1837(8) 0.150(8) Uani 0.81(2) 1 d PD A 1 H87A H -0.3495 0.9928 0.1490 0.225 Uiso 0.81(2) 1 calc PR A 1 H87B H -0.3735 1.1434 0.1688 0.225 Uiso 0.81(2) 1 calc PR A 1 H87C H -0.3716 1.0053 0.2115 0.225 Uiso 0.81(2) 1 calc PR A 1 C85B C -0.260(2) 1.053(7) 0.253(3) 0.130(17) Uani 0.19(2) 1 d PDU A 2 H85C H -0.2893 1.0483 0.2800 0.156 Uiso 0.19(2) 1 calc PR A 2 H85D H -0.2587 1.1514 0.2370 0.156 Uiso 0.19(2) 1 calc PR A 2 C86B C -0.2733(16) 0.943(6) 0.204(2) 0.130(17) Uani 0.19(2) 1 d PDU A 2 H86C H -0.2656 0.8452 0.2213 0.156 Uiso 0.19(2) 1 calc PR A 2 H86D H -0.2464 0.9578 0.1749 0.156 Uiso 0.19(2) 1 calc PR A 2 C87B C -0.3439(17) 0.960(7) 0.169(3) 0.130(17) Uani 0.19(2) 1 d PDU A 2 H87D H -0.3598 0.8673 0.1515 0.196 Uiso 0.19(2) 1 calc PR A 2 H87E H -0.3475 1.0313 0.1366 0.196 Uiso 0.19(2) 1 calc PR A 2 H87F H -0.3679 0.9914 0.1982 0.196 Uiso 0.19(2) 1 calc PR A 2 C88A C 0.4527(11) 0.998(4) 0.0410(12) 0.126(9) Uani 0.744(7) 1 d PU B 3 H88A H 0.4763 1.0854 0.0569 0.151 Uiso 0.744(7) 1 calc PR B 3 H88B H 0.4354 1.0095 -0.0035 0.151 Uiso 0.744(7) 1 calc PR B 3 C89A C 0.4988(13) 0.846(5) 0.0561(15) 0.189(13) Uani 0.744(7) 1 d PU B 3 H89A H 0.5141 0.8314 0.1005 0.226 Uiso 0.744(7) 1 calc PR B 3 H89B H 0.4759 0.7594 0.0380 0.226 Uiso 0.744(7) 1 calc PR B 3 C90A C 0.5549(9) 0.882(4) 0.0241(11) 0.217(15) Uani 0.744(7) 1 d PU B 3 H90A H 0.5383 0.8995 -0.0196 0.325 Uiso 0.744(7) 1 calc PR B 3 H90B H 0.5834 0.7999 0.0293 0.325 Uiso 0.744(7) 1 calc PR B 3 H90C H 0.5770 0.9672 0.0430 0.325 Uiso 0.744(7) 1 calc PR B 3 C95 C 0.7429(13) 0.809(3) 0.0236(16) 0.40(4) Uani 0.744(7) 1 d PDU B 3 H95 H 0.7410 0.7033 0.0303 0.481 Uiso 0.744(7) 1 calc PR B 3 Cl13 Cl 0.8111(5) 0.8966(13) -0.0076(6) 0.284(6) Uani 0.744(7) 1 d PDU B 3 Cl14 Cl 0.7348(7) 0.917(4) 0.0728(6) 0.54(2) Uani 0.744(7) 1 d PDU B 3 Cl15 Cl 0.6776(9) 0.9138(19) -0.0472(8) 0.386(12) Uani 0.744(7) 1 d PDU B 3 C90B C 0.4695(19) 0.734(6) 0.0376(12) 0.116(12) Uani 0.256(7) 1 d PU B 4 H90D H 0.4505 0.6917 0.0686 0.175 Uiso 0.256(7) 1 calc PR B 4 H90E H 0.5020 0.6697 0.0302 0.175 Uiso 0.256(7) 1 calc PR B 4 H90F H 0.4380 0.7470 -0.0005 0.175 Uiso 0.256(7) 1 calc PR B 4 C88B C 0.453(3) 0.963(9) 0.050(2) 0.087(12) Uani 0.256(7) 1 d PU B 4 H88C H 0.4364 0.9564 0.0053 0.104 Uiso 0.256(7) 1 calc PR B 4 H88D H 0.4721 1.0596 0.0572 0.104 Uiso 0.256(7) 1 calc PR B 4 C89B C 0.4980(15) 0.880(8) 0.0600(12) 0.114(12) Uani 0.256(7) 1 d PU B 4 H89C H 0.5180 0.8768 0.1041 0.136 Uiso 0.256(7) 1 calc PR B 4 H89D H 0.5289 0.9096 0.0371 0.136 Uiso 0.256(7) 1 calc PR B 4 C96 C 0.6752(12) 0.956(5) -0.0390(12) 0.18(3) Uani 0.256(7) 1 d PDU B 4 H96 H 0.7158 0.9595 -0.0509 0.210 Uiso 0.256(7) 1 calc PR B 4 Cl16 Cl 0.5948(11) 0.955(2) -0.1023(8) 0.196(9) Uani 0.256(7) 1 d PDU B 4 Cl17 Cl 0.6616(15) 1.055(3) 0.0125(8) 0.274(18) Uani 0.256(7) 1 d PDU B 4 Cl18 Cl 0.6485(8) 0.771(2) 0.0054(9) 0.170(7) Uani 0.256(7) 1 d PDU B 4 C1 C 0.4855(3) 1.0185(7) 0.7192(3) 0.0631(14) Uani 1 1 d . . . C2 C 0.3740(2) 1.0689(7) 0.6905(3) 0.0587(13) Uani 1 1 d . . . C3 C 0.3489(3) 0.9440(8) 0.6628(3) 0.0716(17) Uani 1 1 d . . . H3 H 0.3714 0.8566 0.6706 0.086 Uiso 1 1 calc R . . C4 C 0.2906(3) 0.9458(8) 0.6233(3) 0.0704(16) Uani 1 1 d . . . H4 H 0.2732 0.8589 0.6048 0.085 Uiso 1 1 calc R . . C5 C 0.2574(2) 1.0727(7) 0.6106(2) 0.0562(12) Uani 1 1 d . . . C6 C 0.2830(3) 1.1967(7) 0.6365(3) 0.0655(15) Uani 1 1 d . . . H6 H 0.2613 1.2848 0.6271 0.079 Uiso 1 1 calc R . . C7 C 0.3414(3) 1.1957(8) 0.6771(3) 0.0695(16) Uani 1 1 d . . . H7 H 0.3586 1.2828 0.6956 0.083 Uiso 1 1 calc R . . C8 C 0.1925(2) 1.0687(6) 0.5698(2) 0.0497(11) Uani 1 1 d . . . C9 C 0.1840(2) 1.0869(6) 0.5069(2) 0.0521(11) Uani 1 1 d . . . C10 C 0.2330(2) 1.1176(7) 0.4774(3) 0.0621(14) Uani 1 1 d . . . H10 H 0.2739 1.1261 0.5017 0.074 Uiso 1 1 calc R . . C11 C 0.2238(3) 1.1349(9) 0.4173(3) 0.0712(17) Uani 1 1 d . . . H11 H 0.2575 1.1607 0.4001 0.085 Uiso 1 1 calc R . . C12 C 0.1643(3) 1.1152(8) 0.3788(3) 0.0709(17) Uani 1 1 d . . . H12 H 0.1586 1.1207 0.3357 0.085 Uiso 1 1 calc R . . C13 C 0.1154(3) 1.0883(7) 0.4040(3) 0.0596(13) Uani 1 1 d . . . H13 H 0.0754 1.0773 0.3781 0.072 Uiso 1 1 calc R . . C14 C 0.1228(2) 1.0763(6) 0.4679(2) 0.0495(11) Uani 1 1 d . . . C15 C 0.0716(2) 1.0569(6) 0.4945(2) 0.0477(10) Uani 1 1 d . . . C16 C 0.0806(2) 1.0462(5) 0.5588(2) 0.0455(10) Uani 1 1 d . . . C17 C 0.0305(2) 1.0313(6) 0.5873(2) 0.0528(11) Uani 1 1 d . . . H17 H -0.0105 1.0316 0.5628 0.063 Uiso 1 1 calc R . . C18 C 0.0395(3) 1.0166(7) 0.6486(3) 0.0608(13) Uani 1 1 d . . . H18 H 0.0050 1.0056 0.6664 0.073 Uiso 1 1 calc R . . C19 C 0.1004(3) 1.0176(8) 0.6862(2) 0.0633(14) Uani 1 1 d . . . H19 H 0.1066 1.0073 0.7292 0.076 Uiso 1 1 calc R . . C20 C 0.1495(2) 1.0332(7) 0.6610(2) 0.0571(13) Uani 1 1 d . . . H20 H 0.1899 1.0327 0.6868 0.068 Uiso 1 1 calc R . . C21 C 0.1427(2) 1.0504(6) 0.5965(2) 0.0474(10) Uani 1 1 d . . . C22 C 0.0078(2) 1.0482(6) 0.4550(2) 0.0462(10) Uani 1 1 d . . . C23 C -0.0144(2) 0.9251(6) 0.4220(2) 0.0489(11) Uani 1 1 d . . . H23 H 0.0120 0.8442 0.4241 0.059 Uiso 1 1 calc R . . C24 C -0.0739(2) 0.9178(6) 0.3864(2) 0.0511(11) Uani 1 1 d . . . H24 H -0.0879 0.8333 0.3638 0.061 Uiso 1 1 calc R . . C25 C -0.1132(2) 1.0349(6) 0.3838(2) 0.0482(11) Uani 1 1 d . . . C26 C -0.0916(2) 1.1595(7) 0.4150(2) 0.0541(12) Uani 1 1 d . . . H26 H -0.1177 1.2412 0.4121 0.065 Uiso 1 1 calc R . . C27 C -0.0319(2) 1.1649(6) 0.4504(2) 0.0527(12) Uani 1 1 d . . . H27 H -0.0176 1.2505 0.4721 0.063 Uiso 1 1 calc R . . C28 C -0.1791(2) 1.0317(7) 0.3477(2) 0.0533(12) Uani 1 1 d . A . C29 C -0.1430(2) 0.9871(7) 0.2550(2) 0.0570(14) Uani 1 1 d . A . C30 C -0.1044(3) 1.1029(8) 0.2542(3) 0.0641(15) Uani 1 1 d . . . H30 H -0.1117 1.1904 0.2731 0.077 Uiso 1 1 calc R . . C31 C -0.0555(3) 1.0940(8) 0.2266(3) 0.0679(16) Uani 1 1 d . . . H31 H -0.0293 1.1747 0.2266 0.081 Uiso 1 1 calc R . . C32 C -0.0446(3) 0.9677(9) 0.1987(3) 0.0666(16) Uani 1 1 d . . . C33 C -0.0839(3) 0.8562(9) 0.1970(3) 0.0737(18) Uani 1 1 d . . . H33 H -0.0777 0.7709 0.1761 0.088 Uiso 1 1 calc R . . C34 C -0.1333(3) 0.8638(9) 0.2253(3) 0.0668(16) Uani 1 1 d . . . H34 H -0.1601 0.7838 0.2240 0.080 Uiso 1 1 calc R . . C35 C 0.0138(3) 0.9557(9) 0.1747(3) 0.0707(17) Uani 1 1 d . . . C36 C 0.0635(3) 0.8768(9) 0.2084(3) 0.0709(18) Uani 1 1 d . . . C37 C 0.0618(3) 0.8119(10) 0.2649(3) 0.0736(18) Uani 1 1 d . . . H37 H 0.0259 0.8229 0.2807 0.088 Uiso 1 1 calc R . . C38 C 0.1107(3) 0.7339(12) 0.2973(3) 0.087(2) Uani 1 1 d . . . H38 H 0.1084 0.6908 0.3350 0.104 Uiso 1 1 calc R . . C39 C 0.1640(3) 0.7176(10) 0.2750(4) 0.086(2) Uani 1 1 d . . . H39 H 0.1975 0.6619 0.2974 0.103 Uiso 1 1 calc R . . C40 C 0.1685(3) 0.7786(10) 0.2229(3) 0.077(2) Uani 1 1 d . . . H40 H 0.2054 0.7656 0.2092 0.092 Uiso 1 1 calc R . . C41 C 0.1193(3) 0.8641(9) 0.1863(3) 0.0717(17) Uani 1 1 d . . . C42 C 0.1236(3) 0.9296(10) 0.1326(3) 0.0749(19) Uani 1 1 d . . . C43 C 0.0723(3) 1.0084(11) 0.0976(3) 0.082(2) Uani 1 1 d . . . C44 C 0.0742(3) 1.0752(13) 0.0405(3) 0.092(3) Uani 1 1 d . . . H44 H 0.1100 1.0647 0.0248 0.111 Uiso 1 1 calc R . . C45 C 0.0266(4) 1.1517(17) 0.0090(4) 0.124(4) Uani 1 1 d . . . H45 H 0.0303 1.2010 -0.0269 0.148 Uiso 1 1 calc R . . C46 C -0.0293(4) 1.1604(18) 0.0286(4) 0.130(5) Uani 1 1 d . . . H46 H -0.0639 1.2094 0.0044 0.157 Uiso 1 1 calc R . . C47 C -0.0335(3) 1.0985(13) 0.0822(3) 0.096(3) Uani 1 1 d . . . H47 H -0.0707 1.1086 0.0957 0.115 Uiso 1 1 calc R . . C48 C 0.0168(3) 1.0183(10) 0.1188(3) 0.0761(19) Uani 1 1 d . . . C49 C 0.1819(3) 