# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Tatsuya Nabeshima' _publ_contact_author_address ; Department of Chemistry University of Tsukuba Tsukuba Ibaraki 305-8571 JAPAN ; _publ_contact_author_email NABESIMA@CHEM.TSUKUBA.AC.JP _publ_section_title ; Self-assembled cyclic boron-dipyrrin oligomers ; loop_ _publ_author_name 'Tatsuya Nabeshima' 'Chusaku Ikeda' data_3mer _database_code_depnum_ccdc_archive 'CCDC 665385' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C81 H51 B3 N6 O6, 2(C2 H3 N), 2(C H Cl3)' _chemical_formula_sum 'C87 H59 B3 Cl6 N8 O6' _chemical_formula_weight 1557.55 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' 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.025(3) _cell_length_b 23.337(6) _cell_length_c 22.624(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.068(8) _cell_angle_gamma 90.00 _cell_volume 7405(3) _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 prismatic _exptl_crystal_colour Red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 0.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8908 _exptl_absorpt_correction_T_max 0.9432 _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 36155 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15623 _reflns_number_gt 13792 _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^)+(0.1144P)^2^+7.6833P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(5) _refine_ls_number_reflns 15623 _refine_ls_number_parameters 993 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1740 _refine_ls_wR_factor_gt 0.1648 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3796(2) 0.37000(13) 0.18988(15) 0.0227(6) Uani 1 1 d . . . C2 C 0.4649(2) 0.39246(14) 0.21443(16) 0.0267(7) Uani 1 1 d . . . H1 H 0.4835 0.3908 0.2548 0.032 Uiso 1 1 calc R . . C3 C 0.5158(2) 0.41726(13) 0.16883(16) 0.0250(7) Uani 1 1 d . . . H2 H 0.5758 0.4359 0.1720 0.030 Uiso 1 1 calc R . . C4 C 0.4625(2) 0.40982(12) 0.11709(15) 0.0212(6) Uani 1 1 d . . . C5 C 0.4813(2) 0.42763(12) 0.05897(15) 0.0200(6) Uani 1 1 d . . . C6 C 0.4181(2) 0.41424(12) 0.01346(15) 0.0206(6) Uani 1 1 d . . . C7 C 0.4241(2) 0.42933(13) -0.04658(16) 0.0241(6) Uani 1 1 d . . . H3 H 0.4746 0.4496 -0.0652 0.029 Uiso 1 1 calc R . . C8 C 0.3414(3) 0.40872(14) -0.07324(16) 0.0258(7) Uani 1 1 d . . . H4 H 0.3245 0.4125 -0.1137 0.031 Uiso 1 1 calc R . . C9 C 0.2873(2) 0.38129(13) -0.02907(15) 0.0229(6) Uani 1 1 d . . . C10 C 0.3038(2) 0.34047(14) 0.22330(15) 0.0240(6) Uani 1 1 d . . . C11 C 0.2848(3) 0.28190(15) 0.21580(16) 0.0293(7) Uani 1 1 d . . . H5 H 0.3200 0.2603 0.1877 0.035 Uiso 1 1 calc R . . C12 C 0.2146(3) 0.25535(16) 0.24928(18) 0.0355(8) Uani 1 1 d . . . H6 H 0.2024 0.2156 0.2442 0.043 Uiso 1 1 calc R . . C13 C 0.1626(3) 0.28625(18) 0.28988(17) 0.0358(8) Uani 1 1 d . . . H7 H 0.1138 0.2679 0.3120 0.043 Uiso 1 1 calc R . . C14 C 0.1811(3) 0.34407(17) 0.29850(17) 0.0333(8) Uani 1 1 d . . . H8 H 0.1455 0.3652 0.3267 0.040 Uiso 1 1 calc R . . C15 C 0.2524(3) 0.37110(14) 0.26551(16) 0.0265(7) Uani 1 1 d . . . H9 H 0.2659 0.4105 0.2719 0.032 Uiso 1 1 calc R . . C16 C 0.1920(2) 0.35610(15) -0.03992(16) 0.0265(7) Uani 1 1 d . . . C17 C 0.1662(3) 0.30069(16) -0.02211(18) 0.0318(8) Uani 1 1 d . . . H10 H 0.2100 0.2775 -0.0008 0.038 Uiso 1 1 calc R . . C18 C 0.0757(3) 0.27976(19) -0.0360(2) 0.0425(10) Uani 1 1 d . . . H11 H 0.0575 0.2426 -0.0231 0.051 Uiso 1 1 calc R . . C19 C 0.0125(3) 0.3126(2) -0.0682(2) 0.0452(11) Uani 1 1 d . . . H12 H -0.0482 0.2974 -0.0782 0.054 Uiso 1 1 calc R . . C20 C 0.0363(3) 0.3675(2) -0.0861(2) 0.0437(10) Uani 1 1 d . . . H13 H -0.0080 0.3902 -0.1076 0.052 Uiso 1 1 calc R . . C21 C 0.1267(3) 0.38899(16) -0.07214(18) 0.0308(7) Uani 1 1 d . . . H14 H 0.1439 0.4264 -0.0847 0.037 Uiso 1 1 calc R . . C22 C 0.5667(2) 0.46380(13) 0.04702(15) 0.0221(6) Uani 1 1 d . . . C23 C 0.6572(2) 0.44064(13) 0.03528(17) 0.0256(7) Uani 1 1 d . . . H15 H 0.6650 0.4002 0.0338 0.031 Uiso 1 1 calc R . . C24 C 0.7355(2) 0.47592(14) 0.02574(17) 0.0260(7) Uani 1 1 d . . . H16 H 0.7962 0.4592 0.0185 0.031 Uiso 1 1 calc R . . C25 C 0.7265(2) 0.53594(13) 0.02665(16) 0.0234(6) Uani 1 1 d . . . H17 H 0.7799 0.5602 0.0204 0.028 Uiso 1 1 calc R . . C26 C 0.6381(2) 0.55788(13) 0.03693(15) 0.0211(6) Uani 1 1 d . . . C27 C 0.5591(2) 0.52288(13) 0.04699(15) 0.0201(6) Uani 1 1 d . . . N1 N 0.37922(19) 0.37981(10) 0.13035(12) 0.0198(5) Uani 1 1 d . . . N2 N 0.33336(19) 0.38405(10) 0.02360(13) 0.0202(5) Uani 1 1 d . . . B1 B 0.2922(2) 0.37538(14) 0.08725(17) 0.0200(6) Uani 1 1 d . . . O1 O 0.47918(15) 0.55430(9) 0.05651(10) 0.0197(4) Uani 1 1 d . . . O2 O 0.61157(15) 0.61439(9) 0.03990(10) 0.0200(4) Uani 1 1 d . . . C28 C 0.5341(2) 0.63847(13) 0.16559(15) 0.0220(6) Uani 1 1 d . . . C29 C 0.4795(3) 0.66263(15) 0.21111(16) 0.0270(7) Uani 1 1 d . . . H18 H 0.4958 0.6635 0.2519 0.032 Uiso 1 1 calc R . . C30 C 0.3969(2) 0.68520(13) 0.18563(16) 0.0240(6) Uani 1 1 d . . . H19 H 0.3463 0.7039 0.2057 0.029 Uiso 1 1 calc R . . C31 C 0.4031(2) 0.67485(12) 0.12466(15) 0.0211(6) Uani 1 1 d . . . C32 C 0.3419(2) 0.68958(12) 0.07866(15) 0.0209(6) Uani 1 1 d . . . C33 C 0.3654(2) 0.67761(12) 0.02028(16) 0.0218(6) Uani 1 1 d . . . C34 C 0.3150(2) 0.68970(14) -0.03225(16) 0.0255(7) Uani 1 1 d . . . H20 H 0.2567 0.7103 -0.0353 0.031 Uiso 1 1 calc R . . C35 C 0.3662(3) 0.66595(15) -0.07854(17) 0.0288(7) Uani 1 1 d . . . H21 H 0.3496 0.6671 -0.1192 0.035 Uiso 1 1 calc R . . C36 C 0.4480(2) 0.63964(14) -0.05378(15) 0.0235(6) Uani 1 1 d . . . C37 C 0.6266(2) 0.60843(14) 0.17150(16) 0.0241(6) Uani 1 1 d . . . C38 C 0.6292(2) 0.55420(14) 0.19681(16) 0.0260(7) Uani 1 1 d . . . H22 H 0.5721 0.5369 0.2106 0.031 Uiso 1 1 calc R . . C39 C 0.7160(3) 0.52513(15) 0.20185(17) 0.0292(7) Uani 1 1 d . . . H23 H 0.7173 0.4875 0.2178 0.035 Uiso 1 1 calc R . . C40 C 0.8003(3) 0.55079(17) 0.18383(18) 0.0317(8) Uani 1 1 d . . . H24 H 0.8592 0.5310 0.1877 0.038 Uiso 1 1 calc R . . C41 C 0.7981(2) 0.60605(16) 0.15999(17) 0.0288(7) Uani 1 1 d . . . H25 H 0.8557 0.6242 0.1482 0.035 Uiso 1 1 calc R . . C42 C 0.7118(2) 0.63443(15) 0.15358(16) 0.0260(7) Uani 1 1 d . . . H26 H 0.7105 0.6718 0.1369 0.031 Uiso 1 1 calc R . . C43 C 0.5200(3) 0.60722(14) -0.08740(15) 0.0260(7) Uani 1 1 d . . . C44 C 0.6168(3) 0.62164(16) -0.08605(16) 0.0300(7) Uani 1 1 d . . . H27 H 0.6381 0.6533 -0.0631 0.036 Uiso 1 1 calc R . . C45 C 0.6815(3) 0.58956(18) -0.11835(18) 0.0379(9) Uani 1 1 d . . . H28 H 0.7474 0.5990 -0.1173 0.045 Uiso 1 1 calc R . . C46 C 0.6498(3) 0.54313(18) -0.15265(19) 0.0396(9) Uani 1 1 d . . . H29 H 0.6945 0.5211 -0.1745 0.048 Uiso 1 1 calc R . . C47 C 0.5553(3) 0.52958(16) -0.15475(18) 0.0366(9) Uani 1 1 d . . . H30 H 0.5346 0.4982 -0.1782 0.044 Uiso 1 1 calc R . . C48 C 0.4887(3) 0.56142(15) -0.12283(16) 0.0301(7) Uani 1 1 d . . . H31 H 0.4228 0.5522 -0.1250 0.036 Uiso 1 1 calc R . . C49 C 0.2483(2) 0.71703(13) 0.09286(15) 0.0221(6) Uani 1 1 d . . . C50 C 0.2363(2) 0.77646(14) 0.09471(16) 0.0257(7) Uani 1 1 d . . . H32 H 0.2878 0.8009 0.0843 0.031 Uiso 1 1 calc R . . C51 C 0.1486(2) 0.80028(13) 0.11181(17) 0.0271(7) Uani 1 1 d . . . H33 H 0.1429 0.8408 0.1146 0.033 Uiso 1 1 calc R . . C52 C 0.0697(2) 0.76621(13) 0.12482(16) 0.0238(6) Uani 1 1 d . . . H34 H 0.0102 0.7826 0.1356 0.029 Uiso 1 1 calc R . . C53 C 0.0819(2) 0.70745(13) 0.12132(14) 0.0206(6) Uani 1 1 d . . . C54 C 0.1689(2) 0.68388(12) 0.10639(15) 0.0200(6) Uani 1 1 d . . . N3 N 0.48844(18) 0.64579(11) 0.11312(13) 0.0201(5) Uani 1 1 d . . . N4 N 0.4482(2) 0.64739(11) 0.00592(13) 0.0216(5) Uani 1 1 d . . . B2 B 0.5095(3) 0.61542(15) 0.05325(16) 0.0201(7) Uani 1 1 d . . . O3 O 0.16416(15) 0.62540(9) 0.10632(10) 0.0200(4) Uani 1 1 d . . . O4 O 0.01591(15) 0.66603(9) 0.13085(10) 0.0207(4) Uani 1 1 d . . . C55 C 0.0883(2) 0.58769(14) 0.23502(15) 0.0249(6) Uani 1 1 d . . . C56 C 0.1092(3) 0.53754(14) 0.26820(16) 0.0272(7) Uani 1 1 d . . . H35 H 0.1293 0.5361 0.3083 0.033 Uiso 1 1 calc R . . C57 C 0.0948(2) 0.49112(14) 0.23125(16) 0.0253(7) Uani 1 1 d . . . H36 H 0.1023 0.4519 0.2415 0.030 Uiso 1 1 calc R . . C58 C 0.0667(2) 0.51269(13) 0.17555(16) 0.0223(6) Uani 1 1 d . . . C59 C 0.0445(2) 0.48414(13) 0.12397(16) 0.0218(6) Uani 1 1 d . . . C60 C 0.0189(2) 0.51426(13) 0.07303(15) 0.0212(6) Uani 1 1 d . . . C61 C -0.0040(2) 0.49410(13) 0.01609(16) 0.0233(6) Uani 1 1 d . . . H37 H -0.0085 0.4552 0.0041 0.028 Uiso 1 1 calc R . . C62 C -0.0189(2) 0.54208(14) -0.01928(16) 0.0260(7) Uani 1 1 d . . . H38 H -0.0358 0.5421 -0.0600 0.031 Uiso 1 1 calc R . . C63 C -0.0041(2) 0.59051(13) 0.01663(15) 0.0221(6) Uani 1 1 d . . . C64 C 0.0931(3) 0.64663(14) 0.25843(15) 0.0269(7) Uani 1 1 d . . . C65 C 0.1780(3) 0.66476(17) 0.28502(18) 0.0339(8) Uani 1 1 d . . . H39 H 0.2315 0.6398 0.2865 0.041 Uiso 1 1 calc R . . C66 C 0.1839(3) 0.71916(18) 0.30916(19) 0.0408(9) Uani 1 1 d . . . H40 H 0.2416 0.7316 0.3271 0.049 Uiso 1 1 calc R . . C67 C 0.1056(4) 0.75574(18) 0.30730(19) 0.0468(11) Uani 1 1 d . . . H41 H 0.1101 0.7932 0.3234 0.056 Uiso 1 1 calc R . . C68 C 0.0205(3) 0.73729(16) 0.28177(18) 0.0380(9) Uani 1 1 d . . . H42 H -0.0333 0.7621 0.2811 0.046 Uiso 1 1 calc R . . C69 C 0.0139(3) 0.68266(15) 0.25724(16) 0.0308(7) Uani 1 1 d . . . H43 H -0.0441 0.6701 0.2398 