# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Biao Wu' _publ_contact_author_email wubiao@lzb.ac.cn loop_ _publ_author_name 'Li Shaoguang' 'Meiying Wei' 'Xiao-Juan Yang' 'Biao Wu' data_(TEA)4LCl4 _database_code_depnum_ccdc_archive 'CCDC 849100' #TrackingRef 'complexes 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H122 Cl4 N18 O11' _chemical_formula_weight 1605.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.207(4) _cell_length_b 18.232(4) _cell_length_c 19.617(5) _cell_angle_alpha 99.111(4) _cell_angle_beta 103.442(5) _cell_angle_gamma 105.631(4) _cell_volume 5276(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3849 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _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 1.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.166 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9520 _exptl_absorpt_correction_T_max 0.9676 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36009 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.32 _reflns_number_total 18716 _reflns_number_gt 8451 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5037P] 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 18716 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1411 _refine_ls_R_factor_gt 0.0780 _refine_ls_wR_factor_ref 0.2272 _refine_ls_wR_factor_gt 0.2044 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.003 _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 Cl1 Cl 0.65532(8) 0.51465(7) 0.71677(7) 0.0693(4) Uani 1 1 d . . . Cl2 Cl 0.35010(9) 0.31514(8) 0.61506(6) 0.0727(4) Uani 1 1 d . . . Cl3 Cl 0.02993(8) 0.15632(7) 0.59489(6) 0.0632(3) Uani 1 1 d . . . Cl4 Cl 0.80643(7) 0.01531(7) 0.71851(6) 0.0595(3) Uani 1 1 d . . . O1 O 1.1619(2) 0.7631(2) 0.8645(2) 0.0955(13) Uani 1 1 d . . . O2 O 1.2135(2) 0.70229(19) 0.93964(17) 0.0644(9) Uani 1 1 d . . . O3 O 0.81663(19) 0.43143(17) 0.92541(15) 0.0557(8) Uani 1 1 d . . . O4 O 0.5222(2) 0.46989(17) 0.86243(17) 0.0637(9) Uani 1 1 d . . . O5 O 0.5927(2) 0.75272(19) 0.83010(19) 0.0779(10) Uani 1 1 d . . . O6 O 0.9388(2) 0.7959(2) 0.74615(19) 0.0838(11) Uani 1 1 d . . . O7 O 1.0665(2) 1.13397(17) 0.84689(15) 0.0567(8) Uani 1 1 d . . . O8 O 0.8618(2) 1.21537(18) 0.94398(17) 0.0632(8) Uani 1 1 d . . . O9 O 0.5558(2) 0.9651(2) 1.0639(2) 0.0718(10) Uani 1 1 d . . . O10 O 0.5037(2) 0.8691(2) 0.9702(2) 0.0804(11) Uani 1 1 d . . . O11 O 0.2284(3) 0.2444(2) 0.7160(2) 0.1000(12) Uani 1 1 d . . . H11B H 0.2562 0.2784 0.6972 0.080 Uiso 1 1 d R . . H11C H 0.1805 0.2156 0.6839 0.080 Uiso 1 1 d R . . N1 N 1.1508(3) 0.7127(2) 0.8990(2) 0.0589(10) Uani 1 1 d . . . N2 N 0.8007(2) 0.5203(2) 0.85705(19) 0.0515(9) Uani 1 1 d . . . H2 H 0.7599 0.5352 0.8300 0.062 Uiso 1 1 calc R . . N3 N 0.6811(2) 0.4173(2) 0.84648(17) 0.0477(9) Uani 1 1 d . . . H3 H 0.6556 0.4398 0.8149 0.057 Uiso 1 1 calc R . . N4 N 0.5006(2) 0.36910(19) 0.76884(17) 0.0456(8) Uani 1 1 d . . . H4 H 0.4890 0.3549 0.7217 0.055 Uiso 1 1 calc R . . N5 N 0.4348(2) 0.4645(2) 0.75247(19) 0.0509(9) Uani 1 1 d . . . H5 H 0.4216 0.4464 0.7056 0.061 Uiso 1 1 calc R . . N6 N 0.5405(2) 0.6199(2) 0.78942(18) 0.0489(9) Uani 1 1 d . . . H6 H 0.5549 0.5796 0.7709 0.059 Uiso 1 1 calc R . . N7 N 0.6784(2) 0.6898(2) 0.78764(19) 0.0562(10) Uani 1 1 d . . . H7 H 0.6835 0.6439 0.7715 0.067 Uiso 1 1 calc R . . N8 N 0.8295(3) 0.8505(2) 0.7344(2) 0.0800(14) Uani 1 1 d . . . H8 H 0.8151 0.8935 0.7321 0.096 Uiso 1 1 calc R . . N9 N 0.9718(2) 0.9265(2) 0.75045(19) 0.0569(10) Uani 1 1 d . . . H9 H 0.9468 0.9632 0.7447 0.068 Uiso 1 1 calc R . . N10 N 1.0534(2) 1.07275(18) 0.73336(17) 0.0397(8) Uani 1 1 d . . . H10 H 1.0257 1.0649 0.6873 0.048 Uiso 1 1 calc R . . N11 N 1.0091(2) 1.18203(19) 0.75311(17) 0.0434(8) Uani 1 1 d . . . H11 H 0.9823 1.1702 0.7065 0.052 Uiso 1 1 calc R . . N12 N 0.8959(2) 1.18436(19) 0.83914(17) 0.0442(8) Uani 1 1 d . . . H12 H 0.8843 1.1452 0.8020 0.053 Uiso 1 1 calc R . . N13 N 0.7915(2) 1.09339(19) 0.86858(16) 0.0429(8) Uani 1 1 d . . . H13 H 0.7897 1.0644 0.8276 0.051 Uiso 1 1 calc R . . N14 N 0.5550(3) 0.9345(3) 1.0034(3) 0.0613(11) Uani 1 1 d . . . N15 N 0.3177(2) 0.3338(2) 0.97757(17) 0.0519(9) Uani 1 1 d . . . N16 N 0.7551(3) 0.9362(3) 0.47263(18) 0.0680(12) Uani 1 1 d . . . N17 N 0.2842(3) 0.7477(3) 0.3336(2) 0.0798(14) Uani 1 1 d . . . N18 N 1.0000 1.0000 1.0000 0.0637(17) Uani 1 2 d S . . N19 N 0.5456(10) 0.4766(7) 0.4874(7) 0.167(8) Uani 0.50 1 d P . . C1 C 1.0597(3) 0.6639(2) 0.8898(2) 0.0489(11) Uani 1 1 d . . . C2 C 0.9898(3) 0.6701(3) 0.8385(3) 0.0624(13) Uani 1 1 d . . . H2A H 0.9999 0.7073 0.8100 0.075 Uiso 1 1 calc R . . C3 C 0.9062(3) 0.6221(3) 0.8292(3) 0.0631(13) Uani 1 1 d . . . H3A H 0.8577 0.6255 0.7932 0.076 Uiso 1 1 calc R . . C4 C 0.8890(3) 0.5672(2) 0.8714(2) 0.0433(10) Uani 1 1 d . . . C5 C 0.9599(3) 0.5654(2) 0.9249(2) 0.0467(10) Uani 1 1 d . . . H5A H 0.9498 0.5309 0.9559 0.056 Uiso 1 1 calc R . . C6 C 1.0453(3) 0.6132(2) 0.9337(2) 0.0475(10) Uani 1 1 d . . . H6A H 1.0942 0.6111 0.9702 0.057 Uiso 1 1 calc R . . C7 C 0.7696(3) 0.4537(2) 0.8798(2) 0.0435(10) Uani 1 1 d . . . C8 C 0.6236(3) 0.3468(2) 0.8560(2) 0.0435(10) Uani 1 1 d . . . C9 C 0.6530(3) 0.3036(3) 0.9019(2) 0.0524(11) Uani 1 1 d . . . H9A H 0.7130 0.3215 0.9320 0.063 Uiso 1 1 calc R . . C10 C 0.5943(4) 0.2339(3) 0.9037(3) 0.0643(13) Uani 1 1 d . . . H10A H 0.6143 0.2041 0.9357 0.077 Uiso 1 1 calc R . . C11 C 0.5071(3) 0.2066(3) 0.8598(2) 0.0583(12) Uani 1 1 d . . . H11A H 0.4680 0.1575 0.8603 0.070 Uiso 1 1 calc R . . C12 C 0.4774(3) 0.2510(2) 0.8154(2) 0.0501(11) Uani 1 1 d . . . H12A H 0.4173 0.2328 0.7854 0.060 Uiso 1 1 calc R . . C13 C 0.5339(3) 0.3213(2) 0.8143(2) 0.0450(10) Uani 1 1 d . . . C14 C 0.4875(3) 0.4357(3) 0.7995(2) 0.0473(10) Uani 1 1 d . . . C15 C 0.4019(3) 0.5237(3) 0.7801(3) 0.0555(12) Uani 1 1 d . . . C16 C 0.3171(4) 0.5051(3) 0.7880(3) 0.0880(18) Uani 1 1 d . . . H16 H 0.2793 0.4521 0.7724 0.106 Uiso 1 1 calc R . . C17 C 0.2857(4) 0.5620(4) 0.8183(4) 0.117(3) Uani 1 1 d . . . H17 H 0.2269 0.5484 0.8233 0.141 Uiso 1 1 calc R . . C18 C 0.3418(5) 0.6393(4) 0.8413(5) 0.127(3) Uani 1 1 d . . . H18 H 0.3210 0.6785 0.8628 0.152 Uiso 1 1 calc R . . C19 C 0.4248(4) 0.6599(3) 0.8337(3) 0.0808(17) Uani 1 1 d . . . H19 H 0.4621 0.7131 0.8503 0.097 Uiso 1 1 calc R . . C20 C 0.4562(3) 0.6031(3) 0.8013(3) 0.0567(12) Uani 1 1 d . . . C21 C 0.6038(3) 0.6928(3) 0.8034(2) 0.0526(11) Uani 1 1 d . . . C22 C 0.7514(3) 0.7599(3) 0.7962(3) 0.0623(13) Uani 1 1 d . . . H22A H 0.8081 0.7533 0.8223 0.075 Uiso 1 1 calc R . . H22B H 0.7426 0.8047 0.8260 0.075 Uiso 1 1 calc R . . C23 C 0.7592(3) 0.7780(3) 0.7269(3) 0.0796(16) Uani 1 1 d . . . H23A H 0.7710 0.7342 0.6982 0.096 