0.9276(10) 0.1108(3) 0.0755(18) Uani 1 1 d . . . C50 C 0.2245(3) 1.0372(11) 0.1250(4) 0.087(2) Uani 1 1 d . . . H50 H 0.2162 1.1156 0.1489 0.104 Uiso 1 1 calc R . . C51 C 0.2786(3) 1.0361(12) 0.1056(4) 0.090(2) Uani 1 1 d . . . H51 H 0.3075 1.1122 0.1169 0.108 Uiso 1 1 calc R . . C52 C 0.2912(3) 0.9257(13) 0.0698(3) 0.089(3) Uani 1 1 d . . . C53 C 0.2503(3) 0.8123(13) 0.0557(3) 0.094(3) Uani 1 1 d . . . H53 H 0.2590 0.7335 0.0322 0.113 Uiso 1 1 calc R . . C54 C 0.1956(3) 0.8160(12) 0.0770(4) 0.090(2) Uani 1 1 d . . . H54 H 0.1673 0.7383 0.0675 0.108 Uiso 1 1 calc R . . C55 C 0.3455(3) 0.9329(15) 0.0410(3) 0.105(3) Uani 1 1 d . B . C56 C 0.4168(3) 0.9722(10) 0.1399(3) 0.075(2) Uani 1 1 d . B . C57 C 0.4144(3) 0.8477(9) 0.1732(3) 0.0704(17) Uani 1 1 d . . . H57 H 0.4022 0.7599 0.1524 0.085 Uiso 1 1 calc R . . C58 C 0.4291(3) 0.8498(8) 0.2348(3) 0.0637(14) Uani 1 1 d . . . H58 H 0.4270 0.7635 0.2567 0.076 Uiso 1 1 calc R . . C59 C 0.4475(2) 0.9771(7) 0.2667(3) 0.0586(13) Uani 1 1 d . . . C60 C 0.4526(3) 1.1017(8) 0.2332(3) 0.0699(16) Uani 1 1 d . . . H60 H 0.4668 1.1885 0.2539 0.084 Uiso 1 1 calc R . . C61 C 0.4370(3) 1.0984(10) 0.1708(4) 0.082(2) Uani 1 1 d . . . H61 H 0.4401 1.1835 0.1483 0.098 Uiso 1 1 calc R . . C62 C 0.4598(2) 0.9818(6) 0.3347(3) 0.0561(12) Uani 1 1 d . . . C63 C 0.4135(2) 0.9504(6) 0.3639(3) 0.0551(12) Uani 1 1 d . . . C64 C 0.3511(3) 0.9195(8) 0.3303(3) 0.0656(15) Uani 1 1 d . . . H64 H 0.3409 0.9241 0.2870 0.079 Uiso 1 1 calc R . . C65 C 0.3064(3) 0.8835(8) 0.3609(3) 0.0730(18) Uani 1 1 d . . . H65 H 0.2654 0.8646 0.3385 0.088 Uiso 1 1 calc R . . C66 C 0.3204(3) 0.8741(8) 0.4248(4) 0.0733(17) Uani 1 1 d . . . H66 H 0.2896 0.8429 0.4449 0.088 Uiso 1 1 calc R . . C67 C 0.3767(3) 0.9086(7) 0.4580(3) 0.0663(15) Uani 1 1 d . . . H67 H 0.3848 0.9048 0.5013 0.080 Uiso 1 1 calc R . . C68 C 0.4253(2) 0.9513(7) 0.4290(3) 0.0570(12) Uani 1 1 d . . . C69 C 0.4837(3) 0.9929(7) 0.4635(3) 0.0593(13) Uani 1 1 d . . . C70 C 0.5312(2) 1.0250(6) 0.4340(3) 0.0570(12) Uani 1 1 d . . . C71 C 0.5918(3) 1.0677(8) 0.4680(3) 0.0655(15) Uani 1 1 d . . . H71 H 0.5998 1.0776 0.5111 0.079 Uiso 1 1 calc R . . C72 C 0.6370(2) 1.0933(8) 0.4390(3) 0.0723(17) Uani 1 1 d . . . H72 H 0.6763 1.1236 0.4620 0.087 Uiso 1 1 calc R . . C73 C 0.6276(3) 1.0766(8) 0.3758(3) 0.0699(16) Uani 1 1 d . . . H73 H 0.6609 1.0911 0.3566 0.084 Uiso 1 1 calc R . . C74 C 0.5707(3) 1.0395(7) 0.3417(3) 0.0631(14) Uani 1 1 d . . . H74 H 0.5646 1.0296 0.2987 0.076 Uiso 1 1 calc R . . C75 C 0.5199(2) 1.0152(6) 0.3697(3) 0.0575(13) Uani 1 1 d . . . C76 C 0.4917(3) 1.0053(7) 0.5309(3) 0.0589(13) Uani 1 1 d . . . C77 C 0.5167(3) 0.8973(7) 0.5711(3) 0.0689(16) Uani 1 1 d . . . H77 H 0.5353 0.8172 0.5562 0.083 Uiso 1 1 calc R . . C78 C 0.5157(3) 0.9018(8) 0.6321(3) 0.0695(16) Uani 1 1 d . . . H78 H 0.5336 0.8263 0.6588 0.083 Uiso 1 1 calc R . . C79 C 0.4881(2) 1.0178(7) 0.6540(3) 0.0569(12) Uani 1 1 d . . . C80 C 0.4667(3) 1.1308(7) 0.6159(3) 0.0614(13) Uani 1 1 d . . . H80 H 0.4509 1.2137 0.6317 0.074 Uiso 1 1 calc R . . C81 C 0.4676(3) 1.1258(7) 0.5549(3) 0.0677(15) Uani 1 1 d . . . H81 H 0.4519 1.2044 0.5290 0.081 Uiso 1 1 calc R . . C82 C 0.4329(3) 1.0837(16) 0.7968(3) 0.112(3) Uani 1 1 d U . . H82A H 0.4065 1.1668 0.8012 0.134 Uiso 1 1 calc R . . H82B H 0.4754 1.1050 0.8203 0.134 Uiso 1 1 calc R . . C83 C 0.4101(6) 0.956(3) 0.8229(7) 0.246(13) Uani 1 1 d U . . H83A H 0.3650 0.9545 0.8055 0.296 Uiso 1 1 calc R . . H83B H 0.4273 0.8730 0.8051 0.296 Uiso 1 1 calc R . . C84 C 0.4170(14) 0.930(5) 0.8767(9) 0.35(3) Uani 1 1 d U . . H84A H 0.4520 0.9852 0.9003 0.524 Uiso 1 1 calc R . . H84B H 0.4253 0.8269 0.8836 0.524 Uiso 1 1 calc R . . H84C H 0.3794 0.9555 0.8898 0.524 Uiso 1 1 calc R . . C91 C 0.8070(3) 0.0537(8) 0.5253(3) 0.0693(16) Uani 1 1 d . . . H91 H 0.7836 0.0331 0.4826 0.083 Uiso 1 1 calc R . . C92 C 0.2161(4) 0.9472(18) 0.8917(4) 0.130(5) Uani 1 1 d . . . H92 H 0.2550 0.9397 0.9244 0.156 Uiso 1 1 calc R . . C93 C 0.9274(6) 0.9565(18) 0.8158(6) 0.136(4) Uani 1 1 d . . . H93 H 0.9111 1.0514 0.7983 0.163 Uiso 1 1 calc R . . C94 C 0.6671(4) 0.9266(12) 0.7431(4) 0.096(2) Uani 1 1 d . . . H94 H 0.6243 0.9222 0.7500 0.116 Uiso 1 1 calc R . . Cl1 Cl 0.75726(8) 0.0187(2) 0.57430(9) 0.0813(5) Uani 1 1 d . . . Cl2 Cl 0.87078(7) -0.0607(2) 0.54183(12) 0.0933(6) Uani 1 1 d . . . Cl3 Cl 0.82803(10) 0.2337(2) 0.52897(10) 0.0891(5) Uani 1 1 d . . . Cl4 Cl 0.2357(2) 0.9940(8) 0.82635(14) 0.220(3) Uani 1 1 d . . . Cl5 Cl 0.1674(4) 1.0621(11) 0.9168(3) 0.306(6) Uani 1 1 d . . . Cl6 Cl 0.1813(5) 0.7722(14) 0.8813(4) 0.389(9) Uani 1 1 d . . . Cl7 Cl 0.8984(3) 0.9325(10) 0.8784(3) 0.231(3) Uani 1 1 d . . . Cl8 Cl 0.8999(2) 0.8332(7) 0.7606(4) 0.256(4) Uani 1 1 d . . . Cl9 Cl 1.00657(18) 0.9693(5) 0.8299(2) 0.1542(13) Uani 1 1 d . . . Cl10 Cl 0.66893(11) 1.0638(3) 0.69307(17) 0.1237(9) Uani 1 1 d . . . Cl11 Cl 0.7176(3) 0.9596(8) 0.8130(2) 0.222(3) Uani 1 1 d . . . Cl12 Cl 0.68291(18) 0.7620(4) 0.7151(2) 0.1547(14) Uani 1 1 d . . . N1 N 0.4336(2) 1.0672(7) 0.7330(2) 0.0673(13) Uani 1 1 d U . . N2 N -0.18992(18) 0.9931(6) 0.2877(2) 0.0613(13) Uani 1 1 d . . . N3 N 0.4018(2) 0.9693(11) 0.0742(3) 0.098(3) Uani 1 1 d U . . O1 O 0.53153(18) 0.9826(6) 0.7592(2) 0.0760(13) Uani 1 1 d . . . O2 O -0.22134(16) 1.0557(6) 0.37312(19) 0.0666(11) Uani 1 1 d . . . O3 O 0.3376(2) 0.9006(13) -0.0142(3) 0.135(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C85A 0.036(4) 0.093(7) 0.067(4) 0.002(4) 0.004(3) 0.001(4) C86A 0.081(7) 0.140(13) 0.110(7) 0.032(8) -0.021(6) 0.040(7) C87A 0.078(7) 0.22(2) 0.139(11) 0.024(13) -0.004(7) 0.050(11) C85B 0.050(15) 0.14(3) 0.15(3) 0.02(2) -0.075(17) -0.001(17) C86B 0.050(14) 0.14(3) 0.15(3) 0.02(2) -0.076(17) -0.002(17) C87B 0.052(15) 0.14(3) 0.15(3) 0.02(2) -0.076(18) 0.000(18) C88A 0.061(8) 0.20(2) 0.120(18) 0.039(13) 0.022(10) -0.037(9) C89A 0.105(17) 0.25(3) 0.23(3) -0.03(2) 0.090(17) 0.022(18) C90A 0.110(12) 0.35(5) 0.21(2) -0.05(3) 0.076(13) -0.014(17) C95 0.21(3) 0.39(6) 0.49(6) -0.30(5) -0.15(4) 0.15(4) Cl13 0.260(9) 0.224(11) 0.442(16) 0.017(10) 0.230(11) 0.018(8) Cl14 0.311(15) 1.08(6) 0.273(13) -0.29(2) 0.145(12) -0.09(3) Cl15 0.51(3) 0.268(17) 0.47(2) -0.138(17) 0.28(2) -0.079(18) C90B 0.11(2) 0.20(3) 0.053(12) 0.016(18) 0.045(15) 0.10(2) C88B 0.073(16) 0.16(3) 0.032(10) 0.014(18) 0.017(12) -0.01(2) C89B 0.029(12) 0.27(4) 0.041(11) 0.064(16) 0.003(8) 0.002(13) C96 0.065(15) 0.40(8) 0.071(15) 0.03(3) 0.037(12) -0.09(3) Cl16 0.221(19) 0.145(14) 0.182(14) -0.016(11) -0.032(13) 0.004(14) Cl17 0.37(4) 0.32(3) 0.138(11) -0.057(16) 0.083(17) -0.22(3) Cl18 0.156(12) 0.137(13) 0.226(17) 0.009(11) 0.060(11) 0.008(10) C1 0.050(3) 0.053(4) 0.078(3) 0.000(3) -0.001(2) -0.007(3) C2 0.041(2) 0.059(4) 0.071(3) 0.000(3) 0.004(2) 0.003(2) C3 0.048(3) 0.055(4) 0.101(4) 0.011(3) -0.005(3) 0.012(3) C4 0.057(3) 0.049(4) 0.092(4) -0.007(3) -0.010(3) 0.004(3) C5 0.042(2) 0.053(3) 0.067(3) 0.003(3) 0.001(2) 0.002(2) C6 0.044(3) 0.052(4) 0.094(4) 0.001(3) 0.003(3) 0.003(3) C7 0.045(3) 0.062(4) 0.093(4) -0.009(3) -0.002(3) 0.001(3) C8 0.042(2) 0.036(3) 0.066(3) 0.001(2) 0.0005(19) 0.004(2) C9 0.045(2) 0.040(3) 0.070(3) -0.001(2) 0.009(2) 0.001(2) C10 0.043(3) 0.057(4) 0.083(3) 0.008(3) 0.009(2) 0.005(2) C11 0.055(3) 0.073(5) 0.089(4) 0.013(3) 0.024(3) 0.009(3) C12 0.074(4) 0.072(5) 0.070(3) 0.016(3) 0.022(3) 0.009(3) C13 0.053(3) 0.055(4) 0.067(3) 0.002(3) 0.007(2) -0.004(3) C14 0.047(2) 0.038(3) 0.061(2) -0.001(2) 0.009(2) 0.000(2) C15 0.044(2) 0.034(3) 0.061(2) 