# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Nabeshima, Tatsuya' _publ_contact_author_email nabesima@chem.tsukuba.ac.jp _publ_section_title ; Cation recognition and pseudorotaxane formation of tris-dipyrrin BF2 macrocycles ; loop_ _publ_author_name N.Sakamoto C.Ikeda T.Nabeshima data_a #TrackingRef '- compound2.CIF' _database_code_depnum_ccdc_archive 'CCDC 680144' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H54 B3 Cl9 F6 N6 O6' _chemical_formula_weight 1564.69 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.94(3) _cell_length_b 20.22(4) _cell_length_c 20.85(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.87(8) _cell_angle_gamma 90.00 _cell_volume 7103(26) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3192 _exptl_absorpt_coefficient_mu 0.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8144 _exptl_absorpt_correction_T_max 0.9789 _exptl_absorpt_process_details scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAC Science DIP-2030' _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52087 _diffrn_reflns_av_R_equivalents 0.1355 _diffrn_reflns_av_sigmaI/netI 0.2003 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12381 _reflns_number_gt 3022 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^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 12381 _refine_ls_number_parameters 1032 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.2535 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.2251 _refine_ls_wR_factor_gt 0.1910 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.005 _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 B1 B 0.0839(6) -0.0751(5) 0.3869(5) 0.068(3) Uani 1 1 d . . . F1 F 0.1444(3) -0.0315(2) 0.37758(18) 0.0883(13) Uani 1 1 d . . . F2 F 0.0122(3) -0.0420(2) 0.37667(19) 0.0902(13) Uani 1 1 d . . . B2 B 0.1780(7) 0.1767(5) 0.1521(5) 0.078(3) Uani 1 1 d . . . F3 F 0.1164(3) 0.1776(2) 0.1883(2) 0.0994(15) Uani 1 1 d . . . F4 F 0.2451(3) 0.1517(2) 0.1848(2) 0.0957(14) Uani 1 1 d . . . B3 B 0.1820(7) 0.2716(6) 0.4834(5) 0.085(3) Uani 1 1 d . . . F5 F 0.2563(3) 0.2396(2) 0.4757(2) 0.0965(14) Uani 1 1 d . . . F6 F 0.1260(3) 0.2463(2) 0.4388(2) 0.0973(15) Uani 1 1 d . . . N1 N 0.0984(4) -0.1022(4) 0.4556(3) 0.0765(19) Uani 1 1 d . . . N2 N 0.0835(4) -0.1330(3) 0.3394(3) 0.0786(19) Uani 1 1 d . . . N3 N 0.1562(4) 0.1299(3) 0.0925(3) 0.0736(18) Uani 1 1 d . . . N4 N 0.1936(4) 0.2443(3) 0.1226(3) 0.0751(19) Uani 1 1 d . . . N5 N 0.1955(3) 0.3458(3) 0.4722(3) 0.0708(17) Uani 1 1 d . A . N6 N 0.1628(4) 0.2594(4) 0.5518(3) 0.0743(18) Uani 1 1 d . A . C1 C 0.1187(5) -0.0709(5) 0.5119(5) 0.079(2) Uani 1 1 d . . . C2 C 0.1275(5) -0.1154(5) 0.5643(4) 0.092(3) Uani 1 1 d . . . H1 H 0.1421 -0.1058 0.6085 0.111 Uiso 1 1 calc R . . C3 C 0.1101(4) -0.1753(4) 0.5366(4) 0.082(2) Uani 1 1 d . . . H2 H 0.1109 -0.2157 0.5599 0.099 Uiso 1 1 calc R . . C4 C 0.0906(5) -0.1706(5) 0.4692(5) 0.082(3) Uani 1 1 d . . . C5 C 0.0777(5) -0.2174(5) 0.4208(4) 0.081(2) Uani 1 1 d . . . C6 C 0.0735(5) -0.1988(5) 0.3588(4) 0.079(2) Uani 1 1 d . . . C7 C 0.0554(4) -0.2353(4) 0.3028(4) 0.080(2) Uani 1 1 d . . . H3 H 0.0463 -0.2816 0.3005 0.096 Uiso 1 1 calc R . . C8 C 0.0529(5) -0.1919(4) 0.2506(4) 0.086(3) Uani 1 1 d . . . H4 H 0.0412 -0.2030 0.2063 0.103 Uiso 1 1 calc R . . C9 C 0.0709(4) -0.1292(4) 0.2756(4) 0.073(2) Uani 1 1 d . . . C10 C 0.0788(5) -0.0712(4) 0.2363(4) 0.077(2) Uani 1 1 d . . . C11 C 0.0191(6) -0.0539(4) 0.1893(4) 0.078(2) Uani 1 1 d . . . O1 O -0.0517(4) -0.0882(3) 0.1822(3) 0.0939(17) Uani 1 1 d . . . C12 C -0.1047(5) -0.0743(4) 0.2269(5) 0.129(4) Uani 1 1 d . . . H5 H -0.0783 -0.0804 0.2706 0.194 Uiso 1 1 calc R . . H6 H -0.1503 -0.1043 0.2202 0.194 Uiso 1 1 calc R . . H7 H -0.1230 -0.0285 0.2215 0.194 Uiso 1 1 calc R . . C13 C 0.0277(6) -0.0041(4) 0.1462(4) 0.077(2) Uani 1 1 d . . . O2 O -0.0320(4) 0.0127(3) 0.0990(3) 0.0880(17) Uani 1 1 d . . . C14 C -0.0860(6) 0.0595(5) 0.1134(5) 0.153(4) Uani 1 1 d . . . H8 H -0.0585 0.0951 0.1386 0.229 Uiso 1 1 calc R . . H9 H -0.1254 0.0392 0.1386 0.229 Uiso 1 1 calc R . . H10 H -0.1127 0.0777 0.0734 0.229 Uiso 1 1 calc R . . C15 C 0.1025(5) 0.0284(4) 0.1475(4) 0.070(2) Uani 1 1 d . . . C16 C 0.1598(5) 0.0125(4) 0.1953(4) 0.074(2) Uani 1 1 d . . . H11 H 0.2088 0.0357 0.1981 0.089 Uiso 1 1 calc R . . C17 C 0.1495(5) -0.0361(4) 0.2399(4) 0.075(2) Uani 1 1 d . . . H12 H 0.1906 -0.0456 0.2731 0.090 Uiso 1 1 calc R . . C18 C 0.1169(4) 0.0696(4) 0.0913(4) 0.072(2) Uani 1 1 d . . . C19 C 0.1030(4) 0.0474(4) 0.0270(4) 0.075(2) Uani 1 1 d . . . H13 H 0.0776 0.0073 0.0130 0.090 Uiso 1 1 calc R . . C20 C 0.1333(4) 0.0948(4) -0.0122(4) 0.077(2) Uani 1 1 d . . . H14 H 0.1329 0.0929 -0.0577 0.092 Uiso 1 1 calc R . . C21 C 0.1647(5) 0.1463(5) 0.0286(4) 0.070(2) Uani 1 1 d . . . C22 C 0.1939(5) 0.2068(5) 0.0125(4) 0.078(2) Uani 1 1 d . . . C23 C 0.2048(5) 0.2550(5) 0.0600(4) 0.073(2) Uani 1 1 d . . . C24 C 0.2232(5) 0.3212(5) 0.0531(4) 0.087(3) Uani 1 1 d . . . H15 H 0.2351 0.3422 0.0144 0.104 Uiso 1 1 calc R . . C25 C 0.2213(5) 0.3508(4) 0.1121(4) 0.089(3) Uani 1 1 d . . . H16 H 0.2302 0.3963 0.1218 0.107 Uiso 1 1 calc R . . C26 C 0.2035(5) 0.3010(5) 0.1553(4) 0.077(2) Uani 1 1 d . . . C27 C 0.1971(5) 0.3133(4) 0.2224(4) 0.069(2) Uani 1 1 d . A . C28 C 0.1483(5) 0.3635(4) 0.2424(5) 0.080(2) Uani 1 1 d . . . O3 O 0.1001(5) 0.3967(3) 0.1961(3) 0.104(2) Uani 1 1 d . . . C29 C 0.0288(7) 0.3611(6) 0.1774(6) 0.196(6) Uani 1 1 d . . . H17 H 0.0414 0.3207 0.1546 0.295 Uiso 1 1 calc R . . H18 H -0.0071 0.3887 0.1489 0.295 Uiso 1 1 calc R . . H19 H 0.0030 0.3494 0.2159 0.295 Uiso 1 1 calc R . . C30 C 0.1538(6) 0.3828(4) 0.3055(5) 0.088(3) Uani 1 1 d D A . O4 O 0.0999(6) 0.4295(4) 0.3237(3) 0.125(3) Uani 1 1 d D . . C31 C 0.0332(14) 0.4144(18) 0.3444(19) 0.17(2) Uani 0.30 1 d PD A 1 H20 H 0.0420 0.3808 0.3783 0.261 Uiso 0.30 1 calc PR A 1 H21 H -0.0029 0.3969 0.3087 0.261 Uiso 0.30 1 calc PR A 1 H22 H 0.0098 0.4539 0.3620 0.261 Uiso 0.30 1 calc PR A 1 C32 C 0.0951(8) 0.4839(6) 0.2957(6) 0.125(5) Uani 0.70 1 d PD A 2 H23 H 0.0736 0.4776 0.2507 0.188 Uiso 0.70 1 calc PR A 2 H24 H 0.1480 0.5039 0.2973 0.188 Uiso 0.70 1 calc PR A 2 H25 H 0.0599 0.5132 0.3172 0.188 Uiso 0.70 1 calc PR A 2 C33 C 0.1985(5) 0.3506(4) 0.3544(4) 0.080(2) Uani 1 1 d . . . C34 C 0.2452(5) 0.2996(4) 0.3359(4) 0.079(2) Uani 1 1 d . A . H26 H 0.2798 0.2773 0.3675 0.094 Uiso 1 1 calc R . . C35 C 0.2422(5) 0.2799(4) 0.2706(4) 0.076(2) Uani 1 1 d . . . H27 H 0.2722 0.2427 0.2597 0.091 Uiso 1 1 calc R A . C36 C 0.2065(5) 0.3800(4) 0.4168(4) 0.076(2) Uani 1 1 d . A . C37 C 0.2221(5) 0.4448(4) 0.4335(4) 0.091(3) Uani 1 1 d . . . H28 H 0.2339 0.4786 0.4044 0.109 Uiso 1 1 calc R A . C38 C 0.2182(5) 0.4535(4) 0.4976(4) 0.088(3) Uani 1 1 d . A . H29 H 0.2260 0.4937 0.5210 0.106 Uiso 1 1 calc R . . C39 C 0.2006(5) 0.3924(5) 0.5221(4) 0.080(2) Uani 1 1 d . . . C40 C 0.1825(5) 0.3729(5) 0.5828(4) 0.082(2) Uani 1 1 d . A . C41 C 0.1612(5) 0.3085(4) 0.5981(4) 0.078(2) Uani 1 1 d . . . C42 C 0.1395(5) 0.2798(5) 0.6539(4) 0.094(3) Uani 1 1 d . A . H30 H 0.1325 0.3024 0.6928 0.113 Uiso 1 1 calc R . . C43 C 0.1303(5) 0.2158(5) 0.6436(4) 0.095(3) Uani 1 1 d . . . H31 H 0.1154 0.1840 0.6737 0.114 Uiso 1 1 calc R A . C44 C 0.1461(5) 0.2035(5) 0.5818(4) 0.087(3) Uani 1 1 d . A . C45 C 0.1462(5) 0.1388(5) 0.5530(4) 0.083(3) Uani 1 1 d . . . C46 C 0.1973(6) 0.0900(6) 0.5852(4) 0.096(3) Uani 1 1 d . A . O5 O 0.2509(5) 0.1076(3) 0.6351(3) 0.121(2) Uani 1 1 d . . . C47 C 0.3138(6) 0.1516(4) 0.6199(5) 0.134(4) Uani 1 1 d . A . H32 H 0.2953 0.1975 0.6209 0.201 Uiso 1 1 calc R . . H33 H 0.3287 0.1413 0.5769 0.201 Uiso 1 1 calc R . . H34 H 0.3600 0.1458 0.6518 0.201 Uiso 1 1 calc R . . C48 C 0.1894(6) 0.0227(6) 0.5694(5) 0.095(3) Uani 1 1 d . . . O6 O 0.2378(5) -0.0212(3) 0.6036(3) 0.119(2) Uani 1 1 d . A . C49 C 0.3103(7) -0.0324(5) 0.5807(6) 0.150(5) Uani 1 1 d . . . H35 H 0.3027 -0.0378 0.5337 0.225 Uiso 1 1 calc R A . H36 H 0.3341 -0.0727 0.6004 0.225 Uiso 1 1 calc R . . H37 H 0.3456 0.0052 0.5916 0.225 Uiso 1 1 calc R . . C50 C 0.1328(5) 0.0005(5) 0.5216(4) 0.081(2) Uani 1 1 d . A . C51 C 0.0860(5) 0.0487(5) 0.4860(4) 0.078(2) Uani 1 1 d . . . H38 H 0.0487 0.0360 0.4510 0.093 Uiso 1 1 calc R A . C52 C 0.0956(5) 0.1154(4) 0.5034(4) 0.078(2) Uani 1 1 d . A . H39 H 0.0641 0.1468 0.4785 0.094 Uiso 1 1 calc R . . C53 C 0.0702(5) -0.2858(5) 0.4415(4) 0.086(3) Uani 1 1 d . . . C54 C 0.1152(5) -0.3325(5) 0.4114(4) 0.096(3) Uani 1 1 d . . . H40 H 0.1473 -0.3195 0.3788 0.115 Uiso 1 1 calc R . . C55 C 0.1117(6) -0.3990(5) 0.4305(5) 0.108(3) Uani 1 1 d . . . H41 H 0.1440 -0.4310 0.4125 0.129 Uiso 1 1 calc R . . C56 C 0.0618(6) -0.4179(5) 0.4750(5) 0.108(3) Uani 1 1 d . . . H42 H 0.0582 -0.4632 0.4863 0.129 Uiso 1 1 calc R . . C57 C 0.0165(5) -0.3710(6) 0.5037(5) 0.108(3) Uani 1 1 d . . . H43 H -0.0172 -0.3839 0.5352 0.129 Uiso 1 1 calc R . . C58 C 0.0213(5) -0.3058(5) 0.4859(4) 0.098(3) Uani 1 1 d . . . H44 H -0.0102 -0.2739 0.5049 0.118 Uiso 1 1 calc R . . C59 C 0.2058(5) 0.2188(4) -0.0543(4) 0.076(2) Uani 1 1 d . . . C60 C 0.1682(5) 0.2694(5) -0.0875(4) 0.096(3) Uani 1 1 d . . . H45 H 0.1339 0.2971 -0.0662 0.115 Uiso 1 1 calc R . . C61 C 0.1784(6) 0.2824(5) -0.1524(5) 0.126(4) Uani 1 1 d . . . H46 H 0.1497 0.3165 -0.1758 0.151 Uiso 1 1 calc R . . C62 C 0.2331(6) 0.2423(5) -0.1811(4) 0.109(3) Uani 1 1 d . . . H47 H 0.2431 0.2501 -0.2245 0.131 Uiso 1 1 calc R . . C63 C 0.2714(5) 0.1927(5) -0.1474(4) 0.099(3) Uani 1 1 d . . . H48 H 0.3077 0.1658 -0.1674 0.119 Uiso 1 1 calc R . . C64 C 0.2584(5) 0.1808(4) -0.0839(4) 0.088(3) Uani 1 1 d . . . H49 H 0.2862 0.1460 -0.0607 0.106 Uiso 1 1 calc R . . C65 C 0.1827(6) 0.4244(5) 0.6343(4) 0.089(3) Uani 1 1 d . . . C66 C 0.1347(7) 0.4805(6) 0.6264(5) 0.139(4) Uani 1 1 d . A . H50 H 0.1019 0.4866 0.5871 0.166 Uiso 1 1 calc R . . C67 C 0.1339(8) 0.5275(6) 0.6750(6) 0.163(5) Uani 1 1 d . . . H51 H 0.1023 0.5661 0.6684 0.196 Uiso 1 1 calc R A . C68 C 0.1790(8) 0.5176(6) 0.7320(6) 0.137(5) Uani 1 1 d . A . H52 H 0.1756 0.5489 0.7656 0.164 Uiso 1 1 calc R . . C69 C 0.2298(7) 0.4637(6) 0.7436(5) 0.120(4) Uani 1 1 d . . . H53 H 0.2632 0.4591 0.7828 0.145 Uiso 1 1 calc R A . C70 C 0.2287(5) 0.4172(5) 0.6944(5) 0.098(3) Uani 1 1 d . A . H54 H 0.2605 0.3786 0.7015 0.118 Uiso 1 1 calc R . . C71 C 0.5041(16) 0.7060(15) 0.2274(16) 0.097(10) Uiso 0.337(13) 1 d P B 2 H55 H 0.4734 0.7170 0.2645 0.116 Uiso 0.337(13) 1 calc PR B 2 Cl1 Cl 0.5157(6) 0.7677(8) 0.1639(5) 