data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H34 Cl2 N4 O5' _chemical_formula_weight 757.64 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 11.4634(16) _cell_length_b 13.4376(19) _cell_length_c 13.962(2) _cell_angle_alpha 112.753(2) _cell_angle_beta 99.306(2) _cell_angle_gamma 101.604(2) _cell_volume 1873.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7324 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 26.82 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.226 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9521 _exptl_absorpt_correction_T_max 0.9691 _exptl_absorpt_process_details 'SADABS(Sheldrick,2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD 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 13339 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6538 _reflns_number_gt 5336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART(Bruker, 2003)' _computing_cell_refinement 'SAINTPLUS(Bruker, 2003)' _computing_data_reduction 'SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL(Bruker, 2008)' _computing_publication_material '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^)+(0.1572P)^2^+1.2283P] 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 6538 _refine_ls_number_parameters 488 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2546 _refine_ls_wR_factor_gt 0.2333 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 C1 C 0.8442(3) 0.8291(2) 0.9588(2) 0.0364(6) Uani 1 1 d . . . C2 C 0.9533(3) 0.8085(2) 1.0185(2) 0.0355(6) Uani 1 1 d . . . H2 H 0.9326 0.7274 0.9984 0.043 Uiso 1 1 calc R . . C3 C 1.0715(3) 0.8401(2) 0.9844(2) 0.0397(6) Uani 1 1 d . . . H3 H 1.1102 0.9211 1.0289 0.048 Uiso 1 1 calc R . . C4 C 1.0425(2) 0.8225(2) 0.8660(2) 0.0369(6) Uani 1 1 d . . . H4A H 1.0469 0.8948 0.8648 0.044 Uiso 1 1 calc R . . H4B H 1.1055 0.7949 0.8343 0.044 Uiso 1 1 calc R . . C5 C 0.9156(2) 0.7400(2) 0.7963(2) 0.0332(6) Uani 1 1 d . . . C6 C 0.8747(2) 0.7528(2) 0.6897(2) 0.0332(6) Uani 1 1 d . . . H6 H 0.9051 0.8326 0.7059 0.040 Uiso 1 1 calc R . . C7 C 0.7343(2) 0.7215(2) 0.6672(2) 0.0351(6) Uani 1 1 d . . . H7 H 0.7024 0.6404 0.6454 0.042 Uiso 1 1 calc R . . C8 C 0.7175(2) 0.7862(2) 0.7804(2) 0.0358(6) Uani 1 1 d . . . H8 H 0.7299 0.8658 0.7958 0.043 Uiso 1 1 calc R . . C9 C 0.9753(3) 0.8686(2) 1.1399(2) 0.0399(6) Uani 1 1 d . . . C10 C 0.9101(3) 0.8137(2) 1.1971(2) 0.0398(6) Uani 1 1 d . . . C11 C 0.8145(3) 0.7132(3) 1.1429(3) 0.0530(8) Uani 1 1 d . . . H11 H 0.7883 0.6808 1.0681 0.064 Uiso 1 1 calc R . . C12 C 0.7582(3) 0.6611(4) 1.1978(4) 0.0679(10) Uani 1 1 d . . . H12 H 0.6950 0.5938 1.1602 0.081 Uiso 1 1 calc R . . C13 C 0.7957(4) 0.7090(4) 1.3092(3) 0.0651(10) Uani 