Uiso 1 1 calc R . . H23B H 0.7013 0.7815 0.6997 0.096 Uiso 1 1 calc R . . C24 C 0.9136(3) 0.8544(3) 0.7443(3) 0.0655(14) Uani 1 1 d . . . C25 C 1.0652(3) 0.9516(3) 0.7645(2) 0.0495(11) Uani 1 1 d . . . C26 C 1.1172(3) 0.9063(3) 0.7884(2) 0.0626(13) Uani 1 1 d . . . H26 H 1.0897 0.8552 0.7934 0.075 Uiso 1 1 calc R . . C27 C 1.2081(3) 0.9357(3) 0.8046(3) 0.0659(13) Uani 1 1 d . . . H27 H 1.2436 0.9053 0.8226 0.079 Uiso 1 1 calc R . . C28 C 1.2497(3) 1.0087(3) 0.7955(2) 0.0616(13) Uani 1 1 d . . . H28 H 1.3129 1.0276 0.8053 0.074 Uiso 1 1 calc R . . C29 C 1.1979(3) 1.0540(3) 0.7720(2) 0.0513(11) Uani 1 1 d . . . H29 H 1.2255 1.1049 0.7666 0.062 Uiso 1 1 calc R . . C30 C 1.1072(3) 1.0253(2) 0.7566(2) 0.0408(9) Uani 1 1 d . . . C31 C 1.0454(3) 1.1302(2) 0.7831(2) 0.0410(10) Uani 1 1 d . . . C32 C 1.0142(3) 1.2534(2) 0.7961(2) 0.0432(10) Uani 1 1 d . . . C33 C 1.0705(3) 1.3226(3) 0.7895(3) 0.0598(12) Uani 1 1 d . . . H33 H 1.1057 1.3213 0.7570 0.072 Uiso 1 1 calc R . . C34 C 1.0749(4) 1.3939(3) 0.8308(3) 0.0754(15) Uani 1 1 d . . . H34 H 1.1140 1.4415 0.8271 0.090 Uiso 1 1 calc R . . C35 C 1.0226(3) 1.3953(3) 0.8769(3) 0.0681(14) Uani 1 1 d . . . H35 H 1.0270 1.4438 0.9062 0.082 Uiso 1 1 calc R . . C36 C 0.9641(3) 1.3267(3) 0.8808(2) 0.0523(11) Uani 1 1 d . . . H36 H 0.9270 1.3286 0.9116 0.063 Uiso 1 1 calc R . . C37 C 0.9583(3) 1.2556(2) 0.8408(2) 0.0422(10) Uani 1 1 d . . . C38 C 0.8513(3) 1.1695(3) 0.8889(2) 0.0448(10) Uani 1 1 d . . . C39 C 0.7352(3) 1.0584(2) 0.9048(2) 0.0419(10) Uani 1 1 d . . . C40 C 0.7225(3) 1.0951(2) 0.9674(2) 0.0441(10) Uani 1 1 d . . . H40 H 0.7539 1.1491 0.9881 0.053 Uiso 1 1 calc R . . C41 C 0.6650(3) 1.0538(3) 0.9993(2) 0.0488(11) Uani 1 1 d . . . H41 H 0.6577 1.0792 1.0427 0.059 Uiso 1 1 calc R . . C42 C 0.6178(3) 0.9759(3) 0.9693(2) 0.0477(11) Uani 1 1 d . . . C43 C 0.6278(3) 0.9373(3) 0.9081(3) 0.0568(12) Uani 1 1 d . . . H43 H 0.5950 0.8834 0.8877 0.068 Uiso 1 1 calc R . . C44 C 0.6874(3) 0.9790(3) 0.8761(2) 0.0543(11) Uani 1 1 d . . . H44 H 0.6957 0.9527 0.8336 0.065 Uiso 1 1 calc R . . C45 C 0.3034(3) 0.2591(3) 0.9228(2) 0.0557(12) Uani 1 1 d . . . H45A H 0.2388 0.2363 0.8967 0.067 Uiso 1 1 calc R . . H45B H 0.3356 0.2728 0.8871 0.067 Uiso 1 1 calc R . . C46 C 0.3340(3) 0.1981(3) 0.9543(3) 0.0659(13) Uani 1 1 d . . . H46A H 0.3996 0.2153 0.9706 0.099 Uiso 1 1 calc R . . H46B H 0.3118 0.1486 0.9176 0.099 Uiso 1 1 calc R . . H46C H 0.3107 0.1904 0.9954 0.099 Uiso 1 1 calc R . . C47 C 0.4129(3) 0.3639(3) 1.0265(2) 0.0594(12) Uani 1 1 d . . . H47A H 0.4197 0.4125 1.0611 0.071 Uiso 1 1 calc R . . H47B H 0.4216 0.3248 1.0547 0.071 Uiso 1 1 calc R . . C48 C 0.4859(3) 0.3811(3) 0.9920(3) 0.0799(16) Uani 1 1 d . . . H48A H 0.4841 0.3327 0.9608 0.120 Uiso 1 1 calc R . . H48B H 0.5437 0.4029 1.0293 0.120 Uiso 1 1 calc R . . H48C H 0.4782 0.4192 0.9629 0.120 Uiso 1 1 calc R . . C49 C 0.2986(4) 0.3936(3) 0.9356(3) 0.0690(14) Uani 1 1 d . . . H49A H 0.3449 0.4073 0.9104 0.083 Uiso 1 1 calc R . . H49B H 0.2402 0.3687 0.8983 0.083 Uiso 1 1 calc R . . C50 C 0.2965(4) 0.4677(3) 0.9798(3) 0.0732(14) Uani 1 1 d . . . H50A H 0.2442 0.4562 0.9981 0.110 Uiso 1 1 calc R . . H50B H 0.2928 0.5055 0.9498 0.110 Uiso 1 1 calc R . . H50C H 0.3512 0.4898 1.0205 0.110 Uiso 1 1 calc R . . C51 C 0.2580(3) 0.3187(3) 1.0257(2) 0.0516(11) Uani 1 1 d . . . H51A H 0.2710 0.2780 1.0503 0.062 Uiso 1 1 calc R . . H51B H 0.2735 0.3673 1.0633 0.062 Uiso 1 1 calc R . . C52 C 0.1594(3) 0.2930(3) 0.9885(3) 0.0632(13) Uani 1 1 d . . . H52A H 0.1451 0.3335 0.9652 0.095 Uiso 1 1 calc R . . H52B H 0.1263 0.2847 1.0240 0.095 Uiso 1 1 calc R . . H52C H 0.1426 0.2440 0.9521 0.095 Uiso 1 1 calc R . . C53 C 0.8051(4) 1.0199(3) 0.4779(3) 0.0880(18) Uani 1 1 d . . . H53A H 0.8421 1.0446 0.5283 0.106 Uiso 1 1 calc R . . H53B H 0.7616 1.0482 0.4653 0.106 Uiso 1 1 calc R . . C54 C 0.8647(5) 1.0286(4) 0.4290(4) 0.139(3) Uani 1 1 d . . . H54A H 0.8931 0.9875 0.4290 0.209 Uiso 1 1 calc R . . H54B H 0.9109 1.0801 0.4464 0.209 Uiso 1 1 calc R . . H54C H 0.8287 1.0238 0.3799 0.209 Uiso 1 1 calc R . . C55 C 0.8187(4) 0.8911(4) 0.4920(3) 0.0903(19) Uani 1 1 d . . . H55A H 0.8526 0.8896 0.4561 0.108 Uiso 1 1 calc R . . H55B H 0.7838 0.8365 0.4891 0.108 Uiso 1 1 calc R . . C56 C 0.8851(4) 0.9260(4) 0.5675(3) 0.109(2) Uani 1 1 d . . . H56A H 0.9246 0.9779 0.5691 0.164 Uiso 1 1 calc R . . H56B H 0.9210 0.8916 0.5785 0.164 Uiso 1 1 calc R . . H56C H 0.8522 0.9308 0.6031 0.164 Uiso 1 1 calc R . . C57 C 0.6972(4) 0.8935(3) 0.3971(2) 0.0782(16) Uani 1 1 d . . . H57A H 0.6634 0.8398 0.3980 0.094 Uiso 1 1 calc R . . H57B H 0.7366 0.8888 0.3660 0.094 Uiso 1 1 calc R . . C58 C 0.6304(5) 0.9327(4) 0.3628(3) 0.114(2) Uani 1 1 d . . . H58A H 0.5955 0.9433 0.3957 0.171 Uiso 1 1 calc R . . H58B H 0.5899 0.8977 0.3171 0.171 Uiso 1 1 calc R . . H58C H 0.6631 0.9821 0.3537 0.171 Uiso 1 1 calc R . . C59 C 0.6988(4) 0.9366(4) 0.5244(3) 0.0736(16) Uani 1 1 d . . . H59A H 0.7376 0.9704 0.5718 0.088 Uiso 1 1 calc R . . H59B H 0.6524 0.9605 0.5065 0.088 Uiso 1 1 calc R . . C60 C 0.6543(4) 0.8590(4) 0.5347(3) 0.104(2) Uani 1 1 d . . . H60A H 0.6176 0.8241 0.4878 0.156 Uiso 1 1 calc R . . H60B H 0.6161 0.8644 0.5660 0.156 Uiso 1 1 calc R . . H60C H 0.6996 0.8369 0.5571 0.156 Uiso 1 1 calc R . . C61 C 0.3604(5) 0.7117(5) 0.3430(5) 0.144(3) Uani 1 1 d . . . H61A H 0.3413 0.6635 0.3604 0.173 Uiso 1 1 calc R . . H61B H 0.3684 0.6957 0.2950 0.173 Uiso 1 1 calc R . . C62 C 0.4463(5) 0.7608(6) 0.3916(4) 0.158(4) Uani 1 1 d . . . H62A H 0.4705 0.8051 0.3717 0.237 Uiso 1 1 calc R . . H62B H 0.4877 0.7301 0.3974 0.237 Uiso 1 1 calc R . . H62C H 0.4392 0.7803 0.4386 0.237 Uiso 1 1 calc R . . C63 C 0.3175(5) 0.8285(5) 0.3162(4) 0.121(3) Uani 1 1 d . . . H63A H 0.2678 0.8510 0.3105 0.145 Uiso 1 1 calc R . . H63B H 0.3663 0.8632 0.3588 0.145 Uiso 1 1 calc R . . C64 C 0.3498(6) 0.8321(5) 0.2533(4) 0.145(3) Uani 1 1 d . . . H64A H 0.3945 0.8049 0.2549 0.217 Uiso 1 1 calc R . . H64B H 0.3771 0.8870 0.2532 0.217 Uiso 1 1 calc R . . H64C H 0.2996 0.8068 0.2095 0.217 Uiso 1 1 calc R . . C65 C 0.2103(6) 0.6953(6) 0.2681(4) 0.141(3) Uani 1 1 d . . . H65A H 0.1633 0.7203 0.2565 0.169 Uiso 1 1 calc R . . H65B H 0.2347 0.6895 0.2265 0.169 Uiso 1 1 calc R . . C66 C 0.1694(6) 0.6158(5) 0.2794(4) 0.129(3) Uani 1 1 d . . . H66A H 0.2138 0.5882 0.2848 0.194 Uiso 1 1 calc R . . H66B H 0.1178 0.5859 0.2378 0.194 Uiso 1 1 calc R . . H66C H 0.1499 0.6214 0.3231 0.194 Uiso 1 1 calc R . . C67 C 0.2541(5) 0.7605(5) 0.3965(4) 0.127(3) Uani 1 1 d . . . H67A H 0.3044 0.7997 0.4353 0.153 Uiso 1 1 calc R . . H67B H 0.2410 0.7109 0.4125 0.153 Uiso 1 1 calc R . . C68 C 0.1752(5) 0.7872(5) 0.3904(5) 0.146(3) Uani 1 1 d . . . H68A H 0.1948 0.8445 0.4065 0.220 Uiso 1 1 calc R . . H68B H 0.1402 0.7638 0.4205 0.220 Uiso 1 1 calc R . . H68C H 0.1382 0.7711 0.3400 0.220 Uiso 1 1 calc R . . C69 C 0.8956(5) 0.9629(7) 0.9566(6) 0.078(3) Uani 0.50 1 d P . . C70 C 1.0055(5) 0.8640(4) 0.9414(4) 0.113(2) Uani 1 1 d . . . C71 C 0.8495(3) 0.9428(4) 1.0241(4) 0.106(2) Uani 1 1 d . . . C72 C 1.0244(6) 0.9164(6) 1.0120(7) 0.144(5) Uani 0.75 1 d P . . C73 C 0.5497(15) 0.4913(13) 0.4257(12) 0.300(10) Uani 1 1 d D . . C74 C 0.635(2) 0.471(2) 0.4083(11) 0.64(3) Uani 1 1 d D . . C75 C 0.509(2) 0.3907(17) 0.4907(16) 0.413(15) Uani 1 1 d . . . C76 C 0.4125(19) 0.363(2) 0.4252(12) 0.50(2) Uani 1 1 d . . . C69A C 0.9613(6) 0.9776(8) 1.0591(6) 0.085(4) Uani 0.50 1 d P . . C72A C 0.9739(9) 0.9474(7) 0.9301(7) 0.024(3) Uani 0.25 1 d P . . 