# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jean-Pierre Sauvage' _publ_contact_author_email jpsauvage@unistra.fr loop_ _publ_author_name C.Roche J.-P.Sauvage A.Sour N.Strutt data_jpscr100503 _database_code_depnum_ccdc_archive 'CCDC 823860' #TrackingRef '- jpscr100503.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H34 N2 O7, C H2 Cl2' _chemical_formula_sum 'C40 H36 Cl2 N2 O7' _chemical_formula_weight 727.61 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3107(3) _cell_length_b 12.3575(4) _cell_length_c 13.5089(4) _cell_angle_alpha 82.6430(10) _cell_angle_beta 73.2010(10) _cell_angle_gamma 74.7660(10) _cell_volume 1741.29(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9914 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 29.99 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8887 _exptl_absorpt_correction_T_max 0.9578 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27849 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 30.01 _reflns_number_total 10107 _reflns_number_gt 8025 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0537P)^2^+1.2123P] 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 10107 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.05786(14) 1.24602(12) 0.89252(11) 0.0266(3) Uani 1 1 d . . . C2 C -0.01486(15) 1.33011(14) 0.96332(12) 0.0330(3) Uani 1 1 d . . . H2 H -0.0477 1.4042 0.9387 0.040 Uiso 1 1 calc R . . C3 C -0.03692(15) 1.30290(14) 1.06735(12) 0.0338(3) Uani 1 1 d . . . H3 H -0.0857 1.3583 1.1154 0.041 Uiso 1 1 calc R . . C4 C 0.01225(14) 1.19347(14) 1.10334(11) 0.0287(3) Uani 1 1 d . . . C5 C -0.01146(16) 1.15836(15) 1.21110(12) 0.0349(3) Uani 1 1 d . . . H5 H -0.0620 1.2109 1.2613 0.042 Uiso 1 1 calc R . . C6 C 0.03685(17) 1.05179(16) 1.24252(12) 0.0367(4) Uani 1 1 d . . . H6 H 0.0193 1.0302 1.3144 0.044 Uiso 1 1 calc R . . C7 C 0.11411(15) 0.97110(14) 1.16862(11) 0.0308(3) Uani 1 1 d . . . C8 C 0.16504(17) 0.85892(15) 1.19790(12) 0.0367(3) Uani 1 1 d . . . H8 H 0.1500 0.8346 1.2691 0.044 Uiso 1 1 calc R . . C9 C 0.23620(17) 0.78515(15) 1.12361(12) 0.0360(3) Uani 1 1 d . . . H9 H 0.2702 0.7091 1.1426 0.043 Uiso 1 1 calc R . . C10 C 0.25865(14) 0.82345(13) 1.01811(11) 0.0284(3) Uani 1 1 d . . . C11 C 0.13929(14) 1.00175(13) 1.06155(11) 0.0265(3) Uani 1 1 d . . . C12 C 0.08592(13) 1.11585(13) 1.02777(11) 0.0261(3) Uani 1 1 d . . . C13 C 0.07854(13) 1.26720(12) 0.77898(11) 0.0256(3) Uani 1 1 d . . . C14 C 0.13945(16) 1.17782(13) 0.71423(12) 0.0332(3) Uani 1 1 d . . . H14 H 0.1727 1.1062 0.7436 0.040 Uiso 1 1 calc R . . C15 C 0.15253(16) 1.19094(13) 0.60830(12) 0.0327(3) Uani 1 1 d . . . H15 H 0.1941 1.1289 0.5660 0.039 Uiso 1 1 calc R . . C16 C 0.10448(14) 1.29526(12) 0.56439(11) 0.0256(3) Uani 1 1 d . . . C17 C 0.04775(13) 1.38651(12) 0.62698(11) 0.0262(3) Uani 