0.131(5) Uani 0.337(13) 1 d PD B 2 Cl2 Cl 0.6168(5) 0.6884(6) 0.2413(9) 0.130(5) Uani 0.337(13) 1 d PD B 2 Cl3 Cl 0.4928(11) 0.6224(10) 0.1868(9) 0.183(8) Uani 0.337(13) 1 d PD B 2 C72 C 0.5222(8) 0.6673(7) 0.2342(7) 0.105(6) Uiso 0.663(13) 1 d PD B 1 H59 H 0.4792 0.6610 0.2631 0.126 Uiso 0.663(13) 1 calc PR B 1 Cl4 Cl 0.4756(6) 0.7221(5) 0.1753(3) 0.165(4) Uani 0.663(13) 1 d PD B 1 Cl5 Cl 0.5320(6) 0.5921(4) 0.2070(4) 0.156(3) Uani 0.663(13) 1 d PD B 1 Cl6 Cl 0.5921(5) 0.7138(3) 0.2844(4) 0.148(3) Uani 0.663(13) 1 d PD B 1 C73 C 0.2329(10) 0.5690(8) 0.0981(8) 0.049(5) Uiso 0.35 1 d PD C 1 H56 H 0.2750 0.5453 0.0768 0.059 Uiso 0.35 1 calc PR C 1 Cl7 Cl 0.1750(7) 0.6062(5) 0.0455(6) 0.249(6) Uani 0.35 1 d PD C 1 Cl8 Cl 0.1741(9) 0.5116(8) 0.1349(9) 0.81(4) Uani 0.35 1 d PD C 1 Cl9 Cl 0.2731(7) 0.6165(4) 0.1537(4) 0.205(5) Uani 0.35 1 d PD C 1 C74 C 0.0791(16) 0.7638(12) -0.0065(11) 0.149(14) Uiso 0.338(6) 1 d PD D 2 H57 H 0.1250 0.7380 0.0145 0.179 Uiso 0.338(6) 1 calc PR D 2 Cl10 Cl 0.0562(9) 0.8271(10) 0.0441(7) 0.263(12) Uani 0.338(6) 1 d PD D 2 Cl11 Cl 0.1015(8) 0.7918(5) -0.0840(5) 0.211(7) Uani 0.338(6) 1 d PD D 2 Cl12 Cl -0.0006(9) 0.7118(8) -0.0243(8) 0.276(9) Uani 0.338(6) 1 d PD D 2 C75 C 0.0246(14) 0.7958(9) 0.0354(9) 0.243(17) Uiso 0.662(6) 1 d PD D 3 H60 H -0.0287 0.8109 0.0461 0.292 Uiso 0.662(6) 1 calc PR D 3 Cl13 Cl 0.0172(3) 0.7740(3) -0.0488(2) 0.142(2) Uani 0.662(6) 1 d PD D 3 Cl14 Cl 0.0909(4) 0.8596(3) 0.0502(3) 0.132(2) Uani 0.662(6) 1 d PD D 3 Cl15 Cl 0.0503(3) 0.7244(3) 0.0795(3) 0.189(3) Uani 0.662(6) 1 d PD D 3 C76 C 0.0452(12) 0.5526(9) 0.0547(9) 0.120(9) Uiso 0.35 1 d PD E 2 H58 H 0.0989 0.5698 0.0475 0.144 Uiso 0.35 1 calc PR E 2 Cl16 Cl -0.0433(7) 0.5842(5) 0.0019(5) 0.191(4) Uani 0.35 1 d PD . 2 Cl17 Cl 0.0267(7) 0.4656(6) 0.0463(6) 0.236(6) Uani 0.35 1 d PD . 2 Cl18 Cl 0.0108(5) 0.5637(4) 0.1313(4) 0.318(5) Uani 0.65 1 d PD . . C77 C 0.0487(12) 0.5640(15) 0.2092(10) 0.180(16) Uiso 0.30 1 d PD E 1 H61 H 0.0671 0.5179 0.2198 0.216 Uiso 0.30 1 calc PR E 1 Cl19 Cl 0.1277(6) 0.6114(5) 0.2165(7) 0.254(8) Uani 0.30 1 d PD E 1 Cl20 Cl -0.0274(5) 0.5797(5) 0.2534(7) 0.227(7) Uani 0.30 1 d PD E 1 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 B1 0.075(7) 0.086(7) 0.047(7) -0.006(6) 0.021(6) -0.008(6) F1 0.118(4) 0.100(3) 0.051(3) 0.000(2) 0.030(3) -0.017(3) F2 0.112(4) 0.112(3) 0.051(3) 0.004(3) 0.029(3) 0.009(3) B2 0.081(8) 0.107(9) 0.050(7) 0.004(6) 0.018(6) 0.011(7) F3 0.129(4) 0.116(4) 0.063(3) -0.017(3) 0.055(3) -0.027(3) F4 0.126(4) 0.101(3) 0.059(3) 0.006(3) 0.005(3) -0.010(3) B3 0.082(8) 0.115(9) 0.060(8) -0.015(7) 0.021(7) 0.015(7) F5 0.119(4) 0.101(3) 0.076(4) 0.015(3) 0.043(3) 0.007(3) F6 0.124(4) 0.124(4) 0.047(3) -0.001(3) 0.024(3) -0.031(3) N1 0.096(5) 0.092(5) 0.046(5) 0.002(4) 0.029(4) -0.007(4) N2 0.098(5) 0.100(5) 0.042(5) 0.004(4) 0.029(4) -0.003(4) N3 0.079(5) 0.096(5) 0.048(5) 0.011(4) 0.015(4) 0.000(4) N4 0.096(5) 0.105(5) 0.028(4) 0.016(4) 0.023(4) 0.004(4) N5 0.090(5) 0.084(5) 0.039(5) -0.003(4) 0.010(4) -0.003(4) N6 0.105(5) 0.090(5) 0.031(4) 0.002(4) 0.024(4) 0.003(4) C1 0.080(6) 0.097(7) 0.059(7) 0.005(6) 0.011(5) -0.003(5) C2 0.109(7) 0.110(7) 0.062(7) 0.014(6) 0.028(6) -0.005(6) C3 0.089(6) 0.101(7) 0.060(7) 0.017(5) 0.023(5) -0.011(5) C4 0.092(6) 0.107(8) 0.053(7) 0.032(6) 0.031(5) 0.004(5) C5 0.102(7) 0.101(7) 0.042(6) 0.012(6) 0.024(5) -0.001(5) C6 0.101(7) 0.093(7) 0.046(6) 0.008(5) 0.026(5) 0.017(5) C7 0.095(6) 0.086(6) 0.062(7) 0.002(5) 0.026(5) -0.003(5) C8 0.114(7) 0.104(7) 0.044(6) -0.006(5) 0.028(5) 0.002(6) C9 0.084(6) 0.101(7) 0.039(6) -0.002(5) 0.026(5) -0.001(5) C10 0.088(7) 0.111(7) 0.035(6) 0.006(5) 0.023(5) -0.015(6) C11 0.092(7) 0.106(7) 0.041(6) 0.010(5) 0.024(5) -0.016(6) O1 0.091(4) 0.122(5) 0.074(5) 0.003(3) 0.032(4) -0.015(4) C12 0.119(8) 0.139(8) 0.143(10) 0.020(7) 0.075(8) -0.001(6) C13 0.097(7) 0.105(7) 0.033(6) 0.007(5) 0.022(5) 0.007(6) O2 0.095(4) 0.128(5) 0.044(4) 0.001(3) 0.019(4) -0.005(4) C14 0.182(11) 0.180(11) 0.091(9) -0.036(8) -0.006(8) 0.068(9) C15 0.090(7) 0.081(6) 0.043(6) 0.008(4) 0.026(5) 0.006(5) C16 0.089(6) 0.099(6) 0.037(5) 0.011(5) 0.018(5) 0.009(5) C17 0.094(7) 0.095(6) 0.041(5) 0.007(5) 0.025(5) 0.002(5) C18 0.061(5) 0.109(7) 0.047(6) -0.009(5) 0.013(4) 0.007(5) C19 0.087(6) 0.093(6) 0.049(6) -0.017(5) 0.021(5) -0.009(5) C20 0.094(6) 0.100(6) 0.042(6) 0.002(5) 0.035(5) 0.001(5) C21 0.080(6) 0.108(7) 0.025(5) 0.012(5) 0.019(4) 0.021(5) C22 0.084(6) 0.112(7) 0.043(6) 0.019(6) 0.025(5) -0.003(5) C23 0.089(6) 0.098(7) 0.034(6) 0.014(5) 0.019(5) -0.006(5) C24 0.107(7) 0.113(7) 0.042(6) 0.011(5) 0.014(5) -0.013(6) C25 0.126(7) 0.101(7) 0.043(6) 0.004(5) 0.023(5) -0.017(5) C26 0.100(7) 0.102(7) 0.032(5) -0.001(5) 0.017(5) -0.011(5) C27 0.079(6) 0.087(6) 0.044(6) 0.015(5) 0.013(5) 0.017(5) C28 0.097(7) 0.089(6) 0.057(7) 0.009(6) 0.015(6) 0.003(5) O3 0.147(6) 0.112(5) 0.055(4) 0.013(4) 0.023(4) 0.020(4) C29 0.171(12) 0.192(12) 0.202(15) -0.016(10) -0.102(10) -0.016(10) C30 0.124(8) 0.083(7) 0.060(8) -0.013(6) 0.022(7) 0.006(6) O4 0.214(9) 0.110(6) 0.050(5) 0.004(4) 0.002(5) 0.037(7) C31 0.10(3) 0.29(5) 0.14(4) -0.07(4) 0.05(3) 0.00(3) C32 0.115(12) 0.179(16) 0.082(13) -0.037(11) 0.016(10) -0.017(12) C33 0.096(7) 0.097(7) 0.050(7) 0.010(6) 0.027(6) 0.005(5) C34 0.085(6) 0.102(7) 0.050(6) 0.004(5) 0.014(5) -0.013(5) C35 0.088(6) 0.090(6) 0.053(6) -0.007(5) 0.025(5) -0.015(5) C36 0.102(6) 0.091(7) 0.035(6) 0.003(5) 0.007(5) -0.006(5) C37 0.123(7) 0.098(7) 0.056(7) -0.004(5) 0.027(6) -0.010(6) C38 0.126(8) 0.093(7) 0.049(6) 0.001(5) 0.022(6) 0.005(6) C39 0.088(6) 0.104(7) 0.049(6) -0.005(6) 0.016(5) -0.002(5) C40 0.082(6) 0.118(8) 0.046(6) -0.013(6) 0.017(5) 0.003(5) C41 0.088(6) 0.089(7) 0.059(7) 0.008(6) 0.017(5) -0.015(5) C42 0.110(7) 0.139(8) 0.036(6) 0.002(6) 0.019(5) -0.013(7) C43 0.134(8) 0.112(7) 0.040(6) -0.005(5) 0.021(5) -0.033(6) C44 0.130(8) 0.099(7) 0.036(6) -0.008(6) 0.026(5) -0.020(6) C45 0.096(7) 0.120(8) 0.035(6) 0.015(6) 0.010(5) -0.019(6) C46 0.132(9) 0.116(9) 0.038(6) -0.003(6) 0.000(6) -0.030(7) O5 0.176(7) 0.117(5) 0.066(5) 0.018(4) -0.017(5) -0.012(5) C47 0.134(9) 0.119(8) 0.142(10) 0.030(7) -0.019(8) -0.034(7) C48 0.123(8) 0.111(8) 0.048(7) 0.002(6) 0.000(6) -0.016(7) O6 0.156(7) 0.111(5) 0.084(5) 0.027(4) -0.022(5) 0.009(5) C49 0.174(12) 0.129(9) 0.138(12) -0.014(8) -0.032(10) 0.025(9) C50 0.092(7) 0.109(8) 0.048(6) 0.011(6) 0.028(5) -0.013(6) C51 0.083(6) 0.117(7) 0.038(5) -0.011(5) 0.024(5) -0.022(6) C52 0.095(7) 0.094(7) 0.053(6) 0.001(5) 0.040(5) -0.010(5) C53 0.099(7) 0.093(7) 0.072(7) 0.023(6) 0.035(6) -0.001(6) C54 0.119(8) 0.099(7) 0.071(7) 0.021(6) 0.007(6) 0.005(6) C55 0.108(8) 0.106(8) 0.112(9) 0.013(7) 0.023(7) 0.017(6) C56 0.102(8) 0.104(8) 0.117(10) 0.029(7) 0.016(7) -0.022(7) C57 0.096(7) 0.125(9) 0.104(9) 0.040(7) 0.021(6) 0.009(7) C58 0.107(7) 0.114(8) 0.077(7) 0.019(6) 0.032(6) -0.016(6) C59 0.093(7) 0.097(6) 0.039(6) 0.018(5) 0.008(5) 0.002(5) C60 0.129(8) 0.127(8) 0.035(6) -0.001(5) 0.016(6) -0.009(6) C61 0.147(10) 0.157(10) 0.075(9) 0.033(7) 0.021(7) 0.025(8) C62 0.141(9) 0.146(9) 0.044(7) 0.029(6) 0.026(7) -0.007(7) C63 0.103(7) 0.143(9) 0.055(7) 0.008(6) 0.028(6) -0.002(6) C64 0.114(7) 0.104(7) 0.051(6) 0.005(5) 0.036(6) -0.004(5) C65 0.107(7) 0.118(8) 0.043(6) 0.004(6) 0.019(6) -0.015(6) C66 0.212(12) 0.136(9) 0.066(8) -0.019(7) 0.003(8) 0.039(9) C67 0.265(15) 0.148(10) 0.071(9) -0.048(8) -0.007(10) 0.050(9) C68 0.186(13) 0.158(11) 0.074(9) -0.042(9) 0.053(9) -0.023(9) C69 0.142(10) 0.167(11) 0.057(7) -0.043(8) 0.031(7) -0.059(8) C70 0.106(7) 0.126(8) 0.065(7) 0.008(6) 0.023(6) -0.030(6) Cl1 0.116(7) 0.215(13) 0.067(6) 0.023(6) 0.038(5) -0.007(7) Cl2 0.090(6) 0.167(9) 0.140(13) 0.012(8) 0.043(6) 0.003(5) Cl3 0.172(14) 0.28(2) 0.108(13) -0.032(12) 0.067(10) -0.003(13) Cl4 0.205(8) 0.223(8) 0.067(4) 0.030(4) 0.018(4) 0.085(6) Cl5 0.200(7) 0.199(6) 0.072(4) 0.007(4) 0.029(4) 0.032(5) Cl6 0.170(6) 0.171(5) 0.101(5) 0.018(4) 0.006(4) -0.015(4) Cl7 0.250(13) 0.214(11) 0.306(17) -0.067(11) 0.135(13) -0.039(10) Cl8 0.52(4) 1.34(9) 0.49(4) -0.46(6) -0.24(4) 0.69(6) Cl9 0.371(15) 0.132(7) 0.108(8) -0.023(6) 0.003(9) 0.051(8) Cl10 0.164(13) 0.38(3) 0.226(19) 0.136(19) -0.082(12) -0.098(16) Cl11 0.298(17) 0.185(10) 0.146(11) -0.006(8) 0.002(11) 0.008(10) Cl12 0.238(15) 0.32(2) 0.29(2) 0.032(16) 0.141(14) 0.019(14) Cl13 0.137(4) 0.201(5) 0.085(4) -0.029(3) 0.003(3) 0.022(4) Cl14 0.147(5) 0.126(4) 0.117(4) -0.011(3) -0.014(4) 0.026(4) Cl15 0.183(5) 0.239(6) 0.149(6) -0.023(4) 0.038(4) -0.075(4) Cl16 0.272(13) 0.170(9) 0.133(10) 0.010(7) 0.025(9) -0.044(9) Cl17 0.245(13) 0.259(15) 0.215(15) 0.045(11) 0.084(12) 0.056(11) Cl18 0.282(8) 0.422(11) 0.227(8) 0.149(8) -0.076(7) -0.066(8) Cl19 0.151(9) 0.145(9) 0.47(2) -0.146(12) 0.024(12) -0.066(7) Cl20 0.110(8) 0.172(10) 0.40(2) 0.074(11) 0.061(11) 0.024(7) _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 B1 F1 1.380(9) . ? B1 F2 1.385(10) . ? B1 N1 1.530(11) . ? B1 N2 1.533(10) . ? B2 F3 1.350(10) . ? B2 F4 1.362(10) . ? B2 N4 1.534(11) . ? B2 N3 1.574(11) . ? B3 F6 1.358(11) . ? B3 F5 1.439(10) . ? B3 N6 1.515(12) . ? B3 N5 1.538(12) . ? N1 C1 1.347(9) . ? N1 C4 1.421(9) . ? N2 C9 1.328(9) . ? N2 C6 1.405(9) . ? N3 C18 1.388(9) . ? N3 C21 1.396(9) . ? N4 C26 1.335(9) . ? N4 C23 1.356(9) . ? N5 C36 1.376(9) . ? N5 C39 1.398(9) . ? N6 C44 1.335(9) . ? N6 C41 1.386(9) . ? C1 C2 1.411(10) . ? C1 C50 1.474(11) . ? C2 C3 1.361(9) . ? C2 H1 0.9500 . ? C3 C4 1.414(11) . ? C3 H2 0.9500 . ? C4 C5 1.384(11) . ? C5 C6 1.342(10) . ? C5 C53 1.458(10) . ? C6 C7 1.388(10) . ? C7 C8 1.396(10) . ? C7 H3 0.9500 . ? C8 C9 1.392(9) . ? C8 H4 0.9500 . ? C9 C10 1.445(10) . ? C10 C11 1.380(10) . ? C10 C17 1.387(9) . ? C11 C13 1.367(10) . ? C11 O1 1.381(9) . ? O1 C12 1.387(9) . ? C12 H5 0.9800 . ? C12 H6 0.9800 . ? C12 H7 0.9800 . ? C13 O2 1.379(9) . ? C13 C15 1.424(10) . ? O2 C14 1.372(9) . ? C14 H8 0.9800 . ? C14 H9 0.9800 . ? C14 H10 0.9800 . ? C15 C16 1.357(9) . ? C15 C18 1.480(10) . ? C16 C17 1.377(9) . ? C16 H11 0.9500 . ? C17 H12 0.9500 . ? C18 C19 1.410(10) . ? C19 C20 1.390(9) . ? C19 H13 0.9500 . ? C20 C21 1.413(10) . ? C20 H14 0.9500 . ? C21 C22 1.374(10) . ? C22 C23 1.387(10) . ? C22 C59 1.448(11) . ? C23 C24 1.386(10) . ? C24 C25 1.372(10) . ? C24 H15 0.9500 . ? C25 C26 1.405(9) . ? C25 H16 0.9500 . ? C26 C27 1.436(10) . ? C27 C35 1.374(9) . ? C27 C28 1.399(10) . ? C28 C30 1.366(11) . ? C28 O3 1.375(9) . ? O3 C29 1.426(10) . ? C29 H17 