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 Cl1 0.0558(7) 0.0601(8) 0.0848(9) 0.0297(7) 0.0034(6) 0.0142(6) Cl2 0.0688(8) 0.0668(9) 0.0603(8) 0.0019(6) 0.0002(6) 0.0094(7) Cl3 0.0723(8) 0.0703(9) 0.0551(7) 0.0142(6) 0.0329(6) 0.0236(7) Cl4 0.0565(7) 0.0626(8) 0.0479(6) -0.0006(5) 0.0136(5) 0.0098(6) O1 0.057(2) 0.078(3) 0.144(4) 0.070(3) 0.010(2) 0.001(2) O2 0.0449(19) 0.065(2) 0.078(2) 0.0175(18) 0.0080(16) 0.0174(17) O3 0.0479(18) 0.056(2) 0.0634(19) 0.0223(16) 0.0126(15) 0.0154(16) O4 0.075(2) 0.0419(19) 0.059(2) 0.0039(16) -0.0053(17) 0.0219(17) O5 0.091(3) 0.031(2) 0.104(3) 0.0076(18) 0.042(2) -0.0006(18) O6 0.073(2) 0.061(2) 0.102(3) 0.044(2) 0.007(2) -0.001(2) O7 0.077(2) 0.052(2) 0.0426(18) 0.0120(15) 0.0124(15) 0.0254(17) O8 0.068(2) 0.052(2) 0.059(2) 0.0006(16) 0.0325(17) -0.0008(17) O9 0.061(2) 0.093(3) 0.093(3) 0.053(2) 0.046(2) 0.037(2) O10 0.065(2) 0.055(2) 0.135(3) 0.040(2) 0.053(2) 0.011(2) O11 0.087(3) 0.111(3) 0.091(3) 0.019(2) 0.033(2) 0.011(2) N1 0.047(2) 0.041(2) 0.079(3) 0.015(2) 0.008(2) 0.007(2) N2 0.043(2) 0.042(2) 0.070(2) 0.0256(19) 0.0093(18) 0.0123(18) N3 0.046(2) 0.041(2) 0.052(2) 0.0203(17) 0.0068(17) 0.0097(18) N4 0.053(2) 0.034(2) 0.0415(19) 0.0085(16) 0.0069(16) 0.0067(17) N5 0.046(2) 0.038(2) 0.060(2) 0.0154(18) 0.0041(17) 0.0061(18) N6 0.043(2) 0.033(2) 0.071(2) 0.0159(18) 0.0204(18) 0.0067(17) N7 0.049(2) 0.040(2) 0.074(3) 0.0174(19) 0.0239(19) -0.0039(18) N8 0.042(3) 0.064(3) 0.127(4) 0.058(3) 0.009(2) -0.003(2) N9 0.042(2) 0.043(2) 0.080(3) 0.035(2) 0.0088(18) 0.0001(18) N10 0.0377(19) 0.0310(19) 0.0432(19) 0.0044(15) 0.0098(15) 0.0035(16) N11 0.043(2) 0.037(2) 0.048(2) 0.0115(17) 0.0132(16) 0.0085(17) N12 0.044(2) 0.039(2) 0.0440(19) 0.0062(16) 0.0176(16) 0.0027(17) N13 0.044(2) 0.040(2) 0.0395(19) 0.0049(16) 0.0177(16) 0.0031(17) N14 0.046(2) 0.062(3) 0.096(3) 0.039(3) 0.033(2) 0.027(2) N15 0.064(2) 0.036(2) 0.046(2) 0.0073(17) 0.0170(18) 0.0009(18) N16 0.078(3) 0.080(3) 0.038(2) -0.005(2) 0.013(2) 0.026(3) N17 0.065(3) 0.124(4) 0.055(3) -0.002(3) 0.007(2) 0.058(3) N18 0.026(3) 0.086(4) 0.083(4) 0.060(4) 0.006(3) 0.008(3) N19 0.221(17) 0.084(10) 0.084(8) 0.053(8) -0.071(10) -0.053(9) C1 0.045(3) 0.035(3) 0.062(3) 0.013(2) 0.008(2) 0.011(2) C2 0.050(3) 0.051(3) 0.082(3) 0.035(3) 0.007(2) 0.008(2) C3 0.048(3) 0.056(3) 0.079(3) 0.029(3) 0.000(2) 0.014(3) C4 0.045(3) 0.032(2) 0.049(2) 0.0054(19) 0.010(2) 0.013(2) C5 0.055(3) 0.040(3) 0.042(2) 0.0083(19) 0.010(2) 0.015(2) C6 0.044(3) 0.041(3) 0.050(3) 0.004(2) 0.005(2) 0.013(2) C7 0.041(3) 0.037(3) 0.052(3) 0.015(2) 0.011(2) 0.011(2) C8 0.047(3) 0.040(3) 0.044(2) 0.008(2) 0.013(2) 0.016(2) C9 0.056(3) 0.047(3) 0.058(3) 0.024(2) 0.018(2) 0.015(2) C10 0.081(4) 0.053(3) 0.076(3) 0.035(3) 0.034(3) 0.029(3) C11 0.063(3) 0.047(3) 0.069(3) 0.017(2) 0.024(3) 0.017(3) C12 0.063(3) 0.032(3) 0.054(3) 0.008(2) 0.021(2) 0.011(2) C13 0.055(3) 0.033(2) 0.045(2) 0.0089(19) 0.013(2) 0.012(2) C14 0.042(2) 0.037(3) 0.051(3) 0.013(2) 0.001(2) 0.004(2) C15 0.042(3) 0.051(3) 0.078(3) 0.032(3) 0.016(2) 0.013(2) C16 0.056(3) 0.063(4) 0.152(6) 0.060(4) 0.031(3) 0.010(3) C17 0.074(4) 0.103(6) 0.236(8) 0.097(6) 0.091(5) 0.054(4) C18 0.097(5) 0.077(5) 0.261(10) 0.077(6) 0.105(6) 0.050(4) C19 0.065(4) 0.048(3) 0.152(5) 0.038(3) 0.052(4) 0.028(3) C20 0.048(3) 0.046(3) 0.083(3) 0.031(3) 0.026(2) 0.012(2) C21 0.054(3) 0.038(3) 0.058(3) 0.020(2) 0.010(2) 0.004(2) C22 0.050(3) 0.045(3) 0.074(3) 0.020(2) 0.011(2) -0.009(2) C23 0.048(3) 0.077(4) 0.099(4) 0.049(3) 0.007(3) -0.007(3) C24 0.060(3) 0.049(3) 0.085(4) 0.044(3) 0.009(3) 0.008(3) C25 0.049(3) 0.043(3) 0.053(3) 0.014(2) 0.007(2) 0.016(2) C26 0.052(3) 0.057(3) 0.068(3) 0.019(3) 0.001(2) 0.012(3) C27 0.061(3) 0.056(3) 0.079(3) 0.019(3) 0.009(3) 0.024(3) C28 0.043(3) 0.064(4) 0.069(3) 0.001(3) 0.009(2) 0.019(3) C29 0.045(3) 0.046(3) 0.051(3) 0.003(2) 0.008(2) 0.007(2) C30 0.038(2) 0.035(2) 0.042(2) 0.0066(19) 0.0079(18) 0.005(2) C31 0.037(2) 0.033(2) 0.045(3) 0.011(2) 0.0083(19) 0.0008(19) C32 0.042(2) 0.040(3) 0.048(2) 0.015(2) 0.0128(19) 0.012(2) C33 0.060(3) 0.054(3) 0.073(3) 0.026(3) 0.036(3) 0.011(3) C34 0.095(4) 0.039(3) 0.095(4) 0.021(3) 0.042(3) 0.010(3) C35 0.077(4) 0.038(3) 0.090(4) 0.010(3) 0.031(3) 0.016(3) C36 0.065(3) 0.038(3) 0.061(3) 0.016(2) 0.027(2) 0.017(2) C37 0.041(2) 0.036(3) 0.046(2) 0.009(2) 0.0116(19) 0.009(2) C38 0.047(3) 0.046(3) 0.045(3) 0.011(2) 0.019(2) 0.015(2) C39 0.035(2) 0.041(3) 0.046(2) 0.011(2) 0.0057(19) 0.011(2) C40 0.040(2) 0.040(3) 0.055(3) 0.015(2) 0.018(2) 0.009(2) C41 0.037(2) 0.061(3) 0.057(3) 0.024(2) 0.020(2) 0.019(2) C42 0.035(2) 0.049(3) 0.067(3) 0.027(2) 0.020(2) 0.015(2) C43 0.046(3) 0.049(3) 0.077(3) 0.020(3) 0.024(2) 0.009(2) C44 0.046(3) 0.052(3) 0.065(3) 0.009(2) 0.020(2) 0.015(2) C45 0.062(3) 0.042(3) 0.052(3) -0.004(2) 0.014(2) 0.009(2) C46 0.058(3) 0.045(3) 0.085(4) 0.003(3) 0.025(3) 0.004(2) C47 0.062(3) 0.036(3) 0.057(3) -0.004(2) 0.014(2) -0.009(2) C48 0.070(3) 0.072(4) 0.071(3) -0.005(3) 0.034(3) -0.018(3) C49 0.091(4) 0.060(3) 0.070(3) 0.023(3) 0.038(3) 0.029(3) C50 0.084(4) 0.042(3) 0.087(4) 0.012(3) 0.028(3) 0.007(3) C51 0.061(3) 0.045(3) 0.047(2) 0.011(2) 0.025(2) 0.007(2) C52 0.058(3) 0.050(3) 0.072(3) 0.005(2) 0.021(2) 0.004(2) C53 0.112(5) 0.071(4) 0.059(3) -0.009(3) 0.016(3) 0.016(4) C54 0.148(7) 0.121(6) 0.082(5) -0.010(4) 0.035(5) -0.045(5) C55 0.079(4) 0.103(5) 0.086(4) -0.012(3) 0.019(3) 0.047(4) C56 0.082(4) 0.136(6) 0.110(5) 0.002(4) 0.007(4) 0.067(4) C57 0.096(4) 0.073(4) 0.051(3) 0.000(3) 0.015(3) 0.017(3) C58 0.160(6) 0.076(4) 0.058(4) 0.007(3) -0.019(4) 0.011(4) C59 0.071(3) 0.109(5) 0.049(3) 0.006(3) 0.015(3) 0.051(4) C60 0.113(5) 0.117(6) 0.079(4) 0.026(4) 0.041(4) 0.020(5) C61 0.117(7) 0.169(8) 0.148(7) 0.047(6) 0.006(5) 0.070(6) C62 0.082(5) 0.259(12) 0.149(7) 0.077(7) 0.015(5) 0.080(7) C63 0.137(6) 0.151(8) 0.105(5) 0.029(5) 0.052(5) 0.083(6) C64 