1 1 d . . . H17 H 0.0180 1.4587 0.5969 0.031 Uiso 1 1 calc R . . C18 C 0.03460(13) 1.37229(12) 0.73285(11) 0.0260(3) Uani 1 1 d . . . H18 H -0.0049 1.4349 0.7747 0.031 Uiso 1 1 calc R . . C19 C 0.14689(15) 1.22536(13) 0.39543(12) 0.0310(3) Uani 1 1 d . . . H19A H 0.1044 1.2450 0.3388 0.037 Uiso 1 1 calc R . . H19B H 0.1212 1.1586 0.4356 0.037 Uiso 1 1 calc R . . C20 C 0.28892(15) 1.19791(12) 0.35010(11) 0.0296(3) Uani 1 1 d . . . H20A H 0.3156 1.2640 0.3093 0.035 Uiso 1 1 calc R . . H20B H 0.3324 1.1770 0.4061 0.035 Uiso 1 1 calc R . . C21 C 0.45104(15) 1.09031(12) 0.22650(12) 0.0308(3) Uani 1 1 d . . . H21A H 0.5059 1.0761 0.2744 0.037 Uiso 1 1 calc R . . H21B H 0.4633 1.1597 0.1835 0.037 Uiso 1 1 calc R . . C22 C 0.49073(17) 0.99366(13) 0.15762(12) 0.0343(3) Uani 1 1 d . . . H22A H 0.4255 0.9980 0.1208 0.041 Uiso 1 1 calc R . . H22B H 0.5721 0.9964 0.1054 0.041 Uiso 1 1 calc R . . C23 C 0.57666(14) 0.79545(12) 0.17343(12) 0.0287(3) Uani 1 1 d . . . C24 C 0.60528(14) 0.70366(12) 0.24157(12) 0.0281(3) Uani 1 1 d . . . H24 H 0.5739 0.7110 0.3142 0.034 Uiso 1 1 calc R . . C25 C 0.67969(14) 0.60166(12) 0.20287(12) 0.0269(3) Uani 1 1 d . . . C26 C 0.72358(14) 0.59015(13) 0.09623(12) 0.0302(3) Uani 1 1 d . . . H26 H 0.7722 0.5198 0.0695 0.036 Uiso 1 1 calc R . . C27 C 0.69554(14) 0.68242(13) 0.02975(12) 0.0293(3) Uani 1 1 d . . . C28 C 0.62162(15) 0.78605(13) 0.06731(12) 0.0303(3) Uani 1 1 d . . . H28 H 0.6026 0.8487 0.0210 0.036 Uiso 1 1 calc R . . C29 C 0.74790(16) 0.67494(15) -0.08378(13) 0.0357(3) Uani 1 1 d . . . H29 H 0.7328 0.7423 -0.1257 0.043 Uiso 1 1 calc R . . C30 C 0.67045(14) 0.51823(12) 0.37377(12) 0.0290(3) Uani 1 1 d . . . H30A H 0.5765 0.5331 0.3954 0.035 Uiso 1 1 calc R . . H30B H 0.6963 0.5800 0.3956 0.035 Uiso 1 1 calc R . . C31 C 0.72848(16) 0.40643(13) 0.42140(12) 0.0327(3) Uani 1 1 d . . . H31A H 0.7111 0.3447 0.3921 0.039 Uiso 1 1 calc R . . H31B H 0.8218 0.3960 0.4049 0.039 Uiso 1 1 calc R . . C32 C 0.74710(15) 0.44218(14) 0.58390(13) 0.0340(3) Uani 1 1 d . . . H32A H 0.7743 0.5092 0.5455 0.041 Uiso 1 1 calc R . . H32B H 0.8242 0.3830 0.5880 0.041 Uiso 1 1 calc R . . C33 C 0.66706(16) 0.47156(13) 0.69071(13) 0.0325(3) Uani 1 1 d . . . H33A H 0.6318 0.4075 0.7270 0.039 Uiso 1 1 calc R . . H33B H 0.7188 0.4899 0.7313 0.039 Uiso 1 1 calc R . . C34 C 0.49212(15) 0.61983(12) 0.76748(12) 0.0282(3) Uani 1 1 d . . . C35 C 0.39709(15) 0.71280(13) 0.75200(12) 0.0297(3) Uani 1 1 d . . . H35 H 0.3853 0.7326 0.6846 0.036 Uiso 1 1 calc R . . C36 C 0.32014(14) 0.77622(13) 0.83347(12) 0.0290(3) Uani 1 1 d . . . H36 H 0.2554 0.8392 0.8218 0.035 Uiso 1 1 calc R . . C37 C 0.33619(14) 0.74889(12) 0.93384(11) 0.0271(3) Uani 1 1 d . . . C38 C 0.43050(15) 0.65520(13) 0.94820(12) 0.0302(3) Uani 1 1 d . . . H38 H 0.4420 0.6349 1.0156 