data_080417bm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H78 Cl18 N12 O6' _chemical_formula_weight 1629.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 12.6429(15) _cell_length_b 13.0515(16) _cell_length_c 13.7972(16) _cell_angle_alpha 63.541(2) _cell_angle_beta 73.029(2) _cell_angle_gamma 76.461(2) _cell_volume 1935.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2644 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 18.53 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18574 _diffrn_reflns_av_R_equivalents 0.1834 _diffrn_reflns_av_sigmaI/netI 0.1430 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6694 _reflns_number_gt 2714 _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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0967P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6694 _refine_ls_number_parameters 490 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1694 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2379 _refine_ls_wR_factor_gt 0.1938 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2575(4) 0.5101(4) 0.1997(3) 0.0798(13) Uani 1 1 d . . . H1A H 0.2980 0.4398 0.2441 0.096 Uiso 1 1 calc R . . H1B H 0.2789 0.5741 0.2045 0.096 Uiso 1 1 calc R . . C2 C 0.0970(4) 0.4090(4) 0.3262(3) 0.0630(10) Uani 1 1 d . . . C3 C 0.0542(4) 0.6049(4) 0.2284(4) 0.0753(12) Uani 1 1 d . . . H3 H 0.0641 0.6581 0.1500 0.090 Uiso 1 1 calc R . . C4 C 0.0527(5) 0.6683(4) 0.3029(5) 0.1099(18) Uani 1 1 d . . . H4A H 0.0729 0.6116 0.3717 0.132 Uiso 1 1 calc R . . H4B H 0.1087 0.7211 0.2651 0.132 Uiso 1 1 calc R . . C5 C -0.0562(6) 0.7334(5) 0.3292(5) 0.1163(19) Uani 1 1 d . . . H5A H -0.0526 0.7653 0.3795 0.140 Uiso 1 1 calc R . . H5B H -0.0723 0.7970 0.2617 0.140 Uiso 1 1 calc R . . C6 C -0.1453(5) 0.6606(5) 0.3797(5) 0.1091(18) Uani 1 1 d . . . H6A H -0.2149 0.7054 0.3979 0.131 Uiso 1 1 calc R . . H6B H -0.1301 0.5979 0.4481 0.131 Uiso 1 1 calc R . . C7 C -0.1564(4) 0.6127(4) 0.3044(4) 0.0894(14) Uani 1 1 d . . . H7A H -0.1793 0.6754 0.2397 0.107 Uiso 1 1 calc R . . H7B H -0.2144 0.5623 0.3420 0.107 Uiso 1 1 calc R . . C8 C -0.0498(3) 0.5457(3) 0.2668(3) 0.0664(11) Uani 1 1 d . . . H8 H -0.0585 0.5303 0.2064 0.080 Uiso 1 1 calc R . . C9 C -0.0844(4) 0.3439(4) 0.4066(3) 0.0701(11) Uani 1 1 d . . . H9A H -0.1551 0.3679 0.4471 0.084 Uiso 1 1 calc R . . H9B H -0.0478 0.2779 0.4596 0.084 Uiso 1 1 calc R . . C10 C -0.2092(4) 0.3106(4) 0.3176(3) 0.0683(11) Uani 1 1 d . . . C11 C -0.0810(4) 0.2519(4) 0.1883(4) 0.0706(12) Uani 1 1 d . . . H11 H -0.0701 0.3267 0.1257 0.085 Uiso 1 1 calc R . . C12 C -0.0421(4) 0.1591(4) 0.1433(4) 0.0960(15) Uani 1 1 d . . . H12A H -0.0974 0.1599 0.1067 0.115 Uiso 1 1 calc R . . H12B H 0.0268 0.1768 0.0882 0.115 Uiso 1 1 calc R . . C13 C -0.0236(6) 0.0414(5) 0.2313(5) 0.1165(19) Uani 1 1 d . . . H13A H 0.0093 -0.0128 0.1970 0.140 Uiso 1 1 calc R . . H13B H -0.0947 0.0179 0.2792 0.140 Uiso 1 1 calc R . . C14 C 0.0522(6) 0.0375(5) 0.3002(6) 0.122(2) Uani 1 1 d . . . H14A H 0.0636 -0.0402 0.3557 0.146 Uiso 1 1 calc R . . H14B H 0.1241 0.0591 0.2529 0.146 Uiso 1 1 calc R . . C15 C 0.0009(5) 0.1193(4) 0.3562(4) 0.0935(15) Uani 1 1 d . . . H15A H 0.0512 0.1177 0.3984 0.112 Uiso 1 1 calc R . . H15B H -0.0680 0.0935 0.4078 0.112 Uiso 1 1 calc R . . C16 C -0.0229(3) 0.2417(4) 0.2741(3) 0.0696(12) Uani 1 1 d . . . H16 H 0.0462 0.2776 0.2377 0.084 Uiso 1 1 calc R . . C17 C -0.2887(4) 0.2750(4) 0.1964(4) 0.0811(13) Uani 1 1 d . . . H17A H -0.3586 0.2867 0.2454 0.097 Uiso 1 1 calc R . . H17B H -0.2891 0.2062 0.1862 0.097 Uiso 1 1 calc R . . C18 C 0.2807(4) 0.6335(5) 0.0057(4) 0.0725(12) Uani 1 1 d . . . C19 C 0.2985(4) 0.5062(4) -0.0782(4) 0.0901(14) Uani 1 1 d . . . H19 H 0.2496 0.4969 -0.1165 0.108 Uiso 1 1 calc R . . C20 C 0.4160(5) 0.4685(5) -0.1210(4) 0.0998(16) Uani 1 1 d . . . H20A H 0.4646 0.5037 -0.1050 0.120 Uiso 1 1 calc R . . H20B H 0.4289 0.4960 -0.2009 0.120 Uiso 1 1 calc R . . C21 C 0.4457(5) 0.3410(6) -0.0727(5) 0.1181(19) Uani 1 1 d . . . H21A H 0.5241 0.3222 -0.1012 0.142 Uiso 1 1 calc R . . H21B H 0.4028 0.3057 -0.0950 0.142 Uiso 1 1 calc R . . C22 C 0.4232(5) 0.2932(5) 0.0507(5) 0.1212(19) Uani 1 1 d . . . H22A H 0.4679 0.3261 0.0735 0.145 Uiso 1 1 calc R . . H22B H 0.4434 0.2103 0.0801 0.145 Uiso 1 1 calc R . . C23 C 0.2978(5) 0.3218(5) 0.0974(5) 0.1092(17) Uani 1 1 d . . . H23A H 0.2547 0.2789 0.0840 0.131 Uiso 1 1 calc R . . H23B H 0.2857 0.2966 0.1770 0.131 Uiso 1 1 calc R . . C24 C 0.2573(4) 0.4446(4) 0.0485(4) 0.0829(13) Uani 1 1 d . . . H24 H 0.1757 0.4522 0.0644 0.099 Uiso 1 1 calc R . . C25 C 0.5977(4) 0.3256(5) 0.5990(4) 0.1114(19) Uani 1 1 d D . . H25 H 0.6172 0.3205 0.5270 0.134 Uiso 1 1 calc R A 1 C26 C 0.7106(6) 0.0272(5) 0.0380(5) 0.125(2) Uani 1 1 d . . . H26 H 0.7017 0.1103 0.0182 0.150 Uiso 1 1 calc R B 1 C27 C 0.3374(6) 0.1313(6) 0.4398(6) 0.144(3) Uani 1 1 d . . . H27 H 0.2694 0.1859 0.4293 0.173 Uiso 1 1 calc R C 1 Cl1 Cl 0.6333(7) 0.4537(6) 0.5915(8) 0.136(3) Uani 0.48(2) 1 d PD D 1 Cl2 Cl 0.6747(7) 0.2241(8) 0.6900(9) 0.176(3) Uani 0.48(2) 1 d PD D 1 Cl3 Cl 