1 1 d . . . H13 H 0.7575 0.6735 1.3462 0.078 Uiso 1 1 calc R . . C14 C 0.8877(4) 0.8073(3) 1.3650(3) 0.0610(9) Uani 1 1 d . . . H14 H 0.9119 0.8388 1.4399 0.073 Uiso 1 1 calc R . . C15 C 0.9466(3) 0.8615(3) 1.3104(3) 0.0501(8) Uani 1 1 d . . . C16 C 1.1643(3) 0.7805(3) 1.0102(2) 0.0566(9) Uani 1 1 d . . . C17 C 1.1290(5) 0.6682(4) 0.9935(3) 0.0763(12) Uani 1 1 d . . . H17 H 1.0454 0.6291 0.9693 0.092 Uiso 1 1 calc R . . C18 C 1.2133(7) 0.6133(6) 1.0114(4) 0.103(2) Uani 1 1 d . . . H18 H 1.1869 0.5377 0.9972 0.124 Uiso 1 1 calc R . . C19 C 1.3299(8) 0.6679(8) 1.0482(4) 0.113(2) Uani 1 1 d . . . C20 C 1.3753(5) 0.7778(9) 1.0677(4) 0.129(3) Uani 1 1 d . . . H20 H 1.4597 0.8140 1.0933 0.155 Uiso 1 1 calc R . . C21 C 1.2871(4) 0.8371(5) 1.0469(4) 0.0900(15) Uani 1 1 d . . . H21 H 1.3145 0.9119 1.0586 0.108 Uiso 1 1 calc R . . C22 C 0.9121(3) 0.6180(2) 0.7730(2) 0.0367(6) Uani 1 1 d . . . C23 C 0.8208(3) 0.5455(2) 0.7877(2) 0.0451(7) Uani 1 1 d . . . H23 H 0.7548 0.5680 0.8108 0.054 Uiso 1 1 calc R . . C24 C 0.8300(4) 0.4379(3) 0.7671(3) 0.0589(9) Uani 1 1 d . . . H24 H 0.7707 0.3876 0.7776 0.071 Uiso 1 1 calc R . . C25 C 0.9276(4) 0.4068(3) 0.7312(3) 0.0640(10) Uani 1 1 d . . . H25 H 0.9368 0.3359 0.7182 0.077 Uiso 1 1 calc R . . C26 C 1.0107(3) 0.4829(3) 0.7151(3) 0.0586(9) Uani 1 1 d . . . H26 H 1.0749 0.4605 0.6881 0.070 Uiso 1 1 calc R . . C27 C 0.5911(3) 0.7382(3) 0.7897(2) 0.0452(7) Uani 1 1 d . . . C28 C 0.5058(3) 0.7983(4) 0.7960(4) 0.0705(11) Uani 1 1 d . . . H28 H 0.5270 0.8707 0.8004 0.085 Uiso 1 1 calc R . . C29 C 0.3880(4) 0.7479(6) 0.7957(4) 0.0976(18) Uani 1 1 d . . . H29 H 0.3277 0.7851 0.7976 0.117 Uiso 1 1 calc R . . C30 C 0.3611(4) 0.6421(6) 0.7925(4) 0.0937(17) Uani 1 1 d . . . H30 H 0.2837 0.6073 0.7953 0.112 Uiso 1 1 calc R . . C31 C 0.4497(5) 0.5911(5) 0.7854(5) 0.1050(18) Uani 1 1 d . . . H31 H 0.4302 0.5182 0.7800 0.126 Uiso 1 1 calc R . . C32 C 0.9230(3) 0.6856(3) 0.5981(2) 0.0424(7) Uani 1 1 d . . . C33 C 1.2364(4) 0.7257(6) 0.5459(4) 0.0942(17) Uani 1 1 d . . . H33 H 1.2886 0.6843 0.5175 0.113 Uiso 1 1 calc R . . C34 C 1.2720(5) 0.8398(7) 0.5836(6) 0.109(2) Uani 1 1 d . . . H34 H 1.3466 0.8766 0.5779 0.131 Uiso 1 1 calc R . . C35 C 1.1974(5) 0.8989(6) 0.6296(7) 0.123(3) Uani 1 1 d . . . H35 H 1.2246 0.9772 0.6590 0.147 Uiso 1 1 calc R . . C36 C 1.0855(4) 0.8493(3) 0.6348(4) 0.0693(11) Uani 1 1 d . . . H36 H 1.0353 0.8919 0.6656 0.083 Uiso 1 1 calc R . . C37 C 1.0496(3) 0.7379(3) 0.5945(3) 0.0513(8) Uani 1 1 d . . . C38 C 0.6671(2) 0.7500(2) 0.5833(2) 0.0369(6) Uani 1 1 d . . . C39 C 0.6869(3) 0.8596(3) 0.5961(3) 0.0520(8) Uani 1 1 d . . . H39 H 0.7446 0.9175 0.6570 0.062 Uiso 1 1 calc R . . C40 C 0.6226(4) 0.8855(3) 