0.167(8) 0.192(9) 0.109(6) 0.042(6) 0.037(5) 0.109(7) C65 0.132(7) 0.184(10) 0.093(5) -0.011(6) -0.002(5) 0.081(7) C66 0.145(7) 0.124(7) 0.114(6) -0.004(5) 0.040(5) 0.053(6) C67 0.125(6) 0.143(7) 0.110(5) -0.001(5) 0.051(5) 0.040(5) C68 0.093(5) 0.160(8) 0.195(8) -0.013(6) 0.074(5) 0.057(5) C69 0.016(4) 0.106(9) 0.130(9) 0.089(7) 0.016(5) 0.017(5) C70 0.097(5) 0.094(5) 0.108(5) -0.021(4) 0.018(4) 0.001(4) C71 0.043(3) 0.140(6) 0.164(6) 0.103(5) 0.048(3) 0.024(3) C72 0.089(7) 0.111(8) 0.208(12) 0.089(9) -0.027(7) 0.025(6) C73 0.34(2) 0.247(18) 0.234(19) -0.006(15) -0.043(16) 0.110(18) C74 1.11(9) 0.59(5) 0.198(19) 0.29(3) 0.07(3) 0.24(5) C75 0.54(4) 0.40(3) 0.45(3) 0.29(3) 0.22(3) 0.22(3) C76 0.41(3) 0.61(5) 0.26(2) -0.05(2) -0.13(2) 0.10(3) C69A 0.042(6) 0.129(11) 0.091(8) 0.068(8) 0.018(5) 0.016(7) C72A 0.031(8) 0.012(7) 0.013(7) 0.010(6) -0.010(5) -0.011(6) _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 O1 N1 1.225(4) . ? O2 N1 1.216(4) . ? O3 C7 1.229(4) . ? O4 C14 1.214(5) . ? O5 C21 1.213(5) . ? O6 C24 1.243(5) . ? O7 C31 1.203(4) . ? O8 C38 1.203(4) . ? O9 N14 1.225(5) . ? O10 N14 1.226(5) . ? N1 C1 1.456(6) . ? N2 C7 1.369(5) . ? N2 C4 1.391(5) . ? N3 C7 1.356(5) . ? N3 C8 1.438(5) . ? N4 C14 1.360(5) . ? N4 C13 1.457(5) . ? N5 C14 1.373(5) . ? N5 C15 1.415(5) . ? N6 C21 1.382(5) . ? N6 C20 1.400(5) . ? N7 C21 1.328(5) . ? N7 C22 1.444(5) . ? N8 C24 1.312(6) . ? N8 C23 1.456(6) . ? N9 C24 1.365(6) . ? N9 C25 1.403(5) . ? N10 C31 1.370(5) . ? N10 C30 1.435(5) . ? N11 C31 1.378(5) . ? N11 C32 1.404(5) . ? N12 C38 1.362(5) . ? N12 C37 1.405(5) . ? N13 C39 1.370(5) . ? N13 C38 1.394(5) . ? N14 C42 1.454(6) . ? N15 C51 1.506(5) . ? N15 C47 1.513(5) . ? N15 C49 1.520(5) . ? N15 C45 1.521(5) . ? N16 C53 1.497(7) . ? N16 C55 1.502(6) . ? N16 C57 1.509(6) . ? N16 C59 1.515(6) . ? N17 C67 1.438(7) . ? N17 C65 1.508(8) . ? N17 C61 1.536(8) . ? N17 C63 1.547(9) . ? N18 C72A 1.440(13) . ? N18 C72A 1.440(13) 2_777 ? N18 C69A 1.502(10) . ? N18 C69A 1.502(10) 2_777 ? N18 C69 1.605(9) . ? N18 C69 1.605(9) 2_777 ? N18 C72 1.711(9) 2_777 ? N18 C72 1.711(9) . ? N19 C73 1.29(2) . ? N19 C75 1.53(3) . ? C1 C6 1.371(6) . ? C1 C2 1.373(6) . ? C2 C3 1.353(6) . ? C3 C4 1.407(6) . ? C4 C5 1.377(5) . ? C5 C6 1.378(6) . ? C8 C9 1.373(5) . ? C8 C13 1.400(5) . ? C9 C10 1.378(6) . ? C10 C11 1.381(6) . ? C11 C12 1.372(6) . ? C12 C13 1.366(6) . ? C15 C16 1.375(6) . ? C15 C20 1.412(6) . ? C16 C17 1.385(8) . ? C17 C18 1.391(9) . ? C18 C19 1.346(7) . ? C19 C20 1.402(6) . ? C22 C23 1.473(6) . ? C25 C30 1.385(6) . ? C25 C26 1.388(6) . ? C26 C27 1.365(6) . ? C27 C28 1.380(7) . ? C28 C29 1.383(6) . ? C29 C30 1.362(5) . ? C32 C33 1.387(6) . ? C32 C37 1.404(5) . ? C33 C34 1.393(6) . ? C34 C35 1.378(6) . ? C35 C36 1.376(6) . ? C36 C37 1.372(5) . ? C39 C40 1.387(5) . ? C39 C44 1.396(6) . ? C40 C41 1.368(5) . ? C41 C42 1.375(6) . ? C42 C43 1.360(6) . ? C43 C44 1.393(6) . ? C45 C46 1.496(6) . ? C47 C48 1.482(6) . ? C49 C50 1.500(6) . ? C51 C52 1.499(6) . ? C53 C54 1.508(8) . ? C55 C56 1.532(7) . ? C57 C58 1.538(7) . ? C59 C60 1.473(8) . ? C61 C62 1.446(10) . ? C63 C64 1.452(9) . ? C65 C66 1.497(11) . ? C67 C68 1.472(8) . ? C69 C72A 1.554(17) . ? C69 C71 1.706(11) . ? C69 C69A 1.982(14) . ? C70 C72 1.467(14) . ? C70 C72A 1.760(14) . ? C71 C69A 1.679(11) . ? C72 C72A 1.870(14) . ? C72 C69A 1.969(18) . ? C73 C74 1.616(19) . ? C75 C76 1.67(3) . ? C69A C72A 1.430(17) 2_777 ? C72A C69A 1.430(17) 2_777 ? 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 O2 N1 O1 121.7(4) . . ? O2 N1 C1 120.0(4) . . ? O1 N1 C1 118.3(4) . . ? C7 N2 C4 128.1(3) . . ? C7 N3 C8 128.4(3) . . ? C14 N4 C13 119.8(3) . . ? C14 N5 C15 119.3(4) . . ? C21 N6 C20 127.4(4) . . ? C21 N7 C22 121.9(4) . . ? C24 N8 C23 122.5(4) . . ? C24 N9 C25 130.3(4) . . ? C31 N10 C30 119.8(3) . . ? C31 N11 C32 120.8(3) . . ? C38 N12 C37 126.9(3) . . ? C39 N13 C38 127.7(3) . . ? O9 N14 O10 122.5(4) . . ? O9 N14 C42 119.4(5) . . ? O10 N14 C42 118.1(5) . . ? C51 N15 C47 106.4(3) . . ? C51 N15 C49 111.3(3) . . ? C47 N15 C49 110.5(4) . . ? C51 N15 C45 111.0(3) . . ? C47 N15 C45 110.3(3) . . ? C49 N15 C45 107.3(3) . . ? C53 N16 C55 110.8(4) . . ? C53 N16 C57 112.7(4) . . ? C55 N16 C57 105.1(4) . . ? C53 N16 C59 107.1(4) . . ? C55 N16 C59 110.5(4) . . ? C57 N16 C59 110.7(4) . . ? C67 N17 C65 112.8(6) . . ? C67 N17 C61 114.1(5) . . ? C65 N17 C61 106.8(5) . . ? C67 N17 C63 106.9(5) . . ? C65 N17 C63 107.1(6) . . ? C61 N17 C63 108.7(5) . . ? C72A N18 C72A 179.999(7) . 2_777 ? C72A N18 C69A 121.9(7) . . ? C72A N18 C69A 58.1(7) 2_777 . ? C72A N18 C69A 58.1(7) . 2_777 ? C72A N18 C69A 121.9(7) 2_777 2_777 ? C69A N18 C69A 179.997(7) . 2_777 ? C72A N18 C69 61.1(7) . . ? C72A N18 C69 118.9(7) 2_777 . ? C69A N18 C69 79.2(5) . . ? C69A N18 C69 100.8(5) 2_777 . ? C72A N18 C69 118.9(7) . 2_777 ? C72A N18 C69 61.1(7) 2_777 2_777 ? C69A N18 C69 100.8(5) . 2_777 ? C69A N18 C69 79.2(5) 2_777 2_777 ? C69 N18 C69 179.997(2) . 2_777 ? C72A N18 C72 107.8(6) . 2_777 ? C72A N18 C72 72.2(6) 2_777 2_777 ? C69A N18 C72 104.7(6) . 2_777 ? C69A N18 C72 75.3(6) 2_777 2_777 ? C69 N18 C72 80.1(5) . 2_777 ? C69 N18 C72 99.9(5) 2_777 2_777 ? C72A N18 C72 72.2(6) . . ? C72A N18 C72 107.8(6) 2_777 . ? C69A N18 C72 75.2(6) . . ? C69A N18 C72 104.7(6) 2_777 . ? C69 N18 C72 99.9(5) . . ? C69 N18 C72 80.1(5) 2_777 . ? C72 N18 C72 179.998(6) 2_777 . ? C73 N19 C75 118.1(19) . . ? C6 C1 C2 121.1(4) . . ? C6 C1 N1 119.0(4) . . ? C2 C1 N1 119.9(4) . . ? C3 C2 C1 118.7(4) . . ? C2 C3 C4 121.9(4) . . ? C5 C4 N2 124.7(4) . . ? C5 C4 C3 117.9(4) . . ? N2 C4 C3 117.3(4) . . ? C4 C5 C6 120.3(4) . . ? C1 C6 C5 119.9(4) . . ? O3 C7 N3 125.3(4) . . ? O3 C7 N2 123.5(4) . . ? N3 C7 N2 111.2(3) . . ? C9 C8 C13 119.7(4) . . ? C9 C8 N3 123.3(4) . . ? C13 C8 N3 117.0(3) . . ? C8 C9 C10 119.2(4) . . ? C9 C10 C11 121.1(4) . . ? C12 C11 C10 119.5(5) . . ? C13 C12 C11 120.2(4) . . ? C12 C13 C8 120.2(4) . . ? C12 C13 N4 119.7(4) . . ? C8 C13 N4 120.2(4) . . ? O4 C14 N4 123.8(4) . . ? O4 C14 N5 121.6(4) . . ? N4 C14 N5 114.5(4) . . ? C16 C15 C20 118.7(5) . . ? C16 C15 N5 120.8(5) . . ? C20 C15 N5 120.5(4) . . ? C15 C16 C17 121.4(6) . . ? C16 C17 C18 118.8(5) . . ? C19 C18 C17 121.5(6) . . ? C18 C19 C20 120.1(6) . . ? N6 C20 C19 123.6(4) . . ? N6 C20 C15 116.9(4) . . ? C19 C20 C15 119.4(4) . . ? O5 C21 N7 123.9(4) . . ? O5 C21 N6 122.6(4) . . ? N7 C21 N6 113.4(4) . . ? N7 C22 C23 112.9(4) . . ? N8 C23 C22 113.8(4) . . ? O6 C24 N8 122.5(5) . . ? O6 C24 N9 121.8(5) . . ? N8 C24 N9 115.7(4) . . ? C30 C25 C26 118.9(4) . . ? C30 C25 N9 118.7(4) . . ? C26 C25 N9 122.4(4) . . ? C27 C26 C25 119.5(5) . . ? C26 C27 C28 121.5(4) . . ? C27 C28 C29 119.0(4) . . ? C30 C29 C28 