0.036 Uiso 1 1 calc R . . C39 C 0.50861(16) 0.59024(12) 0.86638(12) 0.0310(3) Uani 1 1 d . . . H39 H 0.5725 0.5264 0.8779 0.037 Uiso 1 1 calc R . . C40 C 0.30543(18) 0.86701(15) 0.42590(14) 0.0422(4) Uani 1 1 d . . . H40A H 0.3421 0.7877 0.4080 0.051 Uiso 1 1 calc R . . H40B H 0.3131 0.9143 0.3605 0.051 Uiso 1 1 calc R . . N1 N 0.10745(12) 1.14248(11) 0.92482(9) 0.0265(2) Uani 1 1 d . . . N2 N 0.21149(12) 0.92910(11) 0.98825(9) 0.0272(2) Uani 1 1 d . . . O1 O 0.10696(11) 1.31764(9) 0.46180(8) 0.0317(2) Uani 1 1 d . . . O2 O 0.32169(10) 1.10653(8) 0.28514(8) 0.0286(2) Uani 1 1 d . . . O3 O 0.50526(12) 0.89164(9) 0.22068(9) 0.0369(3) Uani 1 1 d . . . O4 O 0.80824(13) 0.59025(12) -0.12742(10) 0.0469(3) Uani 1 1 d . . . O5 O 0.71709(11) 0.50969(9) 0.26388(9) 0.0321(2) Uani 1 1 d . . . O6 O 0.67597(11) 0.40320(9) 0.53079(9) 0.0311(2) Uani 1 1 d . . . O7 O 0.56679(11) 0.56635(9) 0.68025(9) 0.0332(2) Uani 1 1 d . . . Cl1 Cl 0.39234(8) 0.90378(6) 0.49939(6) 0.0756(2) Uani 1 1 d . . . Cl2 Cl 0.14368(5) 0.88396(5) 0.49215(4) 0.05764(15) 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 0.0239(6) 0.0315(7) 0.0233(6) -0.0068(5) -0.0036(5) -0.0053(5) C2 0.0320(8) 0.0341(7) 0.0279(7) -0.0078(6) -0.0053(6) 0.0003(6) C3 0.0314(8) 0.0389(8) 0.0272(7) -0.0120(6) -0.0046(6) -0.0003(6) C4 0.0252(7) 0.0396(8) 0.0217(6) -0.0074(6) -0.0058(5) -0.0063(6) C5 0.0319(8) 0.0495(9) 0.0217(7) -0.0108(6) -0.0053(6) -0.0051(7) C6 0.0379(8) 0.0525(10) 0.0181(6) -0.0062(6) -0.0059(6) -0.0078(7) C7 0.0307(7) 0.0423(8) 0.0203(6) -0.0026(6) -0.0069(5) -0.0101(6) C8 0.0403(9) 0.0471(9) 0.0214(7) 0.0022(6) -0.0085(6) -0.0095(7) C9 0.0402(9) 0.0379(8) 0.0263(7) 0.0044(6) -0.0075(6) -0.0077(7) C10 0.0274(7) 0.0333(7) 0.0244(7) -0.0002(5) -0.0072(5) -0.0075(6) C11 0.0243(6) 0.0343(7) 0.0214(6) -0.0033(5) -0.0054(5) -0.0080(5) C12 0.0242(6) 0.0337(7) 0.0208(6) -0.0049(5) -0.0049(5) -0.0072(5) C13 0.0232(6) 0.0293(7) 0.0225(6) -0.0056(5) -0.0028(5) -0.0047(5) C14 0.0391(8) 0.0275(7) 0.0244(7) -0.0025(5) -0.0025(6) 0.0002(6) C15 0.0410(8) 0.0248(6) 0.0245(7) -0.0068(5) -0.0011(6) -0.0004(6) C16 0.0256(6) 0.0269(6) 0.0221(6) -0.0043(5) -0.0020(5) -0.0058(5) C17 0.0248(6) 0.0243(6) 0.0266(7) -0.0041(5) -0.0046(5) -0.0021(5) C18 0.0242(6) 0.0258(6) 0.0262(7) -0.0078(5) -0.0034(5) -0.0035(5) C19 0.0335(8) 0.0334(7) 0.0248(7) -0.0103(6) -0.0056(6) -0.0043(6) C20 0.0340(8) 0.0281(7) 0.0248(7) -0.0069(5) -0.0013(5) -0.0090(6) C21 0.0317(7) 0.0249(6) 0.0299(7) -0.0019(5) 0.0002(6) -0.0059(5) C22 0.0415(9) 0.0250(7) 0.0256(7) -0.0001(5) 0.0024(6) -0.0027(6) C23 0.0263(7) 0.0244(6) 0.0293(7) -0.0042(5) 0.0002(5) -0.0029(5) C24 0.0271(7) 0.0267(6) 0.0264(7) -0.0043(5) -0.0013(5) -0.0046(5) C25 0.0251(6) 0.0249(6) 0.0304(7) -0.0041(5) -0.0067(5) -0.0048(5) C26 0.0279(7) 0.0282(7) 