0.037 Uiso 1 1 calc R . . C70 C -0.0107(2) 0.65125(14) -0.00135(15) 0.0241(6) Uani 1 1 d . . . C71 C -0.0835(3) 0.68663(15) 0.01966(18) 0.0317(8) Uani 1 1 d . . . H44 H -0.1320 0.6714 0.0444 0.038 Uiso 1 1 calc R . . C72 C -0.0847(3) 0.74426(16) 0.0042(2) 0.0375(9) Uani 1 1 d . . . H45 H -0.1332 0.7686 0.0193 0.045 Uiso 1 1 calc R . . C73 C -0.0156(3) 0.76668(15) -0.03329(19) 0.0360(9) Uani 1 1 d . . . H46 H -0.0173 0.8061 -0.0438 0.043 Uiso 1 1 calc R . . C74 C 0.0551(3) 0.73192(16) -0.05521(17) 0.0326(8) Uani 1 1 d . . . H47 H 0.1019 0.7473 -0.0810 0.039 Uiso 1 1 calc R . . C75 C 0.0585(3) 0.67373(15) -0.03956(16) 0.0284(7) Uani 1 1 d . . . H48 H 0.1074 0.6497 -0.0548 0.034 Uiso 1 1 calc R . . C76 C 0.0519(2) 0.42062(13) 0.12227(16) 0.0224(6) Uani 1 1 d . . . C77 C -0.0262(2) 0.38391(14) 0.13277(17) 0.0267(7) Uani 1 1 d . . . H49 H -0.0874 0.3999 0.1402 0.032 Uiso 1 1 calc R . . C78 C -0.0149(2) 0.32483(14) 0.13244(17) 0.0279(7) Uani 1 1 d . . . H50 H -0.0683 0.3011 0.1406 0.033 Uiso 1 1 calc R . . C79 C 0.0731(2) 0.29952(13) 0.12042(16) 0.0251(7) Uani 1 1 d . . . H51 H 0.0803 0.2590 0.1198 0.030 Uiso 1 1 calc R . . C80 C 0.1489(2) 0.33516(13) 0.10956(15) 0.0204(6) Uani 1 1 d . . . C81 C 0.1386(2) 0.39531(13) 0.11094(15) 0.0209(6) Uani 1 1 d . . . N5 N 0.06265(19) 0.57295(11) 0.17907(13) 0.0209(5) Uani 1 1 d . . . N6 N 0.01774(19) 0.57391(11) 0.07240(13) 0.0220(5) Uani 1 1 d . . . B3 B 0.0637(3) 0.61143(14) 0.12277(17) 0.0207(7) Uani 1 1 d . . . O5 O 0.22260(15) 0.42160(9) 0.09920(11) 0.0210(4) Uani 1 1 d . . . O6 O 0.24072(16) 0.32124(9) 0.09497(11) 0.0213(4) Uani 1 1 d . . . C82 C 0.2520(3) 0.53653(15) 0.00101(17) 0.0296(7) Uani 1 1 d . . . H52 H 0.2242 0.5688 0.0227 0.044 Uiso 1 1 calc R . . H53 H 0.3217 0.5384 0.0036 0.044 Uiso 1 1 calc R . . H54 H 0.2298 0.5004 0.0183 0.044 Uiso 1 1 calc R . . C83 C 0.2228(2) 0.53937(13) -0.06104(18) 0.0281(7) Uani 1 1 d . . . N7 N 0.1991(3) 0.54155(15) -0.10940(16) 0.0395(8) Uani 1 1 d . . . C84 C 0.3241(3) 0.53288(14) 0.17164(17) 0.0279(7) Uani 1 1 d . . . H55 H 0.2852 0.5661 0.1606 0.042 Uiso 1 1 calc R . . H56 H 0.2877 0.4976 0.1650 0.042 Uiso 1 1 calc R . . H57 H 0.3821 0.5322 0.1475 0.042 Uiso 1 1 calc R . . C85 C 0.3501(3) 0.53700(16) 0.23419(18) 0.0308(7) Uani 1 1 d . . . N8 N 0.3708(3) 0.54174(18) 0.28270(18) 0.0468(9) Uani 1 1 d . . . C86 C 0.8933(3) 0.3609(2) 0.2757(2) 0.0456(10) Uani 1 1 d . . . H58 H 0.9478 0.3523 0.2486 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.90472(9) 0.31716(6) 0.33846(6) 0.0551(3) Uani 1 1 d . . . Cl2 Cl 0.89927(9) 0.43377(6) 0.29517(6) 0.0586(3) Uani 1 1 d . . . Cl3 Cl 0.78688(7) 0.34532(5) 0.23794(5) 0.0445(2) Uani 1 1 d . . . C87 C 0.2176(3) 0.10779(18) 0.3875(2) 0.0411(9) Uani 1 1 d . . . H59 H 0.2088 0.0715 0.4104 0.049 Uiso 1 1 calc R . . Cl4 Cl 0.25825(9) 0.16130(5) 0.43598(5) 0.0477(3) Uani 1 1 d . . . Cl5 Cl 0.30251(10) 0.09563(7) 0.33144(7) 0.0664(4) Uani 1 1 d . . . Cl6 Cl 0.10771(9) 0.12711(5) 0.35577(6) 0.0542(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0245(15) 0.0193(14) 0.0242(15) -0.0024(12) 0.0052(13) 0.0006(12) C2 0.0263(16) 0.0241(15) 0.0298(17) -0.0021(13) 0.0013(14) -0.0016(12) C3 0.0228(15) 0.0193(13) 0.0329(18) -0.0035(13) 0.0033(14) 0.0015(12) C4 0.0194(14) 0.0148(12) 0.0295(16) 0.0000(11) 0.0053(13) 0.0008(11) C5 0.0165(13) 0.0146(12) 0.0289(16) 0.0010(11) 0.0059(12) 0.0018(11) C6 0.0176(13) 0.0149(12) 0.0294(16) 0.0017(11) 0.0064(12) -0.0008(11) C7 0.0239(15) 0.0193(14) 0.0291(17) 0.0033(12) 0.0058(13) 0.0010(12) C8 0.0299(17) 0.0209(14) 0.0266(16) 0.0024(12) 0.0018(14) -0.0003(12) C9 0.0207(15) 0.0194(13) 0.0286(16) -0.0016(12) 0.0023(13) 0.0001(11) C10 0.0248(16) 0.0233(15) 0.0240(16) 0.0020(12) 0.0023(13) 0.0003(12) C11 0.0351(18) 0.0240(16) 0.0289(18) 0.0005(13) 0.0054(15) -0.0022(13) C12 0.048(2) 0.0250(16) 0.0336(19) -0.0023(14) 0.0065(17) -0.0110(15) C13 0.038(2) 0.041(2) 0.0283(18) 0.0059(16) 0.0086(16) -0.0092(16) C14 0.0347(19) 0.0373(19) 0.0279(18) -0.0005(15) 0.0105(16) 0.0002(15) C15 0.0280(16) 0.0232(15) 0.0284(17) 0.0008(13) 0.0034(14) 0.0010(12) C16 0.0232(16) 0.0280(16) 0.0282(17) -0.0070(13) 0.0048(13) -0.0029(13) C17 0.0339(18) 0.0257(16) 0.0358(19) -0.0074(14) 0.0015(16) -0.0092(14) C18 0.042(2) 0.041(2) 0.045(2) -0.0177(18) 0.0134(19) -0.0228(18) C19 0.0261(18) 0.058(3) 0.051(3) -0.022(2) 0.0032(18) -0.0096(18) C20 0.0279(19) 0.051(2) 0.052(3) -0.021(2) -0.0048(19) 0.0043(17) C21 0.0267(17) 0.0311(17) 0.0346(19) -0.0075(15) 0.0003(15) 0.0001(14) C22 0.0219(15) 0.0185(13) 0.0260(16) 0.0018(12) 0.0013(13) -0.0013(12) C23 0.0218(16) 0.0193(13) 0.0355(18) 0.0008(13) 0.0064(14) 0.0029(12) C24 0.0172(14) 0.0227(14) 0.0381(19) 0.0032(13) 0.0081(14) 0.0023(12) C25 0.0156(13) 0.0213(14) 0.0332(17) -0.0007(12) 0.0056(13) -0.0013(11) C26 0.0186(14) 0.0201(13) 0.0248(15) 0.0010(11) 0.0014(12) -0.0022(11) C27 0.0171(13) 0.0193(13) 0.0240(15) -0.0019(11) 0.0027(12) 0.0013(11) N1 0.0184(12) 0.0150(11) 0.0260(13) 0.0000(10) 0.0032(11) 0.0011(9) N2 0.0183(12) 0.0161(11) 0.0263(13) 0.0007(10) 0.0038(11) -0.0013(9) B1 0.0165(15) 0.0153(14) 0.0280(17) 0.0008(13) 0.0048(14) -0.0012(12) O1 0.0136(9) 0.0157(9) 0.0297(12) 0.0006(8) 0.0045(9) -0.0005(7) O2 0.0167(10) 0.0153(9) 0.0280(11) 0.0005(8) 0.0049(9) -0.0021(8) C28 0.0193(14) 0.0167(13) 0.0298(17) 0.0016(12) 0.0015(13) -0.0001(11) C29 0.0272(17) 0.0285(16) 0.0252(16) -0.0027(13) -0.0001(14) 0.0014(13) C30 0.0219(14) 0.0185(14) 0.0315(17) -0.0019(12) 0.0049(13) 0.0019(11) C31 0.0171(13) 0.0153(12) 0.0308(17) -0.0005(12) 0.0046(13) -0.0033(10) C32 0.0197(14) 0.0128(12) 0.0302(16) -0.0005(11) 0.0039(13) -0.0022(11) C33 0.0197(14) 0.0139(12) 0.0318(17) 0.0012(12) 0.0035(13) 0.0001(11) C34 0.0219(15) 0.0205(14) 0.0342(18) 0.0009(13) 0.0002(14) 0.0004(12) C35 0.0293(17) 0.0275(16) 0.0295(18) 0.0031(13) 0.0007(14) 0.0006(13) C36 0.0199(14) 0.0218(14) 0.0289(17) 0.0019(12) 0.0013(13) -0.0019(11) C37 0.0210(15) 0.0245(15) 0.0267(16) -0.0033(13) -0.0001(13) 0.0004(12) C38 0.0195(15) 0.0259(15) 0.0327(18) 0.0008(13) -0.0002(14) -0.0004(12) C39 0.0260(16) 0.0277(16) 0.0340(19) 0.0011(14) -0.0018(15) 0.0055(13) C40 0.0199(15) 0.0412(19) 0.0340(19) -0.0058(15) -0.0030(14) 0.0050(14) C41 0.0185(15) 0.0371(18) 0.0309(18) -0.0027(14) 0.0029(14) -0.0001(13) C42 0.0233(16) 0.0285(16) 0.0261(16) -0.0005(13) 0.0048(13) -0.0026(13) C43 0.0289(16) 0.0242(15) 0.0247(16) 0.0047(13) 0.0071(14) 0.0018(13) C44 0.0336(18) 0.0311(17) 0.0253(17) 0.0070(14) 0.0080(15) 0.0016(14) C45 0.040(2) 0.041(2) 0.0320(19) 0.0088(16) 0.0142(17) 0.0077(17) C46 0.042(2) 0.042(2) 0.035(2) 0.0039(16) 0.0191(18) 0.0160(17) C47 0.052(2) 0.0294(18) 0.0286(18) -0.0001(14) 0.0040(17) 0.0053(16) C48 0.0396(19) 0.0249(15) 0.0257(17) 0.0015(13) 0.0034(15) -0.0013(14) C49 0.0206(15) 0.0179(13) 0.0279(16) 0.0006(12) 0.0005(13) 0.0006(11) C50 0.0236(15) 0.0197(14) 0.0339(18) 0.0015(13) 0.0025(14) -0.0012(12) C51 0.0277(17) 0.0153(13) 0.0383(19) -0.0012(13) 0.0029(15) 0.0025(12) C52 0.0196(14) 0.0161(13) 0.0356(18) 0.0010(12) 0.0027(14) 0.0036(11) C53 0.0197(14) 0.0180(13) 0.0240(15) -0.0011(11) 0.0008(12) -0.0004(11) C54 0.0219(14) 0.0139(13) 0.0243(15) -0.0010(11) 0.0009(12) 0.0003(11) N3 0.0154(11) 0.0169(11) 0.0282(14) -0.0001(10) 0.0052(11) -0.0010(9) N4 0.0202(12) 0.0182(11) 0.0266(14) 0.0030(10) 0.0073(11) -0.0004(10) B2 0.0200(16) 0.0180(15) 0.0223(17) 0.0017(12) 0.0025(14) -0.0017(12) O3 0.0164(10) 0.0137(9) 0.0298(12) -0.0013(8) 0.0031(9) 0.0015(8) O4 0.0168(10) 0.0177(9) 0.0275(12) -0.0009(8) 0.0019(9) -0.0001(8) C55 0.0220(15) 0.0268(15) 0.0257(16) 0.0012(13) 0.0026(13) -0.0033(12) C56 0.0282(16) 0.0257(15) 0.0276(17) 0.0031(13) -0.0013(14) 0.0001(13) C57 0.0222(15) 0.0222(14) 0.0315(17) 0.0024(13) 0.0054(13) 0.0000(12) C58 0.0174(13) 0.0186(13) 0.0308(16) 0.0017(12) 0.0037(13) 0.0010(11) C59 0.0135(13) 0.0182(13) 0.0337(17) 0.0012(13) 0.0051(12) 0.0008(11) C60 0.0157(13) 0.0178(13) 0.0300(17) -0.0014(12) 0.0059(12) 0.0010(11) C61 0.0206(14) 0.0205(14) 0.0288(16) -0.0016(12) 0.0048(13) -0.0019(11) C62 0.0238(15) 0.0257(15) 0.0286(17) -0.0023(13) 0.0001(14) 0.0030(12) C63 0.0173(13) 0.0222(14) 0.0270(16) -0.0041(12) 0.0034(12) 0.0026(11) C64 0.0357(18) 0.0237(15) 0.0214(15) 0.0026(12) 0.0032(14) -0.0035(13) C65 0.036(2) 0.0348(18) 0.0306(18) -0.0014(15) 0.0003(16) -0.0073(15) C66 0.048(2) 0.039(2) 0.035(2) -0.0053(16) 0.0050(19) -0.0162(18) C67 0.079(3) 0.0297(19) 0.032(2) -0.0058(16) 0.006(2) -0.010(2) C68 0.057(3) 0.0255(17) 0.0310(19) -0.0040(15) 0.0041(18) 0.0082(16) C69 0.0405(19) 0.0282(17) 0.0236(16) -0.0008(13) 0.0010(15) 0.0031(14) C70 0.0246(15) 0.0217(14) 0.0261(16) -0.0008(12) -0.0029(13) 0.0028(12) C71 0.0331(18) 0.0275(16) 0.0346(19) 0.0011(14) 0.0014(16) 0.0060(14) C72 0.042(2) 0.0271(17) 0.043(2) 0.0015(15) -0.0003(18) 0.0111(15) C73 0.046(2) 0.0196(15) 0.043(2) 0.0029(14) -0.0081(18) 0.0035(14) C74 0.040(2) 0.0271(16) 0.0311(18) 0.0051(14) -0.0039(16) -0.0034(14) C75 0.0322(17) 0.0263(16) 0.0267(17) 0.0022(13) 0.0019(14) -0.0005(13) C76 0.0192(14) 0.0168(13) 0.0314(17) -0.0005(12) 0.0051(13) -0.0012(11) C77 0.0203(15) 0.0226(15) 0.0373(18) 0.0025(13) 0.0063(14) 0.0013(12) C78 0.0214(15) 0.0212(14) 0.041(2) -0.0004(14) 0.0062(14) -0.0066(12) C79 