119.8(4) . . ? C29 C30 C25 121.3(4) . . ? C29 C30 N10 119.9(4) . . ? C25 C30 N10 118.8(3) . . ? O7 C31 N10 122.9(4) . . ? O7 C31 N11 123.4(4) . . ? N10 C31 N11 113.7(3) . . ? C33 C32 N11 119.0(4) . . ? C33 C32 C37 120.2(4) . . ? N11 C32 C37 120.7(4) . . ? C32 C33 C34 119.5(4) . . ? C35 C34 C33 119.9(5) . . ? C36 C35 C34 120.2(4) . . ? C37 C36 C35 121.2(4) . . ? C36 C37 C32 118.9(4) . . ? C36 C37 N12 123.5(4) . . ? C32 C37 N12 117.5(3) . . ? O8 C38 N12 125.0(4) . . ? O8 C38 N13 123.5(4) . . ? N12 C38 N13 111.5(3) . . ? N13 C39 C40 125.6(4) . . ? N13 C39 C44 116.5(4) . . ? C40 C39 C44 117.9(4) . . ? C41 C40 C39 120.4(4) . . ? C40 C41 C42 120.5(4) . . ? C43 C42 C41 121.3(4) . . ? C43 C42 N14 119.5(4) . . ? C41 C42 N14 119.1(4) . . ? C42 C43 C44 118.2(4) . . ? C43 C44 C39 121.7(4) . . ? C46 C45 N15 114.7(4) . . ? C48 C47 N15 117.4(4) . . ? C50 C49 N15 115.3(4) . . ? C52 C51 N15 115.5(3) . . ? N16 C53 C54 112.9(5) . . ? N16 C55 C56 113.4(4) . . ? N16 C57 C58 114.9(4) . . ? C60 C59 N16 115.1(4) . . ? C62 C61 N17 116.7(7) . . ? C64 C63 N17 118.4(6) . . ? C66 C65 N17 112.3(7) . . ? N17 C67 C68 118.1(6) . . ? C72A C69 N18 54.2(5) . . ? C72A C69 C71 136.3(7) . . ? N18 C69 C71 101.5(6) . . ? C72A C69 C69A 92.5(6) . . ? N18 C69 C69A 48.1(4) . . ? C71 C69 C69A 53.5(5) . . ? C72 C70 C72A 70.2(6) . . ? C69A C71 C69 71.7(5) . . ? C70 C72 N18 109.3(7) . . ? C70 C72 C72A 62.3(7) . . ? N18 C72 C72A 47.2(5) . . ? C70 C72 C69A 136.2(7) . . ? N18 C72 C69A 47.5(4) . . ? C72A C72 C69A 84.1(6) . . ? N19 C73 C74 108.1(18) . . ? N19 C75 C76 99.8(17) . . ? C72A C69A N18 58.8(6) 2_777 . ? C72A C69A C71 133.1(9) 2_777 . ? N18 C69A C71 107.3(6) . . ? C72A C69A C72 96.0(8) 2_777 . ? N18 C69A C72 57.2(5) . . ? C71 C69A C72 113.5(8) . . ? C72A C69A C69 99.2(7) 2_777 . ? N18 C69A C69 52.7(4) . . ? C71 C69A C69 54.8(4) . . ? C72 C69A C69 80.0(6) . . ? C69A C72A N18 63.1(7) 2_777 . ? C69A C72A C69 106.7(10) 2_777 . ? N18 C72A C69 64.7(7) . . ? C69A C72A C70 121.8(10) 2_777 . ? N18 C72A C70 108.0(7) . . ? C69 C72A C70 120.9(8) . . ? C69A C72A C72 100.2(8) 2_777 . ? N18 C72A C72 60.6(6) . . ? C69 C72A C72 95.3(8) . . ? C70 C72A C72 47.5(5) . . ? 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 O2 N1 C1 C6 7.7(6) . . . . ? O1 N1 C1 C6 -172.9(4) . . . . ? O2 N1 C1 C2 -173.2(4) . . . . ? O1 N1 C1 C2 6.3(6) . . . . ? C6 C1 C2 C3 -3.3(7) . . . . ? N1 C1 C2 C3 177.6(4) . . . . ? C1 C2 C3 C4 1.0(7) . . . . ? C7 N2 C4 C5 -15.9(7) . . . . ? C7 N2 C4 C3 166.0(4) . . . . ? C2 C3 C4 C5 2.3(7) . . . . ? C2 C3 C4 N2 -179.5(4) . . . . ? N2 C4 C5 C6 178.6(4) . . . . ? C3 C4 C5 C6 -3.3(6) . . . . ? C2 C1 C6 C5 2.3(6) . . . . ? N1 C1 C6 C5 -178.6(4) . . . . ? C4 C5 C6 C1 1.1(6) . . . . ? C8 N3 C7 O3 -0.1(7) . . . . ? C8 N3 C7 N2 -179.2(3) . . . . ? C4 N2 C7 O3 10.1(7) . . . . ? C4 N2 C7 N3 -170.8(4) . . . . ? C7 N3 C8 C9 -1.4(6) . . . . ? C7 N3 C8 C13 -179.7(4) . . . . ? C13 C8 C9 C10 2.8(6) . . . . ? N3 C8 C9 C10 -175.5(4) . . . . ? C8 C9 C10 C11 0.6(7) . . . . ? C9 C10 C11 C12 -2.3(7) . . . . ? C10 C11 C12 C13 0.6(6) . . . . ? C11 C12 C13 C8 2.8(6) . . . . ? C11 C12 C13 N4 -177.8(4) . . . . ? C9 C8 C13 C12 -4.5(6) . . . . ? N3 C8 C13 C12 173.9(3) . . . . ? C9 C8 C13 N4 176.1(4) . . . . ? N3 C8 C13 N4 -5.5(5) . . . . ? C14 N4 C13 C12 107.3(4) . . . . ? C14 N4 C13 C8 -73.2(5) . . . . ? C13 N4 C14 O4 19.7(6) . . . . ? C13 N4 C14 N5 -163.5(4) . . . . ? C15 N5 C14 O4 -15.7(6) . . . . ? C15 N5 C14 N4 167.4(4) . . . . ? C14 N5 C15 C16 -96.9(5) . . . . ? C14 N5 C15 C20 82.1(5) . . . . ? C20 C15 C16 C17 -2.2(8) . . . . ? N5 C15 C16 C17 176.8(5) . . . . ? C15 C16 C17 C18 -0.3(10) . . . . ? C16 C17 C18 C19 1.0(12) . . . . ? C17 C18 C19 C20 0.7(11) . . . . ? C21 N6 C20 C19 -3.4(7) . . . . ? C21 N6 C20 C15 177.8(4) . . . . ? C18 C19 C20 N6 178.1(6) . . . . ? C18 C19 C20 C15 -3.2(9) . . . . ? C16 C15 C20 N6 -177.3(4) . . . . ? N5 C15 C20 N6 3.8(6) . . . . ? C16 C15 C20 C19 3.9(7) . . . . ? N5 C15 C20 C19 -175.1(4) . . . . ? C22 N7 C21 O5 -4.8(7) . . . . ? C22 N7 C21 N6 177.9(3) . . . . ? C20 N6 C21 O5 1.4(7) . . . . ? C20 N6 C21 N7 178.8(4) . . . . ? C21 N7 C22 C23 -106.8(5) . . . . ? C24 N8 C23 C22 82.9(7) . . . . ? N7 C22 C23 N8 177.0(4) . . . . ? C23 N8 C24 O6 2.0(8) . . . . ? C23 N8 C24 N9 -179.9(4) . . . . ? C25 N9 C24 O6 -5.2(8) . . . . ? C25 N9 C24 N8 176.7(4) . . . . ? C24 N9 C25 C30 169.7(4) . . . . ? C24 N9 C25 C26 -12.6(7) . . . . ? C30 C25 C26 C27 1.1(6) . . . . ? N9 C25 C26 C27 -176.6(4) . . . . ? C25 C26 C27 C28 -2.2(7) . . . . ? C26 C27 C28 C29 2.5(7) . . . . ? C27 C28 C29 C30 -1.6(6) . . . . ? C28 C29 C30 C25 0.5(6) . . . . ? C28 C29 C30 N10 178.9(4) . . . . ? C26 C25 C30 C29 -0.2(6) . . . . ? N9 C25 C30 C29 177.5(4) . . . . ? C26 C25 C30 N10 -178.7(4) . . . . ? N9 C25 C30 N10 -0.9(6) . . . . ? C31 N10 C30 C29 -79.3(5) . . . . ? C31 N10 C30 C25 99.1(4) . . . . ? C30 N10 C31 O7 -14.9(6) . . . . ? C30 N10 C31 N11 166.5(3) . . . . ? C32 N11 C31 O7 15.5(6) . . . . ? C32 N11 C31 N10 -165.8(3) . . . . ? C31 N11 C32 C33 109.1(4) . . . . ? C31 N11 C32 C37 -76.0(5) . . . . ? N11 C32 C33 C34 178.8(4) . . . . ? C37 C32 C33 C34 3.8(6) . . . . ? C32 C33 C34 C35 -1.0(7) . . . . ? C33 C34 C35 C36 -1.9(8) . . . . ? C34 C35 C36 C37 2.0(7) . . . . ? C35 C36 C37 C32 0.8(6) . . . . ? C35 C36 C37 N12 -175.8(4) . . . . ? C33 C32 C37 C36 -3.7(6) . . . . ? N11 C32 C37 C36 -178.6(4) . . . . ? C33 C32 C37 N12 173.1(4) . . . . ? N11 C32 C37 N12 -1.8(5) . . . . ? C38 N12 C37 C36 -20.4(6) . . . . ? C38 N12 C37 C32 162.9(4) . . . . ? C37 N12 C38 O8 -3.1(6) . . . . ? C37 N12 C38 N13 177.4(3) . . . . ? C39 N13 C38 O8 1.1(6) . . . . ? C39 N13 C38 N12 -179.4(3) . . . . ? C38 N13 C39 C40 5.0(6) . . . . ? C38 N13 C39 C44 -174.5(4) . . . . ? N13 C39 C40 C41 -179.3(4) . . . . ? C44 C39 C40 C41 0.3(5) . . . . ? C39 C40 C41 C42 -1.2(6) . . . . ? C40 C41 C42 C43 1.1(6) . . . . ? C40 C41 C42 N14 -178.0(3) . . . . ? O9 N14 C42 C43 168.9(4) . . . . ? O10 N14 C42 C43 -10.3(6) . . . . ? O9 N14 C42 C41 -12.0(5) . . . . ? O10 N14 C42 C41 168.9(4) . . . . ? C41 C42 C43 C44 -0.1(6) . . . . ? N14 C42 C43 C44 179.0(4) . . . . ? C42 C43 C44 C39 -0.8(6) . . . . ? N13 C39 C44 C43 -179.7(4) . . . . ? C40 C39 C44 C43 0.8(6) . . . . ? C51 N15 C45 C46 -68.0(5) . . . . ? C47 N15 C45 C46 49.7(5) . . . . ? C49 N15 C45 C46 170.1(4) . . . . ? C51 N15 C47 C48 178.1(4) . . . . ? C49 N15 C47 C48 -60.9(5) . . . . ? C45 N15 C47 C48 57.6(5) . . . . ? C51 N15 C49 C50 50.1(6) . . . . ? C47 N15 C49 C50 -68.0(5) . . . . ? C45 N15 C49 C50 171.7(4) . . . . ? C47 N15 C51 C52 176.3(4) . . . . ? C49 N15 C51 C52 55.8(5) . . . . ? C45 N15 C51 C52 -63.6(5) . . . . ? C55 N16 C53 C54 59.3(6) . . . . ? C57 N16 C53 C54 -58.2(6) . . . . ? C59 N16 C53 C54 