0.9800 . ? C29 H18 0.9800 . ? C29 H19 0.9800 . ? C30 C33 1.371(10) . ? C30 O4 1.393(9) . ? O4 C32 1.244(11) . ? O4 C31 1.286(17) . ? C31 H20 0.9800 . ? C31 H21 0.9800 . ? C31 H22 0.9800 . ? C32 H23 0.9800 . ? C32 H24 0.9800 . ? C32 H25 0.9800 . ? C33 C34 1.378(10) . ? C33 C36 1.424(11) . ? C34 C35 1.415(10) . ? C34 H26 0.9500 . ? C35 H27 0.9500 . ? C36 C37 1.373(9) . ? C37 C38 1.356(10) . ? C37 H28 0.9500 . ? C38 C39 1.381(10) . ? C38 H29 0.9500 . ? C39 C40 1.389(11) . ? C40 C41 1.399(10) . ? C40 C65 1.495(11) . ? C41 C42 1.382(10) . ? C42 C43 1.320(10) . ? C42 H30 0.9500 . ? C43 C44 1.366(10) . ? C43 H31 0.9500 . ? C44 C45 1.439(11) . ? C45 C52 1.360(10) . ? C45 C46 1.434(11) . ? C46 O5 1.356(10) . ? C46 C48 1.402(11) . ? O5 C47 1.447(9) . ? C47 H32 0.9800 . ? C47 H33 0.9800 . ? C47 H34 0.9800 . ? C48 O6 1.359(10) . ? C48 C50 1.386(11) . ? O6 C49 1.382(11) . ? C49 H35 0.9800 . ? C49 H36 0.9800 . ? C49 H37 0.9800 . ? C50 C51 1.418(10) . ? C51 C52 1.401(9) . ? C51 H38 0.9500 . ? C52 H39 0.9500 . ? C53 C58 1.365(10) . ? C53 C54 1.402(10) . ? C54 C55 1.406(10) . ? C54 H40 0.9500 . ? C55 C56 1.371(11) . ? C55 H41 0.9500 . ? C56 C57 1.393(11) . ? C56 H42 0.9500 . ? C57 C58 1.373(10) . ? C57 H43 0.9500 . ? C58 H44 0.9500 . ? C59 C60 1.358(10) . ? C59 C64 1.371(10) . ? C60 C61 1.406(11) . ? C60 H45 0.9500 . ? C61 C62 1.410(11) . ? C61 H46 0.9500 . ? C62 C63 1.352(10) . ? C62 H47 0.9500 . ? C63 C64 1.384(10) . ? C63 H48 0.9500 . ? C64 H49 0.9500 . ? C65 C66 1.395(11) . ? C65 C70 1.414(11) . ? C66 C67 1.390(12) . ? C66 H50 0.9500 . ? C67 C68 1.360(13) . ? C67 H51 0.9500 . ? C68 C69 1.394(13) . ? C68 H52 0.9500 . ? C69 C70 1.392(11) . ? C69 H53 0.9500 . ? C70 H54 0.9500 . ? C71 Cl1 1.84(3) . ? C71 Cl3 1.89(3) . ? C71 Cl2 1.94(3) . ? C71 H55 1.0000 . ? C72 Cl5 1.636(14) . ? C72 Cl6 1.768(13) . ? C72 Cl4 1.778(13) . ? C72 H59 1.0000 . ? C73 Cl7 1.584(15) . ? C73 Cl9 1.602(15) . ? C73 Cl8 1.758(17) . ? C73 H56 1.0000 . ? C74 Cl12 1.721(19) . ? C74 Cl10 1.727(18) . ? C74 Cl11 1.788(19) . ? C74 H57 1.0000 . ? C75 Cl14 1.717(18) . ? C75 Cl15 1.743(18) . ? C75 Cl13 1.801(19) . ? C75 H60 1.0000 . ? C76 Cl18 1.770(18) . ? C76 Cl17 1.793(17) . ? C76 Cl16 1.877(17) . ? C76 H58 1.0000 . ? Cl16 Cl17 1.469(13) 3_565 ? Cl17 Cl16 1.469(13) 3_565 ? Cl18 C77 1.683(19) . ? C77 Cl19 1.641(18) . ? C77 Cl20 1.690(19) . ? C77 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 F1 B1 F2 108.7(8) . . ? F1 B1 N1 108.1(7) . . ? F2 B1 N1 111.8(7) . . ? F1 B1 N2 110.6(7) . . ? F2 B1 N2 108.9(7) . . ? N1 B1 N2 108.7(7) . . ? F3 B2 F4 112.2(9) . . ? F3 B2 N4 112.8(8) . . ? F4 B2 N4 111.2(8) . . ? F3 B2 N3 108.5(8) . . ? F4 B2 N3 106.7(7) . . ? N4 B2 N3 104.8(8) . . ? F6 B3 F5 108.1(8) . . ? F6 B3 N6 112.3(8) . . ? F5 B3 N6 107.8(8) . . ? F6 B3 N5 111.6(8) . . ? F5 B3 N5 106.1(8) . . ? N6 B3 N5 110.6(8) . . ? C1 N1 C4 107.7(8) . . ? C1 N1 B1 130.5(8) . . ? C4 N1 B1 121.7(7) . . ? C9 N2 C6 109.4(7) . . ? C9 N2 B1 126.3(8) . . ? C6 N2 B1 122.0(7) . . ? C18 N3 C21 106.6(7) . . ? C18 N3 B2 128.0(7) . . ? C21 N3 B2 124.9(8) . . ? C26 N4 C23 109.5(7) . . ? C26 N4 B2 125.4(7) . . ? C23 N4 B2 125.0(8) . . ? C36 N5 C39 106.4(7) . . ? C36 N5 B3 130.8(7) . . ? C39 N5 B3 122.8(8) . . ? C44 N6 C41 105.1(7) . . ? C44 N6 B3 130.9(8) . . ? C41 N6 B3 124.0(8) . . ? N1 C1 C2 111.9(8) . . ? N1 C1 C50 127.1(9) . . ? C2 C1 C50 121.1(9) . . ? C3 C2 C1 103.8(9) . . ? C3 C2 H1 128.1 . . ? C1 C2 H1 128.1 . . ? C2 C3 C4 112.3(8) . . ? C2 C3 H2 123.8 . . ? C4 C3 H2 123.8 . . ? C5 C4 C3 133.0(9) . . ? C5 C4 N1 122.1(8) . . ? C3 C4 N1 104.3(8) . . ? C6 C5 C4 119.9(9) . . ? C6 C5 C53 123.7(9) . . ? C4 C5 C53 116.4(8) . . ? C5 C6 C7 130.2(9) . . ? C5 C6 N2 123.2(9) . . ? C7 C6 N2 106.5(7) . . ? C8 C7 C6 107.9(8) . . ? C8 C7 H3 126.0 . . ? C6 C7 H3 126.0 . . ? C7 C8 C9 107.0(8) . . ? C7 C8 H4 126.5 . . ? C9 C8 H4 126.5 . . ? N2 C9 C8 109.2(8) . . ? N2 C9 C10 126.9(9) . . ? C8 C9 C10 123.8(8) . . ? C11 C10 C17 118.4(8) . . ? C11 C10 C9 120.3(8) . . ? C17 C10 C9 120.9(8) . . ? C13 C11 C10 122.2(9) . . ? C13 C11 O1 116.8(9) . . ? C10 C11 O1 120.9(8) . . ? C11 O1 C12 116.2(7) . . ? O1 C12 H5 109.5 . . ? O1 C12 H6 109.5 . . ? H5 C12 H6 109.5 . . ? O1 C12 H7 109.5 . . ? H5 C12 H7 109.5 . . ? H6 C12 H7 109.5 . . ? C11 C13 O2 122.0(9) . . ? C11 C13 C15 118.8(9) . . ? O2 C13 C15 119.0(8) . . ? C14 O2 C13 118.0(7) . . ? O2 C14 H8 109.5 . . ? O2 C14 H9 109.5 . . ? H8 C14 H9 109.5 . . ? O2 C14 H10 109.5 . . ? H8 C14 H10 109.5 . . ? H9 C14 H10 109.5 . . ? C16 C15 C13 118.2(8) . . ? C16 C15 C18 123.5(8) . . ? C13 C15 C18 117.6(8) . . ? C15 C16 C17 122.3(8) . . ? C15 C16 H11 118.9 . . ? C17 C16 H11 118.9 . . ? C16 C17 C10 119.8(8) . . ? C16 C17 H12 120.1 . . ? C10 C17 H12 120.1 . . ? N3 C18 C19 109.3(7) . . ? N3 C18 C15 126.7(8) . . ? C19 C18 C15 123.3(8) . . ? C20 C19 C18 107.7(7) . . ? C20 C19 H13 126.2 . . ? C18 C19 H13 126.2 . . ? C19 C20 C21 107.0(7) . . ? C19 C20 H14 126.5 . . ? C21 C20 H14 126.5 . . ? C22 C21 N3 121.2(8) . . ? C22 C21 C20 129.3(8) . . ? N3 C21 C20 109.3(8) . . ? C21 C22 C23 118.5(8) . . ? C21 C22 C59 118.2(8) . . ? C23 C22 C59 123.2(8) . . ? N4 C23 C22 123.7(8) . . ? N4 C23 C24 108.0(8) . . ? C22 C23 C24 128.2(8) . . ? C25 C24 C23 107.6(8) . . ? C25 C24 H15 126.2 . . ? C23 C24 H15 126.2 . . ? C24 C25 C26 106.8(8) . . ? C24 C25 H16 126.6 . . ? C26 C25 H16 126.6 . . ? N4 C26 C25 108.1(7) . . ? N4 C26 C27 128.9(8) . . ? C25 C26 C27 123.0(8) . . ? C35 C27 C28 116.1(8) . . ? C35 C27 C26 122.3(8) . . ? C28 C27 C26 121.4(8) . . ? C30 C28 O3 120.9(9) . . ? C30 C28 C27 120.6(9) . . ? O3 C28 C27 118.2(8) . . ? C28 O3 C29 111.7(7) . . ? O3 C29 H17 109.5 . . ? O3 C29 H18 109.5 . . ? H17 C29 H18 109.5 . . ? O3 C29 H19 109.5 . . ? H17 C29 H19 109.5 . . ? H18 C29 H19 109.5 . . ? C28 C30 C33 124.0(9) . . ? C28 C30 O4 118.3(9) . . ? C33 C30 O4 116.5(9) . . ? C32 O4 C31 110(2) . . ? C32 O4 C30 119.0(10) . . ? C31 O4 C30 123.5(17) . . ? O4 C31 H20 109.5 . . ? O4 C31 H21 109.5 . . ? H20 C31 H21 109.5 . . ? O4 C31 H22 109.5 . . ? H20 C31 H22 109.5 . . ? H21 C31 H22 109.5 . . ? O4 C32 H23 109.5 . . ? O4 C32 H24 109.5 . . ? H23 C32 H24 109.5 . . ? O4 C32 H25 109.5 . . ? H23 C32 H25 109.5 . . ? H24 C32 H25 109.5 . . ? C34 C33 C30 115.8(9) . . ? C34 C33 C36 124.4(9) . . ? C30 C33 C36 118.3(9) . . ? C33 C34 C35 121.0(8) . . ? C33 C34 H26 119.5 . . ? C35 C34 H26 119.5 . . ? C27 C35 C34 121.8(8) . . ? C27 C35 H27 119.1 . . ? C34 C35 H27 119.1 . . ? N5 C36 C37 107.8(7) . . ? N5 C36 C33 123.2(8) . . ? C37 C36 C33 129.0(8) . . ? C38 C37 C36 110.3(8) . . ? C38 C37 H28 124.9 . . ? C36 C37 H28 124.9 . . ? C37 C38 C39 106.3(8) . . ? C37 C38 H29 126.8 . . ? C39 C38 H29 126.8 . . ? C38 C39 C40 131.7(9) . . ? C38 C39 N5 109.1(8) . . ? C40 C39 N5 119.0(8) . . ? C39 C40 C41 123.9(8) . . ? C39 C40 C65 118.2(9) . . ? C41 C40 C65 117.8(8) . . ? C42 C41 N6 108.1(8) . . ? C42 C41 C40 132.8(10) . . ? N6 C41 C40 119.0(8) . . ? C43 C42 C41 108.2(9) . . ? C43 C42 H30 125.9 . . ? C41 C42 H30 125.9 . . ? C42 C43 C44 107.4(9) . . ? C42 C43 H31 126.3 . . ? C44 C43 H31 126.3 . . ? N6 C44 C43 111.1(8) . . ? N6 C44 C45 124.4(8) . . ? C43 C44 C45 124.5(9) . . ? C52 C45 C46 114.8(9) . . ? C52 C45 C44 127.4(9) . . ? C46 C45 C44 117.2(9) . . ? O5 C46 C48 118.4(10) . . ? O5 C46 C45 120.1(9) . . ? C48 C46 C45 121.3(10) . . ? C46 O5 C47 116.4(7) . . ? O5 C47 H32 109.5 . . ? O5 C47 H33 109.5 . . ? H32 C47 H33 109.5 . . ? O5 C47 H34 109.5 . . ? H32 C47 H34 109.5 . . ? H33 C47 H34 109.5 . . ? O6 C48 C50 120.0(10) . . ? O6 C48 C46 118.2(9) . . ? C50 C48 C46 121.7(10) . . ? C48 O6 C49 115.8(9) . . ? O6 C49 H35 109.5 . . ? O6 C49 H36 109.5 . . ? H35 C49 H36 109.5 . . ? O6 C49 H37 109.5 . . ? H35 C49 H37 109.5 . . ? H36 C49 H37 109.5 . . ? C48 C50 C51 117.5(9) . . ? C48 C50 C1 120.5(10) . . ? C51 C50 C1 121.9(9) . . ? C52 C51 C50 118.8(8) . . ? C52 C51 H38 120.6 . . ? C50 C51 H38 120.6 . . ? C45 C52 C51 125.5(9) . . ? C45 C52 H39 117.3 . . ? C51 C52 H39 117.3 . . ? C58 C53 C54 120.0(9) . . ? C58 C53 C5 124.0(9) . . ? C54 C53 C5 116.0(8) . . ? C55 C54 C53 118.4(9) . . ? C55 C54 H40 120.8 . . ? C53 C54 H40 120.8 . . ? C56 C55 C54 120.4(9) . . ? C56 C55 H41 119.8 . . ? C54 C55 H41 119.8 . . ? C55 C56 C57 120.4(10) . . ? C55 C56 H42 119.8 . . ? C57 C56 H42 119.8 . . ? C58 C57 C56 119.1(10) . . ? C58 C57 H43 120.5 . . ? C56 C57 H43 120.5 . . ? C53 C58 C57 121.7(9) . . ? C53 C58 H44 119.2 . . ? C57 C58 H44 119.2 . . ? C60 C59 C64 119.0(8) . . ? C60 C59 C22 120.9(9) . . ? C64 C59 C22 120.0(8) . . ? C59 C60 C61 122.3(9) . . ? C59 C60 H45 118.8 . . ? C61 C60 H45 118.8 . . ? C60 C61 C62 116.9(9) . . ? C60 C61 H46 121.6 . . ? C62 C61 H46 121.6 . . ? C63 C62 C61 120.4(9) . . ? C63 C62 H47 119.8 . . ? C61 C62 H47 119.8 . . ? C62 C63 C64 120.8(9) . . ? C62 C63 H48 119.6 . . ? C64 C63 H48 119.6 . . ? C59 C64 C63 120.4(9) . . ? C59 C64 H49 119.8 . . ? C63 C64 H49 119.8 . . ? C66 C65 C70 116.7(9) . . ? C66 C65 C40 121.6(9) . . ? C70 C65 C40 121.6(10) . . ? C67 C66 C65 121.3(11) . . ? C67 C66 H50 119.4 . . ? C65 C66 H50 119.4 . . ? C68 C67 C66 119.4(12) . . ? C68 C67 H51 120.3 . . ? C66 C67 H51 120.3 . . ? C67 C68 C69 123.2(12) . . ? C67 C68 H52 118.4 . . ? C69 C68 H52 118.4 . . ? C70 C69 C68 116.1(11) . . ? C70 C69 H53 122.0 . . ? C68 C69 H53 122.0 . . ? C69 C70 C65 123.2(10) . . ? C69 C70 H54 118.4 . . ? C65 C70 H54 118.4 . . ? Cl1 C71 Cl3 107.2(18) . . ? Cl1 C71 Cl2 93.2(13) . . ? Cl3 C71 Cl2 87.4(14) . . ? Cl1 C71 H55 120.5 . . ? Cl3 C71 H55 120.5 . . ? Cl2 C71 H55 120.5 . . ? Cl5 C72 Cl6 127.9(9) . . ? Cl5 C72 Cl4 113.1(8) . . ? Cl6 C72 Cl4 107.5(7) . . ? Cl5 C72 H59 101.3 . . ? Cl6 C72 H59 101.3 . . ? Cl4 C72 H59 101.3 . . ? Cl7 C73 Cl9 113.8(11) . . ? Cl7 C73 Cl8 106.1(11) . . ? Cl9 C73 Cl8 107.3(12) . . ? Cl7 C73 H56 109.8 . . ? Cl9 C73 H56 109.8 . . ? Cl8 C73 H56 109.8 . . ? Cl12 C74 Cl10 111.4(15) . . ? Cl12 C74 Cl11 103.5(14) . . ? Cl10 C74 Cl11 113.5(15) . . ? Cl12 C74 H57 109.4 . . ? Cl10 C74 H57 109.4 . . ? Cl11 C74 H57 109.4 . . ? Cl14 C75 Cl15 113.9(12) . . ? Cl14 C75 Cl13 109.8(11) . . ? Cl15 C75 Cl13 107.4(11) . . ? Cl14 C75 H60 108.6 . . ? Cl15 C75 H60 108.6 . . ? Cl13 C75 H60 108.6 . . ? Cl18 C76 Cl17 98.2(11) . . ? Cl18 C76 Cl16 99.8(10) . . ? Cl17 C76 Cl16 99.0(10) . . ? Cl18 C76 H58 118.6 . . ? Cl17 C76 H58 118.6 . . ? Cl16 C76 H58 118.6 . . ? Cl17 Cl16 C76 88.3(11) 3_565 . ? Cl16 Cl17 C76 134.1(11) 3_565 . ? C77 Cl18 C76 138.0(11) . . ? Cl19 C77 Cl18 108.6(14) . . ? Cl19 C77 Cl20 119.9(16) . . ? Cl18 C77 Cl20 106.9(13) . . ? Cl19 C77 H61 106.9 . . ? Cl18 C77 H61 106.9 . . ? Cl20 C77 H61 106.9 . . ? 