0.0228(15) 0.0169(13) 0.0357(18) 0.0021(12) 0.0033(14) -0.0010(11) C80 0.0181(14) 0.0174(13) 0.0258(15) 0.0003(11) 0.0033(12) 0.0002(11) C81 0.0203(14) 0.0185(13) 0.0239(15) 0.0026(11) 0.0038(12) -0.0015(11) N5 0.0184(12) 0.0175(12) 0.0267(14) 0.0004(10) 0.0034(11) -0.0006(9) N6 0.0197(12) 0.0165(12) 0.0297(14) 0.0003(10) 0.0030(11) 0.0033(9) B3 0.0194(15) 0.0176(14) 0.0253(17) -0.0003(13) 0.0019(14) 0.0033(12) O5 0.0178(10) 0.0148(9) 0.0305(12) -0.0018(8) 0.0060(9) 0.0010(8) O6 0.0193(10) 0.0133(9) 0.0314(12) 0.0002(8) 0.0050(9) -0.0018(8) C82 0.0285(17) 0.0255(16) 0.0347(19) -0.0012(14) 0.0038(15) 0.0005(13) C83 0.0242(16) 0.0178(14) 0.042(2) -0.0011(13) 0.0101(15) -0.0007(12) N7 0.047(2) 0.0366(17) 0.0344(19) -0.0024(14) 0.0013(16) -0.0023(15) C84 0.0286(16) 0.0224(14) 0.0327(18) -0.0010(13) 0.0023(14) -0.0008(13) C85 0.0265(16) 0.0316(17) 0.034(2) 0.0015(14) 0.0063(15) 0.0011(13) N8 0.044(2) 0.057(2) 0.040(2) -0.0019(17) 0.0054(17) 0.0039(17) C86 0.029(2) 0.066(3) 0.042(2) 0.005(2) 0.0027(18) -0.0034(19) Cl1 0.0450(6) 0.0769(8) 0.0433(6) 0.0107(6) -0.0026(5) 0.0056(6) Cl2 0.0464(6) 0.0639(7) 0.0655(8) 0.0003(6) 0.0164(6) -0.0208(5) Cl3 0.0321(5) 0.0624(6) 0.0389(5) 0.0046(5) 0.0020(4) -0.0045(4) C87 0.049(2) 0.037(2) 0.037(2) -0.0029(16) -0.0033(19) -0.0045(18) Cl4 0.0559(7) 0.0410(5) 0.0462(6) -0.0048(4) 0.0002(5) -0.0129(5) Cl5 0.0541(7) 0.0869(10) 0.0581(8) -0.0227(7) 0.0180(6) -0.0205(7) Cl6 0.0500(6) 0.0495(6) 0.0631(8) 0.0073(5) -0.0121(6) -0.0071(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.366(4) . ? C1 C2 1.418(5) . ? C1 C10 1.476(5) . ? C2 C3 1.382(5) . ? C2 H1 0.9500 . ? C3 C4 1.399(5) . ? C3 H2 0.9500 . ? C4 N1 1.395(4) . ? C4 C5 1.404(5) . ? C5 C6 1.394(5) . ? C5 C22 1.491(4) . ? C6 N2 1.400(4) . ? C6 C7 1.406(5) . ? C7 C8 1.393(5) . ? C7 H3 0.9500 . ? C8 C9 1.409(5) . ? C8 H4 0.9500 . ? C9 N2 1.356(4) . ? C9 C16 1.480(4) . ? C10 C15 1.394(5) . ? C10 C11 1.403(5) . ? C11 C12 1.389(5) . ? C11 H5 0.9500 . ? C12 C13 1.378(6) . ? C12 H6 0.9500 . ? C13 C14 1.388(6) . ? C13 H7 0.9500 . ? C14 C15 1.399(5) . ? C14 H8 0.9500 . ? C15 H9 0.9500 . ? C16 C21 1.400(5) . ? C16 C17 1.402(5) . ? C17 C18 1.395(5) . ? C17 H10 0.9500 . ? C18 C19 1.380(7) . ? C18 H11 0.9500 . ? C19 C20 1.384(7) . ? C19 H12 0.9500 . ? C20 C21 1.399(5) . ? C20 H13 0.9500 . ? C21 H14 0.9500 . ? C22 C27 1.383(4) . ? C22 C23 1.404(5) . ? C23 C24 1.390(5) . ? C23 H15 0.9500 . ? C24 C25 1.407(4) . ? C24 H16 0.9500 . ? C25 C26 1.362(4) . ? C25 H17 0.9500 . ? C26 O2 1.372(4) . ? C26 C27 1.395(4) . ? C27 O1 1.357(4) . ? N1 B1 1.565(4) . ? N2 B1 1.565(5) . ? B1 O6 1.465(4) . ? B1 O5 1.480(4) . ? O1 B2 1.490(4) . ? O2 B2 1.463(4) . ? C28 N3 1.358(4) . ? C28 C29 1.402(5) . ? C28 C37 1.481(4) . ? C29 C30 1.396(5) . ? C29 H18 0.9500 . ? C30 C31 1.403(5) . ? C30 H19 0.9500 . ? C31 C32 1.392(5) . ? C31 N3 1.400(4) . ? C32 C33 1.390(5) . ? C32 C49 1.495(4) . ? C33 N4 1.398(4) . ? C33 C34 1.411(5) . ? C34 C35 1.387(5) . ? C34 H20 0.9500 . ? C35 C36 1.416(5) . ? C35 H21 0.9500 . ? C36 N4 1.363(5) . ? C36 C43 1.474(5) . ? C37 C38 1.389(5) . ? C37 C42 1.401(5) . ? C38 C39 1.399(5) . ? C38 H22 0.9500 . ? C39 C40 1.387(5) . ? C39 H23 0.9500 . ? C40 C41 1.398(6) . ? C40 H24 0.9500 . ? C41 C42 1.387(5) . ? C41 H25 0.9500 . ? C42 H26 0.9500 . ? C43 C44 1.400(5) . ? C43 C48 1.406(5) . ? C44 C45 1.386(5) . ? C44 H27 0.9500 . ? C45 C46 1.405(6) . ? C45 H28 0.9500 . ? C46 C47 1.363(6) . ? C46 H29 0.9500 . ? C47 C48 1.396(6) . ? C47 H30 0.9500 . ? C48 H31 0.9500 . ? C49 C54 1.390(4) . ? C49 C50 1.398(4) . ? C50 C51 1.405(5) . ? C50 H32 0.9500 . ? C51 C52 1.394(5) . ? C51 H33 0.9500 . ? C52 C53 1.384(4) . ? C52 H34 0.9500 . ? C53 O4 1.356(4) . ? C53 C54 1.381(4) . ? C54 O3 1.367(3) . ? N3 B2 1.558(5) . ? N4 B2 1.562(4) . ? O3 B3 1.493(4) . ? O4 B3 1.452(4) . ? C55 N5 1.360(4) . ? C55 C56 1.421(5) . ? C55 C64 1.475(5) . ? C56 C57 1.383(5) . ? C56 H35 0.9500 . ? C57 C58 1.412(5) . ? C57 H36 0.9500 . ? C58 C59 1.379(5) . ? C58 N5 1.410(4) . ? C59 C60 1.397(5) . ? C59 C76 1.487(4) . ? C60 N6 1.392(4) . ? C60 C61 1.408(5) . ? C61 C62 1.392(5) . ? C61 H37 0.9500 . ? C62 C63 1.407(5) . ? C62 H38 0.9500 . ? C63 N6 1.355(4) . ? C63 C70 1.478(4) . ? C64 C69 1.393(5) . ? C64 C65 1.400(5) . ? C65 C66 1.384(6) . ? C65 H39 0.9500 . ? C66 C67 1.391(7) . ? C66 H40 0.9500 . ? C67 C68 1.393(7) . ? C67 H41 0.9500 . ? C68 C69 1.394(5) . ? C68 H42 0.9500 . ? C69 H43 0.9500 . ? C70 C71 1.397(5) . ? C70 C75 1.403(5) . ? C71 C72 1.390(5) . ? C71 H44 0.9500 . ? C72 C73 1.391(6) . ? C72 H45 0.9500 . ? C73 C74 1.374(6) . ? C73 H46 0.9500 . ? C74 C75 1.404(5) . ? C74 H47 0.9500 . ? C75 H48 0.9500 . ? C76 C81 1.376(4) . ? C76 C77 1.411(4) . ? C77 C78 1.388(4) . ? C77 H49 0.9500 . ? C78 C79 1.396(5) . ? C78 H50 0.9500 . ? C79 C80 1.372(4) . ? C79 H51 0.9500 . ? C80 O6 1.369(4) . ? C80 C81 1.411(4) . ? C81 O5 1.355(4) . ? N5 B3 1.559(4) . ? N6 B3 1.575(4) . ? C82 C83 1.463(6) . ? C82 H52 0.9800 . ? C82 H53 0.9800 . ? C82 H54 0.9800 . ? C83 N7 1.145(5) . ? C84 C85 1.464(5) . ? C84 H55 0.9800 . ? C84 H56 0.9800 . ? C84 H57 0.9800 . ? C85 N8 1.140(6) . ? C86 Cl1 1.756(5) . ? C86 Cl3 1.756(4) . ? C86 Cl2 1.760(5) . ? C86 H58 1.0000 . ? C87 Cl4 1.757(4) . ? C87 Cl6 1.758(5) . ? C87 Cl5 1.764(5) . ? C87 H59 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 N1 C1 C2 109.1(3) . . ? N1 C1 C10 125.5(3) . . ? C2 C1 C10 125.4(3) . . ? C3 C2 C1 107.4(3) . . ? C3 C2 H1 126.3 . . ? C1 C2 H1 126.3 . . ? C2 C3 C4 107.3(3) . . ? C2 C3 H2 126.4 . . ? C4 C3 H2 126.4 . . ? N1 C4 C3 109.2(3) . . ? N1 C4 C5 120.6(3) . . ? C3 C4 C5 130.2(3) . . ? C6 C5 C4 120.4(3) . . ? C6 C5 C22 120.3(3) . . ? C4 C5 C22 119.3(3) . . ? C5 C6 N2 122.1(3) . . ? C5 C6 C7 128.2(3) . . ? N2 C6 C7 109.7(3) . . ? C8 C7 C6 106.3(3) . . ? C8 C7 H3 126.9 . . ? C6 C7 H3 126.9 . . ? C7 C8 C9 107.4(3) . . ? C7 C8 H4 126.3 . . ? C9 C8 H4 126.3 . . ? N2 C9 C8 110.2(3) . . ? N2 C9 C16 126.4(3) . . ? C8 C9 C16 123.3(3) . . ? C15 C10 C11 119.0(3) . . ? C15 C10 C1 119.0(3) . . ? C11 C10 C1 122.0(3) . . ? C12 C11 C10 120.2(3) . . ? C12 C11 H5 119.9 . . ? C10 C11 H5 119.9 . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H6 119.8 . . ? C11 C12 H6 119.8 . . ? C12 C13 C14 120.2(4) . . ? C12 C13 H7 119.9 . . ? C14 C13 H7 119.9 . . ? C13 C14 C15 119.8(3) . . ? C13 C14 H8 120.1 . . ? C15 C14 H8 120.1 . . ? C10 C15 C14 120.3(3) . . ? C10 C15 H9 119.8 . . ? C14 C15 H9 119.8 . . ? C21 C16 C17 119.1(3) . . ? C21 C16 C9 117.3(3) . . ? C17 C16 C9 123.5(3) . . ? C18 C17 C16 119.6(4) . . ? C18 C17 H10 120.2 . . ? C16 C17 H10 120.2 . . ? C19 C18 C17 120.5(4) . . ? C19 C18 H11 119.7 . . ? C17 C18 H11 119.7 . . ? C18 C19 C20 120.9(4) . . ? C18 C19 H12 119.6 . . ? C20 C19 H12 119.6 . . ? C19 C20 C21 119.0(4) . . ? C19 C20 H13 120.5 . . ? C21 C20 H13 120.5 . . ? C20 C21 C16 120.9(4) . . ? C20 C21 H14 119.5 . . ? C16 C21 H14 119.5 . . ? C27 C22 C23 117.0(3) . . ? C27 C22 C5 120.2(3) . . ? C23 C22 C5 122.9(3) . . ? C24 C23 C22 121.0(3) . . ? C24 C23 H15 119.5 . . ? C22 C23 H15 119.5 . . ? C23 C24 C25 121.1(3) . . ? C23 C24 H16 119.5 . . ? C25 C24 H16 119.5 . . ? C26 C25 C24 117.3(3) . . ? C26 C25 H17 121.3 . . ? C24 C25 H17 121.3 . . ? C25 C26 O2 128.1(3) . . ? C25 C26 C27 122.0(3) . . ? O2 C26 C27 109.9(3) . . ? O1 C27 C22 127.1(3) . . ? O1 C27 C26 111.4(3) . . ? C22 C27 C26 121.5(3) . . ? C1 N1 C4 107.1(3) . . ? C1 N1 B1 127.3(3) . . ? C4 N1 B1 123.5(3) . . ? C9 N2 C6 106.5(3) . . ? C9 N2 B1 128.8(3) . . ? C6 N2 B1 122.0(3) . . ? O6 B1 O5 106.4(2) . . ? O6 B1 N1 111.5(3) . . ? O5 B1 N1 110.6(3) . . ? O6 B1 N2 113.8(3) . . ? O5 B1 N2 108.5(2) . . ? N1 B1 N2 106.0(2) . . ? C27 O1 B2 105.9(2) . . ? C26 O2 B2 106.9(2) . . ? N3 C28 C29 109.5(3) . . ? N3 C28 C37 123.4(3) . . ? C29 C28 C37 127.1(3) . . ? C30 C29 C28 107.5(3) . . ? C30 C29 H18 126.2 . . ? C28 C29 H18 126.2 . . ? C29 C30 C31 106.8(3) . . ? C29 C30 H19 126.6 . . ? C31 C30 H19 126.6 . . ? C32 C31 N3 120.5(3) . . ? C32 C31 C30 130.8(3) . . ? N3 C31 C30 108.7(3) . . ? C33 C32 C31 120.9(3) . . ? C33 C32 C49 120.0(3) . . ? C31 C32 C49 119.1(3) . . ? C32 C33 N4 121.4(3) . . ? C32 C33 C34 129.8(3) . . ? N4 C33 C34 108.7(3) . . ? C35 C34 C33 107.2(3) . . ? C35 C34 H20 126.4 . . ? C33 C34 H20 126.4 . . ? C34 C35 C36 107.2(3) . . ? C34 C35 H21 126.4 . . ? C36 C35 H21 126.4 . . ? N4 C36 C35 109.6(3) . . ? N4 C36 C43 125.4(3) . . ? C35 C36 C43 125.0(3) . . ? C38 C37 C42 119.5(3) . . ? C38 C37 C28 119.4(3) . . ? C42 C37 C28 121.1(3) . . ? C37 C38 C39 119.8(3) . . ? C37 C38 H22 120.1 . . ? C39 C38 H22 120.1 . . ? C40 C39 C38 120.6(3) . . ? C40 C39 H23 119.7 . . ? C38 C39 H23 119.7 . . ? C39 C40 C41 119.5(3) . . ? C39 C40 H24 120.2 . . ? C41 C40 H24 120.2 . . ? C42 C41 C40 120.0(3) . . ? C42 C41 H25 120.0 . . ? C40 C41 H25 120.0 . . ? C41 C42 C37 120.5(3) . . ? C41 C42 H26 119.7 . . ? C37 C42 H26 119.7 . . ? C44 C43 C48 119.8(3) . . ? C44 C43 C36 122.1(3) . . ? C48 C43 C36 118.1(3) . . ? C45 C44 C43 119.7(4) . . ? C45 C44 H27 120.2 . . ? C43 C44 H27 120.2 . . ? C44 C45 C46 120.1(4) . . ? C44 C45 H28 120.0 . . ? C46 C45 H28 120.0 . . ? C47 C46 C45 120.3(4) . . ? C47 C46 H29 119.8 . . ? C45 C46 H29 119.8 . . ? C46 C47 C48 120.7(4) . . ? C46 C47 H30 119.7 . . ? C48 C47 H30 119.7 . . ? C47 C48 C43 119.4(4) . . ? C47 C48 H31 120.3 . . ? C43 C48 H31 120.3 . . ? C54 C49 C50 116.7(3) . . ? C54 C49 C32 120.8(3) . . ? C50 C49 C32 122.5(3) . . ? C49 C50 C51 120.4(3) . . ? C49 C50 H32 119.8 . . ? C51 C50 H32 119.8 . . ? C52 C51 C50 121.9(3) . . ? C52 C51 H33 119.1 . . ? C50 C51 H33 119.1 . . ? C53 C52 C51 117.1(3) . . ? C53 C52 H34 121.5 . . ? C51 C52 H34 121.5 . . ? O4 C53 C54 111.0(3) . . ? O4 C53 C52 127.8(3) . . ? C54 C53 C52 121.2(3) . . ? O3 C54 C53 110.8(3) . . ? O3 C54 C49 126.5(3) . . ? C53 C54 C49 122.7(3) . . ? C28 N3 C31 107.4(3) . . ? C28 N3 B2 127.8(3) . . ? C31 N3 B2 123.1(3) . . ? C36 N4 C33 107.2(3) . . ? C36 N4 B2 128.1(3) . . ? C33 N4 B2 122.6(3) . . ? O2 B2 O1 105.9(2) . . ? O2 B2 N3 111.9(3) . . ? O1 B2 N3 109.8(3) . . ? O2 B2 N4 113.8(3) . . ? O1 B2 N4 109.5(3) . . ? N3 B2 N4 105.9(3) . . ? C54 O3 B3 105.3(2) . . ? C53 O4 B3 106.9(2) . . ? N5 C55 C56 109.7(3) . . ? N5 C55 C64 125.6(3) . . ? C56 C55 C64 124.7(3) . . ? C57 C56 C55 107.2(3) . . ? C57 C56 H35 126.4 . . ? C55 C56 H35 126.4 . . ? C56 C57 C58 107.5(3) . . ? C56 C57 H36 126.3 . . ? C58 C57 H36 126.3 . . ? C59 C58 N5 121.4(3) . . ? C59 C58 C57 130.2(3) . . ? N5 C58 C57 108.5(3) . . ? C58 C59 C60 120.9(3) . . ? C58 C59 C76 119.2(3) . . ? C60 C59 C76 119.9(3) . . ? N6 C60 C59 121.0(3) . . ? N6 C60 C61 108.8(3) . . ? C59 C60 C61 130.2(3) . . ? C62 C61 C60 106.9(3) . . ? C62 C61 H37 126.5 . . ? C60 C61 H37 126.5 . . ? C61 C62 C63 107.0(3) . . ? C61 C62 H38 126.5 . . ? C63 C62 H38 126.5 . . ? N6 C63 C62 109.9(3) . . ? N6 C63 C70 123.0(3) . . ? C62 C63 C70 127.0(3) . . ? C69 C64 C65 120.3(3) . . ? C69 C64 C55 121.3(3) . . ? C65 C64 C55 118.3(3) . . ? C66 C65 C64 119.8(4) . . ? C66 C65 H39 120.1 . . ? C64 C65 H39 120.1 . . ? C65 C66 C67 120.3(4) . . ? C65 C66 H40 119.9 . . ? C67 C66 H40 119.9 . . ? C66 C67 C68 119.9(4) . . ? C66 C67 H41 120.1 . . ? C68 C67 H41 120.1 . . ? C69 C68 C67 120.3(4) . . ? C69 C68 H42 119.9 . . ? C67 C68 H42 119.9 . . ? C64 C69 C68 119.5(4) . . ? C64 C69 H43 120.3 . . ? C68 C69 H43 120.3 . . ? C71 C70 C75 119.7(3) . . ? C71 C70 C63 121.3(3) . . ? C75 C70 C63 119.0(3) . . ? C72 C71 C70 119.6(4) . . ? C72 C71 H44 120.2 . . ? C70 C71 H44 120.2 . . ? C71 C72 C73 120.6(4) . . ? C71 C72 H45 119.7 . . ? C73 C72 H45 119.7 . . ? C74 C73 C72 120.1(3) . . ? C74 C73 H46 119.9 . . ? C72 C73 H46 119.9 . . ? C73 C74 C75 120.3(4) . . ? C73 C74 H47 119.9 . . ? C75 C74 H47 119.9 . . ? C70 C75 C74 119.6(3) . . ? C70 C75 H48 120.2 . . ? C74 C75 H48 120.2 . . ? C81 C76 C77 117.2(3) . . ? C81 C76 C59 119.7(3) . . ? C77 C76 C59 123.1(3) . . ? C78 C77 C76 120.9(3) . . ? C78 C77 H49 119.6 . . ? C76 C77 H49 119.6 . . ? C77 C78 C79 121.5(3) . . ? C77 C78 H50 119.2 . . ? C79 C78 H50 119.2 . . ? C80 C79 C78 117.6(3) . . ? C80 C79 H51 121.2 . . ? C78 C79 H51 121.2 . . ? O6 C80 C79 128.9(3) . . ? O6 C80 C81 109.7(3) . . ? C79 C80 C81 121.3(3) . . ? O5 C81 C76 127.6(3) . . ? O5 C81 C80 110.9(3) . . ? C76 C81 C80 121.4(3) . . ? C55 N5 C58 107.1(3) . . ? C55 N5 B3 127.7(3) . . ? C58 N5 B3 121.9(3) . . ? C63 N6 C60 107.3(3) . . ? C63 N6 B3 127.4(3) . . ? C60 N6 B3 122.9(3) . . ? O4 B3 O3 106.0(2) . . ? O4 B3 N5 113.5(3) . . ? O3 B3 N5 109.8(2) . . ? O4 B3 N6 113.0(3) . . ? O3 B3 N6 109.1(3) . . ? N5 B3 N6 105.5(2) . . ? C81 O5 B1 106.2(2) . . ? C80 O6 B1 106.7(2) . . ? C83 C82 H52 109.5 . . ? C83 C82 H53 109.5 . . ? H52 C82 H53 109.5 . . ? C83 C82 H54 109.5 . . ? H52 C82 H54 109.5 . . ? H53 C82 H54 109.5 . . ? N7 C83 C82 179.3(4) . . ? C85 C84 H55 109.5 . . ? C85 C84 H56 109.5 . . ? H55 C84 H56 109.5 . . ? C85 C84 H57 109.5 . . ? H55 C84 H57 109.5 . . ? H56 C84 H57 109.5 . . ? N8 C85 C84 178.2(4) . . ? Cl1 C86 Cl3 110.5(3) . . ? Cl1 C86 Cl2 110.7(3) . . ? Cl3 C86 Cl2 111.2(3) . . ? Cl1 C86 H58 108.1 . . ? Cl3 C86 H58 108.1 . . ? Cl2 C86 H58 108.1 . . ? Cl4 C87 Cl6 110.9(3) . . ? Cl4 C87 Cl5 110.1(3) . . ? Cl6 C87 Cl5 109.9(2) . . ? Cl4 C87 H59 108.6 . . ? Cl6 C87 H59 108.6 . . ? Cl5 C87 H59 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.2(4) . . . . ? C10 C1 C2 C3 -179.1(3) . . . . ? C1 C2 C3 C4 -0.2(4) . . . . ? C2 C3 C4 N1 -0.8(4) . . . . ? C2 C3 C4 C5 178.9(3) . . . . ? N1 C4 C5 C6 -1.7(4) . . . . ? C3 C4 C5 C6 178.7(3) . . . . ? N1 C4 C5 C22 174.9(3) . . . . ? C3 C4 C5 C22 -4.7(5) . . . . ? C4 C5 C6 N2 1.4(4) . . . . ? C22 C5 C6 N2 -175.1(3) . . . . ? C4 C5 C6 C7 178.6(3) . . . . ? C22 C5 C6 C7 2.0(5) . . . . ? C5 C6 C7 C8 -176.7(3) . . . . ? N2 C6 C7 C8 0.8(4) . . . . ? C6 C7 C8 C9 -0.4(4) . . . . ? C7 C8 C9 N2 -0.1(4) . . . . ? C7 C8 C9 C16 177.2(3) . . . . ? N1 C1 C10 C15 -115.5(4) . . . . ? C2 C1 C10 C15 64.9(5) . . . . ? N1 C1 C10 C11 67.5(5) . . . . ? C2 C1 C10 C11 -112.1(4) . . . . ? C15 C10 C11 C12 1.1(5) . . . . ? C1 C10 C11 C12 178.2(3) . . . . ? C10 C11 C12 C13 0.4(6) . . . . ? C11 C12 C13 C14 -1.3(6) . . . . ? C12 C13 C14 C15 0.5(6) . . . . ? C11 C10 C15 C14 -1.9(5) . . . . ? C1 C10 C15 C14 -179.0(3) . . . . ? C13 C14 C15 C10 1.1(6) . . . . ? N2 C9 C16 C21 131.1(4) . . . . ? C8 C9 C16 C21 -45.7(5) . . . . ? N2 C9 C16 C17 -52.0(5) . . . . ? C8 C9 C16 C17 131.2(4) . . . . ? C21 C16 C17 C18 -1.0(6) . . . . ? C9 C16 C17 C18 -177.9(3) . . . . ? C16 C17 C18 C19 1.6(6) . . . . ? C17 C18 C19 C20 -1.8(7) . . . . ? C18 C19 C20 C21 1.3(7) . . . . ? C19 C20 C21 C16 -0.8(6) . . . . ? C17 C16 C21 C20 0.6(6) . . . . ? C9 C16 C21 C20 177.7(4) . . . . ? C6 C5 C22 C27 83.9(4) . . . . ? C4 C5 C22 C27 -92.7(4) . . . . ? C6 C5 C22 C23 -95.9(4) . . . . ? C4 C5 C22 C23 87.5(4) . . . . ? C27 C22 C23 C24 1.7(5) . . . . ? C5 C22 C23 C24 -178.5(3) . . . . ? C22 C23 C24 C25 -1.0(6) . . . . ? C23 C24 C25 C26 -0.3(5) . . . . ? C24 C25 C26 O2 180.0(3) . . . . ? C24 C25 C26 C27 0.8(5) . . . . ? C23 C22 C27 O1 179.2(3) . . . . ? C5 C22 C27 O1 -0.6(5) . . . . ? C23 C22 C27 C26 -1.2(5) . . . . ? C5 C22 C27 C26 178.9(3) . . . . ? C25 C26 C27 O1 179.6(3) . . . . ? O2 C26 C27 O1 0.3(4) . . . . ? C25 C26 C27 C22 0.0(5) . . . . ? O2 C26 C27 C22 -179.3(3) . . . . ? C2 C1 N1 C4 -1.6(3) . . . . ? C10 C1 N1 C4 178.7(3) . . . . ? C2 C1 N1 B1 -165.2(3) . . . . ? C10 C1 N1 B1 15.1(5) . . . . ? C3 C4 N1 C1 1.5(3) . . . . ? C5 C4 N1 C1 -178.2(3) . . . . ? C3 C4 N1 B1 165.9(3) . . . . ? C5 C4 N1 B1 -13.9(4) . . . . ? C8 C9 N2 C6 0.6(3) . . . . ? C16 C9 N2 C6 -176.6(3) . . . . ? C8 C9 N2 B1 161.6(3) . . . . ? C16 C9 N2 B1 -15.6(5) . . . . ? C5 C6 N2 C9 176.8(3) . . . . ? C7 C6 N2 C9 -0.9(3) . . . . ? C5 C6 N2 B1 14.2(4) . . . . ? C7 C6 N2 B1 -163.5(3) . . . . ? C1 N1 B1 O6 -49.3(4) . . . . ? C4 N1 B1 O6 149.5(3) . . . . ? C1 N1 B1 O5 68.8(4) . . . . ? C4 N1 B1 O5 -92.3(3) . . . . ? C1 N1 B1 N2 -173.7(3) . . . . ? C4 N1 B1 N2 25.2(4) . . . . ? C9 N2 B1 O6 53.7(4) . . . . ? C6 N2 B1 O6 -147.9(3) . . . . ? C9 N2 B1 O5 -64.6(4) . . . . ? C6 N2 B1 O5 93.9(3) . . . . ? C9 N2 B1 N1 176.6(3) . . . . ? C6 N2 B1 N1 -25.0(3) . . . . ? C22 C27 O1 B2 178.6(3) . . . . ? C26 C27 O1 B2 -1.0(4) . . . . ? C25 C26 O2 B2 -178.7(3) . . . . ? C27 C26 O2 B2 0.6(3) . . . . ? N3 C28 C29 C30 0.5(4) . . . . ? C37 C28 C29 C30 -178.6(3) . . . . ? C28 C29 C30 C31 -0.6(4) . . . . ? C29 C30 C31 C32 -178.1(3) . . . . ? C29 C30 C31 N3 0.5(3) . . . . ? N3 C31 C32 C33 -2.2(4) . . . . ? C30 C31 C32 C33 176.2(3) . . . . ? N3 C31 C32 C49 175.9(3) . . . . ? C30 C31 C32 C49 -5.7(5) . . . . ? C31 C32 C33 N4 3.9(4) . . . . ? C49 C32 C33 N4 -174.2(3) . . . . ? C31 C32 C33 C34 -178.7(3) . . . . ? C49 C32 C33 C34 3.2(5) . . . . ? C32 C33 C34 C35 -176.6(3) . . . . ? N4 C33 C34 C35 1.0(4) . . . . ? C33 C34 C35 C36 -0.2(4) . . . . ? C34 C35 C36 N4 -0.7(4) . . . . ? C34 C35 C36 C43 177.4(3) . . . . ? N3 C28 C37 C38 -107.3(4) . . . . ? C29 C28 C37 C38 71.7(5) . . . . ? N3 C28 C37 C42 74.6(4) . . . . ? C29 C28 C37 C42 -106.4(4) . . . . ? C42 C37 C38 C39 -2.7(5) . . . . ? C28 C37 C38 C39 179.1(3) . . . . ? C37 C38 C39 C40 2.4(6) . . . . ? C38 C39 C40 C41 -0.5(6) . . . . ? C39 C40 C41 C42 -1.1(6) . . . . ? C40 C41 C42 C37 0.8(5) . . . . ? C38 C37 C42 C41 1.1(5) . . . . ? C28 C37 C42 C41 179.3(3) . . . . ? N4 C36 C43 C44 -58.4(5) . . . . ? C35 C36 C43 C44 123.7(4) . . . . ? N4 C36 C43 C48 123.2(4) . . . . ? C35 C36 C43 C48 -54.7(5) . . . . ? C48 C43 C44 C45 -1.9(5) . . . . ? C36 C43 C44 C45 179.8(3) . . . . ? C43 C44 C45 C46 0.5(6) . . . . ? C44 C45 C46 C47 0.5(6) . . . . ? C45 C46 C47 C48 -0.2(6) . . . . ? C46 C47 C48 C43 -1.2(6) . . . . ? C44 C43 C48 C47 2.2(5) . . . . ? C36 C43 C48 C47 -179.4(3) . . . . ? C33 C32 C49 C54 92.5(4) . . . . ? C31 C32 C49 C54 -85.6(4) . . . . ? C33 C32 C49 C50 -89.1(4) . . . . ? C31 C32 C49 C50 92.8(4) . . . . ? C54 C49 C50 C51 2.4(5) . . . . ? C32 C49 C50 C51 -176.1(3) . . . . ? C49 C50 C51 C52 -3.0(6) . . . . ? C50 C51 C52 C53 1.3(5) . . . . ? C51 C52 C53 O4 -178.8(3) . . . . ? C51 C52 C53 C54 0.9(5) . . . . ? O4 C53 C54 O3 -0.9(4) . . . . ? C52 C53 C54 O3 179.4(3) . . . . ? O4 C53 C54 C49 178.3(3) . . . . ? C52 C53 C54 C49 -1.4(5) . . . . ? C50 C49 C54 O3 178.8(3) . . . . ? C32 C49 C54 O3 -2.7(5) . . . . ? C50 C49 C54 C53 -0.3(5) . . . . ? C32 C49 C54 C53 178.2(3) . . . . ? C29 C28 N3 C31 -0.2(3) . . . . ? C37 C28 N3 C31 179.0(3) . . . . ? C29 C28 N3 B2 -165.6(3) . . . . ? C37 C28 N3 B2 13.6(5) . . . . ? C32 C31 N3 C28 178.6(3) . . . . ? C30 C31 N3 