0.0323(7) -0.0103(6) -0.0073(6) 0.0005(5) C27 0.0263(7) 0.0329(7) 0.0272(7) -0.0084(6) -0.0060(5) -0.0026(6) C28 0.0286(7) 0.0287(7) 0.0290(7) -0.0041(5) -0.0037(6) -0.0021(5) C29 0.0333(8) 0.0420(8) 0.0278(7) -0.0090(6) -0.0083(6) 0.0015(6) C30 0.0278(7) 0.0280(7) 0.0302(7) -0.0038(5) -0.0081(6) -0.0036(5) C31 0.0386(8) 0.0267(7) 0.0323(8) -0.0060(6) -0.0122(6) -0.0020(6) C32 0.0291(7) 0.0384(8) 0.0372(8) -0.0090(6) -0.0108(6) -0.0069(6) C33 0.0338(8) 0.0305(7) 0.0338(8) -0.0042(6) -0.0132(6) -0.0026(6) C34 0.0317(7) 0.0257(6) 0.0292(7) -0.0041(5) -0.0094(6) -0.0079(5) C35 0.0330(7) 0.0316(7) 0.0272(7) -0.0035(5) -0.0131(6) -0.0057(6) C36 0.0273(7) 0.0307(7) 0.0297(7) -0.0019(5) -0.0109(6) -0.0044(5) C37 0.0278(7) 0.0285(6) 0.0251(6) -0.0001(5) -0.0057(5) -0.0091(5) C38 0.0357(8) 0.0298(7) 0.0248(7) 0.0042(5) -0.0093(6) -0.0088(6) C39 0.0361(8) 0.0256(6) 0.0303(7) 0.0028(5) -0.0108(6) -0.0056(6) C40 0.0452(10) 0.0336(8) 0.0372(9) -0.0037(7) 0.0059(7) -0.0092(7) N1 0.0263(6) 0.0307(6) 0.0211(5) -0.0044(4) -0.0043(4) -0.0056(5) N2 0.0266(6) 0.0321(6) 0.0223(5) -0.0017(5) -0.0053(4) -0.0075(5) O1 0.0410(6) 0.0287(5) 0.0205(5) -0.0056(4) -0.0049(4) -0.0013(4) O2 0.0314(5) 0.0243(5) 0.0264(5) -0.0063(4) 0.0005(4) -0.0074(4) O3 0.0460(7) 0.0227(5) 0.0267(5) -0.0019(4) 0.0048(5) 0.0022(4) O4 0.0485(8) 0.0492(7) 0.0358(6) -0.0188(6) -0.0088(6) 0.0059(6) O5 0.0360(6) 0.0259(5) 0.0301(5) -0.0041(4) -0.0075(4) -0.0002(4) O6 0.0344(6) 0.0293(5) 0.0325(5) -0.0036(4) -0.0114(4) -0.0087(4) O7 0.0390(6) 0.0290(5) 0.0300(5) -0.0055(4) -0.0122(5) 0.0000(4) Cl1 0.0867(5) 0.0779(4) 0.0736(4) 0.0098(3) -0.0414(4) -0.0237(4) Cl2 0.0436(3) 0.0659(3) 0.0404(2) 0.0025(2) 0.00842(19) 0.0020(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 1.3280(19) . ? C1 C2 1.422(2) . ? C1 C13 1.4825(19) . ? C2 C3 1.368(2) . ? C2 H2 0.9500 . ? C3 C4 1.403(2) . ? C3 H3 0.9500 . ? C4 C12 1.413(2) . ? C4 C5 1.433(2) . ? C5 C6 1.351(3) . ? C5 H5 0.9500 . ? C6 C7 1.431(2) . ? C6 H6 0.9500 . ? C7 C8 1.408(2) . ? C7 C11 1.412(2) . ? C8 C9 1.367(2) . ? C8 H8 0.9500 . ? C9 C10 1.415(2) . ? C9 H9 0.9500 . ? C10 N2 1.3324(19) . ? C10 C37 1.477(2) . ? C11 N2 1.3522(19) . ? C11 C12 1.452(2) . ? C12 N1 1.3530(18) . ? C13 C18 1.398(2) . ? C13 C14 1.400(2) . ? C14 C15 1.388(2) . ? C14 H14 0.9500 . ? C15 C16 1.390(2) . ? C15 H15 0.9500 . ? C16 O1 1.3716(17) . ? C16 C17 1.3960(19) . ? C17 C18 1.387(2) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O1 1.4372(17) . ? C19 C20 1.506(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O2 1.4241(17) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O2 1.4229(18) . ? C21 C22 1.502(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O3 1.4280(18) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O3 1.3654(17) . ? C23 C28 1.385(2) . ? C23 