0.000(2) 0.0033(19) 0.003(2) C16 0.046(2) 0.029(3) 0.059(2) 0.0002(19) 0.0062(18) 0.0013(19) C17 0.045(2) 0.042(3) 0.065(3) -0.003(2) 0.0005(19) 0.001(2) C18 0.057(3) 0.058(4) 0.069(3) 0.000(3) 0.018(2) 0.007(3) C19 0.064(3) 0.062(4) 0.059(3) 0.001(3) 0.003(2) 0.002(3) C20 0.052(3) 0.052(3) 0.061(3) -0.001(2) -0.001(2) 0.003(2) C21 0.042(2) 0.032(3) 0.061(2) 0.000(2) -0.0025(18) 0.0001(19) C22 0.041(2) 0.037(3) 0.059(2) 0.004(2) 0.0092(18) -0.003(2) C23 0.045(2) 0.035(3) 0.063(2) 0.002(2) 0.0055(19) 0.003(2) C24 0.050(3) 0.039(3) 0.063(3) -0.002(2) 0.010(2) -0.006(2) C25 0.041(2) 0.046(3) 0.056(2) 0.005(2) 0.0097(18) -0.003(2) C26 0.046(3) 0.048(3) 0.066(3) 0.000(2) 0.008(2) 0.007(2) C27 0.048(3) 0.044(3) 0.061(3) -0.009(2) 0.003(2) 0.000(2) C28 0.040(2) 0.051(3) 0.069(3) 0.008(2) 0.013(2) -0.004(2) C29 0.042(2) 0.067(4) 0.054(2) 0.009(3) -0.0033(19) -0.001(2) C30 0.054(3) 0.065(4) 0.069(3) 0.005(3) 0.004(2) 0.004(3) C31 0.053(3) 0.074(5) 0.075(3) 0.004(3) 0.011(2) -0.007(3) C32 0.044(3) 0.087(5) 0.068(3) 0.001(3) 0.012(2) -0.002(3) C33 0.052(3) 0.087(5) 0.081(4) -0.015(4) 0.013(3) 0.004(3) C34 0.048(3) 0.078(5) 0.072(3) -0.005(3) 0.009(2) -0.009(3) C35 0.048(3) 0.098(5) 0.063(3) -0.005(3) 0.008(2) -0.003(3) C36 0.045(3) 0.089(5) 0.074(3) -0.014(3) 0.004(2) -0.010(3) C37 0.051(3) 0.095(6) 0.072(3) 0.001(3) 0.007(2) -0.011(3) C38 0.066(4) 0.112(7) 0.076(4) 0.009(4) 0.002(3) -0.009(4) C39 0.058(3) 0.093(6) 0.097(5) 0.015(4) 0.001(3) -0.014(4) C40 0.040(3) 0.098(6) 0.090(4) -0.014(4) 0.009(3) -0.006(3) C41 0.046(3) 0.086(5) 0.077(4) -0.010(3) 0.002(2) -0.007(3) C42 0.050(3) 0.102(6) 0.069(3) -0.014(4) 0.007(2) -0.006(3) C43 0.052(3) 0.122(7) 0.067(3) -0.014(4) 0.005(2) 0.000(4) C44 0.068(4) 0.138(8) 0.072(3) 0.004(4) 0.017(3) 0.004(5) C45 0.089(5) 0.201(13) 0.077(4) 0.033(6) 0.011(4) 0.005(7) C46 0.069(4) 0.243(16) 0.075(4) 0.042(7) 0.007(3) 0.026(7) C47 0.053(3) 0.155(9) 0.075(4) 0.016(5) 0.007(3) 0.010(5) C48 0.051(3) 0.108(6) 0.068(3) -0.007(4) 0.011(2) 0.005(4) C49 0.053(3) 0.101(6) 0.070(3) -0.002(4) 0.008(2) 0.001(4) C50 0.053(3) 0.101(6) 0.102(5) 0.002(4) 0.008(3) -0.003(4) C51 0.057(3) 0.109(7) 0.101(5) -0.002(5) 0.012(3) -0.017(4) C52 0.046(3) 0.141(8) 0.072(3) 0.007(4) 0.001(3) -0.007(4) C53 0.055(3) 0.144(9) 0.081(4) -0.022(5) 0.012(3) -0.010(5) C54 0.054(3) 0.121(7) 0.095(5) -0.016(5) 0.017(3) -0.013(4) C55 0.062(4) 0.186(11) 0.064(4) 0.014(5) 0.008(3) 0.010(5) C56 0.041(3) 0.107(6) 0.077(3) -0.003(4) 0.014(2) -0.006(3) C57 0.050(3) 0.081(5) 0.081(4) -0.014(3) 0.014(3) -0.002(3) C58 0.052(3) 0.059(4) 0.078(3) 0.000(3) 0.010(2) -0.002(3) C59 0.042(2) 0.045(3) 0.088(3) 0.000(3) 0.012(2) -0.003(2) C60 0.052(3) 0.061(4) 0.093(4) 0.004(3) 0.010(3) -0.002(3) C61 0.051(3) 0.090(6) 0.102(5) 0.027(4) 0.016(3) -0.005(3) C62 0.050(3) 0.036(3) 0.077(3) 0.000(2) 0.004(2) 0.001(2) C63 0.040(2) 0.039(3) 0.082(3) -0.007(2) 0.006(2) 0.001(2) C64 0.045(3) 0.058(4) 0.090(4) -0.012(3) 0.007(2) -0.003(3) C65 0.040(3) 0.068(5) 0.109(5) -0.012(4) 0.012(3) -0.011(3) C66 0.059(3) 0.055(4) 0.109(5) -0.007(3) 0.027(3) -0.015(3) C67 0.059(3) 0.049(4) 0.093(4) 0.001(3) 0.021(3) -0.003(3) C68 0.047(3) 0.039(3) 0.087(3) -0.002(3) 0.018(2) 0.000(2) C69 0.049(3) 0.043(3) 0.082(3) -0.002(3) 0.006(2) 0.003(2) C70 0.049(3) 0.037(3) 0.081(3) 0.002(2) 0.008(2) 0.003(2) C71 0.053(3) 0.057(4) 0.080(3) 0.000(3) 0.002(2) 0.006(3) C72 0.036(2) 0.071(5) 0.102(4) 0.003(4) 0.001(3) 0.000(3) C73 0.039(2) 0.063(4) 0.105(4) 0.003(3) 0.013(3) 0.003(3) C74 0.050(3) 0.052(4) 0.088(3) -0.001(3) 0.016(2) 0.004(3) C75 0.044(2) 0.038(3) 0.088(3) 0.004(3) 0.010(2) 0.001(2) C76 0.051(3) 0.044(3) 0.081(3) -0.002(3) 0.013(2) -0.003(2) C77 0.071(4) 0.047(4) 0.081(4) -0.004(3) 0.001(3) 0.016(3) C78 0.067(3) 0.053(4) 0.077(3) 0.002(3) -0.006(3) 0.013(3) C79 0.042(2) 0.046(3) 0.076(3) 0.001(3) 0.000(2) -0.002(2) C80 0.056(3) 0.043(3) 0.085(4) 0.001(3) 0.015(3) -0.001(3) C81 0.071(4) 0.041(3) 0.093(4) -0.002(3) 0.023(3) 0.002(3) C82 0.054(3) 0.209(11) 0.065(3) 0.004(5) -0.001(3) 0.005(5) C83 0.117(9) 0.45(3) 0.141(8) 0.141(16) -0.034(8) -0.123(15) C84 0.32(3) 0.53(6) 0.154(10) 0.15(2) -0.030(18) -0.19(4) C91 0.058(3) 0.065(4) 0.082(3) -0.007(3) 0.011(3) 0.009(3) C92 0.084(5) 0.202(13) 0.081(4) -0.011(6) -0.029(4) 0.033(7) C93 0.114(8) 0.136(11) 0.153(9) -0.005(8) 0.020(7) 0.038(8) C94 0.064(4) 0.094(6) 0.136(7) 0.001(5) 0.032(4) 0.003(4) Cl1 0.0670(8) 0.0775(12) 0.1039(11) 0.0018(9) 0.0287(7) 0.0050(8) Cl2 0.0543(8) 0.0628(11) 0.1663(18) 0.0188(11) 0.0324(9) 0.0098(8) Cl3 0.1117(14) 0.0517(10) 0.1162(13) 0.0008(9) 0.0514(11) 0.0088(9) Cl4 0.175(3) 0.380(9) 0.1069(17) 0.066(3) 0.0369(19) 0.130(5) Cl5 0.316(8) 0.453(13) 0.179(4) 0.106(6) 0.119(5) 0.261(9) Cl6 0.368(11) 0.559(19) 0.280(8) -0.256(11) 0.158(8) -0.319(13) Cl7 0.178(4) 0.320(9) 0.191(4) 0.077(5) 0.034(3) 0.006(5) Cl8 0.162(4) 0.207(5) 0.334(7) -0.147(5) -0.074(4) 0.054(4) Cl9 0.130(2) 0.130(3) 0.198(3) -0.005(2) 0.029(2) 0.002(2) Cl10 0.0838(13) 0.0882(17) 0.207(3) 0.0312(17) 0.0494(15) 0.0010(12) Cl11 0.208(5) 0.240(7) 0.179(4) -0.020(4) -0.035(3) -0.052(5) Cl12 0.141(2) 0.0766(18) 0.261(4) -0.003(2) 0.076(3) 0.0135(16) N1 0.042(2) 0.082(4) 0.070(2) 0.001(3) -0.0030(18) -0.002(2) N2 0.0313(18) 0.080(4) 0.067(2) 0.004(2) 0.0012(16) -0.004(2) N3 0.052(3) 0.164(8) 0.077(3) 0.015(4) 0.014(2) -0.010(4) O1 0.048(2) 0.088(4) 0.079(2) 0.007(2) -0.0119(17) 0.008(2) O2 0.0408(17) 0.074(3) 0.086(2) -0.006(2) 0.0157(16) 0.0007(19) O3 0.064(3) 0.259(12) 0.081(3) 0.012(5) 0.017(2) -0.009(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 C85A N2 1.478(8) . ? C85A C86A 1.493(15) . ? C85A H85A 0.9900 . ? C85A H85B 0.9900 . ? C86A C87A 1.588(15) . ? C86A H86A 0.9900 . ? C86A H86B 0.9900 . ? C87A H87A 0.9800 . ? C87A H87B 0.9800 . ? C87A H87C 0.9800 . ? C85B C86B 1.49(2) . ? C85B N2 1.66(4) . ? C85B H85C 0.9900 . ? C85B H85D 0.9900 . ? C86B C87B 1.59(2) . ? C86B H86C 0.9900 . ? C86B H86D 0.9900 . ? C87B H87D 0.9800 . ? C87B H87E 0.9800 . ? C87B H87F 0.9800 . ? C88A N3 1.52(3) . ? C88A C89A 1.73(5) . ? C88A H88A 0.9900 . ? C88A H88B 0.9900 . ? C89A C90A 1.61(3) . ? C89A H89A 0.9900 . ? C89A H89B 0.9900 . ? C90A H90A 0.9800 . ? C90A H90B 0.9800 . ? C90A H90C 0.9800 . ? C95 Cl14 1.53(3) . ? C95 Cl13 1.99(3) . ? C95 Cl15 2.13(3) . ? C95 H95 1.0000 . ? C90B C89B 1.54(9) . ? C90B H90D 0.9800 . ? C90B H90E 0.9800 . ? C90B H90F 0.9800 . ? C88B C89B 1.23(9) . ? C88B N3 1.38(6) . ? C88B H88C 0.9900 . ? C88B H88D 0.9900 . ? C89B H89C 0.9900 . ? C89B H89D 0.9900 . ? C96 Cl17 1.57(3) . ? C96 Cl16 2.01(3) . ? C96 Cl18 2.14(3) . ? C96 H96 1.0000 . ? C1 O1 1.242(7) . ? C1 N1 1.344(8) . ? C1 C79 1.483(9) . ? C2 C3 1.375(10) . ? C2 C7 1.381(9) . ? C2 N1 1.443(7) . ? C3 C4 1.393(8) . ? C3 H3 0.9500 . ? C4 C5 1.387(9) . ? C4 H4 0.9500 . ? C5 C6 1.358(9) . ? C5 C8 1.520(6) . ? C6 C7 1.404(8) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C21 1.389(7) . ? C8 C9 1.397(8) . ? C9 C10 1.430(8) . ? C9 C14 1.443(7) . ? C10 C11 1.329(9) . ? C10 H10 0.9500 . ? C11 C12 1.416(10) . ? C11 H11 0.9500 . ? C12 C13 1.364(9) . ? C12 H12 0.9500 . ? C13 C14 1.413(8) . ? C13 H13 0.9500 . ? C14 C15 1.415(7) . ? C15 C16 1.419(7) . ? C15 C22 1.492(6) . ? C16 C17 1.417(7) . ? C16 C21 1.443(6) . ? C17 C18 1.354(8) . ? C17 H17 0.9500 . ? C18 C19 1.422(8) . ? C18 H18 0.9500 . ? C19 C20 1.350(9) . ? C19 H19 0.9500 . ? C20 C21 1.434(7) . ? C20 H20 0.9500 . ? C22 C27 1.388(8) . ? C22 C23 1.392(7) . ? C23 C24 1.381(7) . ? C23 H23 0.9500 . ? C24 C25 1.390(8) . ? C24 H24 0.9500 . ? C25 C26 1.383(8) . ? C25 C28 1.502(6) . ? C26 C27 1.382(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 O2 1.228(7) . ? C28 N2 1.365(7) . ? C29 C34 1.372(10) . ? C29 C30 1.381(9) . ? C29 N2 1.411(7) . ? C30 C31 1.375(9) . ? C30 H30 0.9500 . ? C31 C32 1.381(11) . ? C31 H31 0.9500 . ? C32 C33 1.352(11) . ? C32 C35 1.522(8) . ? C33 C34 1.393(9) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.396(10) . ? C35 C48 1.403(10) . ? C36 C37 1.418(10) . ? C36 C41 1.444(9) . ? C37 C38 1.369(11) . ? C37 H37 0.9500 . ? C38 C39 1.401(11) . ? C38 H38 0.9500 . ? C39 C40 1.326(11) . ? C39 H39 0.9500 . ? C40 C41 1.446(10) . ? C40 H40 0.9500 . ? C41 C42 1.378(11) . ? C42 C43 1.430(11) . ? C42 C49 1.491(9) . ? C43 C48 1.426(9) . ? C43 C44 1.438(11) . ? C44 C45 1.334(14) . ? C44 H44 0.9500 . ? C45 C46 1.416(13) . ? C45 H45 0.9500 . ? C46 C47 1.358(12) . ? C46 H46 0.9500 . ? C47 C48 1.436(11) . ? C47 H47 0.9500 . ? C49 C54 1.363(13) . ? C49 C50 1.378(12) . ? C50 C51 1.372(11) . ? C50 H50 0.9500 . ? C51 C52 1.375(14) . ? C51 H51 0.9500 . ? C52 C53 1.381(14) . ? C52 C55 1.500(10) . ? C53 C54 1.410(10) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 O3 1.251(10) . ? C55 N3 1.343(10) . ? C56 C61 1.386(12) . ? C56 C57 1.389(12) . ? C56 N3 1.440(9) . ? C57 C58 1.348(9) . ? C57 H57 0.9500 . ? C58 C59 1.397(9) . ? C58 H58 0.9500 . ? C59 C60 1.402(10) . ? C59 C62 1.494(8) . ? C60 C61 1.368(11) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C63 1.376(8) . ? C62 C75 1.419(8) . ? C63 C68 1.428(8) . ? C63 C64 1.447(7) . ? C64 C65 1.377(9) . ? C64 H64 0.9500 . ? C65 C66 1.402(11) . ? C65 H65 0.9500 . ? C66 C67 1.341(9) . ? C66 H66 0.9500 . ? C67 C68 1.441(8) . ? C67 H67 0.9500 . ? C68 C69 1.406(8) . ? C69 C70 1.404(8) . ? C69 C76 1.490(8) . ? C70 C75 1.413(9) . ? C70 C71 1.443(8) . ? C71 C72 1.340(9) . ? C71 H71 0.9500 . ? C72 C73 1.399(10) . ? C72 H72 0.9500 . ? C73 C74 1.364(9) . ? C73 H73 0.9500 . ? C74 C75 1.434(8) . ? C74 H74 0.9500 . ? C76 C77 1.380(9) . ? C76 C81 1.405(9) . ? C77 C78 1.381(10) . ? C77 H77 0.9500 . ? C78 C79 1.387(9) . ? C78 H78 0.9500 . ? C79 C80 1.372(9) . ? C80 C81 1.379(9) . ? C80 H80 0.9500 . ? C81 H81 0.9500 . ? C82 N1 1.447(9) . ? C82 C83 1.46(2) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.21(2) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C91 Cl3 1.737(8) . ? C91 Cl2 1.743(7) . ? C91 Cl1 1.764(7) . ? C91 H91 1.0000 . ? C92 Cl4 1.685(12) . ? C92 Cl5 1.709(13) . ? C92 Cl6 1.796(19) . ? C92 H92 1.0000 . ? C93 Cl7 1.696(15) . ? C93 Cl8 1.699(15) . ? C93 Cl9 1.720(13) . ? C93 H93 1.0000 . ? C94 Cl10 1.709(11) . ? C94 Cl12 1.725(11) . ? C94 Cl11 1.736(10) . ? C94 H94 1.0000 . ? 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 N2 C85A C86A 111.7(9) . . ? N2 C85A H85A 109.3 . . ? C86A C85A H85A 109.3 . . ? N2 C85A H85B 109.3 . . ? C86A C85A H85B 109.3 . . ? H85A C85A H85B 107.9 . . ? C85A C86A C87A 108.0(12) . . ? C85A C86A H86A 110.1 . . ? C87A C86A H86A 110.1 . . ? C85A C86A H86B 110.1 . . ? C87A C86A H86B 110.1 . . ? H86A C86A H86B 108.4 . . ? C86B C85B N2 97(3) . . ? C86B C85B H85C 112.3 . . ? N2 C85B H85C 112.3 . . ? C86B C85B H85D 112.3 . . ? N2 C85B H85D 112.3 . . ? H85C C85B H85D 109.9 . . ? C85B C86B C87B 107(3) . . ? C85B C86B H86C 110.2 . . ? C87B C86B H86C 110.2 . . ? C85B C86B H86D 110.2 . . ? C87B C86B H86D 110.2 . . ? H86C C86B H86D 108.5 . . ? C86B C87B H87D 109.5 . . ? C86B C87B H87E 109.5 . . ? H87D C87B H87E 109.5 . . ? C86B C87B H87F 109.5 . . ? H87D C87B H87F 109.5 . . ? H87E C87B H87F 109.5 . . ? N3 C88A C89A 104(2) . . ? N3 C88A H88A 111.0 . . ? C89A C88A H88A 111.0 . . ? N3 C88A H88B 111.0 . . ? C89A C88A H88B 111.0 . . ? H88A C88A H88B 109.0 . . ? C90A C89A C88A 103(3) . . ? C90A C89A H89A 111.1 . . ? C88A C89A H89A 111.1 . . ? C90A C89A H89B 111.1 . . ? C88A C89A H89B 111.1 . . ? H89A C89A H89B 109.1 . . ? Cl14 C95 Cl13 102.5(18) . . ? Cl14 C95 Cl15 94.0(16) . . ? Cl13 C95 Cl15 89.5(15) . . ? Cl14 C95 H95 121.2 . . ? Cl13 C95 H95 121.2 . . ? Cl15 C95 H95 121.2 . . ? C89B C88B N3 131(6) . . ? C89B C88B H88C 104.4 . . ? N3 C88B H88C 104.4 . . ? C89B C88B H88D 104.4 . . ? N3 C88B H88D 104.4 . . ? H88C C88B H88D 105.6 . . ? C88B C89B C90B 104(4) . . ? C88B C89B H89C 111.0 . . ? C90B C89B H89C 111.0 . . ? C88B C89B H89D 111.0 . . ? C90B C89B H89D 111.0 . . ? H89C C89B H89D 109.0 . . ? Cl17 C96 Cl16 103.5(18) . . ? Cl17 C96 Cl18 90.5(13) . . ? Cl16 C96 Cl18 91.8(15) . . ? Cl17 C96 H96 121.2 . . ? Cl16 C96 H96 121.2 . . ? Cl18 C96 H96 121.2 . . ? O1 C1 N1 122.0(6) . . ? O1 C1 C79 120.1(6) . . ? N1 C1 C79 117.8(5) . . ? C3 C2 C7 119.1(5) . . ? C3 C2 N1 120.3(6) . . ? C7 C2 N1 120.6(6) . . ? C2 C3 C4 119.9(6) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.9(6) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 119.0(5) . . ? C6 C5 C8 121.7(5) . . ? C4 C5 C8 119.2(5) . . ? C5 C6 C7 120.4(6) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C2 C7 C6 120.5(6) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C21 C8 C9 121.3(4) . . ? C21 C8 C5 118.9(4) . . ? C9 C8 C5 119.7(5) . . ? C8 C9 C10 123.9(5) . . ? C8 C9 C14 119.7(5) . . ? C10 C9 C14 116.4(5) . . ? C11 C10 C9 122.9(5) . . ? C11 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C10 C11 C12 120.6(6) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 119.4(6) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 121.6(5) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C13 C14 C15 121.8(4) . . ? C13 C14 C9 118.9(5) . . ? C15 C14 C9 119.3(4) . . ? C14 C15 C16 120.3(4) . . ? C14 C15 C22 120.1(4) . . ? C16 C15 C22 119.6(4) . . ? C17 C16 C15 122.0(4) . . ? C17 C16 C21 118.8(4) . . ? C15 C16 C21 119.2(4) . . ? C18 C17 C16 121.7(5) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C19 120.1(5) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 120.0(5) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 122.3(5) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C8 C21 C20 123.0(4) . . ? C8 C21 C16 120.0(4) . . ? C20 C21 C16 117.0(4) . . ? C27 C22 C23 117.7(4) . . ? C27 C22 C15 120.1(5) . . ? C23 C22 C15 122.1(5) . . ? C24 C23 C22 121.5(5) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 119.6(5) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 119.7(4) . . ? C26 C25 C28 118.2(5) . . ? C24 C25 C28 122.1(5) . . ? C27 C26 C25 119.9(5) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C22 121.5(5) . . ? C26 C27 H27 119.2 . . ? C22 C27 H27 119.2 . . ? O2 C28 N2 122.1(4) . . ? O2 C28 C25 120.0(5) . . ? N2 C28 C25 117.8(4) . . ? C34 C29 C30 118.5(6) . . ? C34 C29 N2 120.5(6) . . ? C30 C29 N2 120.9(6) . . ? C31 C30 C29 121.2(7) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C30 C31 C32 119.9(6) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C33 C32 C31 119.0(6) . . ? C33 C32 C35 122.2(7) . . ? C31 C32 C35 118.6(6) . . ? C32 C33 C34 121.5(7) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C29 C34 C33 119.7(6) . . ? C29 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C36 C35 C48 120.6(6) . . ? C36 C35 C32 118.6(6) . . ? C48 C35 C32 120.8(6) . . ? C35 C36 C37 121.9(6) . . ? C35 C36 C41 119.5(6) . . ? C37 C36 C41 118.6(6) . . ? C38 C37 C36 121.3(6) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C37 C38 C39 120.0(7) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 121.0(7) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C39 C40 C41 122.4(6) . . ? C39 C40 H40 118.8 . . ? C41 C40 H40 118.8 . . ? C42 C41 C36 120.4(6) . . ? C42 C41 C40 123.1(6) . . ? C36 C41 C40 116.5(6) . . ? C41 