0.5203(3) 0.0613(9) Uani 1 1 d . . . H40 H 0.6371 0.9598 0.5302 0.074 Uiso 1 1 calc R . . C41 C 0.5372(3) 0.8001(3) 0.4305(3) 0.0560(8) Uani 1 1 d . . . C42 C 0.5159(3) 0.6905(3) 0.4149(3) 0.0572(8) Uani 1 1 d . . . H42 H 0.4584 0.6330 0.3537 0.069 Uiso 1 1 calc R . . C43 C 0.5807(3) 0.6659(3) 0.4910(2) 0.0470(7) Uani 1 1 d . . . H43 H 0.5662 0.5912 0.4803 0.056 Uiso 1 1 calc R . . Cl2 Cl 1.4405(3) 0.6028(3) 1.07360(16) 0.2292(18) Uani 1 1 d . . . Cl4 Cl 0.45540(14) 0.83344(11) 0.33663(10) 0.0967(5) Uani 1 1 d . . . N1 N 0.82016(19) 0.77576(18) 0.85029(17) 0.0334(5) Uani 1 1 d . . . N2 N 0.5650(3) 0.6367(3) 0.7854(3) 0.0769(10) Uani 1 1 d . . . N3 N 1.0060(2) 0.5871(2) 0.7355(2) 0.0473(6) Uani 1 1 d . . . N4 N 1.1212(4) 0.6710(4) 0.5497(3) 0.0935(13) Uani 1 1 d . . . O1 O 0.7806(2) 0.88440(19) 1.00449(17) 0.0513(6) Uani 1 1 d . . . O2 O 1.0518(3) 0.96213(18) 1.18932(18) 0.0611(7) Uani 1 1 d . . . O3 O 1.0365(3) 0.9572(2) 1.3711(2) 0.0807(9) Uani 1 1 d . . . H3A H 1.0629 0.9841 1.3325 0.121 Uiso 1 1 calc R . . O4 O 0.8602(2) 0.5943(2) 0.52754(19) 0.0625(7) Uani 1 1 d . . . O5 O 0.6132(19) 0.9833(16) 0.106(3) 0.63(2) Uani 1 1 d D . . H5A H 0.5993 0.9463 0.1428 0.754 Uiso 1 1 d RD . . H5B H 0.5522 0.9444 0.0512 0.754 Uiso 1 1 d RD . . 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 0.0392(14) 0.0374(13) 0.0342(14) 0.0170(11) 0.0109(11) 0.0108(11) C2 0.0426(15) 0.0321(12) 0.0300(14) 0.0127(11) 0.0074(11) 0.0102(11) C3 0.0349(14) 0.0462(15) 0.0321(14) 0.0146(12) 0.0039(11) 0.0085(11) C4 0.0335(13) 0.0423(14) 0.0348(14) 0.0185(12) 0.0072(11) 0.0088(11) C5 0.0337(13) 0.0379(13) 0.0304(13) 0.0162(11) 0.0092(11) 0.0113(11) C6 0.0338(13) 0.0378(13) 0.0305(13) 0.0166(11) 0.0085(11) 0.0116(10) C7 0.0361(14) 0.0372(13) 0.0318(14) 0.0153(11) 0.0086(11) 0.0100(11) C8 0.0327(13) 0.0423(14) 0.0333(14) 0.0174(12) 0.0075(11) 0.0114(11) C9 0.0501(16) 0.0338(13) 0.0340(15) 0.0135(11) 0.0086(12) 0.0130(12) C10 0.0458(16) 0.0418(14) 0.0354(15) 0.0184(12) 0.0113(12) 0.0165(12) C11 0.0476(17) 0.0625(19) 0.0475(18) 0.0274(16) 0.0097(14) 0.0081(15) C12 0.050(2) 0.080(2) 0.076(3) 0.044(2) 0.0170(18) 0.0032(18) C13 0.066(2) 0.084(3) 0.069(2) 0.049(2) 0.035(2) 0.026(2) C14 0.084(3) 0.071(2) 0.0451(19) 0.0320(17) 0.0320(18) 0.034(2) C15 0.069(2) 0.0475(16) 0.0385(16) 0.0189(14) 0.0178(15) 0.0231(15) C16 0.0501(19) 0.093(3) 0.0338(16) 0.0269(17) 0.0114(14) 0.0369(18) C17 0.101(3) 0.095(3) 0.064(2) 0.046(2) 0.027(2) 0.065(3) C18 0.137(5) 0.142(5) 0.064(3) 0.049(3) 0.026(3) 0.104(4) C19 0.132(6) 0.165(6) 0.051(3) 0.028(4) 0.014(3) 0.103(5) C20 0.061(3) 0.237(9) 0.059(3) 0.027(4) 0.000(2) 0.067(4) C21 0.051(2) 0.148(5) 0.057(2) 0.030(3) 0.0053(19) 0.039(3) C22 