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 F1 B1 N1 C1 45.5(12) . . . . ? F2 B1 N1 C1 -74.2(11) . . . . ? N2 B1 N1 C1 165.6(7) . . . . ? F1 B1 N1 C4 -135.1(7) . . . . ? F2 B1 N1 C4 105.3(8) . . . . ? N2 B1 N1 C4 -15.0(11) . . . . ? F1 B1 N2 C9 -63.1(11) . . . . ? F2 B1 N2 C9 56.3(11) . . . . ? N1 B1 N2 C9 178.3(7) . . . . ? F1 B1 N2 C6 136.1(8) . . . . ? F2 B1 N2 C6 -104.5(9) . . . . ? N1 B1 N2 C6 17.6(11) . . . . ? F3 B2 N3 C18 -40.3(11) . . . . ? F4 B2 N3 C18 80.9(10) . . . . ? N4 B2 N3 C18 -161.0(7) . . . . ? F3 B2 N3 C21 131.1(8) . . . . ? F4 B2 N3 C21 -107.7(8) . . . . ? N4 B2 N3 C21 10.4(11) . . . . ? F3 B2 N4 C26 52.5(12) . . . . ? F4 B2 N4 C26 -74.6(10) . . . . ? N3 B2 N4 C26 170.4(7) . . . . ? F3 B2 N4 C23 -132.2(8) . . . . ? F4 B2 N4 C23 100.7(9) . . . . ? N3 B2 N4 C23 -14.3(11) . . . . ? F6 B3 N5 C36 -47.1(12) . . . . ? F5 B3 N5 C36 70.5(11) . . . . ? N6 B3 N5 C36 -172.9(7) . . . . ? F6 B3 N5 C39 134.7(8) . . . . ? F5 B3 N5 C39 -107.8(8) . . . . ? N6 B3 N5 C39 8.8(11) . . . . ? F6 B3 N6 C44 53.7(13) . . . . ? F5 B3 N6 C44 -65.3(12) . . . . ? N5 B3 N6 C44 179.1(8) . . . . ? F6 B3 N6 C41 -128.0(9) . . . . ? F5 B3 N6 C41 113.0(9) . . . . ? N5 B3 N6 C41 -2.6(12) . . . . ? C4 N1 C1 C2 1.6(9) . . . . ? B1 N1 C1 C2 -178.9(8) . . . . ? C4 N1 C1 C50 -179.6(8) . . . . ? B1 N1 C1 C50 -0.1(14) . . . . ? N1 C1 C2 C3 -0.9(10) . . . . ? C50 C1 C2 C3 -179.8(7) . . . . ? C1 C2 C3 C4 -0.1(10) . . . . ? C2 C3 C4 C5 171.7(9) . . . . ? C2 C3 C4 N1 1.0(10) . . . . ? C1 N1 C4 C5 -173.5(8) . . . . ? B1 N1 C4 C5 6.9(12) . . . . ? C1 N1 C4 C3 -1.5(8) . . . . ? B1 N1 C4 C3 178.9(7) . . . . ? C3 C4 C5 C6 -168.3(9) . . . . ? N1 C4 C5 C6 1.1(13) . . . . ? C3 C4 C5 C53 11.0(14) . . . . ? N1 C4 C5 C53 -179.6(7) . . . . ? C4 C5 C6 C7 -174.6(8) . . . . ? C53 C5 C6 C7 6.0(15) . . . . ? C4 C5 C6 N2 1.6(13) . . . . ? C53 C5 C6 N2 -177.7(8) . . . . ? C9 N2 C6 C5 -175.9(8) . . . . ? B1 N2 C6 C5 -12.2(12) . . . . ? C9 N2 C6 C7 1.1(9) . . . . ? B1 N2 C6 C7 164.8(7) . . . . ? C5 C6 C7 C8 175.5(9) . . . . ? N2 C6 C7 C8 -1.2(9) . . . . ? C6 C7 C8 C9 0.9(9) . . . . ? C6 N2 C9 C8 -0.5(9) . . . . ? B1 N2 C9 C8 -163.3(7) . . . . ? C6 N2 C9 C10 -176.9(7) . . . . ? B1 N2 C9 C10 20.3(13) . . . . ? C7 C8 C9 N2 -0.2(10) . . . . ? C7 C8 C9 C10 176.3(7) . . . . ? N2 C9 C10 C11 -131.2(9) . . . . ? C8 C9 C10 C11 52.9(11) . . . . ? N2 C9 C10 C17 56.1(12) . . . . ? C8 C9 C10 C17 -119.8(9) . . . . ? C17 C10 C11 C13 0.6(12) . . . . ? C9 C10 C11 C13 -172.4(7) . . . . ? C17 C10 C11 O1 178.2(7) . . . . ? C9 C10 C11 O1 5.2(12) . . . . ? C13 C11 O1 C12 -105.4(9) . . . . ? C10 C11 O1 C12 76.9(10) . . . . ? C10 C11 C13 O2 179.5(7) . . . . ? O1 C11 C13 O2 1.8(12) . . . . ? C10 C11 C13 C15 3.9(12) . . . . ? O1 C11 C13 C15 -173.8(7) . . . . ? C11 C13 O2 C14 89.9(10) . . . . ? C15 C13 O2 C14 -94.6(9) . . . . ? C11 C13 C15 C16 -5.9(11) . . . . ? O2 C13 C15 C16 178.4(7) . . . . ? C11 C13 C15 C18 165.0(7) . . . . ? O2 C13 C15 C18 -10.7(11) . . . . ? C13 C15 C16 C17 3.7(11) . . . . ? C18 C15 C16 C17 -166.7(7) . . . . ? C15 C16 C17 C10 0.8(11) . . . . ? C11 C10 C17 C16 -3.0(11) . . . . ? C9 C10 C17 C16 169.9(7) . . . . ? C21 N3 C18 C19 1.7(8) . . . . ? B2 N3 C18 C19 174.4(7) . . . . ? C21 N3 C18 C15 172.4(7) . . . . ? B2 N3 C18 C15 -15.0(12) . . . . ? C16 C15 C18 N3 -48.6(11) . . . . ? C13 C15 C18 N3 141.0(8) . . . . ? C16 C15 C18 C19 120.8(9) . . . . ? C13 C15 C18 C19 -49.6(10) . . . . ? N3 C18 C19 C20 -0.6(9) . . . . ? C15 C18 C19 C20 -171.7(7) . . . . ? C18 C19 C20 C21 -0.7(9) . . . . ? C18 N3 C21 C22 173.0(7) . . . . ? B2 N3 C21 C22 0.0(12) . . . . ? C18 N3 C21 C20 -2.2(8) . . . . ? B2 N3 C21 C20 -175.1(7) . . . . ? C19 C20 C21 C22 -172.8(8) . . . . ? C19 C20 C21 N3 1.8(9) . . . . ? N3 C21 C22 C23 -8.6(11) . . . . ? C20 C21 C22 C23 165.4(8) . . . . ? N3 C21 C22 C59 176.2(7) . . . . ? C20 C21 C22 C59 -9.7(13) . . . . ? C26 N4 C23 C22 -175.9(8) . . . . ? B2 N4 C23 C22 8.2(13) . . . . ? C26 N4 C23 C24 0.5(9) . . . . ? B2 N4 C23 C24 -175.4(7) . . . . ? C21 C22 C23 N4 4.9(12) . . . . ? C59 C22 C23 N4 179.8(7) . . . . ? C21 C22 C23 C24 -170.8(8) . . . . ? C59 C22 C23 C24 4.1(14) . . . . ? N4 C23 C24 C25 -1.4(9) . . . . ? C22 C23 C24 C25 174.9(8) . . . . ? C23 C24 C25 C26 1.6(10) . . . . ? C23 N4 C26 C25 0.5(9) . . . . ? B2 N4 C26 C25 176.4(7) . . . . ? C23 N4 C26 C27 179.6(8) . . . . ? B2 N4 C26 C27 -4.4(14) . . . . ? C24 C25 C26 N4 -1.3(10) . . . . ? C24 C25 C26 C27 179.5(8) . . . . ? N4 C26 C27 C35 57.5(13) . . . . ? C25 C26 C27 C35 -123.4(9) . . . . ? N4 C26 C27 C28 -126.9(9) . . . . ? C25 C26 C27 C28 52.1(12) . . . . ? C35 C27 C28 C30 8.0(12) . . . . ? C26 C27 C28 C30 -167.7(8) . . . . ? C35 C27 C28 O3 -177.9(7) . . . . ? C26 C27 C28 O3 6.4(12) . . . . ? C30 C28 O3 C29 -103.8(10) . . . . ? C27 C28 O3 C29 82.1(10) . . . . ? O3 C28 C30 C33 177.7(8) . . . . ? C27 C28 C30 C33 -8.3(14) . . . . ? O3 C28 C30 O4 10.6(13) . . . . ? C27 C28 C30 O4 -175.4(7) . . . . ? C28 C30 O4 C32 -56.6(14) . . . . ? C33 C30 O4 C32 135.4(11) . . . . ? C28 C30 O4 C31 91(2) . . . . ? C33 C30 O4 C31 -77(3) . . . . ? C28 C30 C33 C34 5.9(13) . . . . ? O4 C30 C33 C34 173.2(7) . . . . ? C28 C30 C33 C36 172.8(8) . . . . ? O4 C30 C33 C36 -19.9(12) . . . . ? C30 C33 C34 C35 -3.9(12) . . . . ? C36 C33 C34 C35 -169.8(7) . . . . ? C28 C27 C35 C34 -6.3(11) . . . . ? C26 C27 C35 C34 169.5(7) . . . . ? C33 C34 C35 C27 4.4(12) . . . . ? C39 N5 C36 C37 3.1(9) . . . . ? B3 N5 C36 C37 -175.4(8) . . . . ? C39 N5 C36 C33 -174.3(8) . . . . ? B3 N5 C36 C33 7.3(14) . . . . ? C34 C33 C36 N5 -62.5(12) . . . . ? C30 C33 C36 N5 131.9(9) . . . . ? C34 C33 C36 C37 120.8(10) . . . . ? C30 C33 C36 C37 -44.9(13) . . . . ? N5 C36 C37 C38 -2.4(10) . . . . ? C33 C36 C37 C38 174.7(9) . . . . ? C36 C37 C38 C39 0.7(10) . . . . ? C37 C38 C39 C40 -173.2(9) . . . . ? C37 C38 C39 N5 1.2(10) . . . . ? C36 N5 C39 C38 -2.7(9) . . . . ? B3 N5 C39 C38 175.9(7) . . . . ? C36 N5 C39 C40 172.6(7) . . . . ? B3 N5 C39 C40 -8.8(11) . . . . ? C38 C39 C40 C41 175.8(9) . . . . ? N5 C39 C40 C41 1.8(12) . . . . ? C38 C39 C40 C65 -1.7(14) . . . . ? N5 C39 C40 C65 -175.7(7) . . . . ? C44 N6 C41 C42 -2.9(9) . . . . ? B3 N6 C41 C42 178.4(8) . . . . ? C44 N6 C41 C40 175.1(8) . . . . ? B3 N6 C41 C40 -3.6(12) . . . . ? C39 C40 C41 C42 -178.2(9) . . . . ? C65 C40 C41 C42 -0.8(14) . . . . ? C39 C40 C41 N6 4.4(12) . . . . ? C65 C40 C41 N6 -178.2(8) . . . . ? N6 C41 C42 C43 1.7(11) . . . . ? C40 C41 C42 C43 -175.9(9) . . . . ? C41 C42 C43 C44 0.1(11) . . . . ? C41 N6 C44 C43 3.0(10) . . . . ? B3 N6 C44 C43 -178.4(9) . . . . ? C41 N6 C44 C45 -176.0(8) . . . . ? B3 N6 C44 C45 2.6(15) . . . . ? C42 C43 C44 N6 -2.1(11) . . . . ? C42 C43 C44 C45 177.0(9) . . . . ? N6 C44 C45 C52 -67.0(13) . . . . ? C43 C44 C45 C52 114.1(11) . . . . ? N6 C44 C45 C46 122.8(9) . . . . ? C43 C44 C45 C46 -56.1(13) . . . . ? C52 C45 C46 O5 179.4(7) . . . . ? C44 C45 C46 O5 -9.1(12) . . . . ? C52 C45 C46 C48 -5.4(12) . . . . ? C44 C45 C46 C48 166.1(8) . . . . ? C48 C46 O5 C47 119.5(9) . . . . ? C45 C46 O5 C47 -65.2(11) . . . . ? O5 C46 C48 O6 -2.1(13) . . . . ? C45 C46 C48 O6 -177.4(8) . . . . ? O5 C46 C48 C50 176.2(8) . . . . ? C45 C46 C48 C50 0.9(13) . . . . ? C50 C48 O6 C49 93.9(11) . . . . ? C46 C48 O6 C49 -87.7(11) . . . . ? O6 C48 C50 C51 -177.8(8) . . . . ? C46 C48 C50 C51 3.9(12) . . . . ? O6 C48 C50 C1 6.5(13) . . . . ? C46 C48 C50 C1 -171.8(8) . . . . ? N1 C1 C50 C48 -146.0(9) . . . . ? C2 C1 C50 C48 32.7(12) . . . . ? N1 C1 C50 C51 38.4(12) . . . . ? C2 C1 C50 C51 -142.9(8) . . . . ? C48 C50 C51 C52 -4.0(11) . . . . ? C1 C50 C51 C52 171.7(7) . . . . ? C46 C45 C52 C51 5.4(12) . . . . ? C44 C45 C52 C51 -165.0(8) . . . . ? C50 C51 C52 C45 -0.8(11) . . . . ? C6 C5 C53 C58 -130.7(10) . . . . ? C4 C5 C53 C58 49.9(12) . . . . ? C6 C5 C53 C54 47.2(12) . . . . ? C4 C5 C53 C54 -132.1(9) . . . . ? C58 C53 C54 C55 -3.3(13) . . . . ? C5 C53 C54 C55 178.6(8) . . . . ? C53 C54 C55 C56 3.6(13) . . . . ? C54 C55 C56 C57 -2.6(14) . . . . ? C55 C56 C57 C58 1.3(15) . . . . ? C54 C53 C58 C57 2.1(14) . . . . ? C5 C53 C58 C57 180.0(8) . . . . ? C56 C57 C58 C53 -1.1(14) . . . . ? C21 C22 C59 C60 121.2(9) . . . . ? C23 C22 C59 C60 -53.7(12) . . . . ? C21 C22 C59 C64 -61.9(11) . . . . ? C23 C22 C59 C64 123.2(10) . . . . ? C64 C59 C60 C61 3.2(14) . . . . ? C22 C59 C60 C61 -179.9(9) . . . . ? C59 C60 C61 C62 -3.2(15) . . . . ? C60 C61 C62 C63 1.9(15) . . . . ? C61 C62 C63 C64 -0.7(15) . . . . ? C60 C59 C64 C63 -1.7(13) . . . . ? C22 C59 C64 C63 -178.7(8) . . . . ? C62 C63 C64 C59 0.5(14) . . . . ? C39 C40 C65 C66 57.4(12) . . . . ? C41 C40 C65 C66 -120.2(10) . . . . ? C39 C40 C65 C70 -125.5(9) . . . . ? C41 C40 C65 C70 56.9(11) . . . . ? C70 C65 C66 C67 1.4(15) . . . . ? C40 C65 C66 C67 178.7(10) . . . . ? C65 C66 C67 C68 -2.1(19) . . . . ? C66 C67 C68 C69 3(2) . . . . ? C67 C68 C69 C70 -4.0(18) . . . . ? C68 C69 C70 C65 3.3(14) . . . . ? C66 C65 C70 C69 -2.2(13) . . . . ? C40 C65 C70 C69 -179.5(8) . . . . ? Cl18 C76 Cl16 Cl17 -145.6(12) . . . 3_565 ? Cl17 C76 Cl16 Cl17 -45.5(12) . . . 3_565 ? Cl18 C76 Cl17 Cl16 -175.1(14) . . . 3_565 ? Cl16 C76 Cl17 Cl16 83.6(17) . . . 3_565 ? Cl17 C76 Cl18 C77 93(2) . . . . ? Cl16 C76 Cl18 C77 -166.2(17) . . . . ? C76 Cl18 C77 Cl19 49(3) . . . . ? C76 Cl18 C77 Cl20 179.4(12) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.515 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.062 # Attachment '- pseudorotaxane_2+3.CIF' # Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_2+3 #TrackingRef '- pseudorotaxane_2+3.CIF' _database_code_depnum_ccdc_archive 'CCDC 767041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H79 B3 F12 N7 O6 P' _chemical_formula_weight 1573.94 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.3798(13) _cell_length_b 15.9613(15) _cell_length_c 19.3185(17) _cell_angle_alpha 90.00 _cell_angle_beta 102.479(3) _cell_angle_gamma 90.00 _cell_volume 3727.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1636 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9504 _exptl_absorpt_correction_T_max 0.9873 _exptl_absorpt_process_details scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAC Science DIP-2030' _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29402 _diffrn_reflns_av_R_equivalents 0.1331 _diffrn_reflns_av_sigmaI/netI 0.1884 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13051 _reflns_number_gt 5335 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+2.