0.4573(5) 0.3277(13) 0.6561(6) 0.184(4) Uani 0.48(2) 1 d PD D 1 Cl4 Cl 0.6897(7) 0.0070(12) -0.0709(7) 0.249(5) Uani 0.538(13) 1 d PD E 1 Cl5 Cl 0.8450(7) -0.0273(7) 0.0534(8) 0.196(4) Uani 0.538(13) 1 d PD E 1 Cl6 Cl 0.6142(9) -0.0309(9) 0.1519(7) 0.260(5) Uani 0.538(13) 1 d PD E 1 Cl7 Cl 0.4372(5) 0.2027(9) 0.3842(8) 0.288(8) Uani 0.550(12) 1 d PD F 1 Cl8 Cl 0.3311(6) 0.0581(6) 0.5879(6) 0.183(3) Uani 0.550(12) 1 d PD F 1 Cl9 Cl 0.3307(11) 0.0287(10) 0.3993(15) 0.317(8) Uani 0.550(12) 1 d PD F 1 Cl1' Cl 0.4670(7) 0.2872(13) 0.6574(9) 0.243(6) Uani 0.52(2) 1 d PD D 2 Cl2' Cl 0.6879(8) 0.2019(8) 0.6461(13) 0.238(5) Uani 0.52(2) 1 d PD D 2 Cl3' Cl 0.6235(10) 0.4301(13) 0.6201(13) 0.263(8) Uani 0.52(2) 1 d PD D 2 Cl4' Cl 0.6362(16) -0.0225(10) -0.0017(13) 0.332(9) Uani 0.462(13) 1 d PD E 2 Cl5' Cl 0.6783(10) -0.0196(6) 0.1871(7) 0.192(4) Uani 0.462(13) 1 d PD E 2 Cl6' Cl 0.8479(10) -0.0054(16) 0.0042(15) 0.316(8) Uani 0.462(13) 1 d PD E 2 Cl7' Cl 0.4296(8) 0.1960(10) 0.4582(12) 0.224(5) Uani 0.450(12) 1 d PD F 2 Cl8' Cl 0.2960(6) 0.0168(9) 0.5450(7) 0.200(5) Uani 0.450(12) 1 d PD F 2 Cl9' Cl 0.4144(9) 0.0962(10) 0.3265(6) 0.211(5) Uani 0.450(12) 1 d PD F 2 N1 N 0.1400(3) 0.5054(3) 0.2454(3) 0.0690(9) Uani 1 1 d . . . N2 N -0.0164(3) 0.4362(3) 0.3540(2) 0.0619(9) Uani 1 1 d . . . N3 N -0.1048(3) 0.3104(3) 0.3283(3) 0.0699(9) Uani 1 1 d . . . N4 N -0.1980(3) 0.2572(3) 0.2480(3) 0.0721(10) Uani 1 1 d . . . N5 N 0.2899(3) 0.5237(3) 0.0848(3) 0.0748(10) Uani 1 1 d . . . N6 N 0.2811(3) 0.6269(3) -0.0899(3) 0.0755(10) Uani 1 1 d . . . O1 O 0.1484(2) 0.3148(3) 0.3673(2) 0.0809(9) Uani 1 1 d . . . O2 O -0.2968(3) 0.3512(3) 0.3620(2) 0.0892(10) Uani 1 1 d . . . O3 O 0.2757(3) 0.7217(3) 0.0161(3) 0.1002(11) 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 C1 0.070(3) 0.105(3) 0.066(3) -0.033(2) -0.017(2) -0.015(2) C2 0.066(3) 0.073(3) 0.053(2) -0.032(2) -0.013(2) 0.001(2) C3 0.076(3) 0.068(3) 0.079(3) -0.024(2) -0.019(2) -0.011(2) C4 0.113(5) 0.083(3) 0.151(5) -0.044(4) -0.048(4) -0.026(3) C5 0.154(6) 0.088(4) 0.123(5) -0.059(4) -0.039(4) 0.003(4) C6 0.114(4) 0.085(3) 0.135(5) -0.065(4) -0.020(4) 0.009(3) C7 0.077(3) 0.075(3) 0.112(4) -0.040(3) -0.025(3) 0.006(2) C8 0.071(3) 0.073(3) 0.064(3) -0.036(2) -0.019(2) -0.002(2) C9 0.071(3) 0.083(3) 0.056(2) -0.032(2) -0.005(2) -0.013(2) C10 0.081(4) 0.070(3) 0.051(2) -0.022(2) -0.004(2) -0.020(2) C11 0.075(3) 0.071(3) 0.065(3) -0.034(2) -0.003(2) -0.009(2) C12 0.099(4) 0.107(4) 0.096(4) -0.064(3) 0.000(3) -0.020(3) C13 0.147(5) 0.088(4) 