C42 C43 120.2(6) . . ? C41 C42 C49 121.8(6) . . ? C43 C42 C49 117.9(6) . . ? C48 C43 C42 119.3(7) . . ? C48 C43 C44 118.6(7) . . ? C42 C43 C44 122.1(6) . . ? C45 C44 C43 121.4(7) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C44 C45 C46 120.7(9) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C47 C46 C45 119.9(8) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 121.7(7) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C35 C48 C43 120.0(6) . . ? C35 C48 C47 122.5(6) . . ? C43 C48 C47 117.4(6) . . ? C54 C49 C50 117.6(7) . . ? C54 C49 C42 121.1(7) . . ? C50 C49 C42 121.3(8) . . ? C51 C50 C49 121.8(9) . . ? C51 C50 H50 119.1 . . ? C49 C50 H50 119.1 . . ? C50 C51 C52 120.4(8) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C51 C52 C53 119.5(7) . . ? C51 C52 C55 121.0(9) . . ? C53 C52 C55 119.2(9) . . ? C52 C53 C54 118.6(9) . . ? C52 C53 H53 120.7 . . ? C54 C53 H53 120.7 . . ? C49 C54 C53 122.0(9) . . ? C49 C54 H54 119.0 . . ? C53 C54 H54 119.0 . . ? O3 C55 N3 120.7(7) . . ? O3 C55 C52 118.5(7) . . ? N3 C55 C52 120.7(6) . . ? C61 C56 C57 119.0(6) . . ? C61 C56 N3 120.1(8) . . ? C57 C56 N3 120.8(8) . . ? C58 C57 C56 120.9(7) . . ? C58 C57 H57 119.6 . . ? C56 C57 H57 119.6 . . ? C57 C58 C59 120.9(7) . . ? C57 C58 H58 119.6 . . ? C59 C58 H58 119.6 . . ? C58 C59 C60 118.4(6) . . ? C58 C59 C62 121.0(5) . . ? C60 C59 C62 120.6(6) . . ? C61 C60 C59 120.1(7) . . ? C61 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C60 C61 C56 120.6(7) . . ? C60 C61 H61 119.7 . . ? C56 C61 H61 119.7 . . ? C63 C62 C75 119.7(5) . . ? C63 C62 C59 120.3(5) . . ? C75 C62 C59 120.0(5) . . ? C62 C63 C68 120.6(5) . . ? C62 C63 C64 121.8(5) . . ? C68 C63 C64 117.6(5) . . ? C65 C64 C63 120.2(6) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C64 C65 C66 121.0(5) . . ? C64 C65 H65 119.5 . . ? C66 C65 H65 119.5 . . ? C67 C66 C65 120.9(6) . . ? C67 C66 H66 119.5 . . ? C65 C66 H66 119.5 . . ? C66 C67 C68 120.9(6) . . ? C66 C67 H67 119.5 . . ? C68 C67 H67 119.5 . . ? C69 C68 C63 119.6(5) . . ? C69 C68 C67 121.3(6) . . ? C63 C68 C67 119.1(5) . . ? C70 C69 C68 119.9(5) . . ? C70 C69 C76 122.7(5) . . ? C68 C69 C76 117.4(5) . . ? C69 C70 C75 119.8(5) . . ? C69 C70 C71 121.3(5) . . ? C75 C70 C71 118.8(5) . . ? C72 C71 C70 120.3(6) . . ? C72 C71 H71 119.8 . . ? C70 C71 H71 119.8 . . ? C71 C72 C73 121.6(5) . . ? C71 C72 H72 119.2 . . ? C73 C72 H72 119.2 . . ? C74 C73 C72 120.0(6) . . ? C74 C73 H73 120.0 . . ? C72 C73 H73 120.0 . . ? C73 C74 C75 121.1(6) . . ? C73 C74 H74 119.5 . . ? C75 C74 H74 119.5 . . ? C70 C75 C62 120.1(5) . . ? C70 C75 C74 118.0(5) . . ? C62 C75 C74 121.9(6) . . ? C77 C76 C81 117.4(6) . . ? C77 C76 C69 123.1(6) . . ? C81 C76 C69 119.2(5) . . ? C76 C77 C78 122.2(6) . . ? C76 C77 H77 118.9 . . ? C78 C77 H77 118.9 . . ? C77 C78 C79 119.2(6) . . ? C77 C78 H78 120.4 . . ? C79 C78 H78 120.4 . . ? C80 C79 C78 119.6(6) . . ? C80 C79 C1 121.9(6) . . ? C78 C79 C1 118.5(5) . . ? C79 C80 C81 120.9(6) . . ? C79 C80 H80 119.6 . . ? C81 C80 H80 119.6 . . ? C80 C81 C76 120.4(6) . . ? C80 C81 H81 119.8 . . ? C76 C81 H81 119.8 . . ? N1 C82 C83 113.3(13) . . ? N1 C82 H82A 108.9 . . ? C83 C82 H82A 108.9 . . ? N1 C82 H82B 108.9 . . ? C83 C82 H82B 108.9 . . ? H82A C82 H82B 107.7 . . ? C84 C83 C82 126(2) . . ? C84 C83 H83A 105.7 . . ? C82 C83 H83A 105.7 . . ? C84 C83 H83B 105.7 . . ? C82 C83 H83B 105.7 . . ? H83A C83 H83B 106.2 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? Cl3 C91 Cl2 112.5(4) . . ? Cl3 C91 Cl1 110.5(4) . . ? Cl2 C91 Cl1 110.6(4) . . ? Cl3 C91 H91 107.7 . . ? Cl2 C91 H91 107.7 . . ? Cl1 C91 H91 107.7 . . ? Cl4 C92 Cl5 116.0(9) . . ? Cl4 C92 Cl6 108.2(7) . . ? Cl5 C92 Cl6 108.9(8) . . ? Cl4 C92 H92 107.8 . . ? Cl5 C92 H92 107.8 . . ? Cl6 C92 H92 107.8 . . ? Cl7 C93 Cl8 112.3(10) . . ? Cl7 C93 Cl9 115.3(8) . . ? Cl8 C93 Cl9 111.1(8) . . ? Cl7 C93 H93 105.8 . . ? Cl8 C93 H93 105.8 . . ? Cl9 C93 H93 105.8 . . ? Cl10 C94 Cl12 112.6(6) . . ? Cl10 C94 Cl11 110.9(6) . . ? Cl12 C94 Cl11 110.2(6) . . ? Cl10 C94 H94 107.7 . . ? Cl12 C94 H94 107.7 . . ? Cl11 C94 H94 107.7 . . ? C1 N1 C2 123.7(5) . . ? C1 N1 C82 118.3(5) . . ? C2 N1 C82 116.0(5) . . ? C28 N2 C29 123.1(4) . . ? C28 N2 C85A 118.6(5) . . ? C29 N2 C85A 118.2(5) . . ? C28 N2 C85B 108(2) . . ? C29 N2 C85B 120(3) . . ? C85A N2 C85B 29(2) . . ? C55 N3 C88B 121(2) . . ? C55 N3 C56 122.7(6) . . ? C88B N3 C56 113(2) . . ? C55 N3 C88A 118.4(11) . . ? C88B N3 C88A 14(4) . . ? C56 N3 C88A 118.8(11) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.786 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.083 _database_code_depnum_ccdc_archive 'CCDC 961419' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_u130705mas1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C126 H98 Cl18 N4 O4' _chemical_formula_weight 2370.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 10.5211(2) _cell_length_b 13.4415(3) _cell_length_c 21.8375(4) _cell_angle_alpha 92.4470(10) _cell_angle_beta 96.5220(10) _cell_angle_gamma 111.4330(10) _cell_volume 2844.21(10) _cell_formula_units_Z 1 _cell_measurement_temperature 120 _cell_measurement_reflns_used 8087 _cell_measurement_theta_min 3.93 _cell_measurement_theta_max 66.98 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 4.417 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4720 _exptl_absorpt_correction_T_max 0.6664 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 35078 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 68.03 _reflns_number_total 9867 _reflns_number_gt 6803 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.1768P)^2^+2.5308P] 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 9867 _refine_ls_number_parameters 790 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.2948 _refine_ls_wR_factor_gt 0.2627 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.004 _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 C58A C -0.3302(15) 0.6930(18) 0.7223(10) 0.051(4) Uani 0.509(19) 1 d PD A 1 H58A H -0.3806 0.7387 0.7075 0.062 Uiso 0.509(19) 1 calc PR A 1 H58B H -0.3922 0.6353 0.7439 0.062 Uiso 0.509(19) 1 calc PR A 1 C59A C -0.2045(14) 0.7589(12) 0.7662(7) 0.085(5) Uani 0.509(19) 1 d PD A 1 H59A H -0.2321 0.7981 0.7983 0.101 Uiso 0.509(19) 1 calc PR A 1 H59B H -0.1663 0.7100 0.7872 0.101 Uiso 0.509(19) 1 calc PR A 1 C60A C -0.098(2) 0.8349(17) 0.7382(9) 0.112(7) Uani 0.509(19) 1 d PD A 1 H60A H -0.0727 0.7977 0.7049 0.168 Uiso 0.509(19) 1 calc PR A 1 H60B H -0.0171 0.8706 0.7693 0.168 Uiso 0.509(19) 1 calc PR A 1 H60C H -0.1313 0.8886 0.7210 0.168 Uiso 0.509(19) 1 calc PR A 1 C58B C -0.324(2) 0.7174(19) 0.7089(13) 0.074(8) Uani 0.491(19) 1 d PD A 2 H58C H -0.3738 0.6747 0.7408 0.089 Uiso 0.491(19) 1 calc PR A 2 H58D H -0.3911 0.7410 0.6839 0.089 Uiso 0.491(19) 1 calc PR A 2 C59B C -0.2140(13) 0.8153(12) 0.7418(6) 0.071(4) Uani 0.491(19) 1 d PD A 2 H59C H -0.1901 0.8708 0.7121 0.085 Uiso 0.491(19) 1 calc PR A 2 H59D H -0.2531 0.8423 0.7750 0.085 Uiso 0.491(19) 1 calc PR A 2 C60B C -0.0878(12) 0.8066(14) 0.7692(8) 0.080(5) Uani 0.491(19) 1 d PD A 2 H60D H -0.1093 0.7457 0.7946 0.120 Uiso 0.491(19) 1 calc PR A 2 H60E H -0.0315 0.8728 0.7953 0.120 Uiso 0.491(19) 1 calc PR A 2 H60F H -0.0367 0.7954 0.7365 0.120 Uiso 0.491(19) 1 calc PR A 2 C62A C 0.3794(11) 0.3384(7) 0.0991(4) 0.080(3) Uani 0.619(15) 1 d PD B 3 H62A H 0.4108 0.3164 0.1394 0.096 Uiso 0.619(15) 1 calc PR B 3 Cl4A Cl 0.3005(7) 0.2267(5) 0.0458(4) 0.0859(14) Uani 0.619(15) 1 d PD B 3 Cl5A Cl 0.3148(8) 0.4231(4) 0.1106(3) 0.0901(16) Uani 0.619(15) 1 