C28 -0.2(3) . . . . ? C32 C31 N3 B2 -15.2(4) . . . . ? C30 C31 N3 B2 166.1(3) . . . . ? C35 C36 N4 C33 1.4(4) . . . . ? C43 C36 N4 C33 -176.8(3) . . . . ? C35 C36 N4 B2 165.0(3) . . . . ? C43 C36 N4 B2 -13.1(5) . . . . ? C32 C33 N4 C36 176.4(3) . . . . ? C34 C33 N4 C36 -1.5(3) . . . . ? C32 C33 N4 B2 11.6(4) . . . . ? C34 C33 N4 B2 -166.2(3) . . . . ? C26 O2 B2 O1 -1.1(3) . . . . ? C26 O2 B2 N3 118.5(3) . . . . ? C26 O2 B2 N4 -121.5(3) . . . . ? C27 O1 B2 O2 1.3(3) . . . . ? C27 O1 B2 N3 -119.7(3) . . . . ? C27 O1 B2 N4 124.4(3) . . . . ? C28 N3 B2 O2 -45.8(4) . . . . ? C31 N3 B2 O2 150.8(3) . . . . ? C28 N3 B2 O1 71.4(4) . . . . ? C31 N3 B2 O1 -91.9(3) . . . . ? C28 N3 B2 N4 -170.4(3) . . . . ? C31 N3 B2 N4 26.3(4) . . . . ? C36 N4 B2 O2 50.9(4) . . . . ? C33 N4 B2 O2 -147.8(3) . . . . ? C36 N4 B2 O1 -67.4(4) . . . . ? C33 N4 B2 O1 93.9(3) . . . . ? C36 N4 B2 N3 174.3(3) . . . . ? C33 N4 B2 N3 -24.4(4) . . . . ? C53 C54 O3 B3 0.2(3) . . . . ? C49 C54 O3 B3 -179.1(3) . . . . ? C54 C53 O4 B3 1.3(4) . . . . ? C52 C53 O4 B3 -179.1(3) . . . . ? N5 C55 C56 C57 -0.6(4) . . . . ? C64 C55 C56 C57 178.9(3) . . . . ? C55 C56 C57 C58 0.9(4) . . . . ? C56 C57 C58 C59 179.7(3) . . . . ? C56 C57 C58 N5 -0.9(4) . . . . ? N5 C58 C59 C60 1.2(5) . . . . ? C57 C58 C59 C60 -179.5(3) . . . . ? N5 C58 C59 C76 178.7(3) . . . . ? C57 C58 C59 C76 -2.0(5) . . . . ? C58 C59 C60 N6 1.8(5) . . . . ? C76 C59 C60 N6 -175.6(3) . . . . ? C58 C59 C60 C61 178.4(3) . . . . ? C76 C59 C60 C61 0.9(5) . . . . ? N6 C60 C61 C62 0.2(4) . . . . ? C59 C60 C61 C62 -176.7(3) . . . . ? C60 C61 C62 C63 0.4(4) . . . . ? C61 C62 C63 N6 -0.9(4) . . . . ? C61 C62 C63 C70 179.3(3) . . . . ? N5 C55 C64 C69 57.1(5) . . . . ? C56 C55 C64 C69 -122.3(4) . . . . ? N5 C55 C64 C65 -126.4(4) . . . . ? C56 C55 C64 C65 54.3(5) . . . . ? C69 C64 C65 C66 -1.3(6) . . . . ? C55 C64 C65 C66 -177.9(4) . . . . ? C64 C65 C66 C67 0.3(6) . . . . ? C65 C66 C67 C68 0.9(7) . . . . ? C66 C67 C68 C69 -1.0(7) . . . . ? C65 C64 C69 C68 1.2(6) . . . . ? C55 C64 C69 C68 177.7(4) . . . . ? C67 C68 C69 C64 0.0(6) . . . . ? N6 C63 C70 C71 -68.2(5) . . . . ? C62 C63 C70 C71 111.6(4) . . . . ? N6 C63 C70 C75 110.8(4) . . . . ? C62 C63 C70 C75 -69.4(5) . . . . ? C75 C70 C71 C72 -2.3(6) . . . . ? C63 C70 C71 C72 176.7(3) . . . . ? C70 C71 C72 C73 1.7(6) . . . . ? C71 C72 C73 C74 -0.3(6) . . . . ? C72 C73 C74 C75 -0.5(6) . . . . ? C71 C70 C75 C74 1.5(5) . . . . ? C63 C70 C75 C74 -177.6(3) . . . . ? C73 C74 C75 C70 -0.1(5) . . . . ? C58 C59 C76 C81 -84.3(4) . . . . ? C60 C59 C76 C81 93.2(4) . . . . ? C58 C59 C76 C77 94.6(4) . . . . ? C60 C59 C76 C77 -87.9(4) . . . . ? C81 C76 C77 C78 0.9(5) . . . . ? C59 C76 C77 C78 -178.0(3) . . . . ? C76 C77 C78 C79 -1.5(6) . . . . ? C77 C78 C79 C80 0.8(6) . . . . ? C78 C79 C80 O6 -177.7(3) . . . . ? C78 C79 C80 C81 0.5(5) . . . . ? C77 C76 C81 O5 179.4(3) . . . . ? C59 C76 C81 O5 -1.6(5) . . . . ? C77 C76 C81 C80 0.3(5) . . . . ? C59 C76 C81 C80 179.3(3) . . . . ? O6 C80 C81 O5 -1.8(4) . . . . ? C79 C80 C81 O5 179.7(3) . . . . ? O6 C80 C81 C76 177.4(3) . . . . ? C79 C80 C81 C76 -1.1(5) . . . . ? C56 C55 N5 C58 0.0(4) . . . . ? C64 C55 N5 C58 -179.4(3) . . . . ? C56 C55 N5 B3 -159.6(3) . . . . ? C64 C55 N5 B3 20.9(5) . . . . ? C59 C58 N5 C55 180.0(3) . . . . ? C57 C58 N5 C55 0.6(4) . . . . ? C59 C58 N5 B3 -18.9(5) . . . . ? C57 C58 N5 B3 161.6(3) . . . . ? C62 C63 N6 C60 1.0(4) . . . . ? C70 C63 N6 C60 -179.2(3) . . . . ? C62 C63 N6 B3 163.8(3) . . . . ? C70 C63 N6 B3 -16.4(5) . . . . ? C59 C60 N6 C63 176.5(3) . . . . ? C61 C60 N6 C63 -0.7(4) . . . . ? C59 C60 N6 B3 12.7(5) . . . . ? C61 C60 N6 B3 -164.5(3) . . . . ? C53 O4 B3 O3 -1.1(3) . . . . ? C53 O4 B3 N5 119.5(3) . . . . ? C53 O4 B3 N6 -120.5(3) . . . . ? C54 O3 B3 O4 0.6(3) . . . . ? C54 O3 B3 N5 -122.4(3) . . . . ? C54 O3 B3 N6 122.5(3) . . . . ? C55 N5 B3 O4 -50.5(4) . . . . ? C58 N5 B3 O4 152.6(3) . . . . ? C55 N5 B3 O3 67.9(4) . . . . ? C58 N5 B3 O3 -89.0(3) . . . . ? C55 N5 B3 N6 -174.7(3) . . . . ? C58 N5 B3 N6 28.4(4) . . . . ? C63 N6 B3 O4 49.5(4) . . . . ? C60 N6 B3 O4 -150.1(3) . . . . ? C63 N6 B3 O3 -68.1(4) . . . . ? C60 N6 B3 O3 92.3(3) . . . . ? C63 N6 B3 N5 174.0(3) . . . . ? C60 N6 B3 N5 -25.6(4) . . . . ? C76 C81 O5 B1 -177.1(3) . . . . ? C80 C81 O5 B1 2.0(4) . . . . ? O6 B1 O5 C81 -1.6(3) . . . . ? N1 B1 O5 C81 -122.8(3) . . . . ? N2 B1 O5 C81 121.2(3) . . . . ? C79 C80 O6 B1 179.0(4) . . . . ? C81 C80 O6 B1 0.7(4) . . . . ? O5 B1 O6 C80 0.6(3) . . . . ? N1 B1 O6 C80 121.2(3) . . . . ? N2 B1 O6 C80 -118.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.615 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.082 # Attachment '4M_revised.CIF' data_4mer _database_code_depnum_ccdc_archive 'CCDC 665386' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H68 B4 N8 O8, 4(C6 H6), 2(C4 H8 O2)' _chemical_formula_sum 'C140 H108 B4 N8 O12' _chemical_formula_weight 2137.58 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' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 27.870(5) _cell_length_b 27.870(5) _cell_length_c 28.442(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 22092(8) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour Red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8960 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9760 _exptl_absorpt_correction_T_max 0.9839 _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 78962 _diffrn_reflns_av_R_equivalents 0.1126 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9697 _reflns_number_gt 5558 _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^)+(0.1882P)^2^+17.3243P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9697 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1591 _refine_ls_R_factor_gt 0.1038 _refine_ls_wR_factor_ref 0.3183 _refine_ls_wR_factor_gt 0.2736 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.81527(16) 0.17907(16) 0.04454(15) 0.0547(11) Uani 1 1 d . . . C2 C 0.81326(19) 0.21169(17) 0.00743(17) 0.0649(13) Uani 1 1 d . . . H1 H 0.8088 0.2038 -0.0248 0.078 Uiso 1 1 calc R . . C3 C 0.81885(18) 0.25689(18) 0.02523(16) 0.0610(12) Uani 1 1 d . . . H2 H 0.8187 0.2860 0.0079 0.073 Uiso 1 1 calc R . . C4 C 0.82486(15) 0.25222(16) 0.07380(15) 0.0513(11) Uani 1 1 d . . . C5 C 0.83159(14) 0.28791(15) 0.10795(15) 0.0482(10) Uani 1 1 d . . . C6 C 0.83778(15) 0.27470(16) 0.15481(15) 0.0497(10) Uani 1 1 d . . . C7 C 0.83748(18) 0.30422(17) 0.19479(16) 0.0607(12) Uani 1 1 d . . . H3 H 0.8375 0.3383 0.1952 0.073 Uiso 1 1 calc R . . C8 C 0.8372(2) 0.27424(17) 0.23319(17) 0.0664(13) Uani 1 1 d . . . H4 H 0.8366 0.2838 0.2652 0.080 Uiso 1 1 calc R . . C9 C 0.83781(16) 0.22690(16) 0.21632(15) 0.0528(11) Uani 1 1 d . . . C10 C 0.80821(17) 0.12708(17) 0.03883(15) 0.0559(12) Uani 1 1 d . . . C11 C 0.77300(18) 0.10136(17) 0.06396(17) 0.0592(12) Uani 1 1 d . . . H5 H 0.7544 0.1170 0.0874 0.071 Uiso 1 1 calc R . . C12 C 0.76569(18) 0.05342(17) 0.05441(17) 0.0619(13) Uani 1 1 d . . . H6 H 0.7420 0.0363 0.0715 0.074 Uiso 1 1 calc R . . C13 C 0.79212(19) 0.02990(19) 0.02058(18) 0.0661(13) Uani 1 1 d . . . H7 H 0.7867 -0.0032 0.0145 0.079 Uiso 1 1 calc R . . C14 C 0.82647(19) 0.05468(19) -0.00445(19) 0.0691(14) Uani 1 1 d . . . H8 H 0.8450 0.0384 -0.0276 0.083 Uiso 1 1 calc R . . C15 C 0.83425(18) 0.10295(18) 0.00378(16) 0.0631(13) Uani 1 1 d . . . H9 H 0.8573 0.1199 -0.0144 0.076 Uiso 1 1 calc R . . C16 C 0.83565(17) 0.18378(16) 0.24696(14) 0.0540(11) Uani 1 1 d . . . C17 C 0.87491(18) 0.15386(17) 0.25403(15) 0.0577(12) Uani 1 1 d . . . H10 H 0.9038 0.1592 0.2371 0.069 Uiso 1 1 calc R . . C18 C 0.8719(2) 0.11635(18) 0.28580(16) 0.0649(13) Uani 1 1 d . . . H11 H 0.8989 0.0961 0.2909 0.078 Uiso 1 1 calc R . . C19 C 0.8300(2) 0.10831(18) 0.31007(16) 0.0670(14) Uani 1 1 d . . . H12 H 0.8279 0.0821 0.3314 0.080 Uiso 1 1 calc R . . C20 C 0.7908(2) 0.13784(19) 0.30374(17) 0.0678(13) Uani 1 1 d . . . H13 H 0.7621 0.1325 0.3210 0.081 Uiso 1 1 calc R . . C21 C 0.79375(19) 0.17508(18) 0.27227(17) 0.0637(13) Uani 1 1 d . . . H14 H 0.7667 0.1953 0.2677 0.076 Uiso 1 1 calc R . . N1 N 0.82277(13) 0.20337(13) 0.08563(12) 0.0495(9) Uani 1 1 d . . . N2 N 0.83845(12) 0.22706(12) 0.16887(12) 0.0484(9) Uani 1 1 d . . . C22 C 0.82681(15) 0.33909(16) 0.09522(14) 0.0486(10) Uani 1 1 d . . . C23 C 0.78299(16) 0.35651(17) 0.07668(15) 0.0545(11) Uani 1 1 d . . . H15 H 0.7577 0.3345 0.0707 0.065 Uiso 1 1 calc R . . C24 C 0.77599(16) 0.40411(17) 0.06708(16) 0.0554(11) Uani 1 1 d . . . H16 H 0.7456 0.4145 0.0558 0.067 Uiso 1 1 calc R . . C25 C 0.81265(16) 0.43785(16) 0.07353(14) 0.0516(11) Uani 1 1 d . . . H17 H 0.8078 0.4709 0.0667 0.062 Uiso 1 1 calc R . . C26 C 0.85578(15) 0.42140(16) 0.09001(14) 0.0475(10) Uani 1 1 d . . . C27 C 0.86290(15) 0.37309(15) 0.10170(13) 0.0460(10) Uani 1 1 d . . . O1 O 0.90807(10) 0.36570(10) 0.11789(9) 0.0477(7) Uani 1 1 d . . . O2 O 0.89690(10) 0.44670(10) 0.09765(10) 0.0494(7) Uani 1 1 d . . . B1 B 0.93328(18) 0.41287(17) 0.11501(16) 0.0470(11) Uani 1 1 d . . . C28 C 0.3507(2) 0.77915(18) 0.21663(17) 0.0764(16) Uani 1 1 d . . . C29 C 0.3430(3) 0.7311(2) 0.22899(19) 0.098(2) Uani 1 1 d . . . H18 H 0.3428 0.7187 0.2601 0.118 Uiso 1 1 calc R . . C30 C 0.3361(2) 0.7051(2) 