179.8(5) . . . . ? C53 N16 C55 C56 57.3(6) . . . . ? C57 N16 C55 C56 179.3(5) . . . . ? C59 N16 C55 C56 -61.2(7) . . . . ? C53 N16 C57 C58 -54.9(6) . . . . ? C55 N16 C57 C58 -175.6(5) . . . . ? C59 N16 C57 C58 65.0(6) . . . . ? C53 N16 C59 C60 -171.6(5) . . . . ? C55 N16 C59 C60 -50.9(6) . . . . ? C57 N16 C59 C60 65.1(6) . . . . ? C67 N17 C61 C62 -68.7(9) . . . . ? C65 N17 C61 C62 165.8(8) . . . . ? C63 N17 C61 C62 50.5(9) . . . . ? C67 N17 C63 C64 -178.4(6) . . . . ? C65 N17 C63 C64 -57.2(7) . . . . ? C61 N17 C63 C64 57.9(8) . . . . ? C67 N17 C65 C66 -60.0(8) . . . . ? C61 N17 C65 C66 66.2(8) . . . . ? C63 N17 C65 C66 -177.4(6) . . . . ? C65 N17 C67 C68 -51.6(9) . . . . ? C61 N17 C67 C68 -173.8(7) . . . . ? C63 N17 C67 C68 65.9(8) . . . . ? C72A N18 C69 C72A 180.001(6) 2_777 . . . ? C69A N18 C69 C72A -136.0(7) . . . . ? C69A N18 C69 C72A 44.0(7) 2_777 . . . ? C69 N18 C69 C72A 31(32) 2_777 . . . ? C72 N18 C69 C72A 116.8(7) 2_777 . . . ? C72 N18 C69 C72A -63.2(7) . . . . ? C72A N18 C69 C71 139.8(8) . . . . ? C72A N18 C69 C71 -40.2(8) 2_777 . . . ? C69A N18 C69 C71 3.7(7) . . . . ? C69A N18 C69 C71 -176.3(7) 2_777 . . . ? C69 N18 C69 C71 170(32) 2_777 . . . ? C72 N18 C69 C71 -103.5(7) 2_777 . . . ? C72 N18 C69 C71 76.5(7) . . . . ? C72A N18 C69 C69A 136.0(7) . . . . ? C72A N18 C69 C69A -44.0(7) 2_777 . . . ? C69A N18 C69 C69A 179.997(5) 2_777 . . . ? C69 N18 C69 C69A 167(32) 2_777 . . . ? C72 N18 C69 C69A -107.2(7) 2_777 . . . ? C72 N18 C69 C69A 72.8(7) . . . . ? C72A C69 C71 C69A 45.9(13) . . . . ? N18 C69 C71 C69A -3.5(6) . . . . ? C72A C70 C72 N18 -3.8(6) . . . . ? C72A C70 C72 C69A 44.3(11) . . . . ? C72A N18 C72 C70 4.6(8) . . . . ? C72A N18 C72 C70 -175.4(8) 2_777 . . . ? C69A N18 C72 C70 135.7(8) . . . . ? C69A N18 C72 C70 -44.3(8) 2_777 . . . ? C69 N18 C72 C70 59.8(8) . . . . ? C69 N18 C72 C70 -120.2(8) 2_777 . . . ? C72 N18 C72 C70 -166(15) 2_777 . . . ? C72A N18 C72 C72A 179.999(14) 2_777 . . . ? C69A N18 C72 C72A 131.1(7) . . . . ? C69A N18 C72 C72A -48.9(7) 2_777 . . . ? C69 N18 C72 C72A 55.2(7) . . . . ? C69 N18 C72 C72A -124.8(7) 2_777 . . . ? C72 N18 C72 C72A -170(16) 2_777 . . . ? C72A N18 C72 C69A -131.1(7) . . . . ? C72A N18 C72 C69A 48.9(7) 2_777 . . . ? C69A N18 C72 C69A 180.000(12) 2_777 . . . ? C69 N18 C72 C69A -76.0(6) . . . . ? C69 N18 C72 C69A 104.0(6) 2_777 . . . ? C72 N18 C72 C69A 59(17) 2_777 . . . ? C75 N19 C73 C74 -76(3) . . . . ? C73 N19 C75 C76 -53(3) . . . . ? C72A N18 C69A C72A 180.001(6) . . . 2_777 ? C69A N18 C69A C72A 126(17) 2_777 . . 2_777 ? C69 N18 C69A C72A -134.3(8) . . . 2_777 ? C69 N18 C69A C72A 45.7(8) 2_777 . . 2_777 ? C72 N18 C69A C72A -57.6(7) 2_777 . . 2_777 ? C72 N18 C69A C72A 122.4(7) . . . 2_777 ? C72A N18 C69A C71 -49.6(10) . . . . ? C72A N18 C69A C71 130.4(10) 2_777 . . . ? C69A N18 C69A C71 -103(17) 2_777 . . . ? C69 N18 C69A C71 -3.9(7) . . . . ? C69 N18 C69A C71 176.1(7) 2_777 . . . ? C72 N18 C69A C71 72.8(8) 2_777 . . . ? C72 N18 C69A C71 -107.2(8) . . . . ? C72A N18 C69A C72 57.6(7) . . . . ? C72A N18 C69A C72 -122.4(7) 2_777 . . . ? C69A N18 C69A C72 4(17) 2_777 . . . ? C69 N18 C69A C72 103.3(6) . . . . ? C69 N18 C69A C72 -76.7(6) 2_777 . . . ? C72 N18 C69A C72 180.002(13) 2_777 . . . ? C72A N18 C69A C69 -45.7(8) . . . . ? C72A N18 C69A C69 134.3(8) 2_777 . . . ? C69A N18 C69A C69 -99(17) 2_777 . . . ? C69 N18 C69A C69 180.001(5) 2_777 . . . ? C72 N18 C69A C69 76.7(6) 2_777 . . . ? C72 N18 C69A C69 -103.3(6) . . . . ? C69 C71 C69A C72A 66.9(13) . . . 2_777 ? C69 C71 C69A N18 3.8(7) . . . . ? C69 C71 C69A C72 -57.3(7) . . . . ? C70 C72 C69A C72A -118.7(12) . . . 2_777 ? N18 C72 C69A C72A -46.6(6) . . . 2_777 ? C72A C72 C69A C72A -80.3(8) . . . 2_777 ? C70 C72 C69A N18 -72.2(11) . . . . ? C72A C72 C69A N18 -33.7(5) . . . . ? C70 C72 C69A C71 23.9(14) . . . . ? N18 C72 C69A C71 96.1(6) . . . . ? C72A C72 C69A C71 62.4(7) . . . . ? C70 C72 C69A C69 -20.3(12) . . . . ? N18 C72 C69A C69 51.8(4) . . . . ? C72A C72 C69A C69 18.1(6) . . . . ? C72A C69 C69A C72A 72.7(11) . . . 2_777 ? N18 C69 C69A C72A 38.3(7) . . . 2_777 ? C71 C69 C69A C72A -137.1(10) . . . 2_777 ? C72A C69 C69A N18 34.3(6) . . . . ? C71 C69 C69A N18 -175.4(8) . . . . ? C72A C69 C69A C71 -150.2(9) . . . . ? N18 C69 C69A C71 175.4(8) . . . . ? C72A C69 C69A C72 -21.8(7) . . . . ? N18 C69 C69A C72 -56.2(4) . . . . ? C71 C69 C69A C72 128.4(7) . . . . ? C72A N18 C72A C69A 154(46) 2_777 . . 2_777 ? C69A N18 C72A C69A 180.003(5) . . . 2_777 ? C69 N18 C72A C69A 126.5(7) . . . 2_777 ? C69 N18 C72A C69A -53.5(7) 2_777 . . 2_777 ? C72 N18 C72A C69A 59.0(7) 2_777 . . 2_777 ? C72 N18 C72A C69A -121.0(7) . . . 2_777 ? C72A N18 C72A C69 27(46) 2_777 . . . ? C69A N18 C72A C69 53.5(7) . . . . ? C69A N18 C72A C69 -126.5(7) 2_777 . . . ? C69 N18 C72A C69 180.002(6) 2_777 . . . ? C72 N18 C72A C69 -67.5(6) 2_777 . . . ? C72 N18 C72A C69 112.5(6) . . . . ? C72A N18 C72A C70 -89(46) 2_777 . . . ? C69A N18 C72A C70 -62.8(10) . . . . ? C69A N18 C72A C70 117.2(10) 2_777 . . . ? C69 N18 C72A C70 -116.3(9) . . . . ? C69 N18 C72A C70 63.7(9) 2_777 . . . ? C72 N18 C72A C70 176.2(7) 2_777 . . . ? C72 N18 C72A C70 -3.8(7) . . . . ? C72A N18 C72A C72 -85(46) 2_777 . . . ? C69A N18 C72A C72 -59.0(7) . . . . ? C69A N18 C72A C72 121.0(7) 2_777 . . . ? C69 N18 C72A C72 -112.5(6) . . . . ? C69 N18 C72A C72 67.5(6) 2_777 . . . ? C72 N18 C72A C72 180.000(12) 2_777 . . . ? N18 C69 C72A C69A -48.4(7) . . . 2_777 ? C71 C69 C72A C69A -114.9(12) . . . 2_777 ? C69A C69 C72A C69A -79.6(9) . . . 2_777 ? C71 C69 C72A N18 -66.5(12) . . . . ? C69A C69 C72A N18 -31.2(5) . . . . ? N18 C69 C72A C70 96.7(9) . . . . ? C71 C69 C72A C70 30.2(18) . . . . ? C69A C69 C72A C70 65.5(10) . . . . ? N18 C69 C72A C72 53.9(5) . . . . ? C71 C69 C72A C72 -12.6(15) . . . . ? C69A C69 C72A C72 22.8(7) . . . . ? C72 C70 C72A C69A 73.5(11) . . . 2_777 ? C72 C70 C72A N18 4.5(8) . . . . ? C72 C70 C72A C69 -66.3(10) . . . . ? C70 C72 C72A C69A -124.1(10) . . . 2_777 ? N18 C72 C72A C69A 51.0(7) . . . 2_777 ? C69A C72 C72A C69A 85.0(9) . . . 2_777 ? C70 C72 C72A N18 -175.1(8) . . . . ? C69A C72 C72A N18 34.0(5) . . . . ? C70 C72 C72A C69 127.9(9) . . . . ? N18 C72 C72A C69 -57.0(7) . . . . ? C69A C72 C72A C69 -23.1(8) . . . . ? N18 C72 C72A C70 175.1(8) . . . . ? C69A C72 C72A C70 -150.9(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N13 H13 Cl4 0.88 2.29 3.153(3) 166.7 1_565 N12 H12 Cl4 0.88 2.47 3.300(4) 158.0 1_565 N9 H9 Cl4 0.88 2.67 3.475(4) 153.2 1_565 N8 H8 Cl4 0.88 2.32 3.179(4) 167.0 1_565 N11 H11 Cl3 0.88 2.48 3.175(3) 136.0 1_665 N10 H10 Cl3 0.88 2.65 3.315(3) 133.2 1_665 O11 H11C Cl3 0.85 2.49 3.320(4) 167.7 . O11 H11B Cl2 0.85 2.51 3.276(4) 150.5 . N5 H5 Cl2 0.88 2.53 3.241(4) 137.9 . N4 H4 Cl1 0.88 3.43 3.583(4) 93.1 . N7 H7 Cl1 0.88 2.30 3.159(4) 164.4 . N6 H6 Cl1 0.88 2.57 3.386(4) 154.0 . N3 H3 Cl1 0.88 2.53 3.336(3) 152.7 . N2 H2 Cl1 0.88 2.36 3.147(4) 148.3 . _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.510 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.068 ############ data_(TPA)3LCl3 _database_code_depnum_ccdc_archive 'CCDC 849101' #TrackingRef 'complexes 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H124 Cl3 N17 O10' _chemical_formula_weight 1590.