d PD B 3 Cl6A Cl 0.5409(7) 0.4111(4) 0.0556(2) 0.0968(17) Uani 0.619(15) 1 d PD B 3 C62B C 0.276(3) 0.335(2) 0.0631(14) 0.38(3) Uani 0.381(15) 1 d PDU B 4 H62B H 0.2134 0.3356 0.0252 0.450 Uiso 0.381(15) 1 calc PR B 4 Cl4B Cl 0.2702(11) 0.2052(8) 0.0674(6) 0.089(2) Uani 0.381(15) 1 d PD B 4 Cl5B Cl 0.2506(16) 0.4001(9) 0.1169(5) 0.103(3) Uani 0.381(15) 1 d PDU B 4 Cl6B Cl 0.466(3) 0.4091(11) 0.0481(5) 0.158(5) Uani 0.381(15) 1 d PD B 4 C63A C 0.6334(19) 0.8336(13) 0.4574(9) 0.091(4) Uani 0.553(5) 1 d P C 5 H63A H 0.6512 0.7975 0.4947 0.109 Uiso 0.553(5) 1 calc PR C 5 Cl7A Cl 0.6105(13) 0.9535(6) 0.4820(6) 0.176(4) Uani 0.553(5) 1 d P C 5 Cl8A Cl 0.4927(5) 0.7476(4) 0.4110(2) 0.1324(17) Uani 0.553(5) 1 d P C 5 Cl9A Cl 0.7745(4) 0.8650(3) 0.4168(2) 0.1056(13) Uani 0.553(5) 1 d P C 5 C63B C 0.683(3) 0.8587(15) 0.4877(10) 0.098(7) Uani 0.447(5) 1 d P C 6 H63B H 0.6702 0.8007 0.5163 0.118 Uiso 0.447(5) 1 calc PR C 6 Cl7B Cl 0.6117(17) 0.9373(10) 0.5119(5) 0.148(4) Uani 0.447(5) 1 d P C 6 Cl8B Cl 0.6284(9) 0.8004(5) 0.4138(3) 0.147(4) Uani 0.447(5) 1 d P C 6 Cl9B Cl 0.8714(5) 0.9429(3) 0.4943(2) 0.1056(16) Uani 0.447(5) 1 d P C 6 C1 C 0.2550(5) -0.0469(4) 0.9775(2) 0.0594(11) Uani 1 1 d . . . C2 C 0.1970(5) 0.0021(3) 0.9264(2) 0.0573(11) Uani 1 1 d . . . C3 C 0.0653(5) 0.0013(4) 0.9275(2) 0.0632(12) Uani 1 1 d . . . H3 H 0.0081 -0.0423 0.9544 0.076 Uiso 1 1 calc R . . C4 C 0.0171(5) 0.0625(4) 0.8905(2) 0.0656(12) Uani 1 1 d . . . H4 H -0.0737 0.0607 0.8917 0.079 Uiso 1 1 calc R . . C5 C 0.0995(5) 0.1284(4) 0.8504(2) 0.0618(11) Uani 1 1 d . . . C6 C 0.2258(5) 0.1239(4) 0.8474(2) 0.0664(12) Uani 1 1 d . . . H6 H 0.2815 0.1649 0.8192 0.080 Uiso 1 1 calc R . . C7 C 0.2749(5) 0.0617(4) 0.8839(2) 0.0635(12) Uani 1 1 d . . . H7 H 0.3629 0.0594 0.8802 0.076 Uiso 1 1 calc R . . C8 C 0.0492(5) 0.2048(4) 0.8170(2) 0.0619(11) Uani 1 1 d . . . C9 C 0.0454(5) 0.2947(4) 0.8515(2) 0.0583(11) Uani 1 1 d . . . C10 C 0.0989(6) 0.3192(4) 0.9154(2) 0.0724(13) Uani 1 1 d . . . H10 H 0.1367 0.2734 0.9360 0.087 Uiso 1 1 calc R . . C11 C 0.0964(7) 0.4083(5) 0.9477(3) 0.0831(16) Uani 1 1 d . . . H11 H 0.1321 0.4230 0.9905 0.100 Uiso 1 1 calc R . . C12 C 0.0425(6) 0.4772(4) 0.9189(2) 0.0781(15) Uani 1 1 d . . . H12 H 0.0430 0.5390 0.9419 0.094 Uiso 1 1 calc R . . C13 C -0.0118(5) 0.4565(4) 0.8570(2) 0.0652(12) Uani 1 1 d . . . H13 H -0.0495 0.5035 0.8376 0.078 Uiso 1 1 calc R . . C14 C -0.0113(4) 0.3640(4) 0.8219(2) 0.0562(11) Uani 1 1 d . . . C15 C -0.0644(5) 0.3435(4) 0.7578(2) 0.0586(11) Uani 1 1 d . . . C16 C -0.0496(5) 0.2588(4) 0.7231(2) 0.0616(11) Uani 1 1 d . . . C17 C -0.1006(6) 0.2354(5) 0.6582(3) 0.0765(14) Uani 1 1 d . . . H17 H -0.1399 0.2804 0.6377 0.092 Uiso 1 1 calc R . . C18 C -0.0931(8) 0.1489(5) 0.6257(3) 0.0900(18) Uani 1 1 d . . . H18 H -0.1282 0.1342 0.5828 0.108 Uiso 1 1 calc R . . C19 C -0.0348(8) 0.0824(6) 0.6544(3) 0.097(2) Uani 1 1 d . . . H19 H -0.0288 0.0237 0.6307 0.116 Uiso 1 1 calc R . . C20 C 0.0143(6) 0.1000(5) 0.7162(3) 0.0777(15) Uani 1 1 d . . . H20 H 0.0521 0.0527 0.7351 0.093 Uiso 1 1 calc R . . C21 C 0.0091(5) 0.1900(4) 0.7533(2) 0.0610(11) Uani 1 1 d . . . C22 C -0.1279(4) 0.4151(4) 0.7289(2) 0.0572(11) Uani 1 1 d . . . C23 C -0.2559(5) 0.4136(5) 0.7431(3) 0.0702(13) Uani 1 1 d . . . H23 H -0.3063 0.3612 0.7682 0.084 Uiso 1 1 calc R . . C24 C -0.3082(5) 0.4857(5) 0.7215(3) 0.0705(14) Uani 1 1 d . . . H24 H -0.3952 0.4824 0.7314 0.085 Uiso 1 1 calc R . . C25 C -0.2379(4) 0.5639(4) 0.6854(2) 0.0612(12) Uani 1 1 d . A . C26 C -0.1124(4) 0.5650(4) 0.6695(2) 0.0557(10) Uani 1 1 d . . . H26 H -0.0624 0.6174 0.6444 0.067 Uiso 1 1 calc R . . C27 C -0.0617(4) 0.4900(4) 0.6903(2) 0.0550(11) Uani 1 1 d . . . H27 H 0.0217 0.4896 0.6777 0.066 Uiso 1 1 calc R . . C28 C -0.2891(6) 0.6792(5) 0.6099(3) 0.0762(16) Uani 1 1 d . . . C29 C 0.2723(5) -0.6118(5) 0.4424(2) 0.0675(14) Uani 1 1 d . . . C30 C 0.1792(5) -0.6612(5) 0.4817(3) 0.0739(15) Uani 1 1 d . . . H30 H 0.1199 -0.7342 0.4717 0.089 Uiso 1 1 calc R . . C31 C 0.1698(5) -0.6068(4) 0.5360(2) 0.0690(13) Uani 1 1 d . . . H31 H 0.1028 -0.6414 0.5618 0.083 Uiso 1 1 calc R . . C32 C 0.2614(5) -0.4998(4) 0.5518(2) 0.0607(12) Uani 1 1 d . . . C33 C 0.3535(5) -0.4503(4) 0.5111(2) 0.0601(11) Uani 1 1 d . . . H33 H 0.4151 -0.3779 0.5209 0.072 Uiso 1 1 calc R . . C34 C 0.3562(5) -0.5059(5) 0.4562(2) 0.0665(13) Uani 1 1 d . . . H34 H 0.4167 -0.4701 0.4282 0.080 Uiso 1 1 calc R . . C35 C 0.2648(4) -0.4420(4) 0.6121(2) 0.0580(11) Uani 1 1 d . . . C36 C 0.2937(4) -0.4841(4) 0.6682(2) 0.0532(10) Uani 1 1 d . . . C37 C 0.3169(4) -0.5821(4) 0.6701(2) 0.0592(11) Uani 1 1 d . . . H37 H 0.3181 -0.6193 0.6323 0.071 Uiso 1 1 calc R . . C38 C 0.3370(5) -0.6232(4) 0.7232(2) 0.0627(12) Uani 1 1 d . . . H38 H 0.3503 -0.6895 0.7226 0.075 Uiso 1 1 calc R . . C39 C 0.3387(5) -0.5687(4) 0.7806(2) 0.0627(11) Uani 1 1 d . . . H39 H 0.3517 -0.5991 0.8182 0.075 Uiso 1 1 calc R . . C40 C 0.3220(4) -0.4736(4) 0.7820(2) 0.0584(11) Uani 1 1 d . . . H40 H 0.3244 -0.4373 0.8207 0.070 Uiso 1 1 calc R . . C41 C 0.3009(4) -0.4269(3) 0.7262(2) 0.0530(10) Uani 1 1 d . . . C42 C 0.2818(4) -0.3283(4) 0.7276(2) 0.0536(10) Uani 1 1 d . . . C43 C 0.2503(4) -0.2872(4) 0.6719(2) 0.0548(10) Uani 1 1 d . . . C44 C 0.2275(5) -0.1893(4) 0.6720(2) 0.0615(11) Uani 1 1 d . . . H44 H 0.2361 -0.1494 0.7102 0.074 Uiso 1 1 calc R . . C45 C 0.1940(6) -0.1523(4) 0.6186(3) 0.0702(13) Uani 1 1 d . . . H45 H 0.1801 -0.0863 0.6194 0.084 Uiso 1 1 calc R . . C46 C 0.1795(6) -0.2113(5) 0.5614(2) 0.0730(14) Uani 1 1 d . . . H46 H 0.1532 -0.1853 0.5242 0.088 Uiso 1 1 calc R . . C47 C 0.2021(5) -0.3034(4) 0.5586(2) 0.0655(12) Uani 1 1 d . . . H47 H 0.1923 -0.3412 0.5195 0.079 Uiso 1 1 calc R . . C48 C 0.2408(4) -0.3454(4) 0.6137(2) 0.0560(11) Uani 1 1 d . . . C49 C 0.2921(5) -0.2678(3) 0.7881(2) 0.0545(10) Uani 1 1 d . . . C50 C 0.4196(5) -0.2025(3) 0.8197(2) 0.0535(10) Uani 1 1 d . . . H50 H 0.5007 -0.1944 0.8019 0.064 Uiso 1 1 calc R . . C51 C 0.4303(5) -0.1488(3) 0.8768(2) 0.0544(10) Uani 1 1 d . . . H51 H 0.5183 -0.1041 0.8979 0.065 Uiso 1 1 calc R . . C52 C 0.3121(5) -0.1606(3) 0.9031(2) 0.0525(10) Uani 1 1 d . . . C53 C 0.1846(5) -0.2243(4) 0.8716(2) 0.0610(11) Uani 1 1 d . . . H53 H 0.1034 -0.2320 0.8893 0.073 Uiso 1 1 calc R . . C54 C 0.1747(5) -0.2767(4) 0.8145(2) 0.0628(12) Uani 1 1 d . . . H54 H 0.0864 -0.3195 0.7929 0.075 Uiso 1 1 calc R . . C55 C 0.3907(5) -0.1480(4) 1.0152(2) 0.0598(11) Uani 1 1 d . . . H55A H 0.4214 -0.0927 1.0508 0.072 Uiso 1 1 calc R . . H55B H 0.4735 -0.1575 1.0028 0.072 Uiso 1 1 calc R . . C56 C 0.2951(6) -0.2542(4) 1.0354(3) 0.0768(15) Uani 1 1 d . . . H56A H 0.2128 -0.2448 1.0485 0.092 Uiso 1 1 calc R . . H56B H 0.2637 -0.3097 0.9999 0.092 Uiso 1 1 calc R . . C57 C 0.3685(8) -0.2914(5) 1.0888(3) 0.097(2) Uani 1 1 d . . . H57A H 0.4522 -0.2976 1.0766 0.145 Uiso 1 1 calc R . . H57B H 0.3070 -0.3614 1.0992 0.145 Uiso 1 1 calc R . . H57C H 0.3933 -0.2390 1.1251 0.145 Uiso 1 1 calc R . . C61 C 0.3931(7) 0.9212(5) 0.2665(3) 0.0932(18) Uani 1 1 d . . . H61 H 0.3287 0.8563 0.2830 0.112 Uiso 1 1 calc R . . Cl1 Cl 0.32099(17) 0.92981(15) 0.19071(9) 0.1003(5) Uani 1 1 d . . . Cl2 Cl 0.55053(19) 0.90575(15) 0.26434(9) 0.1020(5) Uani 1 1 d . . . Cl3 Cl 0.4140(2) 1.03467(16) 0.31580(10) 0.1079(6) Uani 1 1 d . . . N1 N 0.3250(4) -0.1106(3) 0.96398(17) 0.0547(9) Uani 1 1 d . . . N2 N -0.2896(4) 0.6442(4) 0.6678(2) 0.0671(11) Uani 1 1 d . . . O1 O 0.2449(4) -0.0225(3) 1.03120(15) 0.0697(9) Uani 1 1 d . . . O2 O -0.3086(5) 0.7622(4) 