0.18914(17) 0.0833(18) Uani 1 1 d . . . H19 H 0.3304 0.6716 0.1873 0.100 Uiso 1 1 calc R . . C31 C 0.33889(19) 0.73702(17) 0.15129(16) 0.0614(12) Uani 1 1 d . . . C32 C 0.32832(17) 0.72900(17) 0.10464(16) 0.0572(12) Uani 1 1 d . . . C33 C 0.32313(17) 0.76839(17) 0.07376(16) 0.0580(12) Uani 1 1 d . . . C34 C 0.31239(19) 0.76866(19) 0.02591(17) 0.0661(13) Uani 1 1 d . . . H20 H 0.3068 0.7413 0.0067 0.079 Uiso 1 1 calc R . . C35 C 0.3113(2) 0.81542(19) 0.01180(17) 0.0692(14) Uani 1 1 d . . . H21 H 0.3052 0.8263 -0.0193 0.083 Uiso 1 1 calc R . . C36 C 0.32075(17) 0.84443(17) 0.05045(16) 0.0565(11) Uani 1 1 d . . . C37 C 0.32152(17) 0.89748(18) 0.04820(16) 0.0599(12) Uani 1 1 d . . . C38 C 0.34564(18) 0.91871(19) 0.01096(18) 0.0657(13) Uani 1 1 d . . . H22 H 0.3620 0.8993 -0.0113 0.079 Uiso 1 1 calc R . . C39 C 0.34582(18) 0.96885(19) 0.0062(2) 0.0684(14) Uani 1 1 d . . . H23 H 0.3631 0.9834 -0.0188 0.082 Uiso 1 1 calc R . . C40 C 0.3214(2) 0.9965(2) 0.0370(2) 0.0793(16) Uani 1 1 d . . . H24 H 0.3216 1.0304 0.0333 0.095 Uiso 1 1 calc R . . C41 C 0.2962(2) 0.9761(2) 0.0738(2) 0.0779(16) Uani 1 1 d . . . H25 H 0.2791 0.9959 0.0953 0.094 Uiso 1 1 calc R . . C42 C 0.2959(2) 0.92651(19) 0.07935(19) 0.0708(14) Uani 1 1 d . . . H26 H 0.2782 0.9124 0.1043 0.085 Uiso 1 1 calc R . . C43 C 0.3606(3) 0.8177(2) 0.25019(17) 0.0763(16) Uani 1 1 d . . . C44 C 0.3276(2) 0.8260(2) 0.28655(17) 0.0804(17) Uani 1 1 d . . . H27 H 0.2984 0.8085 0.2874 0.097 Uiso 1 1 calc R . . C45 C 0.3374(3) 0.8593(2) 0.3209(2) 0.091(2) Uani 1 1 d . . . H28 H 0.3148 0.8646 0.3454 0.109 Uiso 1 1 calc R . . C46 C 0.3794(3) 0.8849(2) 0.3203(2) 0.0900(19) Uani 1 1 d . . . H29 H 0.3857 0.9078 0.3442 0.108 Uiso 1 1 calc R . . C47 C 0.4122(3) 0.8773(2) 0.2852(2) 0.096(2) Uani 1 1 d . . . H30 H 0.4414 0.8950 0.2846 0.115 Uiso 1 1 calc R . . C48 C 0.4024(3) 0.8430(2) 0.24963(19) 0.0852(18) Uani 1 1 d . . . H31 H 0.4251 0.8377 0.2253 0.102 Uiso 1 1 calc R . . N3 N 0.34802(15) 0.78315(14) 0.16918(13) 0.0597(10) Uani 1 1 d . . . N4 N 0.32780(13) 0.81584(13) 0.08911(13) 0.0537(9) Uani 1 1 d . . . C49 C 0.32011(17) 0.67931(17) 0.08792(15) 0.0575(12) Uani 1 1 d . . . C50 C 0.35342(17) 0.64263(16) 0.09473(15) 0.0527(11) Uani 1 1 d . . . C51 C 0.34488(16) 0.59656(16) 0.07765(15) 0.0518(11) Uani 1 1 d . . . C52 C 0.30299(17) 0.58470(17) 0.05589(16) 0.0576(12) Uani 1 1 d . . . H32 H 0.2972 0.5529 0.0454 0.069 Uiso 1 1 calc R . . C53 C 0.26914(18) 0.62025(18) 0.04952(17) 0.0631(13) Uani 1 1 d . . . H33 H 0.2397 0.6127 0.0344 0.076 Uiso 1 1 calc R . . C54 C 0.27721(18) 0.66682(18) 0.06480(17) 0.0624(12) Uani 1 1 d . . . H34 H 0.2534 0.6907 0.0596 0.075 Uiso 1 1 calc R . . O3 O 0.38343(11) 0.56775(11) 0.08704(10) 0.0547(8) Uani 1 1 d . . . O4 O 0.39770(10) 0.64568(10) 0.11514(10) 0.0525(7) Uani 1 1 d . . . B2 B 0.41940(19) 0.5977(2) 0.11098(18) 0.0533(12) Uani 1 1 d . . . C55 C 0.0905(3) 0.7281(3) 0.1222(4) 0.138(3) Uani 1 1 d . . . H35 H 0.0719 0.7388 0.0949 0.207 Uiso 1 1 calc R . . H36 H 0.0768 0.7420 0.1509 0.207 Uiso 1 1 calc R . . H37 H 0.0894 0.6930 0.1242 0.207 Uiso 1 1 calc R . . C56 C 0.1431(4) 0.7447(4) 0.1168(4) 0.131(3) Uani 1 1 d . . . O5 O 0.1722(3) 0.7288(3) 0.0888(2) 0.158(3) Uani 1 1 d . . . O6 O 0.1558(2) 0.7778(2) 0.1462(2) 0.143(2) Uani 1 1 d . . . C57 C 0.2078(3) 0.7903(4) 0.1442(3) 0.130(3) Uani 1 1 d . . . H38 H 0.2250 0.7722 0.1194 0.155 Uiso 1 1 calc R . . H39 H 0.2240 0.7858 0.1748 0.155 Uiso 1 1 calc R . . C58 C 0.2017(6) 0.8422(8) 0.1319(6) 0.284(10) Uani 1 1 d . . . H40 H 0.2333 0.8568 0.1271 0.426 Uiso 1 1 calc R . . H41 H 0.1850 0.8587 0.1575 0.426 Uiso 1 1 calc R . . H42 H 0.1828 0.8449 0.1029 0.426 Uiso 1 1 calc R . . C59 C 1.0362(5) 0.2453(7) 0.0607(8) 0.201(14) Uani 0.50 1 d PG A -1 H49 H 1.0633 0.2446 0.0809 0.241 Uiso 0.50 1 calc PR A -1 C60 C 0.9965(7) 0.2168(5) 0.0705(6) 0.175(11) Uani 0.50 1 d PG A -1 H50 H 0.9965 0.1966 0.0974 0.210 Uiso 0.50 1 calc PR A -1 C61 C 0.9568(6) 0.2178(5) 0.0409(6) 0.139(10) Uani 0.50 1 d PG A -1 H51 H 0.9297 0.1983 0.0476 0.167 Uiso 0.50 1 calc PR A -1 C62 C 0.9568(6) 0.2473(7) 0.0015(6) 0.224(18) Uani 0.50 1 d PG A -1 H52 H 0.9297 0.2481 -0.0187 0.269 Uiso 0.50 1 calc PR A -1 C63 C 0.9965(7) 0.2759(7) -0.0083(8) 0.33(3) Uani 0.50 1 d PG A -1 H53 H 0.9965 0.2960 -0.0352 0.393 Uiso 0.50 1 calc PR A -1 C64 C 1.0362(6) 0.2748(7) 0.0213(10) 0.36(4) Uani 0.50 1 d PG A -1 H54 H 1.0633 0.2943 0.0146 0.431 Uiso 0.50 1 calc PR A -1 C65 C 0.4838(6) 0.7594(7) 0.0563(6) 0.29(2) Uiso 0.50 1 d PG B -1 H55 H 0.4647 0.7730 0.0805 0.352 Uiso 0.50 1 calc PR B -1 C66 C 0.4733(5) 0.7689(6) 0.0095(7) 0.131(6) Uiso 0.50 1 d PG B -1 H56 H 0.4470 0.7891 0.0017 0.158 Uiso 0.50 1 calc PR B -1 C67 C 0.5012(7) 0.7489(8) -0.0259(5) 0.192(7) Uiso 1 2 d SG B -1 H57 H 0.4940 0.7554 -0.0580 0.230 Uiso 0.50 1 calc PR B -1 C68 C 0.5396(6) 0.7193(6) -0.0145(4) 0.161(8) Uiso 0.50 1 d PG B -1 H58 H 0.5587 0.7056 -0.0387 0.193 Uiso 0.50 1 calc PR B -1 C69 C 0.5501(4) 0.7097(5) 0.0323(5) 0.132(6) Uiso 0.50 1 d PG B -1 H59 H 0.5764 0.6895 0.0401 0.159 Uiso 0.50 1 calc PR B -1 C70 C 0.5222(7) 0.7298(8) 0.0678(4) 0.167(9) Uiso 0.50 1 d PG B -1 H60 H 0.5294 0.7232 0.0998 0.201 Uiso 0.50 1 calc PR B -1 C71 C 0.6123(2) 0.6815(3) -0.1283(4) 0.340(14) Uani 1 1 d G . . H61 H 0.5849 0.6614 -0.1251 0.408 Uiso 1 1 calc R . . C72 C 0.6067(3) 0.7309(3) -0.1316(5) 0.42(2) Uani 1 1 d G . . H62 H 0.5755 0.7447 -0.1307 0.505 Uiso 1 1 calc R . . C73 C 0.6467(4) 0.7603(2) -0.1363(3) 0.263(10) Uani 1 1 d G . . H63 H 0.6429 0.7941 -0.1386 0.315 Uiso 1 1 calc R . . C74 C 0.6923(3) 0.7402(4) -0.1377(3) 0.196(7) Uani 1 1 d G . . H64 H 0.7197 0.7603 -0.1409 0.235 Uiso 1 1 calc R . . C75 C 0.6979(2) 0.6908(4) -0.1344(3) 0.240(9) Uani 1 1 d G . . H65 H 0.7291 0.6771 -0.1354 0.288 Uiso 1 1 calc R . . C76 C 0.6579(3) 0.6614(2) -0.1297(3) 0.180(5) Uani 1 1 d G . . H66 H 0.6617 0.6276 -0.1275 0.216 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 0.061(3) 0.057(3) 0.046(2) -0.001(2) -0.012(2) 0.000(2) C2 0.090(4) 0.058(3) 0.047(3) -0.003(2) -0.012(2) -0.004(2) C3 0.077(3) 0.057(3) 0.050(3) 0.010(2) -0.011(2) -0.004(2) C4 0.052(3) 0.051(3) 0.050(3) 0.001(2) -0.004(2) -0.0015(19) C5 0.040(2) 0.051(3) 0.054(3) -0.001(2) -0.0005(19) 0.0005(18) C6 0.053(3) 0.050(3) 0.047(2) -0.004(2) 0.0042(19) 0.0048(19) C7 0.082(3) 0.050(3) 0.050(3) -0.002(2) 0.000(2) 0.004(2) C8 0.098(4) 0.058(3) 0.043(3) 0.002(2) 0.003(2) 0.004(3) C9 0.063(3) 0.052(3) 0.043(2) -0.001(2) -0.004(2) 0.005(2) C10 0.062(3) 0.059(3) 0.046(2) -0.005(2) -0.020(2) -0.002(2) C11 0.067(3) 0.057(3) 0.054(3) -0.002(2) -0.011(2) 0.000(2) C12 0.071(3) 0.056(3) 0.059(3) 0.000(2) -0.014(2) -0.007(2) C13 0.075(3) 0.059(3) 0.065(3) -0.012(2) -0.015(3) 0.001(3) C14 0.069(3) 0.067(3) 0.071(3) -0.021(3) -0.008(3) 0.004(3) C15 0.068(3) 0.069(3) 0.052(3) -0.008(2) -0.009(2) -0.005(2) C16 0.070(3) 0.054(3) 0.037(2) -0.0034(19) -0.008(2) -0.001(2) C17 0.072(3) 0.056(3) 0.045(2) 0.001(2) 0.001(2) 0.000(2) C18 0.086(4) 0.059(3) 0.050(3) -0.001(2) -0.008(3) 0.005(2) C19 0.102(4) 0.056(3) 0.043(3) 0.004(2) -0.006(3) -0.005(3) C20 0.082(4) 0.064(3) 0.057(3) 0.007(2) 0.005(3) -0.007(3) C21 0.067(3) 0.069(3) 0.055(3) 0.002(2) -0.002(2) -0.004(2) N1 0.054(2) 0.051(2) 0.044(2) -0.0029(16) -0.0058(16) -0.0003(16) N2 0.053(2) 0.049(2) 0.0430(19) -0.0005(16) -0.0008(16) -0.0007(16) C22 0.046(3) 0.058(3) 0.041(2) 0.0021(19) -0.0033(18) 0.000(2) C23 0.052(3) 0.058(3) 0.054(3) 0.001(2) -0.006(2) -0.001(2) C24 0.048(3) 0.062(3) 0.056(3) 0.001(2) -0.008(2) 0.003(2) C25 0.059(3) 0.052(3) 0.043(2) 0.0018(19) -0.005(2) 0.003(2) C26 0.045(3) 0.058(3) 0.040(2) -0.0001(19) 0.0008(18) -0.002(2) C27 0.042(2) 0.057(3) 0.040(2) -0.0001(19) -0.0007(18) 0.0013(19) O1 0.0488(17) 0.0475(17) 0.0468(16) 0.0006(13) -0.0013(13) 0.0018(12) O2 0.0497(18) 0.0518(18) 0.0468(16) 0.0003(13) 0.0009(13) 0.0017(13) B1 0.053(3) 0.046(3) 0.043(3) -0.004(2) 0.000(2) 0.001(2) C28 0.131(5) 0.055(3) 0.044(3) 0.003(2) 0.004(3) 0.019(3) C29 0.190(7) 0.059(4) 0.045(3) 0.007(3) 0.018(4) 0.019(4) C30 0.148(6) 0.053(3) 0.049(3) 0.005(2) 0.011(3) 0.012(3) C31 0.082(4) 0.051(3) 0.052(3) 0.005(2) 0.005(2) 0.006(2) C32 0.061(3) 0.055(3) 0.055(3) 0.003(2) 0.000(2) 0.000(2) C33 0.061(3) 0.059(3) 0.054(3) 0.002(2) -0.006(2) 0.002(2) C34 0.078(3) 0.066(3) 0.054(3) -0.001(2) -0.020(2) 0.000(3) C35 0.084(4) 0.071(4) 0.053(3) 0.009(2) -0.019(3) 0.001(3) C36 0.056(3) 0.063(3) 0.050(3) 0.009(2) -0.006(2) 0.002(2) C37 0.061(3) 0.062(3) 0.056(3) 0.008(2) -0.014(2) 0.002(2) C38 0.060(3) 0.075(4) 0.062(3) 0.011(3) -0.017(2) 0.000(2) C39 0.060(3) 0.064(3) 0.081(4) 0.023(3) -0.015(3) -0.004(2) C40 0.091(4) 0.062(3) 0.084(4) 0.006(3) -0.030(3) 0.006(3) C41 0.098(4) 0.072(4) 0.064(3) 0.002(3) -0.017(3) 0.022(3) C42 0.082(4) 0.066(3) 0.064(3) 0.009(3) -0.012(3) 0.013(3) C43 0.123(5) 0.063(3) 0.043(3) 0.002(2) -0.003(3) 0.020(3) C44 0.115(5) 0.078(4) 0.048(3) -0.004(3) -0.008(3) 0.030(3) C45 0.118(6) 0.099(5) 0.056(3) -0.018(3) -0.003(3) 0.035(4) C46 0.132(6) 0.085(4) 0.053(3) -0.011(3) -0.006(4) 0.020(4) C47 0.142(6) 0.090(4) 0.056(3) -0.005(3) -0.003(4) 0.006(4) C48 0.134(6) 0.074(4) 0.047(3) 0.000(3) -0.003(3) 0.010(4) N3 0.083(3) 0.052(2) 0.044(2) 0.0046(17) 0.0063(19) 