0.0388(14) 0.0403(14) 0.0301(13) 0.0151(11) 0.0051(11) 0.0130(11) C23 0.0493(17) 0.0421(15) 0.0440(17) 0.0208(13) 0.0101(13) 0.0110(13) C24 0.069(2) 0.0444(17) 0.062(2) 0.0282(16) 0.0096(18) 0.0100(16) C25 0.080(3) 0.0462(18) 0.065(2) 0.0227(17) 0.0087(19) 0.0277(18) C26 0.062(2) 0.0545(19) 0.060(2) 0.0194(16) 0.0141(17) 0.0312(16) C27 0.0345(15) 0.0659(19) 0.0366(15) 0.0228(14) 0.0117(12) 0.0146(13) C28 0.0469(19) 0.099(3) 0.080(3) 0.045(2) 0.0253(19) 0.033(2) C29 0.045(2) 0.174(6) 0.090(3) 0.062(4) 0.029(2) 0.048(3) C30 0.043(2) 0.137(5) 0.082(3) 0.038(3) 0.025(2) -0.003(3) C31 0.073(3) 0.099(4) 0.144(5) 0.053(3) 0.059(3) 0.003(3) C32 0.0472(16) 0.0542(17) 0.0313(15) 0.0195(14) 0.0116(13) 0.0235(14) C33 0.063(3) 0.158(5) 0.074(3) 0.045(3) 0.041(2) 0.051(3) C34 0.074(3) 0.152(6) 0.152(6) 0.099(5) 0.070(4) 0.041(3) C35 0.087(4) 0.115(4) 0.224(8) 0.109(5) 0.091(5) 0.037(3) C36 0.059(2) 0.067(2) 0.122(4) 0.061(2) 0.059(2) 0.0311(18) C37 0.0495(17) 0.080(2) 0.0409(17) 0.0341(16) 0.0208(14) 0.0305(16) C38 0.0338(13) 0.0451(14) 0.0338(14) 0.0181(12) 0.0094(11) 0.0136(11) C39 0.0554(19) 0.0466(16) 0.0439(17) 0.0199(14) -0.0028(14) 0.0063(14) C40 0.078(2) 0.0562(19) 0.055(2) 0.0322(17) 0.0084(18) 0.0227(18) C41 0.058(2) 0.075(2) 0.0426(18) 0.0302(17) 0.0091(15) 0.0307(17) C42 0.0550(19) 0.063(2) 0.0403(17) 0.0158(15) -0.0031(15) 0.0164(16) C43 0.0457(16) 0.0476(16) 0.0412(17) 0.0165(13) 0.0039(13) 0.0116(13) Cl2 0.244(3) 0.354(4) 0.1085(13) 0.0487(18) 0.0100(15) 0.260(3) Cl4 0.1215(10) 0.1060(9) 0.0670(7) 0.0465(7) -0.0087(7) 0.0509(8) N1 0.0321(11) 0.0390(11) 0.0288(11) 0.0139(9) 0.0082(9) 0.0114(9) N2 0.0562(18) 0.071(2) 0.117(3) 0.049(2) 0.045(2) 0.0134(15) N3 0.0485(14) 0.0491(14) 0.0474(15) 0.0185(12) 0.0147(12) 0.0240(12) N4 0.072(2) 0.137(4) 0.068(2) 0.028(2) 0.0299(19) 0.048(2) O1 0.0586(13) 0.0599(13) 0.0391(11) 0.0161(10) 0.0184(10) 0.0312(11) O2 0.0866(18) 0.0400(12) 0.0364(12) 0.0096(10) 0.0110(12) -0.0053(11) O3 0.120(3) 0.0616(15) 0.0347(13) 0.0135(12) 0.0090(14) -0.0035(16) O4 0.0578(14) 0.0672(15) 0.0437(13) 0.0042(12) 0.0097(11) 0.0229(12) O5 0.48(3) 0.351(19) 1.21(7) 0.30(3) 0.59(4) 0.229(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.221(3) . ? C1 N1 1.353(4) . ? C1 C2 1.523(4) . ? C2 C9 1.521(4) . ? C2 C3 1.540(4) . ? C2 H2 0.9800 . ? C3 C16 1.532(4) . ? C3 C4 1.545(4) . ? C3 H3 0.9800 . ? C4 C5 1.533(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.481(3) . ? C5 C22 1.533(4) . ? C5 C6 1.571(3) . ? C6 C32 1.515(4) . ? C6 C7 1.526(4) . ? C6 H6 0.9800 . ? C7 C38 1.512(4) . ? C7 C8 1.547(4) . ? C7 H7 0.9800 . ? C8 N1 1.469(3) . ? C8 C27 1.510(4) . ? C8 H8 0.9800 . ? C9 O2 1.231(3) . ? C9 C10 1.472(4) . ? C10 C11 