C24 1.397(2) . ? C24 C25 1.3882(19) . ? C24 H24 0.9500 . ? C25 O5 1.3635(18) . ? C25 C26 1.394(2) . ? C26 C27 1.385(2) . ? C26 H26 0.9500 . ? C27 C28 1.398(2) . ? C27 C29 1.481(2) . ? C28 H28 0.9500 . ? C29 O4 1.208(2) . ? C29 H29 0.9500 . ? C30 O5 1.4322(18) . ? C30 C31 1.514(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 O6 1.4241(19) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O6 1.4212(18) . ? C32 C33 1.497(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O7 1.4249(18) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O7 1.3673(18) . ? C34 C39 1.392(2) . ? C34 C35 1.392(2) . ? C35 C36 1.375(2) . ? C35 H35 0.9500 . ? C36 C37 1.406(2) . ? C36 H36 0.9500 . ? C37 C38 1.389(2) . ? C38 C39 1.392(2) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 Cl1 1.753(2) . ? C40 Cl2 1.7585(19) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? 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 C2 121.66(13) . . ? N1 C1 C13 116.11(12) . . ? C2 C1 C13 122.19(13) . . ? C3 C2 C1 119.15(15) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 120.21(14) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C12 116.95(13) . . ? C3 C4 C5 123.00(14) . . ? C12 C4 C5 120.04(14) . . ? C6 C5 C4 121.14(14) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 120.64(14) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C11 117.30(14) . . ? C8 C7 C6 122.49(14) . . ? C11 C7 C6 120.18(15) . . ? C9 C8 C7 119.80(14) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.19(15) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 122.24(14) . . ? N2 C10 C37 115.63(13) . . ? C9 C10 C37 122.13(14) . . ? N2 C11 C7 122.78(14) . . ? N2 C11 C12 118.05(12) . . ? C7 C11 C12 119.17(13) . . ? N1 C12 C4 122.92(14) . . ? N1 C12 C11 118.25(12) . . ? C4 C12 C11 118.82(13) . . ? C18 C13 C14 117.65(13) . . ? C18 C13 C1 122.95(12) . . ? C14 C13 C1 119.32(13) . . ? C15 C14 C13 121.77(14) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 119.68(13) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? O1 C16 C15 125.12(13) . . ? O1 C16 C17 115.44(12) . . ? C15 C16 C17 119.44(13) . . ? C18 C17 C16 120.33(13) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C13 121.04(12) . . ? C17 C18 H18 119.5 . . ? C13 C18 H18 119.5 . . ? O1 C19 C20 110.89(13) . . ? O1 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? O1 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.0 . . ? O2 C20 C19 107.91(12) . . ? O2 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? O2 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? O2 C21 C22 111.97(13) . . ? O2 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? O2 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? O3 C22 C21 108.29(12) . . ? O3 C22 H22A 110.0 . . ? C21 C22 H22A 110.0 . . ? O3 C22 H22B 