0.0059(19) N4 0.057(2) 0.051(2) 0.054(2) 0.0074(17) -0.0042(17) 0.0003(17) C49 0.063(3) 0.059(3) 0.050(3) 0.002(2) 0.001(2) -0.003(2) C50 0.057(3) 0.054(3) 0.047(2) 0.004(2) 0.004(2) -0.005(2) C51 0.052(3) 0.056(3) 0.047(2) -0.001(2) 0.005(2) 0.003(2) C52 0.057(3) 0.058(3) 0.058(3) -0.007(2) 0.001(2) -0.005(2) C53 0.058(3) 0.069(3) 0.062(3) -0.005(2) -0.002(2) -0.007(2) C54 0.058(3) 0.065(3) 0.064(3) 0.001(2) -0.003(2) 0.003(2) O3 0.0536(19) 0.0581(19) 0.0524(17) -0.0058(14) 0.0045(14) -0.0051(14) O4 0.0514(18) 0.0573(19) 0.0487(17) 0.0009(14) -0.0017(14) -0.0050(14) B2 0.054(3) 0.060(3) 0.046(3) 0.002(2) 0.003(2) -0.005(2) C55 0.125(7) 0.112(6) 0.176(9) 0.013(6) 0.000(6) -0.003(5) C56 0.129(8) 0.156(9) 0.110(7) 0.018(6) -0.024(6) -0.002(7) O5 0.204(7) 0.187(7) 0.084(4) 0.010(4) 0.031(4) -0.017(5) O6 0.144(5) 0.147(5) 0.137(5) -0.010(4) -0.029(4) -0.023(4) C57 0.102(6) 0.173(9) 0.114(6) 0.013(6) 0.014(5) -0.042(6) C58 0.241(18) 0.42(3) 0.195(15) -0.025(18) -0.006(13) -0.164(19) C59 0.047(9) 0.16(2) 0.40(5) -0.02(2) -0.026(17) -0.007(11) C60 0.123(17) 0.100(14) 0.30(3) 0.001(16) -0.03(2) 0.030(13) C61 0.17(2) 0.050(9) 0.19(2) 0.007(11) 0.08(2) 0.019(10) C62 0.18(3) 0.29(4) 0.20(3) 0.01(3) 0.11(3) 0.01(3) C63 0.099(16) 0.21(3) 0.67(8) 0.25(4) 0.12(3) 0.031(19) C64 0.18(3) 0.23(4) 0.66(9) 0.06(5) 0.29(5) -0.05(3) C71 0.130(11) 0.183(13) 0.71(4) 0.17(2) -0.050(17) -0.030(9) C72 0.34(2) 0.108(10) 0.81(5) 0.066(18) 0.38(3) 0.012(12) C73 0.44(3) 0.117(8) 0.230(14) -0.075(9) 0.206(17) -0.103(13) C74 0.157(11) 0.313(19) 0.117(8) 0.067(10) -0.066(8) -0.078(11) C75 0.109(8) 0.44(3) 0.174(11) 0.173(14) 0.034(7) 0.104(12) C76 0.077(5) 0.113(7) 0.349(17) 0.040(8) 0.030(8) 0.026(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.367(5) . ? C1 C2 1.394(6) . ? C1 C10 1.471(6) . ? C2 C3 1.366(6) . ? C2 H1 0.9500 . ? C3 C4 1.398(6) . ? C3 H2 0.9500 . ? C4 C5 1.403(6) . ? C4 N1 1.404(6) . ? C5 C6 1.394(6) . ? C5 C22 1.478(6) . ? C6 N2 1.387(5) . ? C6 C7 1.403(6) . ? C7 C8 1.375(6) . ? C7 H3 0.9500 . ? C8 C9 1.404(6) . ? C8 H4 0.9500 . ? C9 N2 1.350(5) . ? C9 C16 1.486(6) . ? C10 C15 1.404(7) . ? C10 C11 1.410(7) . ? C11 C12 1.379(6) . ? C11 H5 0.9500 . ? C12 C13 1.378(7) . ? C12 H6 0.9500 . ? C13 C14 1.378(7) . ? C13 H7 0.9500 . ? C14 C15 1.383(7) . ? C14 H8 0.9500 . ? C15 H9 0.9500 . ? C16 C17 1.390(6) . ? C16 C21 1.393(7) . ? C17 C18 1.384(7) . ? C17 H10 0.9500 . ? C18 C19 1.376(7) . ? C18 H11 0.9500 . ? C19 C20 1.378(7) . ? C19 H12 0.9500 . ? C20 C21 1.373(7) . ? C20 H13 0.9500 . ? C21 H14 0.9500 . ? N1 B1 1.563(6) 16_645 ? N2 B1 1.555(6) 16_645 ? C22 C27 1.394(6) . ? C22 C23 1.416(6) . ? C23 C24 1.368(6) . ? C23 H15 0.9500 . ? C24 C25 1.401(6) . ? C24 H16 0.9500 . ? C25 C26 1.369(6) . ? C25 H17 0.9500 . ? C26 O2 1.363(5) . ? C26 C27 1.401(6) . ? C27 O1 1.356(5) . ? O1 B1 1.493(5) . ? O2 B1 1.470(6) . ? B1 N2 1.555(6) 15_665 ? B1 N1 1.563(6) 15_665 ? C28 N3 1.356(6) . ? C28 C29 1.402(7) . ? C28 C43 1.464(8) . ? C29 C30 1.359(8) . ? C29 H18 0.9500 . ? C30 C31 1.398(7) . ? C30 H19 0.9500 . ? C31 C32 1.377(6) . ? C31 N3 1.406(6) . ? C32 C33 1.413(6) . ? C32 C49 1.482(7) . ? C33 C34 1.394(6) . ? C33 N4 1.399(6) . ? C34 C35 1.364(7) . ? C34 H20 0.9500 . ? C35 C36 1.390(7) . ? C35 H21 0.9500 . ? C36 N4 1.372(6) . ? C36 C37 1.480(7) . ? C37 C38 1.387(7) . ? C37 C42 1.397(7) . ? C38 C39 1.404(7) . ? C38 H22 0.9500 . ? C39 C40 1.351(8) . ? C39 H23 0.9500 . ? C40 C41 1.386(8) . ? C40 H24 0.9500 . ? C41 C42 1.390(7) . ? C41 H25 0.9500 . ? C42 H26 0.9500 . ? C43 C48 1.362(9) . ? C43 C44 1.401(8) . ? C44 C45 1.375(8) . ? C44 H27 0.9500 . ? C45 C46 1.370(9) . ? C45 H28 0.9500 . ? C46 C47 1.372(9) . ? C46 H29 0.9500 . ? C47 C48 1.418(8) . ? C47 H30 0.9500 . ? C48 H31 0.9500 . ? N3 B2 1.576(6) 15_565 ? N4 B2 1.578(6) 15_565 ? C49 C50 1.395(7) . ? C49 C54 1.408(7) . ? C50 O4 1.366(5) . ? C50 C51 1.393(6) . ? C51 C52 1.362(6) . ? C51 O3 1.368(5) . ? C52 C53 1.380(7) . ? C52 H32 0.9500 . ? C53 C54 1.387(7) . ? C53 H33 0.9500 . ? C54 H34 0.9500 . ? O3 B2 1.471(6) . ? O4 B2 1.473(6) . ? B2 N3 1.576(6) 16_655 ? B2 N4 1.578(6) 16_655 ? C55 C56 1.544(13) . ? C55 H35 0.9800 . ? C55 H36 0.9800 . ? C55 H37 0.9800 . ? C56 O5 1.222(11) . ? C56 O6 1.295(11) . ? O6 C57 1.492(10) . ? C57 C58 1.50(2) . ? C57 H38 0.9900 . ? C57 H39 0.9900 . ? C58 H40 0.9800 . ? C58 H41 0.9800 . ? C58 H42 0.9800 . ? C59 C60 1.3900 . ? C59 C64 1.3900 . ? C59 H49 0.9500 . ? C60 C61 1.3900 . ? C60 H50 0.9500 . ? C61 C62 1.3900 . ? C61 H51 0.9500 . ? C62 C63 1.3900 . ? C62 H52 0.9500 . ? C63 C64 1.3900 . ? C63 H53 0.9500 . ? C64 H54 0.9500 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C65 H55 0.9500 . ? C66 C67 1.3900 . ? C66 H56 0.9500 . ? C67 C68 1.3900 . ? C67 H57 0.9500 . ? C68 C69 1.3900 . ? C68 H58 0.9500 . ? C69 C70 1.3900 . ? C69 H59 0.9500 . ? C70 H60 0.9500 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C71 H61 0.9500 . ? C72 C73 1.3900 . ? C72 H62 0.9500 . ? C73 C74 1.3900 . ? C73 H63 0.9500 . ? C74 C75 1.3900 . ? C74 H64 0.9500 . ? C75 C76 1.3900 . ? C75 H65 0.9500 . ? C76 H66 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.3(4) . . ? N1 C1 C10 127.1(4) . . ? C2 C1 C10 123.6(4) . . ? C3 C2 C1 108.4(4) . . ? C3 C2 H1 125.8 . . ? C1 C2 H1 125.8 . . ? C2 C3 C4 107.1(4) . . ? C2 C3 H2 126.5 . . ? C4 C3 H2 126.5 . . ? C3 C4 C5 129.4(4) . . ? C3 C4 N1 108.8(4) . . ? C5 C4 N1 121.8(4) . . ? C6 C5 C4 119.4(4) . . ? C6 C5 C22 120.0(4) . . ? C4 C5 C22 120.2(4) . . ? N2 C6 C5 122.0(4) . . ? N2 C6 C7 109.1(4) . . ? C5 C6 C7 128.3(4) . . ? C8 C7 C6 106.7(4) . . ? C8 C7 H3 126.6 . . ? C6 C7 H3 126.6 . . ? C7 C8 C9 107.4(4) . . ? C7 C8 H4 126.3 . . ? C9 C8 H4 126.3 . . ? N2 C9 C8 109.8(4) . . ? N2 C9 C16 126.1(4) . . ? C8 C9 C16 124.0(4) . . ? C15 C10 C11 118.4(4) . . ? C15 C10 C1 118.7(4) . . ? C11 C10 C1 122.5(4) . . ? C12 C11 C10 119.7(5) . . ? C12 C11 H5 120.1 . . ? C10 C11 H5 120.1 . . ? C13 C12 C11 121.3(5) . . ? C13 C12 H6 119.3 . . ? C11 C12 H6 119.3 . . ? C12 C13 C14 119.6(5) . . ? C12 C13 H7 120.2 . . ? C14 C13 H7 120.2 . . ? C13 C14 C15 120.6(5) . . ? C13 C14 H8 119.7 . . ? C15 C14 H8 119.7 . . ? C14 C15 C10 120.3(5) . . ? C14 C15 H9 119.8 . . ? C10 C15 H9 119.8 . . ? C17 C16 C21 118.7(4) . . ? C17 C16 C9 122.5(4) . . ? C21 C16 C9 118.5(4) . . ? C18 C17 C16 120.0(5) . . ? C18 C17 H10 120.0 . . ? C16 C17 H10 120.0 . . ? C19 C18 C17 120.1(5) . . ? C19 C18 H11 119.9 . . ? C17 C18 H11 119.9 . . ? C18 C19 C20 120.6(5) . . ? C18 C19 H12 119.7 . . ? C20 C19 H12 119.7 . . ? C21 C20 C19 119.4(5) . . ? C21 C20 H13 120.3 . . ? C19 C20 H13 120.3 . . ? C20 C21 C16 121.2(5) . . ? C20 C21 H14 119.4 . . ? C16 C21 H14 119.4 . . ? C1 N1 C4 106.4(3) . . ? C1 N1 B1 129.0(4) . 16_645 ? C4 N1 B1 123.5(3) . 16_645 ? C9 N2 C6 106.9(3) . . ? C9 N2 B1 128.1(4) . 16_645 ? C6 N2 B1 124.9(3) . 16_645 ? C27 C22 C23 116.0(4) . . ? C27 C22 C5 124.0(4) . . ? C23 C22 C5 120.0(4) . . ? C24 C23 C22 122.0(4) . . ? C24 C23 H15 119.0 . . ? C22 C23 H15 119.0 . . ? C23 C24 C25 121.4(4) . . ? C23 C24 H16 119.3 . . ? C25 C24 H16 119.3 . . ? C26 C25 C24 117.4(4) . . ? C26 C25 H17 121.3 . . ? C24 C25 H17 121.3 . . ? O2 C26 C25 128.3(4) . . ? O2 C26 C27 109.9(4) . . ? C25 C26 C27 121.8(4) . . ? O1 C27 C22 127.7(4) . . ? O1 C27 C26 111.0(4) . . ? C22 C27 C26 121.3(4) . . ? C27 O1 B1 106.5(3) . . ? C26 O2 B1 107.6(3) . . ? O2 B1 O1 105.0(3) . . ? O2 B1 N2 110.4(3) . 15_665 ? O1 B1 N2 112.5(3) . 15_665 ? O2 B1 N1 112.6(3) . 15_665 ? O1 B1 N1 110.2(3) . 15_665 ? N2 B1 N1 106.4(3) 15_665 15_665 ? N3 C28 C29 108.6(4) . . ? N3 C28 C43 126.8(5) . . ? C29 C28 C43 124.6(5) . . ? C30 C29 C28 108.8(5) . . ? C30 C29 H18 125.6 . . ? C28 C29 H18 125.6 . . ? C29 C30 C31 107.2(5) . . ? C29 C30 H19 126.4 . . ? C31 C30 H19 126.4 . . ? C32 C31 C30 128.8(5) . . ? C32 C31 N3 122.4(4) . . ? C30 C31 N3 108.2(4) . . ? C31 C32 C33 119.6(4) . . ? C31 C32 C49 119.6(4) . . ? C33 C32 C49 120.7(4) . . ? C34 C33 N4 108.6(4) . . ? C34 C33 C32 129.3(5) . . ? N4 C33 C32 122.1(4) . . ? C35 C34 C33 107.3(4) . . ? C35 C34 H20 126.4 . . ? C33 C34 H20 126.4 . . ? C34 C35 C36 108.6(4) . . ? C34 C35 H21 125.7 . . ? C36 C35 H21 125.7 . . ? N4 C36 C35 108.9(4) . . ? N4 C36 C37 127.8(4) . . ? C35 C36 C37 123.3(4) . . ? C38 C37 C42 119.0(5) . . ? C38 C37 C36 117.8(5) . . ? C42 C37 C36 122.9(5) . . ? C37 C38 C39 120.0(5) . . ? C37 C38 H22 120.0 . . ? C39 C38 H22 120.0 . . ? C40 C39 C38 120.2(5) . . ? C40 C39 H23 119.9 . . ? C38 C39 H23 119.9 . . ? C39 C40 C41 120.8(5) . . ? C39 C40 H24 119.6 . . ? C41 C40 H24 119.6 . . ? C40 C41 C42 119.8(6) . . ? C40 C41 H25 120.1 . . ? C42 C41 H25 120.1 . . ? C41 C42 C37 120.1(5) . . ? C41 C42 H26 120.0 . . ? C37 C42 H26 120.0 . . ? C48 C43 C44 118.9(6) . . ? C48 C43 C28 122.2(5) . . ? C44 C43 C28 118.6(6) . . ? C45 C44 C43 120.4(7) . . ? C45 C44 H27 119.8 . . ? C43 C44 H27 119.8 . . ? C46 C45 C44 120.7(6) . . ? C46 C45 H28 119.6 . . ? C44 C45 H28 119.6 . . ? C45 C46 C47 119.9(6) . . ? C45 C46 H29 120.0 . . ? C47 C46 H29 120.0 . . ? C46 C47 C48 119.6(7) . . ? C46 C47 H30 120.2 . . ? C48 C47 H30 120.2 . . ? C43 C48 C47 120.4(6) . . ? C43 C48 H31 119.8 . . ? C47 C48 H31 119.8 . . ? C28 N3 C31 107.2(4) . . ? C28 N3 B2 127.7(4) . 15_565 ? C31 N3 B2 124.7(4) . 15_565 ? C36 N4 C33 106.6(4) . . ? C36 N4 B2 128.3(4) . 