0.123(5) -0.058(4) -0.013(4) -0.019(4) C14 0.140(5) 0.073(3) 0.136(5) -0.038(4) -0.030(4) 0.009(3) C15 0.107(4) 0.074(3) 0.101(4) -0.035(3) -0.027(3) -0.006(3) C16 0.062(3) 0.076(3) 0.074(3) -0.039(2) 0.000(2) -0.013(2) C17 0.094(3) 0.090(3) 0.067(3) -0.034(3) -0.004(2) -0.036(3) C18 0.069(3) 0.089(4) 0.074(3) -0.043(3) -0.005(2) -0.028(2) C19 0.100(4) 0.101(4) 0.071(3) -0.040(3) -0.009(3) -0.019(3) C20 0.101(4) 0.101(4) 0.086(3) -0.041(3) 0.004(3) -0.016(3) C21 0.110(4) 0.144(6) 0.106(5) -0.071(4) 0.001(3) -0.013(4) C22 0.116(5) 0.114(4) 0.120(5) -0.049(4) -0.017(4) 0.006(4) C23 0.122(5) 0.098(4) 0.097(4) -0.033(3) -0.003(3) -0.033(3) C24 0.083(3) 0.092(4) 0.080(3) -0.048(3) -0.006(2) -0.013(3) C25 0.098(4) 0.163(6) 0.086(4) -0.068(4) 0.004(3) -0.032(4) C26 0.160(6) 0.083(4) 0.122(5) -0.044(3) -0.018(5) -0.009(4) C27 0.102(5) 0.134(6) 0.145(6) -0.024(5) -0.045(5) 0.035(4) Cl1 0.170(5) 0.138(5) 0.096(4) -0.058(3) 0.004(3) -0.034(4) Cl2 0.148(5) 0.215(7) 0.176(7) -0.086(6) -0.072(5) 0.020(4) Cl3 0.076(4) 0.372(11) 0.118(5) -0.131(6) -0.005(3) -0.010(5) Cl4 0.228(7) 0.405(13) 0.179(6) -0.172(8) -0.063(5) -0.020(7) Cl5 0.219(7) 0.197(5) 0.236(7) -0.130(5) -0.140(6) 0.060(5) Cl6 0.261(9) 0.307(9) 0.141(5) -0.056(5) 0.054(5) -0.099(7) Cl7 0.090(3) 0.325(11) 0.231(9) 0.075(8) -0.008(4) -0.055(4) Cl8 0.159(5) 0.158(4) 0.151(4) -0.011(3) -0.021(3) 0.006(3) Cl9 0.257(12) 0.283(10) 0.48(2) -0.216(13) -0.173(14) 0.090(9) Cl1' 0.150(7) 0.367(11) 0.248(9) -0.157(7) 0.054(6) -0.153(8) Cl2' 0.267(9) 0.157(5) 0.174(8) -0.013(5) 0.001(5) 0.012(5) Cl3' 0.318(12) 0.398(16) 0.145(7) -0.149(8) 0.035(6) -0.201(11) Cl4' 0.52(2) 0.282(9) 0.298(16) -0.064(9) -0.183(15) -0.233(12) Cl5' 0.242(8) 0.164(5) 0.165(5) -0.062(4) -0.001(5) -0.078(5) Cl6' 0.224(10) 0.420(18) 0.328(15) -0.277(15) 0.045(9) 0.047(10) Cl7' 0.165(7) 0.261(11) 0.320(13) -0.195(10) -0.083(8) 0.038(6) Cl8' 0.161(5) 0.221(7) 0.124(5) 0.011(5) -0.006(4) -0.051(5) Cl9' 0.187(7) 0.298(10) 0.148(5) -0.123(6) -0.054(4) 0.062(6) N1 0.056(2) 0.077(2) 0.066(2) -0.0254(19) -0.0090(17) -0.0075(18) N2 0.060(2) 0.069(2) 0.0576(19) -0.0288(18) -0.0115(16) -0.0048(17) N3 0.067(2) 0.078(2) 0.069(2) -0.0388(19) -0.0042(18) -0.0102(18) N4 0.078(3) 0.084(2) 0.058(2) -0.0286(19) -0.0071(19) -0.0272(19) N5 0.074(2) 0.090(3) 0.059(2) -0.026(2) -0.0102(18) -0.021(2) N6 0.094(3) 0.072(2) 0.064(2) -0.0258(19) -0.0141(19) -0.0226(19) O1 0.0711(19) 0.085(2) 0.078(2) -0.0303(17) -0.0221(16) 0.0081(16) O2 0.064(2) 0.130(3) 0.081(2) -0.061(2) -0.0004(16) -0.0062(18) O3 0.144(3) 