1.394(4) . ? C10 C15 1.408(4) . ? C11 C12 1.374(5) . ? C11 H11 0.9300 . ? C12 C13 1.384(6) . ? C12 H12 0.9300 . ? C13 C14 1.357(6) . ? C13 H13 0.9300 . ? C14 C15 1.402(5) . ? C14 H14 0.9300 . ? C15 O3 1.333(4) . ? C16 C21 1.362(6) . ? C16 C17 1.395(6) . ? C17 C18 1.376(6) . ? C17 H17 0.9300 . ? C18 C19 1.296(11) . ? C18 H18 0.9300 . ? C19 C20 1.363(10) . ? C19 Cl2 1.744(6) . ? C20 C21 1.466(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 N3 1.341(4) . ? C22 C23 1.379(4) . ? C23 C24 1.390(4) . ? C23 H23 0.9300 . ? C24 C25 1.373(6) . ? C24 H24 0.9300 . ? C25 C26 1.363(6) . ? C25 H25 0.9300 . ? C26 N3 1.331(4) . ? C26 H26 0.9300 . ? C27 N2 1.311(5) . ? C27 C28 1.381(5) . ? C28 C29 1.382(6) . ? C28 H28 0.9300 . ? C29 C30 1.374(8) . ? C29 H29 0.9300 . ? C30 C31 1.331(8) . ? C30 H30 0.9300 . ? C31 N2 1.340(5) . ? C31 H31 0.9300 . ? C32 O4 1.214(4) . ? C32 C37 1.498(5) . ? C33 C34 1.359(8) . ? C33 N4 1.396(7) . ? C33 H33 0.9300 . ? C34 C35 1.353(8) . ? C34 H34 0.9300 . ? C35 C36 1.348(6) . ? C35 H35 0.9300 . ? C36 C37 1.325(5) . ? C36 H36 0.9300 . ? C37 N4 1.379(5) . ? C38 C39 1.379(4) . ? C38 C43 1.388(4) . ? C39 C40 1.385(5) . ? C39 H39 0.9300 . ? C40 C41 1.373(5) . ? C40 H40 0.9300 . ? C41 C42 1.366(5) . ? C41 Cl4 1.739(3) . ? C42 C43 1.380(5) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? O3 H3A 0.8200 . ? O5 H5A 0.8494 . ? O5 H5B 0.8507 . ? 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 O1 C1 N1 123.1(3) . . ? O1 C1 C2 123.1(2) . . ? N1 C1 C2 113.8(2) . . ? C9 C2 C1 111.8(2) . . ? C9 C2 C3 111.2(2) . . ? C1 C2 C3 111.9(2) . . ? C9 C2 H2 107.2 . . ? C1 C2 H2 107.2 . . ? C3 C2 H2 107.2 . . ? C16 C3 C2 111.2(2) . . ? C16 C3 C4 113.3(2) . . ? C2 C3 C4 112.0(2) . . ? C16 C3 H3 106.6 . . ? C2 C3 H3 106.6 . . ? C4 C3 H3 106.6 . . ? C5 C4 C3 114.3(2) . . ? C5 C4 H4A 108.7 . . ? C3 C4 H4A 108.7 . . ? C5 C4 H4B 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? N1 C5 C4 108.8(2) . . ? N1 C5 C22 112.3(2) . . ? C4 C5 C22 111.6(2) . . ? N1 C5 C6 100.45(19) . . ? C4 C5 C6 111.7(2) . . ? C22 C5 C6 111.6(2) . . ? C32 C6 C7 115.0(2) . . ? C32 C6 C5 114.5(2) . . ? C7 C6 C5 102.9(2) . . ? C32 C6 H6 108.0 . . ? C7 C6 H6 108.0 . . ? C5 C6 H6 108.0 . . ? C38 C7 C6 116.2(2) . . ? C38 C7 C8 112.6(2) . . ? C6 C7 C8 101.7(2) . . ? C38 C7 H7 108.7 . . ? C6 C7 H7 108.7 . . ? C8 C7 H7 108.7 . . ? N1 C8 C27 114.5(2) . . ? N1 C8 C7 101.9(2) . . ? C27 C8 C7 112.0(2) . . ? N1 C8 H8 109.4 . . ? C27 C8 H8 109.4 . . ? C7 C8 H8 109.4 . . ? O2 C9 C10 121.0(3) . . ? O2 C9 C2 118.4(2) . . ? C10 C9 C2 120.5(2) . . ? C11 C10 C15 118.0(3) . . ? C11 C10 C9 122.3(3) . . ? C15 C10 C9 119.7(3) . . ? C12 C11 C10 121.3(3) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 