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(4) _refine_ls_number_reflns 13051 _refine_ls_number_parameters 978 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.2206 _refine_ls_R_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.2641 _refine_ls_wR_factor_gt 0.1916 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.294 _refine_ls_shift/su_mean 0.011 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 0.5540(8) -0.1217(6) 0.3708(4) 0.048(2) Uani 1 1 d . . . C2 C 0.5059(9) -0.1959(6) 0.3802(5) 0.057(3) Uani 1 1 d . . . H1 H 0.4748 -0.2103 0.4195 0.068 Uiso 1 1 calc R . . C3 C 0.5097(9) -0.2463(6) 0.3238(4) 0.050(3) Uani 1 1 d . . . H2 H 0.4851 -0.3027 0.3175 0.060 Uiso 1 1 calc R . . C4 C 0.5567(8) -0.1990(5) 0.2774(4) 0.040(2) Uani 1 1 d . . . C5 C 0.5651(8) -0.2147(5) 0.2071(4) 0.043(2) Uani 1 1 d . . . C6 C 0.5924(8) -0.1530(5) 0.1630(4) 0.045(2) Uani 1 1 d . . . C7 C 0.5982(9) -0.1530(6) 0.0910(5) 0.051(3) Uani 1 1 d . . . H3 H 0.5909 -0.2001 0.0603 0.061 Uiso 1 1 calc R . . C8 C 0.6162(9) -0.0722(6) 0.0738(5) 0.052(3) Uani 1 1 d . . . H4 H 0.6234 -0.0532 0.0284 0.063 Uiso 1 1 calc R . . C9 C 0.6227(8) -0.0208(6) 0.1345(4) 0.046(2) Uani 1 1 d . . . C10 C 0.6385(9) 0.0701(6) 0.1370(4) 0.042(2) Uani 1 1 d . . . C11 C 0.5501(9) 0.1211(7) 0.1089(5) 0.050(3) Uani 1 1 d . . . C12 C 0.5666(9) 0.2069(6) 0.1050(5) 0.048(3) Uani 1 1 d . . . C13 C 0.6701(8) 0.2433(5) 0.1275(4) 0.041(2) Uani 1 1 d . . . C14 C 0.7564(8) 0.1902(6) 0.1533(4) 0.047(2) Uani 1 1 d . . . H5 H 0.8288 0.2128 0.1675 0.056 Uiso 1 1 calc R . . C15 C 0.7417(10) 0.1039(6) 0.1595(5) 0.058(3) Uani 1 1 d . . . H6 H 0.8029 0.0691 0.1792 0.070 Uiso 1 1 calc R . . O1 O 0.4469(6) 0.0899(4) 0.0795(3) 0.061(2) Uani 1 1 d . . . C16 C 0.3863(12) 0.0503(8) 0.1226(6) 0.086(4) Uani 1 1 d . . . H7 H 0.4060 -0.0092 0.1269 0.128 Uiso 1 1 calc R . . H8 H 0.3071 0.0560 0.1018 0.128 Uiso 1 1 calc R . . H9 H 0.4029 0.0763 0.1697 0.128 Uiso 1 1 calc R . . O2 O 0.4786(7) 0.2594(5) 0.0714(4) 0.069(2) Uani 1 1 d . . . C17 C 0.3920(13) 0.2710(10) 0.1073(7) 0.114(6) Uani 1 1 d . . . H10 H 0.3636 0.2163 0.1181 0.171 Uiso 1 1 calc R . . H11 H 0.3323 0.3031 0.0772 0.171 Uiso 1 1 calc R . . H12 H 0.4198 0.3016 0.1515 0.171 Uiso 1 1 calc R . . C18 C 0.6880(8) 0.3315(5) 0.1151(4) 0.041(2) Uani 1 1 d . . . C19 C 0.6478(8) 0.3762(6) 0.0512(4) 0.047(2) Uani 1 1 d . . . H13 H 0.5990 0.3549 0.0101 0.056 Uiso 1 1 calc R . . C20 C 0.6915(8) 0.4552(6) 0.0589(4) 0.049(3) Uani 1 1 d . . . H14 H 0.6788 0.4981 0.0240 0.059 Uiso 1 1 calc R . . C21 C 0.7581(8) 0.4618(6) 0.1271(4) 0.041(2) Uani 1 1 d . . . C22 C 0.8220(7) 0.5275(6) 0.1602(4) 0.040(2) Uani 1 1 d . . . C23 C 0.8755(8) 0.5207(6) 0.2326(4) 0.047(2) Uani 1 1 d . . . C24 C 0.9521(9) 0.5732(7) 0.2748(5) 0.063(3) Uani 1 1 d . . . H15 H 0.9802 0.6243 0.2605 0.076 Uiso 1 1 calc R . . C25 C 0.9798(9) 0.5371(7) 0.3415(5) 0.064(3) Uani 1 1 d . . . H16 H 1.0322 0.5580 0.3811 0.077 Uiso 1 1 calc R . . C26 C 0.9164(9) 0.4642(6) 0.3399(4) 0.049(3) Uani 1 1 d . . . C27 C 0.9124(8) 0.4114(5) 0.4037(4) 0.038(2) Uani 1 1 d . . . C28 C 1.0070(8) 0.3863(6) 0.4480(4) 0.046(2) Uani 1 1 d . . . C29 C 1.0034(9) 0.3584(5) 0.5164(4) 0.042(2) Uani 1 1 d . . . C30 C 0.9032(9) 0.3522(5) 0.5371(4) 0.045(3) Uani 1 1 d . . . C31 C 0.8054(8) 0.3744(5) 0.4903(4) 0.044(2) Uani 1 1 d . . . H17 H 0.7365 0.3688 0.5040 0.053 Uiso 1 1 calc R . . C32 C 0.8092(8) 0.4049(5) 0.4231(4) 0.042(2) Uani 1 1 d . . . H18 H 0.7431 0.4210 0.3908 0.050 Uiso 1 1 calc R . . O3 O 1.1078(6) 0.3917(5) 0.4302(3) 0.063(2) Uani 1 1 d . . . C33 C 1.1230(15) 0.3574(10) 0.3647(7) 0.120(6) Uani 1 1 d . . . H19 H 1.1786 0.3128 0.3742 0.181 Uiso 1 1 calc R . . H20 H 1.1481 0.4016 0.3366 0.181 Uiso 1 1 calc R . . H21 H 1.0528 0.3344 0.3382 0.181 Uiso 1 1 calc R . . O4 O 1.1026(6) 0.3438(4) 0.5637(3) 0.0536(18) Uani 1 1 d . . . C34 C 1.1367(15) 0.2620(8) 0.5790(10) 0.159(9) Uani 1 1 d . . . H22 H 1.0728 0.2274 0.5829 0.239 Uiso 1 1 calc R . . H23 H 1.1915 0.2605 0.6239 0.239 Uiso 1 1 calc R . . H24 H 1.1699 0.2402 0.5409 0.239 Uiso 1 1 calc R . . C35 C 0.9007(8) 0.3344(5) 0.6120(4) 0.040(2) Uani 1 1 d . . . C36 C 0.9602(8) 0.3785(6) 0.6719(4) 0.048(3) Uani 1 1 d . . . H25 H 1.0122 0.4222 0.6716 0.058 Uiso 1 1 calc R . . C37 C 0.9280(9) 0.3457(6) 0.7316(4) 0.051(3) Uani 1 1 d . . . H26 H 0.9537 0.3625 0.7795 0.062 Uiso 1 1 calc R . . C38 C 0.8520(7) 0.2846(5) 0.7069(4) 0.036(2) Uani 1 1 d . . . C39 C 0.8031(8) 0.2265(5) 0.7452(4) 0.041(2) Uani 1 1 d . . . C40 C 0.7434(8) 0.1571(6) 0.7117(4) 0.041(2) Uani 1 1 d . . . C41 C 0.6814(9) 0.0982(5) 0.7390(5) 0.048(3) Uani 1 1 d . . . H27 H 0.6752 0.0930 0.7869 0.057 Uiso 1 1 calc R . . C42 C 0.6301(9) 0.0480(6) 0.6821(5) 0.055(3) Uani 1 1 d . . . H28 H 0.5825 0.0020 0.6846 0.066 Uiso 1 1 calc R . . C43 C 0.6609(8) 0.0773(5) 0.6204(4) 0.042(2) Uani 1 1 d . . . C44 C 0.6309(9) 0.0410(6) 0.5508(4) 0.042(2) Uani 1 1 d . . . C45 C 0.5207(10) 0.0198(6) 0.5222(4) 0.050(3) Uani 1 1 d . . . C46 C 0.4962(11) -0.0258(6) 0.4574(5) 0.061(3) Uani 1 1 d . . . C47 C 0.5763(9) -0.0522(6) 0.4236(5) 0.045(2) Uani 1 1 d . . . C48 C 0.6837(9) -0.0278(6) 0.4501(4) 0.051(3) Uani 1 1 d . . . H29 H 0.7401 -0.0434 0.4262 0.062 Uiso 1 1 calc R . . C49 C 0.7102(9) 0.0199(5) 0.5121(4) 0.047(2) Uani 1 1 d . . . H30 H 0.7842 0.0385 0.5285 0.057 Uiso 1 1 calc R . . O5 O 0.4414(6) 0.0359(4) 0.5595(3) 0.0551(18) Uani 1 1 d . . . C50 C 0.3634(10) 0.0990(7) 0.5302(6) 0.070(3) Uani 1 1 d . . . H31 H 0.4026 0.1511 0.5249 0.105 Uiso 1 1 calc R . . H32 H 0.3125 0.1085 0.5619 0.105 Uiso 1 1 calc R . . H33 H 0.3215 0.0807 0.4837 0.105 Uiso 1 1 calc R . . O6 O 0.3864(6) -0.0507(4) 0.4351(3) 0.0562(18) Uani 1 1 d . . . C51 C 0.3305(10) -0.0277(7) 0.3640(5) 0.069(3) Uani 1 1 d . . . H34 H 0.3230 0.0334 0.3607 0.103 Uiso 1 1 calc R . . H35 H 0.2569 -0.0534 0.3528 0.103 Uiso 1 1 calc R . . H36 H 0.3736 -0.0474 0.3302 0.103 Uiso 1 1 calc R . . N1 N 0.5827(6) -0.1188(4) 0.3062(3) 0.0426(19) Uani 1 1 d . . . N2 N 0.6105(6) -0.0701(4) 0.1893(3) 0.043(2) Uani 1 1 d . . . B1 B 0.6292(11) -0.0477(7) 0.2676(5) 0.049(3) Uani 1 1 d . . . F1 F 0.7419(5) -0.0378(4) 0.2960(3) 0.0699(18) Uani 1 1 d . . . F2 F 0.5775(5) 0.0276(3) 0.2776(2) 0.0646(17) Uani 1 1 d . . . N3 N 0.7573(7) 0.3847(5) 0.1626(3) 0.0442(19) Uani 1 1 d . . . N4 N 0.8527(6) 0.4537(4) 0.2735(3) 0.0398(18) Uani 1 1 d . . . B2 B 0.7868(11) 0.3749(7) 0.2434(5) 0.047(3) Uani 1 1 d . . . F3 F 0.8535(6) 0.3058(3) 0.2651(3) 0.083(2) Uani 1 1 d . . . F4 F 0.6924(6) 0.3671(4) 0.2692(2) 0.0719(19) Uani 1 1 d . . . N5 N 0.8356(6) 0.2764(4) 0.6334(3) 0.0378(18) Uani 1 1 d . . . N6 N 0.7309(6) 0.1431(4) 0.6386(3) 0.0410(19) Uani 1 1 d . . . B3 B 0.7746(9) 0.2045(6) 0.5882(5) 0.035(2) Uani 1 1 d . . . F5 F 0.8501(4) 0.1660(3) 0.5547(2) 0.0482(13) Uani 1 1 d . . . F6 F 0.6847(4) 0.2315(3) 0.5366(2) 0.0458(13) Uani 1 1 d . . . C52 C 0.5395(8) -0.3015(6) 0.1791(5) 0.052(3) Uani 1 1 d . . . C53 C 0.4672(8) -0.3158(6) 0.1159(4) 0.044(2) Uani 1 1 d . . . H37 H 0.4324 -0.2691 0.0896 0.053 Uiso 1 1 calc R . . C54 C 0.4429(10) -0.3951(7) 0.0889(6) 0.066(3) Uani 1 1 d . . . H38 H 0.3937 -0.4036 0.0444 0.079 Uiso 1 1 calc R . . C55 C 0.4929(9) -0.4622(7) 0.1292(6) 0.065(3) Uani 1 1 d . . . H39 H 0.4777 -0.5173 0.1111 0.078 Uiso 1 1 calc R . . C56 C 0.5643(9) -0.4523(6) 0.1949(6) 0.059(3) Uani 1 1 d . . . H40 H 0.5955 -0.4993 0.2222 0.071 Uiso 1 1 calc R . . C57 C 0.5885(8) -0.3710(6) 0.2193(5) 0.048(2) Uani 1 1 d . . . H41 H 0.6384 -0.3620 0.2635 0.057 Uiso 1 1 calc R . . C58 C 0.8355(9) 0.6049(6) 0.1202(5) 0.051(3) Uani 1 1 d . . . C59 C 0.8568(9) 0.6007(6) 0.0547(5) 0.055(3) Uani 1 1 d . . . H42 H 0.8628 0.5480 0.0330 0.066 Uiso 1 1 calc R . . C60 C 0.8702(10) 0.6765(8) 0.0185(6) 0.073(3) Uani 1 1 d . . . H43 H 0.8839 0.6744 -0.0280 0.088 Uiso 1 1 calc R . . C61 C 0.8635(10) 0.7529(8) 0.0506(8) 0.079(4) Uani 1 1 d . . . H44 H 0.8724 0.8034 0.0264 0.095 Uiso 1 1 calc R . . C62 C 0.8439(9) 0.7555(7) 0.1176(7) 0.071(3) Uani 1 1 d . . . H45 H 0.8398 0.8082 0.1398 0.085 Uiso 1 1 calc R . . C63 C 0.8300(8) 0.6831(6) 0.1534(5) 0.055(3) Uani 1 1 d . . . H46 H 0.8169 0.6857 0.2000 0.066 Uiso 1 1 calc R . . C64 C 0.8100(7) 0.2384(6) 0.8219(4) 0.041(2) Uani 1 1 d . . . C65 C 0.8470(8) 0.1737(6) 0.8710(4) 0.047(2) Uani 1 1 d . . . H47 H 0.8692 0.1212 0.8555 0.057 Uiso 1 1 calc R . . C66 C 0.8504(9) 0.1882(7) 0.9430(5) 0.060(3) Uani 1 1 d . . . H48 H 0.8744 0.1447 0.9763 0.072 Uiso 1 1 calc R . . C67 C 0.8205(10) 0.2621(7) 0.9658(5) 0.062(3) Uani 1 1 d . . . H49 H 0.8228 0.2701 1.0148 0.075 Uiso 1 1 calc R . . C68 C 0.7862(10) 0.3273(7) 0.9185(5) 0.069(3) Uiso 1 1 d . . . H50 H 0.7659 0.3796 0.9353 0.083 Uiso 1 1 calc R . . C69 C 0.7814(9) 0.3157(6) 0.8460(4) 0.052(3) Uani 1 1 d . . . H51 H 0.7588 0.3603 0.8135 0.062 Uiso 1 1 calc R . . N7 N 0.7158(7) 0.1755(5) 0.3297(4) 0.061(2) Uani 1 1 d . . . H70 H 0.7232 0.2145 0.2960 0.073 Uiso 1 1 calc R . . H71 H 0.6966 0.1253 0.3069 0.073 Uiso 1 1 calc R . . C70 C 0.8271(9) 0.1654(7) 0.3822(5) 0.059(3) Uani 1 1 d . . . H52 H 0.8525 0.2207 0.4026 0.070 Uiso 1 1 calc R . . H53 H 0.8175 0.1284 0.4216 0.070 Uiso 1 1 calc R . . C71 C 0.9125(9) 0.1292(8) 0.3474(6) 0.068(3) Uani 1 1 d . . . H54 H 0.9182 0.1645 0.3063 0.082 Uiso 1 1 calc R . . H55 H 0.8882 0.0727 0.3293 0.082 Uiso 1 1 calc R . . C72 C 1.0279(13) 0.1221(8) 0.3971(7) 0.096(5) Uani 1 1 d . . . H56 H 1.0791 0.0947 0.3712 0.115 Uiso 1 1 calc R . . H57 H 1.0566 0.1792 0.4104 0.115 Uiso 1 1 calc R . . C73 C 1.0266(13) 0.0764(9) 0.4591(7) 0.099(5) Uani 1 1 d . . . H58 H 0.9878 0.1087 0.4894 0.149 Uiso 1 1 calc R . . H59 H 1.1027 0.0656 0.4847 0.149 Uiso 1 1 calc R . . H60 H 0.9884 0.0230 0.4465 0.149 Uiso 1 1 calc R . . C74 C 0.6252(9) 0.2026(7) 0.3653(5) 0.061(3) Uani 1 1 d . . . H61 H 0.6109 0.1570 0.3969 0.073 Uiso 1 1 calc R . . H62 H 0.6508 0.2521 0.3953 0.073 Uiso 1 1 calc R . . C75 C 0.5209(10) 0.2238(7) 0.3156(5) 0.068(3) Uani 1 1 d . . . H63 H 0.4997 0.1768 0.2819 0.082 Uiso 1 1 calc R . . H64 H 0.5329 0.2738 0.2879 0.082 Uiso 1 1 calc R . . C76 C 0.4280(11) 0.2410(9) 0.3518(7) 0.097(5) Uani 1 1 d . . . H65 H 0.3589 0.2497 0.3157 0.116 Uiso 1 1 calc R . . H66 H 0.4172 0.1919 0.3809 0.116 Uiso 1 1 calc R . . C77 C 0.4514(15) 0.3173(10) 0.3984(8) 0.137(7) Uani 1 1 d . . . H67 H 0.5035 0.3026 0.4425 0.206 Uiso 1 1 calc R . . H68 H 0.3823 0.3377 0.4092 0.206 Uiso 1 1 calc R . . H69 H 0.4837 0.3612 0.3737 0.206 Uiso 1 