110.0 . . ? C21 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? O3 C23 C28 124.82(14) . . ? O3 C23 C24 114.41(13) . . ? C28 C23 C24 120.75(13) . . ? C25 C24 C23 119.86(14) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? O5 C25 C24 123.54(13) . . ? O5 C25 C26 116.32(13) . . ? C24 C25 C26 120.11(14) . . ? C27 C26 C25 119.25(13) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 121.42(14) . . ? C26 C27 C29 120.54(14) . . ? C28 C27 C29 118.00(14) . . ? C23 C28 C27 118.59(14) . . ? C23 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? O4 C29 C27 125.34(17) . . ? O4 C29 H29 117.3 . . ? C27 C29 H29 117.3 . . ? O5 C30 C31 106.12(12) . . ? O5 C30 H30A 110.5 . . ? C31 C30 H30A 110.5 . . ? O5 C30 H30B 110.5 . . ? C31 C30 H30B 110.5 . . ? H30A C30 H30B 108.7 . . ? O6 C31 C30 109.79(12) . . ? O6 C31 H31A 109.7 . . ? C30 C31 H31A 109.7 . . ? O6 C31 H31B 109.7 . . ? C30 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? O6 C32 C33 109.62(13) . . ? O6 C32 H32A 109.7 . . ? C33 C32 H32A 109.7 . . ? O6 C32 H32B 109.7 . . ? C33 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? O7 C33 C32 107.33(13) . . ? O7 C33 H33A 110.2 . . ? C32 C33 H33A 110.2 . . ? O7 C33 H33B 110.2 . . ? C32 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? O7 C34 C39 124.73(14) . . ? O7 C34 C35 115.51(13) . . ? C39 C34 C35 119.71(14) . . ? C36 C35 C34 120.55(14) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 120.76(14) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C38 C37 C36 117.98(14) . . ? C38 C37 C10 122.45(13) . . ? C36 C37 C10 119.47(13) . . ? C37 C38 C39 121.73(14) . . ? C37 C38 H38 119.1 . . ? C39 C38 H38 119.1 . . ? C38 C39 C34 119.26(14) . . ? C38 C39 H39 120.4 . . ? C34 C39 H39 120.4 . . ? Cl1 C40 Cl2 112.32(10) . . ? Cl1 C40 H40A 109.1 . . ? Cl2 C40 H40A 109.1 . . ? Cl1 C40 H40B 109.1 . . ? Cl2 C40 H40B 109.1 . . ? H40A C40 H40B 107.9 . . ? C1 N1 C12 119.07(12) . . ? C10 N2 C11 118.66(13) . . ? C16 O1 C19 118.70(12) . . ? C21 O2 C20 109.95(11) . . ? C23 O3 C22 117.84(12) . . ? C25 O5 C30 117.46(11) . . ? C32 O6 C31 112.90(12) . . ? C34 O7 C33 118.23(12) . . ? 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 C1 C2 C3 -1.6(2) . . . . ? C13 C1 C2 C3 175.91(15) . . . . ? C1 C2 C3 C4 0.3(2) . . . . ? C2 C3 C4 C12 1.2(2) . . . . ? C2 C3 C4 C5 -177.50(16) . . . . ? C3 C4 C5 C6 179.42(16) . . . . ? C12 C4 C5 C6 0.8(2) . . . . ? C4 C5 C6 C7 0.5(3) . . . . ? C5 C6 C7 C8 -179.21(17) . . . . ? C5 C6 C7 C11 -0.9(3) . . . . ? C11 C7 C8 C9 0.4(2) . . . . ? C6 C7 C8 C9 178.76(17) . . . . ? C7 C8 C9 C10 0.7(3) . . . . ? C8 C9 C10 N2 -0.8(3) . . . . ? C8 C9 C10 C37 179.09(15) . . . . ? C8 C7 C11 N2 -1.5(2) . . . . ? C6 C7 C11 N2 -179.95(14) . . . . ? C8 C7 C11 C12 178.44(14) . . . . ? C6 C7 C11 C12 0.0(2) . . . . ? C3 C4 C12 N1 -1.5(2) . . . . ? C5 C4 C12 N1 177.25(14) . . . . ? C3 C4 C12 C11 179.67(14) . . . . ? C5 C4 C12 C11 -1.6(2) . . . . ? N2 C11 C12 N1 2.3(2) . . . . ? C7 C11 C12 N1 -177.72(13) . . . . ? N2 C11 C12 C4 -178.81(13) . . . . ? C7 C11 C12 C4 1.2(2) . . . . ? N1 C1 C13 C18 -178.65(14) . . . . ? C2 C1 C13 C18 3.7(2) . . . . ? N1 C1 C13 C14 4.4(2) . . . . ? C2 C1 C13 C14 -173.26(15) . . . . ? C18 C13 C14 C15 -2.2(2) . . . . ? C1 C13 C14 C15 174.92(15) . . . . ? C13 C14 C15 C16 0.1(3) . . . . ? C14 C15 C16 O1 -177.25(15) . . . . ? C14 C15 C16 C17 2.3(2) . . . . ? O1 C16 C17 C18 176.93(13) . . . . ? C15 C16 C17 C18 -2.7(2) . . . . ? C16 C17 C18 C13 0.6(2) . . . . ? C14 C13 C18 C17 1.8(2) . . . . ? C1 C13 C18 C17 -175.17(13) . . . . ? O1 C19 C20 O2 -179.75(12) . . . . ? O2 C21 C22 O3 -74.27(17) . . . . ? O3 C23 C24 C25 -178.61(14) . . . . ? C28 C23 C24 C25 0.0(2) . . . . ? C23 C24 C25 O5 176.70(14) . . . . ? C23 C24 C25 C26 -1.3(2) . . . . ? O5 C25 C26 C27 -176.09(14) . . . . ? C24 C25 C26 C27 2.1(2) . . . . ? C25 C26 C27 C28 -1.6(2) . . . . ? C25 C26 C27 C29 175.91(15) . . . . ? O3 C23 C28 C27 178.98(15) . . . . ? C24 C23 C28 C27 0.5(2) . . . . ? C26 C27 C28 C23 0.3(2) . . . . ? C29 C27 C28 C23 -177.25(15) . . . . ? C26 C27 C29 O4 6.0(3) . . . . ? C28 C27 C29 O4 -176.46(17) . . . . ? O5 C30 C31 O6 -173.63(12) . . . . ? O6 C32 C33 O7 -66.81(17) . . . . ? O7 C34 C35 C36 -176.92(14) . . . . ? C39 C34 C35 C36 0.6(2) . . . . ? C34 C35 C36 C37 0.3(2) . . . . ? C35 C36 C37 C38 -1.0(2) . . . . ? C35 C36 C37 C10 175.39(14) . . . . ? N2 C10 C37 C38 153.78(14) . . . . ? C9 C10 C37 C38 -26.1(2) . . . . ? N2 C10 C37 C36 -22.4(2) . . . . ? C9 C10 C37 C36 157.69(15) . . . . ? C36 C37 C38 C39 0.8(2) . . . . ? C10 C37 C38 C39 -175.48(15) . . . . ? C37 C38 C39 C34 0.1(2) . . . . ? O7 C34 C39 C38 176.48(14) . . . . ? C35 C34 C39 C38 -0.8(2) . . . . ? C2 C1 N1 C12 1.4(2) . . . . ? C13 C1 N1 C12 -176.30(13) . . . . ? C4 C12 N1 C1 0.2(2) . . . . ? C11 C12 N1 C1 179.06(13) . . . . ? C9 C10 N2 C11 -0.3(2) . . . . ? C37 C10 N2 C11 179.81(13) . . . . ? C7 C11 N2 C10 1.5(2) . . . . ? C12 C11 N2 C10 -178.49(13) . . . . ? C15 C16 O1 C19 8.4(2) . . . . ? C17 C16 O1 C19 -171.16(13) . . . . ? C20 C19 O1 C16 -88.32(16) . . . . ? C22 C21 O2 C20 179.26(12) . . . . ? C19 C20 O2 C21 169.80(12) . . . . ? C28 C23 O3 C22 -9.4(2) . . . . ? C24 C23 O3 C22 169.18(14) . . . . ? C21 C22 O3 C23 -160.34(14) . . . . ? C24 C25 O5 C30 3.6(2) . . . . ? C26 C25 O5 C30 -178.29(13) . . . . ? C31 C30 O5 C25 -178.88(13) . . . . ? C33 C32 O6 C31 161.80(13) . . . . ? C30 C31 O6 C32 -90.93(15) . . . . ? C39 C34 O7 C33 1.7(2) . . . . ? C35 C34 O7 C33 179.06(14) . . . . ? C32 C33 O7 C34 -170.05(13) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.861 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.053