0.5994(2) 0.0980(14) 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 C58A 0.047(6) 0.065(9) 0.047(9) -0.014(7) 0.009(5) 0.028(5) C59A 0.093(10) 0.073(8) 0.083(9) -0.034(7) 0.004(7) 0.031(7) C60A 0.122(16) 0.133(16) 0.083(12) -0.017(11) -0.002(11) 0.058(12) C58B 0.097(12) 0.073(12) 0.058(12) -0.010(9) 0.015(8) 0.040(9) C59B 0.076(8) 0.065(8) 0.072(8) -0.012(6) 0.010(6) 0.029(6) C60B 0.056(7) 0.090(10) 0.082(11) -0.041(8) 0.007(7) 0.018(7) C62A 0.111(8) 0.056(5) 0.061(5) -0.010(4) -0.008(5) 0.026(5) Cl4A 0.086(3) 0.064(2) 0.100(4) -0.019(2) -0.008(2) 0.028(2) Cl5A 0.120(4) 0.080(2) 0.075(2) -0.0212(16) -0.008(2) 0.052(3) Cl6A 0.145(4) 0.077(2) 0.0564(16) 0.0139(12) 0.0067(19) 0.029(2) C62B 0.52(7) 0.28(5) 0.22(4) -0.02(4) -0.18(5) 0.10(5) Cl4B 0.084(4) 0.060(3) 0.104(6) -0.019(3) 0.001(3) 0.011(3) Cl5B 0.132(7) 0.102(5) 0.095(4) 0.000(3) 0.036(5) 0.061(5) Cl6B 0.284(16) 0.165(8) 0.076(4) 0.024(4) 0.027(8) 0.141(10) C63A 0.116(12) 0.066(9) 0.100(13) 0.005(9) 0.017(10) 0.044(8) Cl7A 0.166(5) 0.070(2) 0.299(13) 0.005(6) 0.031(8) 0.057(3) Cl8A 0.116(3) 0.122(3) 0.116(3) 0.023(2) 0.007(2) -0.004(2) Cl9A 0.106(3) 0.087(2) 0.142(3) 0.0300(19) 0.032(2) 0.0512(19) C63B 0.18(2) 0.057(10) 0.077(12) 0.002(8) 0.031(12) 0.057(12) Cl7B 0.204(8) 0.136(8) 0.140(6) -0.034(5) 0.013(5) 0.114(7) Cl8B 0.264(12) 0.125(5) 0.079(3) -0.030(3) -0.009(4) 0.118(7) Cl9B 0.156(4) 0.087(2) 0.097(3) 0.0112(19) 0.048(3) 0.063(3) C1 0.061(3) 0.052(2) 0.056(3) -0.010(2) 0.015(2) 0.009(2) C2 0.064(3) 0.050(2) 0.053(2) -0.0142(19) 0.010(2) 0.017(2) C3 0.067(3) 0.058(3) 0.059(3) -0.004(2) 0.016(2) 0.016(2) C4 0.061(3) 0.066(3) 0.069(3) -0.011(2) 0.014(2) 0.023(2) C5 0.069(3) 0.057(3) 0.055(3) -0.010(2) 0.008(2) 0.021(2) C6 0.068(3) 0.064(3) 0.066(3) -0.003(2) 0.020(2) 0.021(2) C7 0.065(3) 0.063(3) 0.065(3) -0.003(2) 0.014(2) 0.025(2) C8 0.062(3) 0.060(3) 0.060(3) -0.008(2) 0.013(2) 0.019(2) C9 0.058(2) 0.053(2) 0.058(3) -0.010(2) 0.011(2) 0.015(2) C10 0.088(3) 0.071(3) 0.055(3) -0.007(2) 0.001(2) 0.029(3) C11 0.109(4) 0.077(4) 0.059(3) -0.019(3) -0.011(3) 0.037(3) C12 0.101(4) 0.066(3) 0.061(3) -0.021(2) 0.004(3) 0.029(3) C13 0.069(3) 0.057(3) 0.064(3) -0.011(2) 0.009(2) 0.019(2) C14 0.054(2) 0.053(2) 0.053(2) -0.0113(19) 0.0104(19) 0.0105(19) C15 0.053(2) 0.055(2) 0.062(3) -0.010(2) 0.011(2) 0.014(2) C16 0.066(3) 0.061(3) 0.053(3) -0.008(2) 0.016(2) 0.017(2) C17 0.097(4) 0.073(3) 0.063(3) -0.007(2) 0.017(3) 0.034(3) C18 0.131(5) 0.089(4) 0.059(3) -0.011(3) 0.018(3) 0.052(4) C19 0.149(6) 0.092(4) 0.067(4) -0.015(3) 0.022(4) 0.066(4) C20 0.101(4) 0.076(3) 0.062(3) -0.011(2) 0.018(3) 0.041(3) C21 0.063(3) 0.064(3) 0.058(3) -0.004(2) 0.017(2) 0.025(2) C22 0.047(2) 0.063(3) 0.055(2) -0.019(2) 0.0030(19) 0.016(2) C23 0.056(3) 0.077(3) 0.072(3) -0.012(3) 0.016(2) 0.018(2) C24 0.045(2) 0.086(4) 0.075(3) -0.027(3) 0.008(2) 0.022(2) C25 0.047(2) 0.073(3) 0.061(3) -0.027(2) -0.004(2) 0.026(2) C26 0.045(2) 0.063(3) 0.054(2) -0.013(2) 0.0008(18) 0.0195(19) C27 0.040(2) 0.064(3) 0.058(3) -0.017(2) 0.0054(18) 0.0180(19) C28 0.071(3) 0.093(4) 0.071(3) -0.033(3) -0.009(3) 0.048(3) C29 0.060(3) 0.092(4) 0.057(3) -0.026(3) -0.010(2) 0.045(3) C30 0.066(3) 0.078(3) 0.076(3) -0.035(3) -0.018(3) 0.037(3) C31 0.049(2) 0.080(3) 0.071(3) -0.026(3) -0.008(2) 0.024(2) C32 0.054(2) 0.078(3) 0.054(3) -0.021(2) -0.009(2) 0.038(2) C33 0.054(2) 0.074(3) 0.056(3) -0.020(2) -0.003(2) 0.034(2) C34 0.061(3) 0.089(4) 0.057(3) -0.020(2) -0.007(2) 0.045(3) C35 0.047(2) 0.066(3) 0.059(3) -0.017(2) 0.0007(19) 0.023(2) C36 0.040(2) 0.058(2) 0.055(2) -0.0121(19) 0.0027(17) 0.0150(18) C37 0.048(2) 0.058(3) 0.070(3) -0.015(2) 0.006(2) 0.021(2) C38 0.051(2) 0.056(3) 0.078(3) -0.009(2) 0.009(2) 0.019(2) C39 0.055(2) 0.060(3) 0.071(3) 0.003(2) 0.009(2) 0.018(2) C40 0.052(2) 0.059(3) 0.057(3) -0.007(2) 0.0062(19) 0.014(2) C41 0.041(2) 0.052(2) 0.061(3) -0.0113(19) 0.0021(18) 0.0136(17) C42 0.047(2) 0.054(2) 0.053(2) -0.0100(19) 0.0034(18) 0.0131(18) C43 0.049(2) 0.056(2) 0.056(3) -0.0087(19) 0.0038(19) 0.0182(19) C44 0.065(3) 0.060(3) 0.058(3) -0.010(2) 0.006(2) 0.023(2) C45 0.080(3) 0.067(3) 0.073(3) 0.001(2) 0.012(3) 0.038(3) C46 0.080(3) 0.092(4) 0.056(3) -0.003(3) 0.003(2) 0.045(3) C47 0.069(3) 0.083(3) 0.052(3) -0.010(2) 0.002(2) 0.040(3) C48 0.049(2) 0.065(3) 0.054(2) -0.013(2) 0.0010(18) 0.025(2) C49 0.059(2) 0.050(2) 0.052(2) -0.0049(18) 0.0044(19) 0.0192(19) C50 0.055(2) 0.050(2) 0.053(2) -0.0064(18) 0.0107(19) 0.0170(19) C51 0.057(2) 0.045(2) 0.054(2) -0.0061(18) 0.0051(19) 0.0136(18) C52 0.061(2) 0.042(2) 0.051(2) -0.0050(17) 0.0123(19) 0.0147(18) C53 0.060(3) 0.058(3) 0.059(3) -0.010(2) 0.017(2) 0.015(2) C54 0.056(2) 0.059(3) 0.062(3) -0.016(2) 0.008(2) 0.011(2) C55 0.072(3) 0.050(2) 0.050(2) -0.0059(19) 0.012(2) 0.014(2) C56 0.092(4) 0.053(3) 0.068(3) 0.003(2) 0.013(3) 0.006(3) C57 0.134(6) 0.059(3) 0.077(4) 0.013(3) 0.017(4) 0.012(3) C61 0.089(4) 0.081(4) 0.102(5) 0.009(3) 0.029(3) 0.018(3) Cl1 0.0828(10) 0.1019(12) 0.1013(12) 0.0060(9) 0.0078(8) 0.0189(8) Cl2 0.1067(12) 0.0946(11) 0.1122(13) -0.0001(9) 0.0127(10) 0.0482(9) Cl3 0.1035(12) 0.1080(13) 0.1155(14) -0.0096(10) 0.0228(10) 0.0431(10) N1 0.065(2) 0.0468(19) 0.0483(19) -0.0088(15) 0.0117(16) 0.0160(16) N2 0.058(2) 0.081(3) 0.065(3) -0.027(2) -0.0033(18) 0.037(2) O1 0.083(2) 0.072(2) 0.0531(19) -0.0114(15) 0.0163(16) 0.0281(18) O2 0.140(4) 0.110(3) 0.074(3) -0.023(2) -0.007(2) 0.092(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C58A C59A 1.496(13) . ? C58A N2 1.51(2) . ? C58A H58A 0.9900 . ? C58A H58B 0.9900 . ? C59A C60A 1.431(16) . ? C59A H59A 0.9900 . ? C59A H59B 0.9900 . ? C60A H60A 0.9800 . ? C60A H60B 0.9800 . ? C60A H60C 0.9800 . ? C58B N2 1.47(3) . ? C58B C59B 1.487(15) . ? C58B H58C 0.9900 . ? C58B H58D 0.9900 . ? C59B C60B 1.440(16) . ? C59B H59C 0.9900 . ? C59B H59D 0.9900 . ? C60B H60D 0.9800 . ? C60B H60E 0.9800 . ? C60B H60F 0.9800 . ? C62A Cl5A 1.550(11) . ? C62A Cl4A 1.737(10) . ? C62A Cl6A 1.994(12) . ? C62A H62A 1.0000 . ? C62B Cl5B 1.54(2) . ? C62B Cl4B 1.73(2) . ? C62B Cl6B 1.96(2) . ? C62B H62B 1.0000 . ? C63A Cl8A 1.693(19) . ? C63A Cl9A 1.745(19) . ? C63A Cl7A 1.784(19) . ? C63A H63A 1.0000 . ? C63B Cl7B 1.60(2) . ? C63B Cl8B 1.702(19) . ? C63B Cl9B 1.88(3) . ? C63B H63B 1.0000 . ? C1 O1 1.230(5) . ? C1 N1 1.361(6) . ? C1 C2 1.503(7) . ? C2 C3 1.385(7) . ? C2 C7 1.389(7) . ? C3 C4 1.364(7) . ? C3 H3 0.9500 . ? C4 C5 1.406(7) . ? C4 H4 0.9500 . ? C5 C6 1.361(7) . ? C5 C8 1.497(7) . ? C6 C7 1.371(7) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C21 1.392(7) . ? C8 C9 1.412(6) . ? C9 C14 1.420(7) . ? C9 C10 1.420(7) . ? C10 C11 1.375(8) . ? C10 H10 0.9500 . ? C11 C12 1.389(8) . ? C11 H11 0.9500 . ? C12 C13 1.382(7) . ? C12 H12 0.9500 . ? C13 C14 1.435(6) . ? C13 H13 0.9500 . ? C14 C15 1.422(7) . ? C15 C16 1.405(6) . ? C15 C22 1.483(7) . ? C16 C21 1.432(7) . ? C16 C17 1.434(7) . ? C17 C18 1.369(8) . ? C17 H17 0.9500 . ? C18 C19 1.389(9) . ? C18 H18 0.9500 . ? C19 C20 1.368(8) . ? C19 H19 0.9500 . ? C20 C21 1.447(7) . ? C20 H20 0.9500 . ? C22 C27 1.379(7) . ? C22 C23 1.410(7) . ? C23 C24 1.354(8) . ? C23 H23 0.9500 . ? C24 C25 1.381(8) . ? C24 H24 0.9500 . ? C25 C26 1.399(6) . ? C25 N2 1.423(7) . ? C26 C27 1.373(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 O2 1.232(7) . ? C28 N2 1.368(8) . ? C28 C29 1.495(6) 2_556 ? C29 C34 1.372(8) . ? C29 C30 1.379(8) . ? C29 C28 1.495(6) 2_556 ? C30 C31 1.398(7) . ? C30 H30 0.9500 . ? C31 C32 1.409(7) . ? C31 H31 0.9500 . ? C32 C33 1.395(7) . ? C32 C35 1.491(6) . ? C33 C34 1.393(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C48 1.410(7) . ? C35 C36 1.419(7) . ? C36 C37 1.426(6) . ? C36 C41 1.433(6) . ? C37 C38 1.335(7) . ? C37 H37 0.9500 . ? C38 C39 1.420(7) . ? C38 H38 0.9500 . ? C39 C40 1.353(7) . ? C39 H39 0.9500 . ? C40 C41 1.425(7) . ? C40 H40 0.9500 . ? C41 C42 1.411(6) . ? C42 C43 1.410(7) . ? C42 C49 1.494(6) . ? C43 C44 1.421(7) . ? C43 C48 1.438(6) . ? C44 C45 1.348(7) . ? C44 H44 0.9500 . ? C45 C46 1.413(7) . ? C45 H45 0.9500 . ? C46 C47 1.344(8) . ? C46 H46 0.9500 . ? C47 C48 1.431(7) . ? C47 H47 0.9500 . ? C49 C50 1.387(6) . ? C49 C54 1.390(7) . ? C50 C51 1.386(6) . ? C50 H50 0.9500 . ? C51 C52 1.388(6) . ? C51 H51 0.9500 . ? C52 C53 1.381(6) . ? C52 N1 1.433(5) . ? C53 C54 1.380(6) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 N1 1.452(6) . ? C55 C56 1.532(7) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.528(9) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C61 Cl2 1.749(7) . ? C61 Cl3 1.759(7) . ? C61 Cl1 1.768(8) . ? C61 H61 1.0000 . ? 