1 calc R . . P1 P 1.1117(5) 0.1118(4) 0.1976(3) 0.066(2) Uiso 0.586(13) 1 d PD A 1 F7 F 1.0108(10) 0.1490(8) 0.1369(7) 0.117(6) Uiso 0.586(13) 1 d PD A 1 F8 F 1.0816(12) 0.1881(8) 0.2451(6) 0.142(6) Uiso 0.586(13) 1 d PD A 1 F9 F 1.1325(11) 0.0353(7) 0.1461(7) 0.118(5) Uiso 0.586(13) 1 d PD A 1 F10 F 1.2015(10) 0.0849(9) 0.2594(6) 0.132(6) Uiso 0.586(13) 1 d PD A 1 F11 F 1.0233(8) 0.0534(7) 0.2236(6) 0.085(4) Uiso 0.586(13) 1 d PD A 1 F12 F 1.1854(6) 0.1615(5) 0.1641(4) 0.119(3) Uiso 1 1 d D . . P2 P 1.0853(9) 0.0814(7) 0.1680(6) 0.094(4) Uiso 0.414(13) 1 d PD A 2 F13 F 1.0535(18) 0.1358(14) 0.2280(10) 0.237(17) Uiso 0.414(13) 1 d PD A 2 F14 F 1.1836(12) 0.0336(10) 0.2209(9) 0.116(8) Uiso 0.414(13) 1 d PD A 2 F15 F 0.9949(12) 0.1244(11) 0.1100(9) 0.109(7) Uiso 0.414(13) 1 d PD A 2 F16 F 1.0003(14) 0.0101(12) 0.1768(12) 0.165(11) Uiso 0.414(13) 1 d PD A 2 F17 F 1.1213(14) 0.0346(10) 0.1044(9) 0.133(9) Uiso 0.414(13) 1 d PD A 2 C78 C 0.9000(12) 0.9523(10) 0.9633(7) 0.115(5) Uiso 1 1 d D . . C79 C 0.9850(11) 0.9051(10) 0.9395(8) 0.125(6) Uiso 1 1 d D . . H72 H 1.0566 0.8991 0.9690 0.150 Uiso 1 1 calc R . . C80 C 0.9610(15) 0.8703(13) 0.8754(9) 0.169(8) Uiso 1 1 d D . . H73 H 1.0156 0.8354 0.8624 0.203 Uiso 1 1 calc R . . C81 C 0.8642(17) 0.8810(14) 0.8271(9) 0.193(9) Uiso 1 1 d D . . H74 H 0.8542 0.8596 0.7803 0.232 Uiso 1 1 calc R . . C82 C 0.7805(14) 0.9245(12) 0.8492(8) 0.168(8) Uiso 1 1 d D . . H75 H 0.7103 0.9307 0.8180 0.202 Uiso 1 1 calc R . . C83 C 0.7986(10) 0.9586(8) 0.9156(6) 0.097(4) Uiso 1 1 d D . . H76 H 0.7398 0.9875 0.9298 0.117 Uiso 1 1 calc R . . C84 C 0.917(2) 0.978(2) 1.0371(10) 0.315(18) Uiso 1 1 d D . . H77 H 0.9088 1.0391 1.0394 0.473 Uiso 1 1 calc R . . H78 H 0.9917 0.9622 1.0622 0.473 Uiso 1 1 calc R . . H79 H 0.8623 0.9508 1.0592 0.473 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.059(7) 0.039(5) 0.049(5) -0.002(5) 0.018(5) -0.006(5) C2 0.073(8) 0.051(6) 0.043(5) 0.002(5) 0.008(5) -0.008(6) C3 0.075(8) 0.037(5) 0.041(5) -0.012(4) 0.021(5) -0.019(5) C4 0.038(6) 0.027(5) 0.053(5) -0.006(4) 0.005(4) -0.008(4) C5 0.046(6) 0.033(5) 0.046(5) -0.017(4) -0.002(4) -0.010(4) C6 0.060(7) 0.031(5) 0.047(5) -0.003(4) 0.017(5) -0.003(5) C7 0.066(8) 0.037(5) 0.045(5) 0.002(4) 0.002(5) -0.008(5) C8 0.059(8) 0.054(6) 0.042(5) -0.002(5) 0.007(5) 0.001(5) C9 0.057(7) 0.040(5) 0.043(5) 0.002(4) 0.014(5) -0.008(5) C10 0.054(7) 0.040(5) 0.032(5) -0.010(4) 0.008(4) -0.009(5) C11 0.048(7) 0.058(7) 0.049(6) -0.008(5) 0.023(5) -0.013(5) C12 0.056(7) 0.044(6) 0.045(5) 0.007(4) 0.009(5) 0.022(5) C13 0.057(7) 0.036(5) 0.030(4) -0.004(4) 0.012(4) 0.003(5) C14 0.044(7) 0.041(6) 0.055(5) 0.006(5) 0.010(5) -0.005(5) C15 0.070(9) 0.046(6) 0.061(6) 0.000(5) 0.022(6) 0.002(6) O1 0.063(5) 0.075(5) 0.046(4) -0.001(4) 0.011(4) -0.016(4) C16 0.112(12) 0.080(9) 0.067(7) -0.002(6) 0.026(7) -0.035(8) O2 0.062(5) 0.067(5) 0.078(5) 0.015(4) 0.016(4) 0.006(4) C17 0.116(13) 0.138(14) 0.102(10) 0.049(9) 0.054(10) 0.066(11) C18 0.041(6) 0.046(6) 0.035(4) 0.004(4) 0.007(4) -0.004(5) C19 0.058(7) 0.047(6) 0.037(5) 0.004(5) 0.015(4) -0.001(5) C20 0.064(7) 0.053(6) 0.030(4) -0.001(4) 0.011(4) 0.002(6) C21 0.056(7) 0.038(5) 0.033(5) 0.007(4) 0.018(4) 0.010(5) C22 0.033(6) 0.048(5) 0.041(5) -0.006(4) 0.012(4) -0.009(5) C23 0.055(7) 0.043(5) 0.045(5) 0.008(5) 0.013(5) -0.006(5) C24 0.064(8) 0.058(7) 0.065(7) 0.016(6) 0.008(6) -0.018(6) C25 0.072(8) 0.059(7) 0.054(6) 0.007(5) -0.004(5) -0.032(6) C26 0.066(8) 0.048(6) 0.035(5) -0.003(4) 0.015(5) -0.005(5) C27 0.050(7) 0.033(5) 0.033(4) 0.003(4) 0.014(4) -0.005(4) C28 0.043(7) 0.059(6) 0.037(5) 0.000(5) 0.010(5) -0.021(5) C29 0.050(7) 0.038(5) 0.037(5) -0.003(4) 0.005(5) -0.002(5) C30 0.064(8) 0.030(5) 0.034(4) -0.005(4) -0.003(5) -0.006(5) C31 0.053(7) 0.041(5) 0.040(5) -0.002(4) 0.011(4) -0.002(5) C32 0.045(7) 0.044(5) 0.038(5) -0.008(4) 0.014(4) 0.000(5) O3 0.059(5) 0.089(5) 0.041(3) 0.004(4) 0.011(3) -0.026(4) C33 0.169(17) 0.102(11) 0.109(11) -0.026(9) 0.074(11) -0.024(11) O4 0.053(5) 0.060(4) 0.044(3) 0.006(3) 0.001(3) -0.008(4) C34 0.167(18) 0.053(9) 0.196(17) 0.003(10) -0.096(14) 0.001(10) C35 0.047(6) 0.037(5) 0.032(4) -0.007(4) -0.001(4) 0.002(5) C36 0.051(7) 0.052(6) 0.039(5) 0.000(5) 0.003(4) -0.022(5) C37 0.070(8) 0.042(6) 0.036(5) -0.006(4) -0.001(5) 0.000(5) C38 0.035(6) 0.044(5) 0.029(4) 0.000(4) 0.005(4) 0.006(4) C39 0.042(6) 0.038(5) 0.037(5) 0.004(4) -0.001(4) 0.005(4) C40 0.045(6) 0.044(5) 0.035(5) 0.004(4) 0.010(4) -0.003(5) C41 0.065(7) 0.039(6) 0.039(5) -0.006(4) 0.010(5) 0.011(5) C42 0.053(7) 0.054(7) 0.064(6) 0.006(5) 0.029(5) 0.001(5) C43 0.045(6) 0.040(5) 0.040(5) 0.000(4) 0.010(4) -0.003(5) C44 0.051(7) 0.041(5) 0.035(4) -0.003(4) 0.014(5) 0.009(5) C45 0.083(9) 0.035(5) 0.034(5) 0.003(4) 0.021(5) 0.003(5) C46 0.087(10) 0.039(6) 0.051(6) 0.004(5) 0.004(6) -0.006(6) C47 0.058(7) 0.032(5) 0.046(5) 0.007(4) 0.019(5) 0.003(5) C48 0.064(8) 0.050(6) 0.041(5) -0.016(5) 0.013(5) 0.004(5) C49 0.058(7) 0.033(5) 0.052(5) 0.000(4) 0.013(5) -0.006(5) O5 0.057(5) 0.062(4) 0.049(4) -0.005(3) 0.016(3) -0.003(4) C50 0.067(9) 0.064(7) 0.086(8) -0.006(6) 0.031(6) 0.018(7) O6 0.056(5) 0.060(4) 0.051(4) -0.012(3) 0.008(3) -0.015(4) C51 0.088(9) 0.060(7) 0.046(6) 0.003(5) -0.015(6) -0.011(6) N1 0.051(5) 0.038(4) 0.040(4) 0.000(3) 0.012(4) 0.001(4) N2 0.050(5) 0.038(4) 0.040(4) -0.002(3) 0.004(4) -0.005(4) B1 0.076(10) 0.038(6) 0.033(5) 0.000(5) 0.013(6) 0.000(6) F1 0.077(5) 0.090(4) 0.041(3) 0.002(3) 0.007(3) -0.036(4) F2 0.117(5) 0.035(3) 0.047(3) -0.003(3) 0.030(3) -0.006(3) N3 0.051(5) 0.040(4) 0.042(4) -0.002(4) 0.013(4) -0.008(4) N4 0.042(5) 0.047(4) 0.030(4) 0.010(3) 0.007(3) -0.008(4) B2 0.073(9) 0.044(6) 0.025(5) 0.003(5) 0.013(5) 0.006(6) F3 0.128(6) 0.045(3) 0.055(3) -0.007(3) -0.025(3) 0.025(4) F4 0.090(5) 0.091(5) 0.036(3) 0.005(3) 0.017(3) -0.046(4) N5 0.040(5) 0.039(4) 0.034(4) 0.003(3) 0.008(3) 0.004(4) N6 0.061(6) 0.027(4) 0.037(4) 0.001(3) 0.016(4) 0.001(4) B3 0.038(7) 0.036(6) 0.036(5) -0.004(4) 0.017(5) -0.006(5) F5 0.059(4) 0.040(3) 0.051(3) 0.001(2) 0.023(3) 0.002(3) F6 0.058(4) 0.038(3) 0.038(3) 0.010(2) 0.004(2) -0.003(3) C52 0.044(7) 0.055(6) 0.063(6) -0.024(5) 0.023(5) -0.008(5) C53 0.041(6) 0.046(6) 0.049(5) -0.014(5) 0.014(5) -0.006(5) C54 0.076(9) 0.051(7) 0.075(7) -0.021(6) 0.028(6) -0.003(6) C55 0.059(8) 0.054(7) 0.092(8) -0.045(7) 0.040(7) -0.012(6) C56 0.071(8) 0.031(6) 0.085(8) 0.000(5) 0.040(7) 0.001(5) C57 0.042(6) 0.044(6) 0.064(6) 0.002(5) 0.029(5) -0.004(5) C58 0.052(7) 0.054(6) 0.044(5) 0.017(5) 0.007(5) 0.006(5) C59 0.058(8) 0.055(6) 0.047(6) 0.014(5) 0.000(5) -0.001(5) C60 0.066(9) 0.080(9) 0.067(7) 0.028(7) 0.002(6) -0.010(7) C61 0.067(9) 0.055(8) 0.115(10) 0.041(7) 0.018(8) 0.000(6) C62 0.061(8) 0.046(7) 0.102(9) 0.029(6) 0.008(7) -0.022(6) C63 0.045(7) 0.052(7) 0.065(6) 0.001(5) 0.004(5) -0.002(5) C64 0.039(6) 0.046(6) 0.038(5) 0.003(4) 0.007(4) -0.004(5) C65 0.052(7) 0.045(6) 0.047(5) 0.002(5) 0.015(5) -0.001(5) C66 0.064(8) 0.069(8) 0.047(6) 0.016(6) 0.013(5) 0.007(6) C67 0.083(9) 0.066(7) 0.041(5) -0.008(5) 0.018(5) -0.030(6) C69 0.078(8) 0.036(5) 0.044(5) -0.003(4) 0.017(5) -0.004(5) N7 0.073(7) 0.061(6) 0.045(4) -0.002(4) 0.008(4) -0.011(5) C70 0.066(8) 0.062(7) 0.048(5) -0.010(5) 0.012(5) -0.006(6) C71 0.058(8) 0.080(8) 0.065(7) 0.007(6) 0.007(6) -0.003(6) C72 0.128(14) 0.067(8) 0.088(9) -0.009(7) 0.014(9) -0.011(8) C73 0.116(13) 0.098(10) 0.078(8) 0.006(8) 0.007(8) 0.021(9) C74 0.077(9) 0.063(7) 0.045(5) -0.001(5) 0.018(6) 0.009(6) C75 0.086(10) 0.055(7) 0.059(6) -0.006(5) 0.005(6) 0.004(6) C76 0.071(10) 0.116(12) 0.103(10) -0.043(9) 0.018(8) -0.009(9) C77 0.124(15) 0.130(14) 0.129(12) -0.044(11) -0.038(11) 0.046(11) _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 C2 1.354(13) . ? C1 N1 1.371(11) . ? C1 C47 1.492(13) . ? C2 C3 1.364(12) . ? C2 H1 0.9500 . ? C3 C4 1.392(12) . ? C3 H2 0.9500 . ? C4 C5 1.406(12) . ? C4 N1 1.406(10) . ? C5 C6 1.391(12) . ? C5 C52 1.497(12) . ? C6 C7 1.408(12) . ? C6 N2 1.418(10) . ? C7 C8 1.362(12) . ? C7 H3 0.9500 . ? C8 C9 1.419(12) . ? C8 H4 0.9500 . ? C9 N2 1.353(10) . ? C9 C10 1.463(12) . ? C10 C15 1.369(14) . ? C10 C11 1.378(13) . ? C11 O1 1.375(12) . ? C11 C12 1.389(13) . ? C12 C13 1.389(13) . ? C12 O2 1.416(11) . ? C13 C14 1.371(12) . ? C13 C18 1.452(12) . ? C14 C15 1.397(13) . ? C14 H5 0.9500 . ? C15 H6 0.9500 . ? O1 C16 1.387(12) . ? C16 H7 0.9800 . ? C16 H8 0.9800 . ? C16 H9 0.9800 . ? O2 C17 1.409(14) . ? C17 H10 0.9800 . ? C17 H11 0.9800 . ? C17 H12 0.9800 . ? C18 N3 1.401(10) . ? C18 C19 1.420(11) . ? C19 C20 1.367(13) . ? C19 H13 0.9500 . ? C20 C21 1.399(11) . ? C20 H14 0.9500 . ? C21 C22 1.385(12) . ? C21 N3 1.409(11) . ? C22 C23 1.417(11) . ? C22 C58 1.486(12) . ? C23 N4 1.394(11) . ? C23 C24 1.391(13) . ? C24 C25 1.386(13) . ? C24 H15 0.9500 . ? C25 C26 1.401(13) . ? C25 H16 0.9500 . ? C26 N4 1.363(10) . ? C26 C27 1.502(11) . ? C27 C28 1.353(12) . ? C27 C32 1.412(12) . ? C28 O3 1.367(11) . ? C28 C29 1.404(12) . ? C29 O4 1.382(10) . ? C29 C30 1.388(13) . ? C30 C31 1.391(12) . ? C30 C35 1.481(12) . ? C31 C32 1.397(11) . ? C31 H17 0.9500 . ? C32 H18 0.9500 . ? O3 C33 1.429(13) . ? C33 H19 0.9800 . ? C33 H20 0.9800 . ? C33 H21 0.9800 . ? O4 C34 1.383(14) . ? C34 H22 0.9800 . ? C34 H23 0.9800 . ? C34 H24 0.9800 . ? C35 N5 1.350(11) . ? C35 C36 1.417(11) . ? C36 C37 1.401(12) . ? C36 H25 0.9500 . ? C37 C38 1.368(12) . ? C37 H26 0.9500 . ? C38 C39 1.402(12) . ? C38 N5 1.397(10) . ? C39 C40 1.409(12) . ? C39 C64 1.478(11) . ? C40 C41 1.388(12) . ? C40 N6 1.405(10) . ? C41 C42 1.397(13) . ? C41 H27 0.9500 . ? C42 C43 1.407(12) . ? C42 H28 0.9500 . ? C43 N6 1.359(11) . ? C43 C44 1.438(12) . ? C44 C49 1.396(12) . ? C44 C45 1.399(13) . ? C45 O5 1.362(11) . ? C45 C46 1.423(12) . ? C46 C47 1.366(14) . ? C46 O6 1.392(13) . ? C47 C48 1.374(13) . ? C48 C49 1.398(12) . ? C48 H29 0.9500 . ? C49 H30 0.9500 . ? O5 C50 1.425(12) . ? C50 H31 0.9800 . ? C50 H32 0.9800 . ? C50 H33 0.9800 . ? O6 C51 1.447(10) . ? C51 H34 0.9800 . ? C51 H35 0.9800 . ? C51 H36 0.9800 . ? N1 B1 1.535(13) . ? N2 B1 1.523(12) . ? B1 F2 1.395(13) . ? B1 F1 1.393(14) . ? N3 B2 1.532(11) . ? N4 B2 1.543(13) . ? B2 F4 1.372(13) . ? B2 F3 1.387(12) . ? N5 B3 1.537(11) . ? N6 B3 1.558(12) . ? B3 F5 1.390(11) . ? B3 F6 1.393(11) . ? C52 C53 1.367(11) . ? C52 C57 1.413(13) . ? C53 C54 1.378(13) . ? C53 H37 0.9500 . ? C54 C55 1.389(15) . ? C54 H38 0.9500 . ? C55 C56 1.390(14) . ? C55 H39 0.9500 . ? C56 C57 1.391(13) . ? C56 