0.091(2) 0.080(2) -0.0417(19) -0.0153(19) -0.039(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.439(5) . ? C1 N5 1.456(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O1 1.214(5) . ? C2 N1 1.356(5) . ? C2 N2 1.376(5) . ? C3 N1 1.461(5) . ? C3 C8 1.521(6) . ? C3 C4 1.575(7) . ? C3 H3 0.9800 . ? C4 C5 1.477(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.452(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.483(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.514(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N2 1.467(5) . ? C8 H8 0.9800 . ? C9 N2 1.434(5) . ? C9 N3 1.436(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O2 1.225(5) . ? C10 N3 1.370(5) . ? C10 N4 1.378(5) . ? C11 N4 1.471(5) . ? C11 C16 1.511(6) . ? C11 C12 1.518(6) . ? C11 H11 0.9800 . ? C12 C13 1.492(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.514(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.509(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.512(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N3 1.465(5) . ? C16 H16 0.9800 . ? C17 N4 1.443(5) . ? C17 N6 1.452(5) 2_565 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O3 1.207(5) . ? C18 N6 1.359(5) . ? C18 N5 1.364(5) . ? C19 N6 1.479(6) . ? C19 C20 1.483(7) . ? C19 C24 1.545(6) . ? C19 H19 0.9800 . ? C20 C21 1.490(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.491(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.552(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.462(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N5 1.506(6) . ? C24 H24 0.9800 . ? C25 Cl3' 1.632(9) . ? C25 Cl1' 1.697(8) . ? C25 Cl2 1.705(8) . ? C25 Cl3 1.717(7) . ? C25 Cl2' 1.722(8) . ? C25 Cl1 1.783(8) . ? C25 H25 0.9800 . ? C26 Cl4' 1.585(9) . ? C26 Cl6' 1.664(13) . ? C26 Cl6 1.668(9) . ? C26 Cl5 1.718(10) . ? C26 Cl4 1.737(9) . ? C26 Cl5' 1.810(10) . ? C26 H26 0.9800 . ? C27 Cl7 1.548(10) . ? C27 Cl8' 1.614(9) . ? C27 Cl9 1.690(11) . ? C27 Cl7' 1.720(12) . ? C27 Cl9' 1.772(10) . ? C27 Cl8 1.816(10) . ? C27 H27 0.9800 . ? N6 C17 1.452(5) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N5 113.3(3) . . ? N1 C1 H1A 108.9 . . ? N5 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? N5 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O1 C2 N1 126.7(4) . . ? O1 C2 N2 125.5(4) . . ? N1 C2 N2 107.8(4) . . ? N1 C3 C8 100.5(3) . . ? N1 C3 C4 111.0(4) . . ? C8 C3 C4 111.5(4) . . ? N1 C3 H3 111.2 . . ? C8 C3 H3 111.2 . . ? C4 C3 H3 111.2 . . ? C5 C4 C3 113.8(4) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 111.6(5) . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 111.3(5) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C6 C7 C8 113.4(4) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N2 C8 C7 114.7(3) . . ? N2 C8 C3 100.4(3) . . ? C7 C8 C3 114.8(4) . . ? N2 C8 H8 108.8 . . ? C7 C8 H8 108.8 . . ? C3 C8 H8 108.8 . . ? N2 C9 N3 112.2(3) . . ? N2 C9 H9A 109.2 . . ? N3 C9 H9A 109.2 . . ? N2 C9 H9B 109.2 . . ? N3 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? O2 C10 N3 126.0(4) . . ? O2 C10 N4 126.2(4) . . ? N3 C10 N4 107.8(4) . . ? N4 C11 C16 100.6(3) . . ? N4 C11 C12 115.8(4) . . ? C16 C11 C12 115.9(4) . . ? N4 C11 H11 108.0 . . ? C16 C11 H11 108.0 . . ? C12 C11 H11 108.0 . . ? C13 C12 C11 112.9(4) . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 C13 C14 111.7(5) . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C13 109.9(5) . . ? C15 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? C15 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C14 C15 C16 112.3(4) . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? N3 C16 C11 101.0(3) . . ? N3 C16 C15 111.3(3) . . ? C11 C16 C15 114.0(4) . . ? N3 C16 H16 110.1 . . ? C11 C16 H16 110.1 . . ? C15 C16 H16 110.1 . . ? N4 C17 N6 112.6(3) . 2_565 ? N4 C17 H17A 109.1 . . ? N6 C17 H17A 109.1 2_565 . ? N4 C17 H17B 109.1 . . ? N6 C17 H17B 109.1 2_565 . ? H17A C17 H17B 107.8 . . ? O3 C18 N6 125.1(5) . . ? O3 C18 N5 127.2(4) . . ? N6 C18 N5 107.7(4) . . ? N6 C19 C20 112.7(4) . . ? N6 C19 C24 99.8(4) . . ? C20 C19 C24 114.6(4) . . ? N6 C19 H19 109.8 . . ? C20 C19 H19 109.8 . . ? C24 C19 H19 109.8 . . ? C19 C20 C21 113.4(4) . . ? C19 C20 H20A 108.9 . . ? C21 C20 H20A 108.9 . . ? C19 C20 H20B 108.9 . . ? C21 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C20 C21 C22 111.3(5) . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 109.8(5) . . ? C21 C22 H22A 109.7 . . ? C23 C22 H22A 109.7 . . ? C21 C22 H22B 109.7 . . ? C23 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C24 C23 C22 113.4(4) . . ? C24 C23 H23A 108.9 . . ? C22 C23 H23A 108.9 . . ? C24 C23 H23B 108.9 . . ? C22 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C23 C24 N5 117.8(4) . . ? C23 C24 C19 115.4(4) . . ? N5 C24 C19 99.5(4) . . ? C23 C24 H24 107.8 . . ? N5 C24 H24 107.8 . . ? C19 C24 H24 107.8 . . ? Cl3' C25 Cl1' 115.5(6) . . ? Cl3' C25 Cl2 92.5(7) . . ? Cl1' C25 Cl2 103.3(6) . . ? Cl3' C25 Cl3 99.7(7) . . ? Cl1' C25 Cl3 17.1(7) . . ? Cl2 C25 Cl3 112.0(5) . . ? Cl3' C25 Cl2' 112.1(7) . . ? Cl1' C25 Cl2' 106.5(6) . . ? Cl2 