119.9(4) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 120.6(3) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 120.4(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? O3 C15 C14 116.6(3) . . ? O3 C15 C10 123.6(3) . . ? C14 C15 C10 119.8(3) . . ? C21 C16 C17 118.0(4) . . ? C21 C16 C3 119.3(4) . . ? C17 C16 C3 122.6(3) . . ? C18 C17 C16 122.4(5) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C19 C18 C17 119.4(7) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 123.4(6) . . ? C18 C19 Cl2 121.3(7) . . ? C20 C19 Cl2 115.3(7) . . ? C19 C20 C21 118.0(6) . . ? C19 C20 H20 121.0 . . ? C21 C20 H20 121.0 . . ? C16 C21 C20 118.7(6) . . ? C16 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? N3 C22 C23 122.5(3) . . ? N3 C22 C5 113.8(2) . . ? C23 C22 C5 123.7(3) . . ? C22 C23 C24 118.4(3) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C25 C24 C23 119.3(3) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C26 C25 C24 118.1(3) . . ? C26 C25 H25 120.9 . . ? C24 C25 H25 120.9 . . ? N3 C26 C25 124.3(3) . . ? N3 C26 H26 117.9 . . ? C25 C26 H26 117.9 . . ? N2 C27 C28 122.5(3) . . ? N2 C27 C8 117.5(3) . . ? C28 C27 C8 119.9(3) . . ? C27 C28 C29 118.2(5) . . ? C27 C28 H28 120.9 . . ? C29 C28 H28 120.9 . . ? C30 C29 C28 119.3(5) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C31 C30 C29 117.6(4) . . ? C31 C30 H30 121.2 . . ? C29 C30 H30 121.2 . . ? C30 C31 N2 125.1(5) . . ? C30 C31 H31 117.4 . . ? N2 C31 H31 117.4 . . ? O4 C32 C37 120.6(3) . . ? O4 C32 C6 121.6(3) . . ? C37 C32 C6 117.7(3) . . ? C34 C33 N4 119.8(4) . . ? C34 C33 H33 120.1 . . ? N4 C33 H33 120.1 . . ? C35 C34 C33 119.1(5) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C36 C35 C34 122.9(6) . . ? C36 C35 H35 118.5 . . ? C34 C35 H35 118.5 . . ? C37 C36 C35 117.6(4) . . ? C37 C36 H36 121.2 . . ? C35 C36 H36 121.2 . . ? C36 C37 N4 123.5(3) . . ? C36 C37 C32 116.1(3) . . ? N4 C37 C32 120.4(3) . . ? C39 C38 C43 117.6(3) . . ? C39 C38 C7 121.7(3) . . ? C43 C38 C7 120.7(2) . . ? C38 C39 C40 121.4(3) . . ? C38 C39 H39 119.3 . . ? C40 C39 H39 119.3 . . ? C41 C40 C39 119.3(3) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C42 C41 C40 120.8(3) . . ? C42 C41 Cl4 120.3(3) . . ? C40 C41 Cl4 119.0(3) . . ? C41 C42 C43 119.4(3) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C42 C43 C38 121.5(3) . . ? C42 C43 H43 119.2 . . ? C38 C43 H43 119.2 . . ? C1 N1 C8 120.8(2) . . ? C1 N1 C5 121.9(2) . . ? C8 N1 C5 113.7(2) . . ? C27 N2 C31 117.2(4) . . ? C26 N3 C22 117.4(3) . . ? C37 N4 C33 117.0(5) . . ? C15 O3 H3A 109.5 . . ? H5A O5 H5B 99.2 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.894 _refine_diff_density_min -0.902 _refine_diff_density_rms 0.115