H40 0.9500 . ? C57 H41 0.9500 . ? C58 C59 1.349(13) . ? C58 C63 1.411(13) . ? C59 C60 1.425(14) . ? C59 H42 0.9500 . ? C60 C61 1.378(17) . ? C60 H43 0.9500 . ? C61 C62 1.368(16) . ? C61 H44 0.9500 . ? C62 C63 1.377(13) . ? C62 H45 0.9500 . ? C63 H46 0.9500 . ? C64 C69 1.392(12) . ? C64 C65 1.410(12) . ? C65 C66 1.402(12) . ? C65 H47 0.9500 . ? C66 C67 1.339(14) . ? C66 H48 0.9500 . ? C67 C68 1.388(14) . ? C67 H49 0.9500 . ? C68 C69 1.402(13) . ? C68 H50 0.9500 . ? C69 H51 0.9500 . ? N7 C74 1.501(13) . ? N7 C70 1.533(12) . ? N7 H70 0.9200 . ? N7 H71 0.9200 . ? C70 C71 1.487(14) . ? C70 H52 0.9900 . ? C70 H53 0.9900 . ? C71 C72 1.544(16) . ? C71 H54 0.9900 . ? C71 H55 0.9900 . ? C72 C73 1.406(16) . ? C72 H56 0.9900 . ? C72 H57 0.9900 . ? C73 H58 0.9800 . ? C73 H59 0.9800 . ? C73 H60 0.9800 . ? C74 C75 1.472(13) . ? C74 H61 0.9900 . ? C74 H62 0.9900 . ? C75 C76 1.494(16) . ? C75 H63 0.9900 . ? C75 H64 0.9900 . ? C76 C77 1.505(17) . ? C76 H65 0.9900 . ? C76 H66 0.9900 . ? C77 H67 0.9800 . ? C77 H68 0.9800 . ? C77 H69 0.9800 . ? P1 F12 1.461(8) . ? P1 F10 1.508(11) . ? P1 F11 1.599(10) . ? P1 F8 1.616(12) . ? P1 F7 1.629(11) . ? P1 F9 1.629(12) . ? F12 P2 1.794(11) . ? P2 F15 1.562(13) . ? P2 F13 1.566(15) . ? P2 F17 1.582(14) . ? P2 F16 1.584(14) . ? P2 F14 1.602(13) . ? C78 C83 1.391(12) . ? C78 C84 1.455(14) . ? C78 C79 1.447(13) . ? C79 C80 1.330(14) . ? C79 H72 0.9500 . ? C80 C81 1.361(14) . ? C80 H73 0.9500 . ? C81 C82 1.389(15) . ? C81 H74 0.9500 . ? C82 C83 1.367(13) . ? C82 H75 0.9500 . ? C83 H76 0.9500 . ? C84 H77 0.9806 . ? C84 H78 0.9806 . ? C84 H79 0.9806 . ? 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 C2 C1 N1 111.1(8) . . ? C2 C1 C47 125.5(9) . . ? N1 C1 C47 123.4(8) . . ? C1 C2 C3 108.5(9) . . ? C1 C2 H1 125.8 . . ? C3 C2 H1 125.8 . . ? C2 C3 C4 106.6(8) . . ? C2 C3 H2 126.7 . . ? C4 C3 H2 126.7 . . ? C3 C4 C5 130.9(8) . . ? C3 C4 N1 109.3(7) . . ? C5 C4 N1 119.0(7) . . ? C6 C5 C4 123.0(7) . . ? C6 C5 C52 119.6(8) . . ? C4 C5 C52 117.4(8) . . ? C5 C6 C7 132.6(8) . . ? C5 C6 N2 118.7(7) . . ? C7 C6 N2 108.5(7) . . ? C8 C7 C6 106.7(8) . . ? C8 C7 H3 126.7 . . ? C6 C7 H3 126.7 . . ? C7 C8 C9 109.2(9) . . ? C7 C8 H4 125.4 . . ? C9 C8 H4 125.4 . . ? N2 C9 C8 108.4(8) . . ? N2 C9 C10 126.0(8) . . ? C8 C9 C10 125.6(8) . . ? C15 C10 C11 119.9(9) . . ? C15 C10 C9 120.7(10) . . ? C11 C10 C9 119.0(9) . . ? C10 C11 O1 122.4(9) . . ? C10 C11 C12 119.4(10) . . ? O1 C11 C12 118.0(10) . . ? C13 C12 C11 122.2(9) . . ? C13 C12 O2 117.5(8) . . ? C11 C12 O2 120.0(10) . . ? C14 C13 C12 116.6(8) . . ? C14 C13 C18 121.7(9) . . ? C12 C13 C18 121.2(8) . . ? C13 C14 C15 122.4(10) . . ? C13 C14 H5 118.8 . . ? C15 C14 H5 118.8 . . ? C10 C15 C14 119.4(10) . . ? C10 C15 H6 120.3 . . ? C14 C15 H6 120.3 . . ? C11 O1 C16 119.4(8) . . ? O1 C16 H7 109.5 . . ? O1 C16 H8 109.5 . . ? H7 C16 H8 109.5 . . ? O1 C16 H9 109.5 . . ? H7 C16 H9 109.5 . . ? H8 C16 H9 109.5 . . ? C17 O2 C12 116.4(8) . . ? O2 C17 H10 109.5 . . ? O2 C17 H11 109.5 . . ? H10 C17 H11 109.5 . . ? O2 C17 H12 109.5 . . ? H10 C17 H12 109.5 . . ? H11 C17 H12 109.5 . . ? N3 C18 C19 108.4(8) . . ? N3 C18 C13 125.0(7) . . ? C19 C18 C13 126.4(8) . . ? C20 C19 C18 108.2(8) . . ? C20 C19 H13 125.9 . . ? C18 C19 H13 125.9 . . ? C19 C20 C21 108.1(8) . . ? C19 C20 H14 125.9 . . ? C21 C20 H14 125.9 . . ? C22 C21 C20 130.8(8) . . ? C22 C21 N3 119.9(7) . . ? C20 C21 N3 109.2(8) . . ? C21 C22 C23 119.8(8) . . ? C21 C22 C58 120.5(7) . . ? C23 C22 C58 119.7(8) . . ? N4 C23 C24 109.0(7) . . ? N4 C23 C22 120.7(8) . . ? C24 C23 C22 130.3(9) . . ? C25 C24 C23 107.1(9) . . ? C25 C24 H15 126.4 . . ? C23 C24 H15 126.4 . . ? C24 C25 C26 107.5(8) . . ? C24 C25 H16 126.2 . . ? C26 C25 H16 126.3 . . ? N4 C26 C25 109.2(8) . . ? N4 C26 C27 126.1(8) . . ? C25 C26 C27 124.5(8) . . ? C28 C27 C32 121.3(8) . . ? C28 C27 C26 120.5(9) . . ? C32 C27 C26 116.8(8) . . ? C27 C28 O3 122.3(8) . . ? C27 C28 C29 119.4(9) . . ? O3 C28 C29 118.2(9) . . ? O4 C29 C30 121.2(7) . . ? O4 C29 C28 118.2(9) . . ? C30 C29 C28 120.4(8) . . ? C29 C30 C31 120.0(8) . . ? C29 C30 C35 120.3(8) . . ? C31 C30 C35 119.0(10) . . ? C32 C31 C30 119.6(9) . . ? C32 C31 H17 120.2 . . ? C30 C31 H17 120.2 . . ? C31 C32 C27 119.1(9) . . ? C31 C32 H18 120.5 . . ? C27 C32 H18 120.5 . . ? C28 O3 C33 120.0(9) . . ? O3 C33 H19 109.5 . . ? O3 C33 H20 109.5 . . ? H19 C33 H20 109.5 . . ? O3 C33 H21 109.5 . . ? H19 C33 H21 109.5 . . ? H20 C33 H21 109.5 . . ? C29 O4 C34 119.1(8) . . ? O4 C34 H22 109.5 . . ? O4 C34 H23 109.5 . . ? H22 C34 H23 109.5 . . ? O4 C34 H24 109.5 . . ? H22 C34 H24 109.5 . . ? H23 C34 H24 109.5 . . ? N5 C35 C36 109.3(7) . . ? N5 C35 C30 124.7(7) . . ? C36 C35 C30 125.9(8) . . ? C37 C36 C35 107.3(8) . . ? C37 C36 H25 126.4 . . ? C35 C36 H25 126.3 . . ? C38 C37 C36 106.0(7) . . ? C38 C37 H26 127.0 . . ? C36 C37 H26 127.0 . . ? C37 C38 C39 129.1(7) . . ? C37 C38 N5 111.1(8) . . ? C39 C38 N5 119.3(8) . . ? C38 C39 C40 121.4(7) . . ? C38 C39 C64 120.4(8) . . ? C40 C39 C64 118.2(8) . . ? C41 C40 N6 108.9(7) . . ? C41 C40 C39 129.5(8) . . ? N6 C40 C39 121.3(8) . . ? C40 C41 C42 106.5(8) . . ? C40 C41 H27 126.8 . . ? C42 C41 H27 126.7 . . ? C41 C42 C43 108.4(9) . . ? C41 C42 H28 125.8 . . ? C43 C42 H28 125.8 . . ? N6 C43 C42 108.2(8) . . ? N6 C43 C44 125.0(8) . . ? C42 C43 C44 126.6(9) . . ? C49 C44 C45 118.0(8) . . ? C49 C44 C43 121.9(9) . . ? C45 C44 C43 119.9(9) . . ? O5 C45 C44 119.9(8) . . ? O5 C45 C46 121.4(10) . . ? C44 C45 C46 118.4(10) . . ? C47 C46 O6 121.7(9) . . ? C47 C46 C45 122.6(11) . . ? O6 C46 C45 115.2(10) . . ? C46 C47 C48 118.6(9) . . ? C46 C47 C1 120.6(10) . . ? C48 C47 C1 119.1(9) . . ? C47 C48 C49 120.2(10) . . ? C47 C48 H29 119.9 . . ? C49 C48 H29 119.9 . . ? C44 C49 C48 121.8(10) . . ? C44 C49 H30 119.1 . . ? C48 C49 H30 119.1 . . ? C45 O5 C50 115.3(7) . . ? O5 C50 H31 109.5 . . ? O5 C50 H32 109.5 . . ? H31 C50 H32 109.5 . . ? O5 C50 H33 109.5 . . ? H31 C50 H33 109.5 . . ? H32 C50 H33 109.5 . . ? C46 O6 C51 117.1(8) . . ? O6 C51 H34 109.5 . . ? O6 C51 H35 109.5 . . ? H34 C51 H35 109.5 . . ? O6 C51 H36 109.5 . . ? H34 C51 H36 109.5 . . ? H35 C51 H36 109.5 . . ? C1 N1 C4 104.3(7) . . ? C1 N1 B1 131.7(7) . . ? C4 N1 B1 124.0(7) . . ? C9 N2 C6 107.3(7) . . ? C9 N2 B1 128.5(7) . . ? C6 N2 B1 123.7(7) . . ? F2 B1 F1 107.4(9) . . ? F2 B1 N2 111.3(8) . . ? F1 B1 N2 110.0(9) . . ? F2 B1 N1 109.8(9) . . ? F1 B1 N1 109.9(8) . . ? N2 B1 N1 108.4(8) . . ? C18 N3 C21 106.1(7) . . ? C18 N3 B2 125.6(8) . . ? C21 N3 B2 124.1(7) . . ? C26 N4 C23 107.1(7) . . ? C26 N4 B2 127.3(7) . . ? C23 N4 B2 124.5(7) . . ? F4 B2 F3 108.4(9) . . ? F4 B2 N3 110.2(9) . . ? F3 B2 N3 112.6(8) . . ? F4 B2 N4 111.0(8) . . ? F3 B2 N4 107.7(8) . . ? N3 B2 N4 106.9(8) . . ? C35 N5 C38 106.3(7) . . ? C35 N5 B3 126.3(7) . . ? C38 N5 B3 126.3(7) . . ? C43 N6 C40 108.0(7) . . ? C43 N6 B3 127.8(7) . . ? C40 N6 B3 123.4(7) . . ? F5 B3 F6 108.5(7) . . ? F5 B3 N5 107.3(8) . . ? F6 B3 N5 113.2(7) . . ? F5 B3 N6 111.8(7) . . ? F6 B3 N6 108.1(8) . . ? N5 B3 N6 108.0(6) . . ? C53 C52 C57 118.7(9) . . ? C53 C52 C5 121.6(9) . . ? C57 C52 C5 119.7(8) . . ? C52 C53 C54 122.6(10) . . ? C52 C53 H37 118.7 . . ? C54 C53 H37 118.7 . . ? C53 C54 C55 117.5(10) . . ? C53 C54 H38 121.3 . . ? C55 C54 H38 121.2 . . ? C56 C55 C54 122.9(9) . . ? C56 C55 H39 118.6 . . ? C54 C55 H39 118.6 . . ? C55 C56 C57 117.6(10) . . ? C55 C56 H40 121.2 . . ? C57 C56 H40 121.2 . . ? C56 C57 C52 120.7(9) . . ? C56 C57 H41 119.7 . . ? C52 C57 H41 119.7 . . ? C59 C58 C63 120.6(10) . . ? C59 C58 C22 120.8(9) . . ? C63 C58 C22 118.5(8) . . ? C58 C59 C60 119.0(11) . . ? C58 C59 H42 120.5 . . ? C60 C59 H42 120.5 . . ? C61 C60 C59 120.4(11) . . ? C61 C60 H43 119.8 . . ? C59 C60 H43 119.8 . . ? C62 C61 C60 119.5(11) . . ? C62 C61 H44 120.2 . . ? C60 C61 H44 120.2 . . ? C61 C62 C63 121.1(12) . . ? C61 C62 H45 119.5 . . ? C63 C62 H45 119.4 . . ? C62 C63 C58 119.4(11) . . ? C62 C63 H46 120.3 . . ? C58 C63 H46 120.3 . . ? C69 C64 C65 119.6(8) . . ? C69 C64 C39 119.0(8) . . ? C65 C64 C39 121.3(8) . . ? C66 C65 C64 118.8(9) . . ? C66 C65 H47 120.6 . . ? C64 C65 H47 120.6 . . ? C67 C66 C65 121.4(9) . . ? C67 C66 H48 119.3 . . ? C65 C66 H48 119.3 . . ? C66 C67 C68 120.7(9) . . ? C66 C67 H49 119.6 . . ? C68 C67 H49 119.6 . . ? C67 C68 C69 120.0(11) . . ? C67 C68 H50 120.0 . . ? C69 C68 H50 120.0 . . ? C64 C69 C68 119.5(9) . . ? C64 C69 H51 120.3 . . ? C68 C69 H51 120.3 . . ? C74 N7 C70 112.4(7) . . ? C74 N7 H70 109.1 . . ? C70 N7 H70 109.1 . . ? C74 N7 H71 109.1 . . ? C70 N7 H71 109.1 . . ? H70 N7 H71 107.9 . . ? C71 C70 N7 111.5(8) . . ? C71 C70 H52 109.3 . . ? N7 C70 H52 109.3 . . ? C71 C70 H53 109.3 . . ? N7 C70 H53 109.3 . . ? H52 C70 H53 108.0 . . ? C70 C71 C72 113.6(10) . . ? C70 C71 H54 108.8 . . ? C72 C71 H54 108.8 . . ? C70 C71 H55 108.8 . . ? C72 C71 H55 108.9 . . ? H54 C71 H55 107.7 . . ? C73 C72 C71 112.8(13) . . ? C73 C72 H56 109.0 . . ? C71 C72 H56 109.0 . . ? C73 C72 H57 109.0 . . ? C71 C72 H57 109.0 . . ? H56 C72 H57 107.8 . . ? C72 C73 H58 109.5 . . ? C72 C73 H59 109.5 . . ? H58 C73 H59 109.5 . . ? C72 C73 H60 109.5 . . ? H58 C73 H60 109.5 . . ? H59 C73 H60 109.5 . . ? C75 C74 N7 113.9(8) . . ? C75 C74 H61 108.8 . . ? N7 C74 H61 108.8 . . ? C75 C74 H62 108.8 . . ? N7 C74 H62 108.8 . . ? H61 C74 H62 107.7 . . ? C74 C75 C76 113.1(10) . . ? C74 C75 H63 108.9 . . ? C76 C75 H63 109.0 . . ? C74 C75 H64 109.0 . . ? C76 C75 H64 108.9 . . ? H63 C75 H64 107.8 . . ? C77 C76 C75 111.1(13) . . ? C77 C76 H65 109.4 . . ? C75 C76 H65 109.4 . . ? C77 C76 H66 109.4 . . ? C75 C76 H66 109.4 . . ? H65 C76 H66 108.0 . . ? C76 C77 H67 109.5 . . ? C76 C77 H68 109.5 . . ? H67 C77 H68 109.5 . . ? C76 C77 H69 109.5 . . ? H67 C77 H69 109.5 . . ? H68 C77 H69 109.5 . . ? F12 P1 F10 94.7(7) . . ? F12 P1 F11 172.3(6) . . ? F10 P1 F11 91.3(6) . . ? F12 P1 F8 94.9(7) . . ? F10 P1 F8 89.1(7) . . ? F11 P1 F8 90.2(6) . . ? F12 P1 F7 86.5(6) . . ? F10 P1 F7 173.2(8) . . ? F11 P1 F7 88.2(6) . . ? F8 P1 F7 84.2(7) . . ? F12 P1 F9 86.6(6) . . ? F10 P1 F9 94.9(7) . . ? F11 P1 F9 88.0(6) . . ? F8 P1 F9 175.7(8) . . ? F7 P1 F9 91.8(7) . . ? P1 F12 P2 24.6(4) . . ? F15 P2 F13 91.8(10) . . ? F15 P2 F17 85.9(9) . . ? F13 P2 F17 174.4(11) . . ? F15 P2 F16 90.2(9) . . ? F13 P2 F16 92.3(9) . . ? F17 P2 F16 92.8(9) . . ? F15 P2 F14 173.9(11) . . ? F13 P2 F14 94.0(10) . . ? F17 P2 F14 88.1(9) . . ? F16 P2 F14 91.2(9) . . ? F15 P2 F12 92.9(8) . . ? F13 P2 F12 85.5(9) . . ? F17 P2 F12 89.5(8) . . ? F16 P2 F12 176.3(9) . . ? F14 P2 F12 86.0(7) . . ? C83 C78 C84 123.2(14) . . ? C83 C78 C79 116.2(10) . . ? C84 C78 C79 119.9(13) . . ? C80 C79 C78 118.8(12) . . ? C80 C79 H72 120.6 . . ? C78 C79 H72 120.5 . . ? C79 C80 C81 124.8(13) . . ? C79 C80 H73 117.6 . . ? C81 C80 H73 117.6 . . ? C80 C81 C82 117.2(12) . . ? C80 C81 H74 121.3 . . ? C82 C81 H74 121.4 . . ? C83 C82 C81 120.4(12) . . ? C83 C82 H75 119.9 . . ? C81 C82 H75 119.8 . . ? C82 C83 C78 122.3(11) . . ? C82 C83 H76 118.8 . . ? C78 C83 H76 118.9 . . ? C78 C84 H77 109.6 . . ? C78 C84 H78 109.5 . . ? H77 C84 H78 109.4 . . ? C78 C84 H79 109.5 . . ? H77 C84 H79 109.4 . . ? H78 C84 H79 109.4 . . ? 