C25 Cl2' 25.1(5) . . ? Cl3 C25 Cl2' 120.7(6) . . ? Cl3' C25 Cl1 11.9(7) . . ? Cl1' C25 Cl1 121.6(6) . . ? Cl2 C25 Cl1 100.1(5) . . ? Cl3 C25 Cl1 104.9(5) . . ? Cl2' C25 Cl1 116.5(7) . . ? Cl3' C25 H25 124.7 . . ? Cl1' C25 H25 105.5 . . ? Cl2 C25 H25 113.0 . . ? Cl3 C25 H25 113.0 . . ? Cl2' C25 H25 88.5 . . ? Cl1 C25 H25 113.0 . . ? Cl4' C26 Cl6' 116.6(8) . . ? Cl4' C26 Cl6 76.3(6) . . ? Cl6' C26 Cl6 132.9(8) . . ? Cl4' C26 Cl5 125.3(8) . . ? Cl6' C26 Cl5 20.4(7) . . ? Cl6 C26 Cl5 114.0(5) . . ? Cl4' C26 Cl4 33.4(5) . . ? Cl6' C26 Cl4 92.2(7) . . ? Cl6 C26 Cl4 109.7(6) . . ? Cl5 C26 Cl4 108.6(5) . . ? Cl4' C26 Cl5' 112.5(6) . . ? Cl6' C26 Cl5' 105.0(6) . . ? Cl6 C26 Cl5' 37.5(4) . . ? Cl5 C26 Cl5' 84.7(5) . . ? Cl4 C26 Cl5' 144.9(5) . . ? Cl4' C26 H26 119.4 . . ? Cl6' C26 H26 103.2 . . ? Cl6 C26 H26 108.1 . . ? Cl5 C26 H26 108.1 . . ? Cl4 C26 H26 108.1 . . ? Cl5' C26 H26 97.6 . . ? Cl7 C27 Cl8' 141.5(6) . . ? Cl7 C27 Cl9 119.8(7) . . ? Cl8' C27 Cl9 68.9(6) . . ? Cl7 C27 Cl7' 33.7(4) . . ? Cl8' C27 Cl7' 115.2(6) . . ? Cl9 C27 Cl7' 142.6(7) . . ? Cl7 C27 Cl9' 73.2(5) . . ? Cl8' C27 Cl9' 110.1(7) . . ? Cl9 C27 Cl9' 47.2(5) . . ? Cl7' C27 Cl9' 102.9(5) . . ? Cl7 C27 Cl8 108.9(6) . . ? Cl8' C27 Cl8 39.6(4) . . ? Cl9 C27 Cl8 105.7(6) . . ? Cl7' C27 Cl8 77.2(5) . . ? Cl9' C27 Cl8 132.6(5) . . ? Cl7 C27 H27 107.3 . . ? Cl8' C27 H27 104.5 . . ? Cl9 C27 H27 107.3 . . ? Cl7' C27 H27 107.2 . . ? Cl9' C27 H27 117.3 . . ? Cl8 C27 H27 107.3 . . ? C2 N1 C1 123.1(4) . . ? C2 N1 C3 110.5(3) . . ? C1 N1 C3 125.5(3) . . ? C2 N2 C9 118.0(3) . . ? C2 N2 C8 108.7(3) . . ? C9 N2 C8 120.9(3) . . ? C10 N3 C9 123.6(4) . . ? C10 N3 C16 109.8(4) . . ? C9 N3 C16 124.4(4) . . ? C10 N4 C17 119.2(4) . . ? C10 N4 C11 108.5(4) . . ? C17 N4 C11 122.0(3) . . ? C18 N5 C1 116.7(4) . . ? C18 N5 C24 108.9(3) . . ? C1 N5 C24 121.6(4) . . ? C18 N6 C17 123.6(4) . 2_565 ? C18 N6 C19 112.0(4) . . ? C17 N6 C19 123.1(4) 2_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 C5 -154.5(4) . . . . ? C8 C3 C4 C5 -43.4(6) . . . . ? C3 C4 C5 C6 54.8(7) . . . . ? C4 C5 C6 C7 -60.8(7) . . . . ? C5 C6 C7 C8 56.4(6) . . . . ? C6 C7 C8 N2 69.3(5) . . . . ? C6 C7 C8 C3 -46.3(6) . . . . ? N1 C3 C8 N2 32.9(4) . . . . ? C4 C3 C8 N2 -84.7(4) . . . . ? N1 C3 C8 C7 156.5(4) . . . . ? C4 C3 C8 C7 38.8(5) . . . . ? N4 C11 C12 C13 -75.4(6) . . . . ? C16 C11 C12 C13 42.2(6) . . . . ? C11 C12 C13 C14 -52.3(6) . . . . ? C12 C13 C14 C15 60.3(6) . . . . ? C13 C14 C15 C16 -57.2(6) . . . . ? N4 C11 C16 N3 -33.2(4) . . . . ? C12 C11 C16 N3 -158.9(4) . . . . ? N4 C11 C16 C15 86.2(4) . . . . ? C12 C11 C16 C15 -39.5(5) . . . . ? C14 C15 C16 N3 160.5(5) . . . . ? C14 C15 C16 C11 47.1(6) . . . . ? N6 C19 C20 C21 157.4(4) . . . . ? C24 C19 C20 C21 44.2(6) . . . . ? C19 C20 C21 C22 -56.4(7) . . . . ? C20 C21 C22 C23 59.5(7) . . . . ? C21 C22 C23 C24 -53.4(7) . . . . ? C22 C23 C24 N5 -74.7(6) . . . . ? C22 C23 C24 C19 42.5(7) . . . . ? N6 C19 C24 C23 -158.8(4) . . . . ? C20 C19 C24 C23 -38.2(6) . . . . ? N6 C19 C24 N5 -31.7(4) . . . . ? C20 C19 C24 N5 88.9(5) . . . . ? O1 C2 N1 C1 -3.1(6) . . . . ? N2 C2 N1 C1 177.0(3) . . . . ? O1 C2 N1 C3 -172.4(4) . . . . ? N2 C2 N1 C3 7.7(4) . . . . ? N5 C1 N1 C2 111.9(4) . . . . ? N5 C1 N1 C3 -80.4(5) . . . . ? C8 C3 N1 C2 -26.4(4) . . . . ? C4 C3 N1 C2 91.6(4) . . . . ? C8 C3 N1 C1 164.6(4) . . . . ? C4 C3 N1 C1 -77.3(5) . . . . ? O1 C2 N2 C9 -21.7(6) . . . . ? N1 C2 N2 C9 158.3(3) . . . . ? O1 C2 N2 C8 -164.1(4) . . . . ? N1 C2 N2 C8 15.8(4) . . . . ? N3 C9 N2 C2 -81.1(4) . . . . ? N3 C9 N2 C8 56.6(5) . . . . ? C7 C8 N2 C2 -154.7(4) . . . . ? C3 C8 N2 C2 -31.1(4) . . . . ? C7 C8 N2 C9 64.1(5) . . . . ? C3 C8 N2 C9 -172.3(3) . . . . ? O2 C10 N3 C9 9.2(6) . . . . ? N4 C10 N3 C9 -170.8(3) . . . . ? O2 C10 N3 C16 173.0(4) . . . . ? N4 C10 N3 C16 -7.1(4) . . . . ? N2 C9 N3 C10 -122.9(4) . . . . ? N2 C9 N3 C16 75.8(5) . . . . ? C11 C16 N3 C10 26.2(4) . . . . ? C15 C16 N3 C10 -95.2(4) . . . . ? C11 C16 N3 C9 -170.3(3) . . . . ? C15 C16 N3 C9 68.4(5) . . . . ? O2 C10 N4 C17 18.1(6) . . . . ? N3 C10 N4 C17 -161.8(3) . . . . ? O2 C10 N4 C11 163.7(4) . . . . ? N3 C10 N4 C11 -16.2(4) . . . . ? N6 C17 N4 C10 90.1(4) 2_565 . . . ? N6 C17 N4 C11 -50.7(5) 2_565 . . . ? C16 C11 N4 C10 31.5(4) . . . . ? C12 C11 N4 C10 157.3(4) . . . . ? C16 C11 N4 C17 176.0(4) . . . . ? C12 C11 N4 C17 -58.3(6) . . . . ? O3 C18 N5 C1 19.9(6) . . . . ? N6 C18 N5 C1 -161.8(3) . . . . ? O3 C18 N5 C24 162.3(5) . . . . ? N6 C18 N5 C24 -19.4(4) . . . . ? N1 C1 N5 C18 85.2(5) . . . . ? N1 C1 N5 C24 -52.1(6) . . . . ? C23 C24 N5 C18 158.3(4) . . . . ? C19 C24 N5 C18 32.9(4) . . . . ? C23 C24 N5 C1 -61.4(6) . . . . ? C19 C24 N5 C1 173.1(4) . . . . ? O3 C18 N6 C17 7.5(7) . . . 2_565 ? N5 C18 N6 C17 -170.8(4) . . . 2_565 ? O3 C18 N6 C19 174.6(4) . . . . ? N5 C18 N6 C19 -3.8(5) . . . . ? C20 C19 N6 C18 -98.3(5) . . . . ? C24 C19 N6 C18 23.8(5) . . . . ? C20 C19 N6 C17 68.9(6) . . . 2_565 ? C24 C19 N6 C17 -169.1(4) . . . 2_565 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.372 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.049