15_565 ? C33 N4 B2 124.0(4) . 15_565 ? C50 C49 C54 116.7(4) . . ? C50 C49 C32 122.5(4) . . ? C54 C49 C32 120.8(4) . . ? O4 C50 C51 111.1(4) . . ? O4 C50 C49 127.9(4) . . ? C51 C50 C49 120.9(4) . . ? C52 C51 O3 128.3(4) . . ? C52 C51 C50 121.9(4) . . ? O3 C51 C50 109.8(4) . . ? C51 C52 C53 118.1(4) . . ? C51 C52 H32 120.9 . . ? C53 C52 H32 120.9 . . ? C52 C53 C54 121.3(5) . . ? C52 C53 H33 119.3 . . ? C54 C53 H33 119.3 . . ? C53 C54 C49 121.0(5) . . ? C53 C54 H34 119.5 . . ? C49 C54 H34 119.5 . . ? C51 O3 B2 107.0(4) . . ? C50 O4 B2 106.3(3) . . ? O3 B2 O4 105.8(4) . . ? O3 B2 N3 108.9(4) . 16_655 ? O4 B2 N3 112.5(4) . 16_655 ? O3 B2 N4 113.3(4) . 16_655 ? O4 B2 N4 110.7(4) . 16_655 ? N3 B2 N4 105.9(4) 16_655 16_655 ? C56 C55 H35 109.5 . . ? C56 C55 H36 109.5 . . ? H35 C55 H36 109.5 . . ? C56 C55 H37 109.5 . . ? H35 C55 H37 109.5 . . ? H36 C55 H37 109.5 . . ? O5 C56 O6 119.9(10) . . ? O5 C56 C55 126.0(11) . . ? O6 C56 C55 114.1(10) . . ? C56 O6 C57 114.0(8) . . ? O6 C57 C58 97.1(9) . . ? O6 C57 H38 112.3 . . ? C58 C57 H38 112.3 . . ? O6 C57 H39 112.3 . . ? C58 C57 H39 112.3 . . ? H38 C57 H39 109.9 . . ? C57 C58 H40 109.5 . . ? C57 C58 H41 109.5 . . ? H40 C58 H41 109.5 . . ? C57 C58 H42 109.5 . . ? H40 C58 H42 109.5 . . ? H41 C58 H42 109.5 . . ? C60 C59 C64 120.0 . . ? C60 C59 H49 120.0 . . ? C64 C59 H49 120.0 . . ? C59 C60 C61 120.0 . . ? C59 C60 H50 120.0 . . ? C61 C60 H50 120.0 . . ? C62 C61 C60 120.0 . . ? C62 C61 H51 120.0 . . ? C60 C61 H51 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H52 120.0 . . ? C63 C62 H52 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 H53 120.0 . . ? C62 C63 H53 120.0 . . ? C63 C64 C59 120.0 . . ? C63 C64 H54 120.0 . . ? C59 C64 H54 120.0 . . ? C66 C65 C70 120.0 . . ? C66 C65 H55 120.0 . . ? C70 C65 H55 120.0 . . ? C65 C66 C67 120.0 . . ? C65 C66 H56 120.0 . . ? C67 C66 H56 120.0 . . ? C68 C67 C66 120.0 . . ? C68 C67 H57 120.0 . . ? C66 C67 H57 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H58 120.0 . . ? C69 C68 H58 120.0 . . ? C68 C69 C70 120.0 . . ? C68 C69 H59 120.0 . . ? C70 C69 H59 120.0 . . ? C69 C70 C65 120.0 . . ? C69 C70 H60 120.0 . . ? C65 C70 H60 120.0 . . ? C72 C71 C76 120.0 . . ? C72 C71 H61 120.0 . . ? C76 C71 H61 120.0 . . ? C71 C72 C73 120.0 . . ? C71 C72 H62 120.0 . . ? C73 C72 H62 120.0 . . ? C72 C73 C74 120.0 . . ? C72 C73 H63 120.0 . . ? C74 C73 H63 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H64 120.0 . . ? C75 C74 H64 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 H65 120.0 . . ? C74 C75 H65 120.0 . . ? C75 C76 C71 120.0 . . ? C75 C76 H66 120.0 . . ? C71 C76 H66 120.0 . . ? 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 -0.8(6) . . . . ? C10 C1 C2 C3 176.9(5) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? C2 C3 C4 C5 -179.5(5) . . . . ? C2 C3 C4 N1 -0.1(6) . . . . ? C3 C4 C5 C6 -178.8(5) . . . . ? N1 C4 C5 C6 1.9(6) . . . . ? C3 C4 C5 C22 7.9(7) . . . . ? N1 C4 C5 C22 -171.4(4) . . . . ? C4 C5 C6 N2 1.3(6) . . . . ? C22 C5 C6 N2 174.6(4) . . . . ? C4 C5 C6 C7 -169.1(5) . . . . ? C22 C5 C6 C7 4.2(7) . . . . ? N2 C6 C7 C8 -0.9(5) . . . . ? C5 C6 C7 C8 170.4(5) . . . . ? C6 C7 C8 C9 0.6(6) . . . . ? C7 C8 C9 N2 -0.1(6) . . . . ? C7 C8 C9 C16 -177.3(5) . . . . ? N1 C1 C10 C15 -132.8(5) . . . . ? C2 C1 C10 C15 49.9(7) . . . . ? N1 C1 C10 C11 53.6(7) . . . . ? C2 C1 C10 C11 -123.7(5) . . . . ? C15 C10 C11 C12 1.4(7) . . . . ? C1 C10 C11 C12 175.0(4) . . . . ? C10 C11 C12 C13 -0.1(7) . . . . ? C11 C12 C13 C14 -0.3(7) . . . . ? C12 C13 C14 C15 -0.7(8) . . . . ? C13 C14 C15 C10 2.0(8) . . . . ? C11 C10 C15 C14 -2.3(7) . . . . ? C1 C10 C15 C14 -176.2(4) . . . . ? N2 C9 C16 C17 74.6(6) . . . . ? C8 C9 C16 C17 -108.6(6) . . . . ? N2 C9 C16 C21 -110.3(5) . . . . ? C8 C9 C16 C21 66.5(6) . . . . ? C21 C16 C17 C18 -0.1(7) . . . . ? C9 C16 C17 C18 175.0(4) . . . . ? C16 C17 C18 C19 0.7(7) . . . . ? C17 C18 C19 C20 -1.2(7) . . . . ? C18 C19 C20 C21 1.1(8) . . . . ? C19 C20 C21 C16 -0.6(8) . . . . ? C17 C16 C21 C20 0.1(7) . . . . ? C9 C16 C21 C20 -175.2(4) . . . . ? C2 C1 N1 C4 0.7(5) . . . . ? C10 C1 N1 C4 -176.9(4) . . . . ? C2 C1 N1 B1 -167.4(4) . . . 16_645 ? C10 C1 N1 B1 15.0(7) . . . 16_645 ? C3 C4 N1 C1 -0.4(5) . . . . ? C5 C4 N1 C1 179.1(4) . . . . ? C3 C4 N1 B1 168.5(4) . . . 16_645 ? C5 C4 N1 B1 -12.0(6) . . . 16_645 ? C8 C9 N2 C6 -0.5(5) . . . . ? C16 C9 N2 C6 176.6(4) . . . . ? C8 C9 N2 B1 -177.2(4) . . . 16_645 ? C16 C9 N2 B1 0.0(7) . . . 16_645 ? C5 C6 N2 C9 -171.1(4) . . . . ? C7 C6 N2 C9 0.9(5) . . . . ? C5 C6 N2 B1 5.7(6) . . . 16_645 ? C7 C6 N2 B1 177.7(4) . . . 16_645 ? C6 C5 C22 C27 63.9(6) . . . . ? C4 C5 C22 C27 -122.9(5) . . . . ? C6 C5 C22 C23 -113.9(5) . . . . ? C4 C5 C22 C23 59.4(6) . . . . ? C27 C22 C23 C24 -2.0(6) . . . . ? C5 C22 C23 C24 176.0(4) . . . . ? C22 C23 C24 C25 2.4(7) . . . . ? C23 C24 C25 C26 -0.3(7) . . . . ? C24 C25 C26 O2 177.7(4) . . . . ? C24 C25 C26 C27 -2.2(6) . . . . ? C23 C22 C27 O1 -178.6(4) . . . . ? C5 C22 C27 O1 3.6(7) . . . . ? C23 C22 C27 C26 -0.5(6) . . . . ? C5 C22 C27 C26 -178.4(4) . . . . ? O2 C26 C27 O1 1.0(5) . . . . ? C25 C26 C27 O1 -179.0(4) . . . . ? O2 C26 C27 C22 -177.3(4) . . . . ? C25 C26 C27 C22 2.7(6) . . . . ? C22 C27 O1 B1 176.1(4) . . . . ? C26 C27 O1 B1 -2.1(4) . . . . ? C25 C26 O2 B1 -179.5(4) . . . . ? C27 C26 O2 B1 0.5(4) . . . . ? C26 O2 B1 O1 -1.7(4) . . . . ? C26 O2 B1 N2 119.7(4) . . . 15_665 ? C26 O2 B1 N1 -121.6(4) . . . 15_665 ? C27 O1 B1 O2 2.3(4) . . . . ? C27 O1 B1 N2 -117.8(4) . . . 15_665 ? C27 O1 B1 N1 123.8(3) . . . 15_665 ? N3 C28 C29 C30 0.7(8) . . . . ? C43 C28 C29 C30 -178.6(6) . . . . ? C28 C29 C30 C31 -0.6(8) . . . . ? C29 C30 C31 C32 -170.9(6) . . . . ? C29 C30 C31 N3 0.3(7) . . . . ? C30 C31 C32 C33 165.8(5) . . . . ? N3 C31 C32 C33 -4.4(7) . . . . ? C30 C31 C32 C49 -11.2(8) . . . . ? N3 C31 C32 C49 178.7(4) . . . . ? C31 C32 C33 C34 -179.6(5) . . . . ? C49 C32 C33 C34 -2.7(8) . . . . ? C31 C32 C33 N4 -0.8(7) . . . . ? C49 C32 C33 N4 176.1(4) . . . . ? N4 C33 C34 C35 1.1(6) . . . . ? C32 C33 C34 C35 -180.0(5) . . . . ? C33 C34 C35 C36 -0.7(6) . . . . ? C34 C35 C36 N4 0.1(6) . . . . ? C34 C35 C36 C37 -178.8(5) . . . . ? N4 C36 C37 C38 136.2(5) . . . . ? C35 C36 C37 C38 -45.2(7) . . . . ? N4 C36 C37 C42 -49.4(7) . . . . ? C35 C36 C37 C42 129.2(5) . . . . ? C42 C37 C38 C39 2.8(7) . . . . ? C36 C37 C38 C39 177.5(4) . . . . ? C37 C38 C39 C40 -1.9(7) . . . . ? C38 C39 C40 C41 0.4(8) . . . . ? C39 C40 C41 C42 0.1(8) . . . . ? C40 C41 C42 C37 0.9(8) . . . . ? C38 C37 C42 C41 -2.4(7) . . . . ? C36 C37 C42 C41 -176.7(5) . . . . ? N3 C28 C43 C48 -61.2(9) . . . . ? C29 C28 C43 C48 117.9(7) . . . . ? N3 C28 C43 C44 124.4(6) . . . . ? C29 C28 C43 C44 -56.4(9) . . . . ? C48 C43 C44 C45 0.2(8) . . . . ? C28 C43 C44 C45 174.8(5) . . . . ? C43 C44 C45 C46 0.0(9) . . . . ? C44 C45 C46 C47 -0.2(10) . . . . ? C45 C46 C47 C48 0.1(10) . . . . ? C44 C43 C48 C47 -0.3(8) . . . . ? C28 C43 C48 C47 -174.6(5) . . . . ? C46 C47 C48 C43 0.1(9) . . . . ? C29 C28 N3 C31 -0.5(7) . . . . ? C43 C28 N3 C31 178.8(6) . . . . ? C29 C28 N3 B2 171.6(5) . . . 15_565 ? C43 C28 N3 B2 -9.1(10) . . . 15_565 ? C32 C31 N3 C28 172.0(5) . . . . ? C30 C31 N3 C28 0.1(6) . . . . ? C32 C31 N3 B2 -0.4(7) . . . 15_565 ? C30 C31 N3 B2 -172.3(5) . . . 15_565 ? C35 C36 N4 C33 0.6(5) . . . . ? C37 C36 N4 C33 179.4(5) . . . . ? C35 C36 N4 B2 169.0(4) . . . 15_565 ? C37 C36 N4 B2 -12.2(8) . . . 15_565 ? C34 C33 N4 C36 -1.1(5) . . . . ? C32 C33 N4 C36 179.9(4) . . . . ? C34 C33 N4 B2 -170.1(4) . . . 15_565 ? C32 C33 N4 B2 10.9(7) . . . 15_565 ? C31 C32 C49 C50 -54.8(7) . . . . ? C33 C32 C49 C50 128.3(5) . . . . ? C31 C32 C49 C54 124.1(5) . . . . ? C33 C32 C49 C54 -52.8(6) . . . . ? C54 C49 C50 O4 178.6(4) . . . . ? C32 C49 C50 O4 -2.5(7) . . . . ? C54 C49 C50 C51 2.4(6) . . . . ? C32 C49 C50 C51 -178.7(4) . . . . ? O4 C50 C51 C52 179.8(4) . . . . ? C49 C50 C51 C52 -3.4(7) . . . . ? O4 C50 C51 O3 0.8(5) . . . . ? C49 C50 C51 O3 177.5(4) . . . . ? O3 C51 C52 C53 -179.0(4) . . . . ? C50 C51 C52 C53 2.2(7) . . . . ? C51 C52 C53 C54 -0.1(7) . . . . ? C52 C53 C54 C49 -0.8(8) . . . . ? C50 C49 C54 C53 -0.4(7) . . . . ? C32 C49 C54 C53 -179.3(4) . . . . ? C52 C51 O3 B2 180.0(5) . . . . ? C50 C51 O3 B2 -1.1(5) . . . . ? C51 C50 O4 B2 -0.1(5) . . . . ? C49 C50 O4 B2 -176.6(4) . . . . ? C51 O3 B2 O4 1.0(4) . . . . ? C51 O3 B2 N3 -120.2(4) . . . 16_655 ? C51 O3 B2 N4 122.4(4) . . . 16_655 ? C50 O4 B2 O3 -0.5(4) . . . . ? C50 O4 B2 N3 118.2(4) . . . 16_655 ? C50 O4 B2 N4 -123.6(4) . . . 16_655 ? O5 C56 O6 C57 -4.5(13) . . . . ? C55 C56 O6 C57 174.2(7) . . . . ? C56 O6 C57 C58 120.3(10) . . . . ? C64 C59 C60 C61 0.0 . . . . ? C59 C60 C61 C62 0.0 . . . . ? C60 C61 C62 C63 0.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C59 0.0 . . . . ? C60 C59 C64 C63 0.0 . . . . ? C70 C65 C66 C67 0.0 . . . . ? C65 C66 C67 C68 0.0 . . . . ? C66 C67 C68 C69 0.0 . . . . ? C67 C68 C69 C70 0.0 . . . . ? C68 C69 C70 C65 0.0 . . . . ? C66 C65 C70 C69 0.0 . . . . ? C76 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C71 0.0 . . . . ? C72 C71 C76 C75 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.584 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.066