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 C59A C58A N2 110.0(12) . . ? C59A C58A H58A 109.7 . . ? N2 C58A H58A 109.7 . . ? C59A C58A H58B 109.7 . . ? N2 C58A H58B 109.7 . . ? H58A C58A H58B 108.2 . . ? C60A C59A C58A 114.7(16) . . ? C60A C59A H59A 108.6 . . ? C58A C59A H59A 108.6 . . ? C60A C59A H59B 108.6 . . ? C58A C59A H59B 108.6 . . ? H59A C59A H59B 107.6 . . ? N2 C58B C59B 120(2) . . ? N2 C58B H58C 107.3 . . ? C59B C58B H58C 107.3 . . ? N2 C58B H58D 107.3 . . ? C59B C58B H58D 107.3 . . ? H58C C58B H58D 106.9 . . ? C60B C59B C58B 118.2(15) . . ? C60B C59B H59C 107.7 . . ? C58B C59B H59C 107.7 . . ? C60B C59B H59D 107.7 . . ? C58B C59B H59D 107.7 . . ? H59C C59B H59D 107.1 . . ? C59B C60B H60D 109.5 . . ? C59B C60B H60E 109.5 . . ? H60D C60B H60E 109.5 . . ? C59B C60B H60F 109.5 . . ? H60D C60B H60F 109.5 . . ? H60E C60B H60F 109.5 . . ? Cl5A C62A Cl4A 122.8(7) . . ? Cl5A C62A Cl6A 105.6(6) . . ? Cl4A C62A Cl6A 97.0(6) . . ? Cl5A C62A H62A 110.0 . . ? Cl4A C62A H62A 110.0 . . ? Cl6A C62A H62A 110.0 . . ? Cl5B C62B Cl4B 123.2(19) . . ? Cl5B C62B Cl6B 107.4(14) . . ? Cl4B C62B Cl6B 101.1(13) . . ? Cl5B C62B H62B 108.1 . . ? Cl4B C62B H62B 108.1 . . ? Cl6B C62B H62B 108.1 . . ? Cl8A C63A Cl9A 108.4(11) . . ? Cl8A C63A Cl7A 111.8(11) . . ? Cl9A C63A Cl7A 109.8(10) . . ? Cl8A C63A H63A 108.9 . . ? Cl9A C63A H63A 108.9 . . ? Cl7A C63A H63A 108.9 . . ? Cl7B C63B Cl8B 117.5(16) . . ? Cl7B C63B Cl9B 105.5(12) . . ? Cl8B C63B Cl9B 108.1(13) . . ? Cl7B C63B H63B 108.5 . . ? Cl8B C63B H63B 108.5 . . ? Cl9B C63B H63B 108.5 . . ? O1 C1 N1 121.9(5) . . ? O1 C1 C2 118.4(4) . . ? N1 C1 C2 119.6(4) . . ? C3 C2 C7 118.2(5) . . ? C3 C2 C1 117.6(4) . . ? C7 C2 C1 123.4(4) . . ? C4 C3 C2 120.6(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 121.1(5) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 117.5(5) . . ? C6 C5 C8 123.4(5) . . ? C4 C5 C8 119.0(4) . . ? C5 C6 C7 121.9(5) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C6 C7 C2 120.5(5) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? C21 C8 C9 119.9(5) . . ? C21 C8 C5 121.6(4) . . ? C9 C8 C5 118.5(4) . . ? C8 C9 C14 119.6(4) . . ? C8 C9 C10 121.9(5) . . ? C14 C9 C10 118.5(4) . . ? C11 C10 C9 120.8(5) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 121.0(5) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 120.5(5) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.0(5) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C9 C14 C15 120.5(4) . . ? C9 C14 C13 119.2(4) . . ? C15 C14 C13 120.3(5) . . ? C16 C15 C14 119.1(5) . . ? C16 C15 C22 121.8(4) . . ? C14 C15 C22 119.0(4) . . ? C15 C16 C21 119.8(4) . . ? C15 C16 C17 121.2(5) . . ? C21 C16 C17 118.9(4) . . ? C18 C17 C16 120.7(6) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 120.9(6) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 C18 121.1(5) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 120.7(6) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C8 C21 C16 120.6(4) . . ? C8 C21 C20 121.5(5) . . ? C16 C21 C20 117.8(5) . . ? C27 C22 C23 117.2(5) . . ? C27 C22 C15 122.0(4) . . ? C23 C22 C15 120.7(5) . . ? C24 C23 C22 120.9(5) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 121.5(4) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C24 C25 C26 118.4(5) . . ? C24 C25 N2 120.2(4) . . ? C26 C25 N2 121.3(5) . . ? C27 C26 C25 119.8(5) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C22 122.1(4) . . ? C26 C27 H27 119.0 . . ? C22 C27 H27 119.0 . . ? O2 C28 N2 121.7(5) . . ? O2 C28 C29 119.2(6) . 2_556 ? N2 C28 C29 119.0(5) . 2_556 ? C34 C29 C30 119.2(4) . . ? C34 C29 C28 122.1(5) . 2_556 ? C30 C29 C28 118.3(5) . 2_556 ? C29 C30 C31 121.8(5) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C30 C31 C32 118.8(5) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? C33 C32 C31 118.7(4) . . ? C33 C32 C35 120.4(4) . . ? C31 C32 C35 120.8(5) . . ? C34 C33 C32 120.7(5) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C29 C34 C33 120.6(5) . . ? C29 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C48 C35 C36 119.9(4) . . ? C48 C35 C32 120.4(4) . . ? C36 C35 C32 119.7(4) . . ? C35 C36 C37 122.9(4) . . ? C35 C36 C41 119.7(4) . . ? C37 C36 C41 117.4(4) . . ? C38 C37 C36 122.1(5) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C37 C38 C39 120.5(5) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 120.2(5) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 121.0(5) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C42 C41 C40 121.0(4) . . ? C42 C41 C36 120.2(4) . . ? C40 C41 C36 118.8(4) . . ? C43 C42 C41 120.4(4) . . ? C43 C42 C49 119.6(4) . . ? C41 C42 C49 120.0(4) . . ? C42 C43 C44 121.5(4) . . ? C42 C43 C48 119.5(4) . . ? C44 C43 C48 119.0(4) . . ? C45 C44 C43 121.0(5) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C44 C45 C46 120.2(5) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C47 C46 C45 121.3(5) . . ? C47 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? C46 C47 C48 120.9(5) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? C35 C48 C47 122.1(4) . . ? C35 C48 C43 120.3(4) . . ? C47 C48 C43 117.5(4) . . ? C50 C49 C54 118.5(4) . . ? C50 C49 C42 120.6(4) . . ? C54 C49 C42 120.9(4) . . ? C51 C50 C49 121.0(4) . . ? C51 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C50 C51 C52 119.8(4) . . ? C50 C51 H51 120.1 . . ? C52 C51 H51 120.1 . . ? C53 C52 C51 119.7(4) . . ? C53 C52 N1 120.9(4) . . ? C51 C52 N1 119.3(4) . . ? C54 C53 C52 120.2(4) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C49 120.9(4) . . ? C53 C54 H54 119.5 . . ? C49 C54 H54 119.5 . . ? N1 C55 C56 112.8(4) . . ? N1 C55 H55A 109.0 . . ? C56 C55 H55A 109.0 . . ? N1 C55 H55B 109.0 . . ? C56 C55 H55B 109.0 . . ? H55A C55 H55B 107.8 . . ? C57 C56 C55 111.2(5) . . ? C57 C56 H56A 109.4 . . ? C55 C56 H56A 109.4 . . ? C57 C56 H56B 109.4 . . ? C55 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? Cl2 C61 Cl3 110.9(4) . . ? Cl2 C61 Cl1 109.6(4) . . ? Cl3 C61 Cl1 111.2(4) . . ? Cl2 C61 H61 108.4 . . ? Cl3 C61 H61 108.4 . . ? Cl1 C61 H61 108.4 . . ? C1 N1 C52 122.8(4) . . ? C1 N1 C55 117.9(4) . . ? C52 N1 C55 117.9(4) . . ? C28 N2 C25 123.4(4) . . ? C28 N2 C58B 108.2(12) . . ? C25 N2 C58B 127.3(12) . . ? C28 N2 C58A 124.7(11) . . ? C25 N2 C58A 111.6(10) . . ? C58B N2 C58A 16.9(18) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 66.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.984 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 961420'