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 4.7(12) . . . . ? C47 C1 C2 C3 -173.9(10) . . . . ? C1 C2 C3 C4 -3.0(12) . . . . ? C2 C3 C4 C5 -169.1(10) . . . . ? C2 C3 C4 N1 0.5(11) . . . . ? C3 C4 C5 C6 165.1(11) . . . . ? N1 C4 C5 C6 -3.6(14) . . . . ? C3 C4 C5 C52 -12.8(15) . . . . ? N1 C4 C5 C52 178.5(8) . . . . ? C4 C5 C6 C7 -175.1(10) . . . . ? C52 C5 C6 C7 2.8(17) . . . . ? C4 C5 C6 N2 -1.3(14) . . . . ? C52 C5 C6 N2 176.6(9) . . . . ? C5 C6 C7 C8 172.7(11) . . . . ? N2 C6 C7 C8 -1.6(12) . . . . ? C6 C7 C8 C9 0.4(12) . . . . ? C7 C8 C9 N2 1.0(12) . . . . ? C7 C8 C9 C10 -178.3(10) . . . . ? N2 C9 C10 C15 84.6(14) . . . . ? C8 C9 C10 C15 -96.1(12) . . . . ? N2 C9 C10 C11 -102.6(11) . . . . ? C8 C9 C10 C11 76.7(14) . . . . ? C15 C10 C11 O1 173.9(9) . . . . ? C9 C10 C11 O1 1.0(14) . . . . ? C15 C10 C11 C12 -1.1(14) . . . . ? C9 C10 C11 C12 -174.0(9) . . . . ? C10 C11 C12 C13 1.0(14) . . . . ? O1 C11 C12 C13 -174.2(8) . . . . ? C10 C11 C12 O2 175.2(8) . . . . ? O1 C11 C12 O2 0.0(14) . . . . ? C11 C12 C13 C14 0.7(13) . . . . ? O2 C12 C13 C14 -173.6(8) . . . . ? C11 C12 C13 C18 172.5(8) . . . . ? O2 C12 C13 C18 -1.8(13) . . . . ? C12 C13 C14 C15 -2.4(13) . . . . ? C18 C13 C14 C15 -174.1(8) . . . . ? C11 C10 C15 C14 -0.4(14) . . . . ? C9 C10 C15 C14 172.3(8) . . . . ? C13 C14 C15 C10 2.3(14) . . . . ? C10 C11 O1 C16 67.4(13) . . . . ? C12 C11 O1 C16 -117.5(11) . . . . ? C13 C12 O2 C17 -114.9(12) . . . . ? C11 C12 O2 C17 70.7(14) . . . . ? C14 C13 C18 N3 -46.1(13) . . . . ? C12 C13 C18 N3 142.5(9) . . . . ? C14 C13 C18 C19 127.2(10) . . . . ? C12 C13 C18 C19 -44.1(14) . . . . ? N3 C18 C19 C20 0.1(11) . . . . ? C13 C18 C19 C20 -174.2(9) . . . . ? C18 C19 C20 C21 -0.5(11) . . . . ? C19 C20 C21 C22 178.4(10) . . . . ? C19 C20 C21 N3 0.8(11) . . . . ? C20 C21 C22 C23 174.8(10) . . . . ? N3 C21 C22 C23 -7.7(14) . . . . ? C20 C21 C22 C58 -5.6(16) . . . . ? N3 C21 C22 C58 171.8(8) . . . . ? C21 C22 C23 N4 -9.0(14) . . . . ? C58 C22 C23 N4 171.5(9) . . . . ? C21 C22 C23 C24 172.3(11) . . . . ? C58 C22 C23 C24 -7.2(17) . . . . ? N4 C23 C24 C25 2.1(13) . . . . ? C22 C23 C24 C25 -179.0(11) . . . . ? C23 C24 C25 C26 -2.2(14) . . . . ? C24 C25 C26 N4 1.5(13) . . . . ? C24 C25 C26 C27 -173.2(10) . . . . ? N4 C26 C27 C28 136.6(10) . . . . ? C25 C26 C27 C28 -49.7(15) . . . . ? N4 C26 C27 C32 -56.6(13) . . . . ? C25 C26 C27 C32 117.1(12) . . . . ? C32 C27 C28 O3 179.7(8) . . . . ? C26 C27 C28 O3 -14.0(14) . . . . ? C32 C27 C28 C29 -4.2(14) . . . . ? C26 C27 C28 C29 162.0(8) . . . . ? C27 C28 C29 O4 -171.5(8) . . . . ? O3 C28 C29 O4 4.7(13) . . . . ? C27 C28 C29 C30 3.5(14) . . . . ? O3 C28 C29 C30 179.7(8) . . . . ? O4 C29 C30 C31 174.3(8) . . . . ? C28 C29 C30 C31 -0.6(13) . . . . ? O4 C29 C30 C35 3.6(12) . . . . ? C28 C29 C30 C35 -171.3(8) . . . . ? C29 C30 C31 C32 -1.6(13) . . . . ? C35 C30 C31 C32 169.3(8) . . . . ? C30 C31 C32 C27 0.9(12) . . . . ? C28 C27 C32 C31 2.1(13) . . . . ? C26 C27 C32 C31 -164.6(8) . . . . ? C27 C28 O3 C33 -51.6(15) . . . . ? C29 C28 O3 C33 132.3(11) . . . . ? C30 C29 O4 C34 80.0(15) . . . . ? C28 C29 O4 C34 -105.1(14) . . . . ? C29 C30 C35 N5 -132.6(9) . . . . ? C31 C30 C35 N5 56.6(12) . . . . ? C29 C30 C35 C36 51.6(14) . . . . ? C31 C30 C35 C36 -119.2(11) . . . . ? N5 C35 C36 C37 -0.6(11) . . . . ? C30 C35 C36 C37 175.7(9) . . . . ? C35 C36 C37 C38 -0.1(11) . . . . ? C36 C37 C38 C39 172.4(9) . . . . ? C36 C37 C38 N5 0.8(11) . . . . ? C37 C38 C39 C40 -167.0(10) . . . . ? N5 C38 C39 C40 4.0(13) . . . . ? C37 C38 C39 C64 15.0(15) . . . . ? N5 C38 C39 C64 -174.0(8) . . . . ? C38 C39 C40 C41 -173.4(9) . . . . ? C64 C39 C40 C41 4.6(15) . . . . ? C38 C39 C40 N6 0.3(13) . . . . ? C64 C39 C40 N6 178.3(8) . . . . ? N6 C40 C41 C42 -0.4(11) . . . . ? C39 C40 C41 C42 174.0(9) . . . . ? C40 C41 C42 C43 -0.3(11) . . . . ? C41 C42 C43 N6 0.9(11) . . . . ? C41 C42 C43 C44 176.8(9) . . . . ? N6 C43 C44 C49 48.4(13) . . . . ? C42 C43 C44 C49 -126.8(11) . . . . ? N6 C43 C44 C45 -136.6(10) . . . . ? C42 C43 C44 C45 48.2(14) . . . . ? C49 C44 C45 O5 177.1(8) . . . . ? C43 C44 C45 O5 2.0(13) . . . . ? C49 C44 C45 C46 3.3(13) . . . . ? C43 C44 C45 C46 -171.9(8) . . . . ? O5 C45 C46 C47 -171.3(9) . . . . ? C44 C45 C46 C47 2.4(14) . . . . ? O5 C45 C46 O6 1.2(12) . . . . ? C44 C45 C46 O6 174.9(8) . . . . ? O6 C46 C47 C48 -177.5(8) . . . . ? C45 C46 C47 C48 -5.5(14) . . . . ? O6 C46 C47 C1 -12.2(13) . . . . ? C45 C46 C47 C1 159.8(8) . . . . ? C2 C1 C47 C46 -47.3(14) . . . . ? N1 C1 C47 C46 134.3(10) . . . . ? C2 C1 C47 C48 117.9(11) . . . . ? N1 C1 C47 C48 -60.5(13) . . . . ? C46 C47 C48 C49 2.8(14) . . . . ? C1 C47 C48 C49 -162.7(8) . . . . ? C45 C44 C49 C48 -6.0(13) . . . . ? C43 C44 C49 C48 169.1(8) . . . . ? C47 C48 C49 C44 3.0(14) . . . . ? C44 C45 O5 C50 111.9(10) . . . . ? C46 C45 O5 C50 -74.4(11) . . . . ? C47 C46 O6 C51 -61.0(12) . . . . ? C45 C46 O6 C51 126.5(9) . . . . ? C2 C1 N1 C4 -4.2(11) . . . . ? C47 C1 N1 C4 174.4(9) . . . . ? C2 C1 N1 B1 173.9(10) . . . . ? C47 C1 N1 B1 -7.5(16) . . . . ? C3 C4 N1 C1 2.2(10) . . . . ? C5 C4 N1 C1 173.2(8) . . . . ? C3 C4 N1 B1 -176.0(9) . . . . ? C5 C4 N1 B1 -5.1(13) . . . . ? C8 C9 N2 C6 -2.0(11) . . . . ? C10 C9 N2 C6 177.4(10) . . . . ? C8 C9 N2 B1 169.3(10) . . . . ? C10 C9 N2 B1 -11.3(17) . . . . ? C5 C6 N2 C9 -173.0(9) . . . . ? C7 C6 N2 C9 2.2(11) . . . . ? C5 C6 N2 B1 15.2(15) . . . . ? C7 C6 N2 B1 -169.6(9) . . . . ? C9 N2 B1 F2 48.1(15) . . . . ? C6 N2 B1 F2 -142.0(9) . . . . ? C9 N2 B1 F1 -70.8(13) . . . . ? C6 N2 B1 F1 99.2(11) . . . . ? C9 N2 B1 N1 168.9(9) . . . . ? C6 N2 B1 N1 -21.1(14) . . . . ? C1 N1 B1 F2 -40.0(14) . . . . ? C4 N1 B1 F2 137.8(8) . . . . ? C1 N1 B1 F1 78.0(13) . . . . ? C4 N1 B1 F1 -104.3(9) . . . . ? C1 N1 B1 N2 -161.8(9) . . . . ? C4 N1 B1 N2 16.0(13) . . . . ? C19 C18 N3 C21 0.3(10) . . . . ? C13 C18 N3 C21 174.7(9) . . . . ? C19 C18 N3 B2 158.1(9) . . . . ? C13 C18 N3 B2 -27.5(15) . . . . ? C22 C21 N3 C18 -178.6(8) . . . . ? C20 C21 N3 C18 -0.7(10) . . . . ? C22 C21 N3 B2 23.2(14) . . . . ? C20 C21 N3 B2 -158.9(9) . . . . ? C25 C26 N4 C23 -0.1(11) . . . . ? C27 C26 N4 C23 174.4(9) . . . . ? C25 C26 N4 B2 167.7(10) . . . . ? C27 C26 N4 B2 -17.8(15) . . . . ? C24 C23 N4 C26 -1.2(11) . . . . ? C22 C23 N4 C26 179.8(9) . . . . ? C24 C23 N4 B2 -169.5(9) . . . . ? C22 C23 N4 B2 11.5(14) . . . . ? C18 N3 B2 F4 -52.1(13) . . . . ? C21 N3 B2 F4 101.8(11) . . . . ? C18 N3 B2 F3 69.0(13) . . . . ? C21 N3 B2 F3 -137.0(9) . . . . ? C18 N3 B2 N4 -172.9(8) . . . . ? C21 N3 B2 N4 -19.0(13) . . . . ? C26 N4 B2 F4 75.7(12) . . . . ? C23 N4 B2 F4 -118.4(9) . . . . ? C26 N4 B2 F3 -42.8(13) . . . . ? C23 N4 B2 F3 123.1(9) . . . . ? C26 N4 B2 N3 -164.0(9) . . . . ? C23 N4 B2 N3 1.8(13) . . . . ? C36 C35 N5 C38 1.1(10) . . . . ? C30 C35 N5 C38 -175.3(9) . . . . ? C36 C35 N5 B3 -167.7(8) . . . . ? C30 C35 N5 B3 16.0(14) . . . . ? C37 C38 N5 C35 -1.2(10) . . . . ? C39 C38 N5 C35 -173.7(8) . . . . ? C37 C38 N5 B3 167.6(8) . . . . ? C39 C38 N5 B3 -5.0(13) . . . . ? C42 C43 N6 C40 -1.1(10) . . . . ? C44 C43 N6 C40 -177.1(9) . . . . ? C42 C43 N6 B3 -170.6(9) . . . . ? C44 C43 N6 B3 13.5(15) . . . . ? C41 C40 N6 C43 0.9(10) . . . . ? C39 C40 N6 C43 -174.0(8) . . . . ? C41 C40 N6 B3 171.0(8) . . . . ? C39 C40 N6 B3 -3.9(13) . . . . ? C35 N5 B3 F5 47.5(11) . . . . ? C38 N5 B3 F5 -119.1(9) . . . . ? C35 N5 B3 F6 -72.2(11) . . . . ? C38 N5 B3 F6 121.3(8) . . . . ? C35 N5 B3 N6 168.1(8) . . . . ? C38 N5 B3 N6 1.6(12) . . . . ? C43 N6 B3 F5 -71.4(12) . . . . ? C40 N6 B3 F5 120.6(8) . . . . ? C43 N6 B3 F6 48.0(12) . . . . ? C40 N6 B3 F6 -120.0(8) . . . . ? C43 N6 B3 N5 170.9(8) . . . . ? C40 N6 B3 N5 2.9(12) . . . . ? C6 C5 C52 C53 -48.6(14) . . . . ? C4 C5 C52 C53 129.4(10) . . . . ? C6 C5 C52 C57 133.0(10) . . . . ? C4 C5 C52 C57 -49.0(13) . . . . ? C57 C52 C53 C54 -2.1(15) . . . . ? C5 C52 C53 C54 179.6(10) . . . . ? C52 C53 C54 C55 1.5(16) . . . . ? C53 C54 C55 C56 0.7(17) . . . . ? C54 C55 C56 C57 -2.2(16) . . . . ? C55 C56 C57 C52 1.5(15) . . . . ? C53 C52 C57 C56 0.5(14) . . . . ? C5 C52 C57 C56 178.9(9) . . . . ? C21 C22 C58 C59 -45.0(14) . . . . ? C23 C22 C58 C59 134.6(10) . . . . ? C21 C22 C58 C63 137.6(10) . . . . ? C23 C22 C58 C63 -42.8(13) . . . . ? C63 C58 C59 C60 -2.0(15) . . . . ? C22 C58 C59 C60 -179.4(9) . . . . ? C58 C59 C60 C61 1.2(16) . . . . ? C59 C60 C61 C62 0.0(18) . . . . ? C60 C61 C62 C63 -0.4(18) . . . . ? C61 C62 C63 C58 -0.4(16) . . . . ? C59 C58 C63 C62 1.7(15) . . . . ? C22 C58 C63 C62 179.1(9) . . . . ? C38 C39 C64 C69 49.9(13) . . . . ? C40 C39 C64 C69 -128.1(10) . . . . ? C38 C39 C64 C65 -128.8(9) . . . . ? C40 C39 C64 C65 53.2(12) . . . . ? C69 C64 C65 C66 2.2(14) . . . . ? C39 C64 C65 C66 -179.1(9) . . . . ? C64 C65 C66 C67 -0.8(16) . . . . ? C65 C66 C67 C68 -0.7(17) . . . . ? C66 C67 C68 C69 0.6(17) . . . . ? C65 C64 C69 C68 -2.2(15) . . . . ? C39 C64 C69 C68 179.1(10) . . . . ? C67 C68 C69 C64 0.8(17) . . . . ? C74 N7 C70 C71 173.4(9) . . . . ? N7 C70 C71 C72 176.8(9) . . . . ? C70 C71 C72 C73 55.5(15) . . . . ? C70 N7 C74 C75 172.3(9) . . . . ? N7 C74 C75 C76 173.3(10) . . . . ? C74 C75 C76 C77 64.2(15) . . . . ? F10 P1 F12 P2 124.5(12) . . . . ? F11 P1 F12 P2 -16(4) . . . . ? F8 P1 F12 P2 -146.0(12) . . . . ? F7 P1 F12 P2 -62.1(10) . . . . ? F9 P1 F12 P2 29.9(10) . . . . ? P1 F12 P2 F15 116.1(14) . . . . ? P1 F12 P2 F13 24.5(12) . . . . ? P1 F12 P2 F17 -158.0(14) . . . . ? P1 F12 P2 F16 -30(15) . . . . ? P1 F12 P2 F14 -69.9(11) . . . . ? C83 C78 C79 C80 -1(3) . . . . ? C84 C78 C79 C80 169(2) . . . . ? C78 C79 C80 C81 6(3) . . . . ? C79 C80 C81 C82 -7(4) . . . . ? C80 C81 C82 C83 3(4) . . . . ? C81 C82 C83 C78 1(3) . . . . ? C84 C78 C83 C82 -172(2) . . . . ? C79 C78 C83 C82 -2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.458 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.075