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 32.425(8) _cell_length_b 19.215(5) _cell_length_c 28.184(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.692(4) _cell_angle_gamma 90.00 _cell_volume 17358(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4219 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.07 _exptl_crystal_description flack _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6832 _exptl_absorpt_coefficient_mu 0.170 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9476 _exptl_absorpt_correction_T_max 0.9815 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42699 _diffrn_reflns_av_R_equivalents 0.0994 _diffrn_reflns_av_sigmaI/netI 0.1290 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.28 _reflns_number_total 15068 _reflns_number_gt 6878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.1355P] 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 15068 _refine_ls_number_parameters 1027 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.2492 _refine_ls_R_factor_gt 0.1456 _refine_ls_wR_factor_ref 0.3879 _refine_ls_wR_factor_gt 0.3504 _refine_ls_goodness_of_fit_ref 1.794 _refine_ls_restrained_S_all 1.838 _refine_ls_shift/su_max 0.002 _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 Cl1 Cl 0.13548(7) 0.77768(10) 0.46534(8) 0.0438(6) Uani 1 1 d . . . Cl2 Cl 0.18890(7) 0.49905(10) 0.42610(9) 0.0492(7) Uani 1 1 d . . . Cl3 Cl 0.20859(7) 0.21847(10) 0.35094(9) 0.0454(6) Uani 1 1 d . . . O1 O -0.0521(2) 1.0951(3) 0.4134(3) 0.073(2) Uani 1 1 d . . . O2 O 0.0064(2) 1.1271(3) 0.4538(3) 0.072(2) Uani 1 1 d . . . O3 O -0.0149(2) 0.7471(3) 0.3987(3) 0.0591(19) Uani 1 1 d . . . O4 O 0.10465(19) 0.6920(3) 0.3412(2) 0.0491(16) Uani 1 1 d . . . O5 O 0.20476(19) 0.9075(3) 0.3423(2) 0.0493(17) Uani 1 1 d . . . O6 O 0.1249(2) 1.0945(3) 0.4647(3) 0.067(2) Uani 1 1 d . . . O7 O 0.1010(2) 1.3103(3) 0.3436(2) 0.0512(17) Uani 1 1 d . . . O8 O 0.1084(4) 1.2523(4) 0.1992(4) 0.150(5) Uani 1 1 d . . . O9 O 0.0889(3) 0.8958(4) 0.1719(4) 0.123(4) Uani 1 1 d . . . O10 O 0.1317(3) 0.8646(4) 0.2334(3) 0.086(3) Uani 1 1 d . . . N1 N -0.0170(3) 1.0825(4) 0.4350(3) 0.053(2) Uani 1 1 d . . . N2 N 0.0404(2) 0.8080(4) 0.4375(3) 0.051(2) Uani 1 1 d . . . H2 H 0.0660 0.8025 0.4525 0.061 Uiso 1 1 calc R . . N3 N 0.0485(2) 0.6938(3) 0.4182(3) 0.0457(19) Uani 1 1 d . . . H3 H 0.0745 0.7019 0.4311 0.055 Uiso 1 1 calc R . . N4 N 0.1130(2) 0.6077(3) 0.3987(3) 0.047(2) Uani 1 1 d . . . H4 H 0.1307 0.5907 0.4227 0.057 Uiso 1 1 calc R . . N5 N 0.1697(2) 0.6576(3) 0.3731(3) 0.0401(18) Uani 1 1 d . . . H5 H 0.1848 0.6409 0.3992 0.048 Uiso 1 1 calc R . . N6 N 0.1818(2) 0.8017(3) 0.3650(3) 0.044(2) Uani 1 1 d . . . H6 H 0.1692 0.7813 0.3868 0.053 Uiso 1 1 calc R . . N7 N 0.1673(2) 0.9008(3) 0.4027(3) 0.050(2) Uani 1 1 d . . . H7 H 0.1636 0.8772 0.4285 0.060 Uiso 1 1 calc R . . N8 N 0.1654(3) 1.0976(4) 0.4054(3) 0.087(3) Uani 1 1 d . . . H8 H 0.1726 1.1206 0.3810 0.104 Uiso 1 1 calc R . . N9 N 0.1376(2) 1.1978(3) 0.4286(3) 0.0384(18) Uani 1 1 d . . . H9 H 0.1517 1.2159 0.4073 0.046 Uiso 1 1 calc R . . N10 N 0.1432(2) 1.3418(3) 0.4120(3) 0.048(2) Uani 1 1 d . . . H10 H 0.1686 1.3555 0.4234 0.058 Uiso 1 1 calc R . . N11 N 0.1509(2) 1.3935(3) 0.3406(3) 0.045(2) Uani 1 1 d . . . H11 H 0.1742 1.4105 0.3563 0.054 Uiso 1 1 calc R . . N12 N 0.1478(2) 1.3036(3) 0.2623(3) 0.0454(19) Uani 1 1 d . . . H12 H 0.1672 1.2957 0.2871 0.054 Uiso 1 1 calc R . . N13 N 0.1522(3) 1.1869(4) 0.2540(3) 0.065(2) Uani 1 1 d . . . H13 H 0.1724 1.1913 0.2785 0.077 Uiso 1 1 calc R . . N14 N 0.1138(3) 0.9099(4) 0.2070(4) 0.075(3) Uani 1 1 d . . . N15 N 0.1996(3) 0.8689(5) 0.1021(4) 0.084(3) Uani 1 1 d D . . N16 N 0.1789(2) 0.3978(4) 0.0665(3) 0.049(2) Uani 1 1 d . . . N18 N -0.0005(8) 0.7678(7) 0.2490(10) 0.151(10) Uani 0.50 1 d PD A -1 C72 C 0.0349(4) 0.8109(7) 0.2754(5) 0.111(5) Uani 1 1 d D A -1 C73 C 0.0216(5) 0.8658(8) 0.3079(6) 0.140(7) Uani 1 1 d D A -1 C74 C 0.0600(12) 0.912(2) 0.3272(11) 0.51(4) Uani 1 1 d D A -1 C75 C 0.0193(11) 0.7281(10) 0.2121(6) 0.39(3) Uani 1 1 d D A -1 C76 C 0.0423(8) 0.6589(11) 0.2317(8) 1.36(13) Uani 1 1 d D A -1 C77 C 0.0103(3) 0.6146(18) 0.2540(8) 0.37(2) Uani 1 1 d D A -1 C81 C 0.0169(7) 0.2365(8) 0.1856(7) 0.23(2) Uani 0.67 1 d PD B -1 C83 C 0.0369(5) 0.3191(11) 0.0989(5) 0.143(12) Uani 0.67 1 d PD B -1 C82 C 0.0016(4) 0.2764(6) 0.1282(6) 0.078(6) Uani 0.67 1 d PD B -1 C80 C 0.0654(7) 0.0628(11) 0.3335(10) 0.135(9) Uani 0.67 1 d PD B -1 C79 C 0.0324(10) 0.1149(10) 0.3231(6) 0.208(18) Uani 0.67 1 d PD B -1 C78 C 0.0292(5) 0.1695(7) 0.2951(5) 0.057(5) Uani 0.67 1 d PD B -1 C71 C 0.0090(18) 0.3927(12) 0.2277(11) 0.27(3) Uani 0.67 1 d PD B -1 C70 C 0.0176(6) 0.3254(11) 0.2570(7) 0.26(3) Uani 0.67 1 d PD B -1 N17 N 0.0277(7) 0.1961(8) 0.2425(6) 0.31(3) Uani 0.50 1 d PD B -1 C69 C -0.0001(8) 0.2602(10) 0.2307(9) 0.95(14) Uani 0.67 1 d PD B -1 C1 C -0.0026(3) 1.0111(4) 0.4365(3) 0.045(2) Uani 1 1 d . . . C2 C -0.0305(3) 0.9596(4) 0.4211(4) 0.049(2) Uani 1 1 d . . . H2A H -0.0589 0.9710 0.4103 0.058 Uiso 1 1 calc R . . C3 C -0.0176(3) 0.8916(4) 0.4214(3) 0.045(2) Uani 1 1 d . . . H3A H -0.0370 0.8560 0.4102 0.054 Uiso 1 1 calc R . . C4 C 0.0238(3) 0.8749(4) 0.4380(3) 0.044(2) Uani 1 1 d . . . C5 C 0.0514(3) 0.9291(5) 0.4550(3) 0.047(2) Uani 1 1 d . . . H5A H 0.0797 0.9186 0.4670 0.057 Uiso 1 1 calc R . . C6 C 0.0382(3) 0.9958(5) 0.4544(3) 0.045(2) Uani 1 1 d . . . H6A H 0.0570 1.0319 0.4662 0.055 Uiso 1 1 calc R . . C7 C 0.0209(3) 0.7492(5) 0.4160(4) 0.047(2) Uani 1 1 d . . . C8 C 0.0389(3) 0.6282(4) 0.4022(3) 0.046(2) Uani 1 1 d . . . C9 C -0.0014(3) 0.6011(5) 0.3978(4) 0.062(3) Uani 1 1 d . . . H9A H -0.0239 0.6303 0.4033 0.074 Uiso 1 1 calc R . . C10 C -0.0089(4) 0.5319(6) 0.3853(5) 0.080(4) Uani 1 1 d . . . H10A H -0.0366 0.5145 0.3822 0.096 Uiso 1 1 calc R . . C11 C 0.0235(4) 0.4873(6) 0.3773(5) 0.080(4) Uani 1 1 d . . . H11A H 0.0182 0.4397 0.3696 0.096 Uiso 1 1 calc R . . C12 C 0.0636(3) 0.5145(5) 0.3808(4) 0.064(3) Uani 1 1 d . . . H12A H 0.0859 0.4854 0.3746 0.077 Uiso 1 1 calc R . . C13 C 0.0715(3) 0.5842(4) 0.3934(3) 0.045(2) Uani 1 1 d . . . C14 C 0.1277(3) 0.6555(4) 0.3690(3) 0.042(2) Uani 1 1 d . . . C15 C 0.1906(3) 0.6865(4) 0.3358(3) 0.039(2) Uani 1 1 d . . . C16 C 0.2058(3) 0.6396(4) 0.3050(4) 0.056(3) Uani 1 1 d . . . H16 H 0.2019 0.5910 0.3087 0.067 Uiso 1 1 calc R . . C17 C 0.2269(3) 0.6643(5) 0.2686(4) 0.063(3) Uani 1 1 d . . . H17 H 0.2379 0.6326 0.2478 0.075 Uiso 1 1 calc R . . C18 C 0.2315(3) 0.7344(5) 0.2631(4) 0.064(3) Uani 1 1 d . . . H18 H 0.2454 0.7516 0.2381 0.076 Uiso 1 1 calc R . . C19 C 0.2159(3) 0.7807(4) 0.2943(4) 0.052(3) Uani 1 1 d . . . H19 H 0.2191 0.8293 0.2899 0.063 Uiso 1 1 calc R . . C20 C 0.1961(3) 0.7574(4) 0.3311(3) 0.040(2) Uani 1 1 d . . . C21 C 0.1854(3) 0.8730(4) 0.3681(3) 0.039(2) Uani 1 1 d . . . C22 C 0.1507(5) 0.9891(11) 0.3938(6) 0.154(9) Uani 1 1 d . . . H22A H 0.1484 1.0051 0.3601 0.185 Uiso 1 1 calc R . . H22B H 0.1252 1.0005 0.4075 0.185 Uiso 1 1 calc R . . C23 C 0.1827(6) 1.0061(12) 0.4188(6) 0.175(10) Uani 1 1 d . . . H23A H 0.2084 0.9929 0.4058 0.210 Uiso 1 1 calc R . . H23B H 0.1844 0.9926 0.4529 0.210 Uiso 1 1 calc R . . C24 C 0.1408(3) 1.1273(4) 0.4353(4) 0.052(3) Uani 1 1 d . . . C25 C 0.1143(3) 1.2438(4) 0.4521(3) 0.043(2) Uani 1 1 d . . . C26 C 0.0876(3) 1.2215(5) 0.4834(4) 0.060(3) Uani 1 1 d . . . H26 H 0.0851 1.1731 0.4893 0.072 Uiso 1 1 calc R . . C27 C 0.0650(4) 1.2679(6) 0.5059(5) 0.102(5) Uani 1 1 d . . . H27 H 0.0470 1.2519 0.5273 0.123 Uiso 1 1 calc R . . C28 C 0.0687(5) 1.3393(6) 0.4970(5) 0.111(6) Uani 1 1 d . . . H28 H 0.0530 1.3721 0.5122 0.133 Uiso 1 1 calc R . . C29 C 0.0944(4) 1.3610(5) 0.4669(4) 0.089(4) Uani 1 1 d . . . H29 H 0.0972 1.4095 0.4617 0.106 Uiso 1 1 calc R . . C30 C 0.1169(3) 1.3153(4) 0.4433(4) 0.052(3) Uani 1 1 d . . . C31 C 0.1287(3) 1.3460(4) 0.3630(4) 0.040(2) Uani 1 1 d . . . C32 C 0.1374(3) 1.4159(4) 0.2933(3) 0.040(2) Uani 1 1 d . . . C33 C 0.1282(3) 1.4864(5) 0.2860(4) 0.058(3) Uani 1 1 d . . . H33 H 0.1311 1.5167 0.3130 0.069 Uiso 1 1 calc R . . C34 C 0.1152(3) 1.5130(5) 0.2419(4) 0.068(3) Uani 1 1 d . . . H34 H 0.1091 1.5612 0.2377 0.082 Uiso 1 1 calc R . . C35 C 0.1111(3) 1.4686(6) 0.2031(4) 0.065(3) Uani 1 1 d . . . H35 H 0.1015 1.4863 0.1719 0.078 Uiso 1 1 calc R . . C36 C 0.1208(3) 1.3983(5) 0.2089(4) 0.052(3) Uani 1 1 d . . . H36 H 0.1184 1.3680 0.1820 0.063 Uiso 1 1 calc R . . C37 C 0.1339(3) 1.3736(4) 0.2546(4) 0.045(2) Uani 1 1 d . . . C38 C 0.1338(4) 1.2478(5) 0.2345(5) 0.073(3) Uani 1 1 d . . . C39 C 0.1420(3) 1.1202(5) 0.2387(4) 0.061(3) Uani 1 1 d . . . C40 C 0.1622(3) 1.0659(5) 0.2670(4) 0.058(3) Uani 1 1 d . . . H40 H 0.1823 1.0770 0.2942 0.070 Uiso 1 1 calc R . . C41 C 0.1535(3) 0.9980(5) 0.2561(4) 0.057(3) Uani 1 1 d . . . H41 H 0.1682 0.9619 0.2745 0.068 Uiso 1 1 calc R . . C42 C 0.1230(4) 0.9821(5) 0.2177(4) 0.066(3) Uani 1 1 d . . . C43 C 0.1024(4) 1.0333(6) 0.1898(5) 0.095(4) Uani 1 1 d . . . H43 H 0.0817 1.0213 0.1635 0.114 Uiso 1 1 calc R . . C44 C 0.1117(4) 1.1025(5) 0.1997(4) 0.102(5) Uani 1 1 d . . . H44 H 0.0977 1.1380 0.1801 0.122 Uiso 1 1 calc R . . C45 C 0.1661(4) 0.9291(6) 0.0864(5) 0.083(4) Uani 1 1 d . . . C46 C 0.1843(4) 0.9967(7) 0.0733(5) 0.094(4) Uani 1 1 d . . . C47 C 0.1458(4) 1.0433(5) 0.0537(5) 0.090(4) Uani 1 1 d . . . C48 C 0.2341(4) 0.8627(7) 0.0701(7) 0.118(6) Uani 1 1 d . . . C49 C 0.2255(8) 0.8456(9) 0.0231(7) 0.190(11) Uani 1 1 d . . . C50 C 0.2628(5) 0.8454(6) -0.0047(5) 0.118(6) Uani 1 1 d . . . C51 C 0.1698(6) 0.8050(8) 0.0912(11) 0.245(16) Uani 1 1 d D . . C52 C 0.1750(8) 0.7346(10) 0.1006(10) 0.52(5) Uani 1 1 d D . . C53 C 0.1333(8) 0.6971(10) 0.113(2) 0.85(8) Uani 1 1 d D . . C54 C 0.2221(8) 0.8848(11) 0.1502(7) 0.194(11) Uani 1 1 d . . . C55 C 0.2319(6) 0.9371(8) 0.1744(7) 0.154(8) Uani 1 1 d . . . C56 C 0.2562(4) 0.9379(5) 0.2257(4) 0.073(3) Uani 1 1 d . . . C57 C 0.1678(4) 0.3262(7) 0.0830(5) 0.088(4) Uani 1 1 d . . . C58 C 0.2004(5) 0.2939(8) 0.1145(5) 0.105(5) Uani 1 1 d . . . C59 C 0.1867(4) 0.2120(6) 0.1243(5) 0.095(4) Uani 1 1 d . . . C60 C 0.1408(4) 0.4294(7) 0.0319(5) 0.089(4) Uani 1 1 d . . . C61 C 0.1038(5) 0.4499(9) 0.0529(6) 0.135(7) Uani 1 1 d . . . C62 C 0.0658(3) 0.4594(6) 0.0159(4) 0.070(3) Uani 1 1 d . . . C63 C 0.1910(4) 0.4464(5) 0.1091(5) 0.083(4) Uani 1 1 d . . . C64 C 0.1981(4) 0.5199(7) 0.1006(5) 0.093(4) Uani 1 1 d . . . C65 C 0.2155(4) 0.5541(6) 0.1496(4) 0.078(4) Uani 1 1 d . . . C66 C 0.2158(4) 0.3964(6) 0.0392(4) 0.074(3) Uani 1 1 d . . . C67 C 0.2136(4) 0.3433(5) 0.0007(5) 0.088(4) Uani 1 1 d . . . C68 C 0.2533(3) 0.3477(5) -0.0247(4) 0.057(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 Cl1 0.0424(13) 0.0427(12) 0.0436(15) 0.0057(11) -0.0017(11) 0.0019(10) Cl2 0.0640(15) 0.0286(10) 0.0508(16) -0.0031(10) -0.0046(13) 0.0005(10) Cl3 0.0461(14) 0.0410(12) 0.0462(16) -0.0013(11) -0.0027(12) -0.0020(10) O1 0.068(5) 0.056(4) 0.086(6) 0.001(4) -0.014(5) 0.019(4) O2 0.071(5) 0.049(4) 0.089(6) -0.017(4) -0.005(4) -0.004(4) O3 0.033(4) 0.069(4) 0.070(6) 0.003(4) -0.011(4) -0.004(3) O4 0.057(4) 0.040(3) 0.047(4) 0.015(3) -0.001(4) 0.003(3) O5 0.068(4) 0.036(3) 0.047(4) 0.008(3) 0.017(4) 0.000(3) O6 0.108(6) 0.031(3) 0.068(5) 0.008(3) 0.041(5) 0.003(4) O7 0.051(4) 0.045(4) 0.056(5) -0.011(3) 0.002(4) -0.011(3) O8 0.240(12) 0.071(5) 0.097(8) -0.042(5) -0.113(9) 0.057(7) O9 0.184(10) 0.060(5) 0.099(8) -0.027(5) -0.063(8) 0.018(6) O10 0.112(6) 0.052(4) 0.084(7) 0.005(4) -0.018(5) 0.011(4) N1 0.052(6) 0.054(5) 0.049(6) 0.000(4) -0.002(5) 0.001(5) N2 0.038(4) 0.050(5) 0.061(6) 0.007(4) -0.007(4) 0.004(4) N3 0.042(5) 0.044(4) 0.048(5) 0.004(4) -0.001(4) 0.000(4) N4 0.060(5) 0.037(4) 0.042(5) 0.005(4) -0.001(4) 0.002(4) N5 0.045(5) 0.038(4) 0.035(5) -0.002(3) 0.001(4) -0.003(3) N6 0.068(5) 0.028(4) 0.040(5) 0.004(3) 0.020(4) 0.002(3) N7 0.082(6) 0.017(3) 0.056(6) -0.001(3) 0.025(5) 0.000(4) N8 0.168(10) 0.021(4) 0.086(8) 0.008(4) 0.068(8) 0.021(5) N9 0.048(5) 0.027(4) 0.040(5) 0.004(3) 0.007(4) 0.001(3) N10 0.070(5) 0.034(4) 0.041(6) 0.001(4) 0.009(5) -0.007(4) N11 0.058(5) 0.032(4) 0.044(6) -0.002(4) 0.002(4) -0.010(4) N12 0.050(5) 0.048(4) 0.036(5) -0.003(4) -0.002(4) -0.002(4) N13 0.088(6) 0.050(5) 0.045(6) -0.010(4) -0.024(5) 0.022(5) N14 0.105(8) 0.047(6) 0.063(8) -0.020(5) -0.018(6) 0.014(5) N15 0.075(7) 0.095(7) 0.077(8) -0.014(6) -0.004(6) 0.015(6) N16 0.040(5) 0.068(5) 0.037(5) -0.010(4) 0.002(4) -0.014(4) N18 0.34(3) 0.045(10) 0.044(13) -0.04(2) -0.062(18) -0.03(5) C72 0.097(10) 0.150(13) 0.068(10) -0.042(9) -0.045(8) 0.065(9) C73 0.167(16) 0.176(16) 0.088(13) -0.042(11) 0.049(12) -0.070(13) C74 0.52(7) 0.87(10) 0.17(3) -0.26(5) 0.14(4) -0.40(7) C75 0.75(7) 0.23(2) 0.113(17) -0.095(17) -0.17(3) 0.37(4) C76 2.0(2) 2.00(19) 0.078(18) 0.09(5) 0.12(5) 2.00(19) C77 0.000(9) 0.94(7) 0.16(2) 0.33(3) -0.036(10) -0.066(15) C81 0.19(2) 0.053(13) 0.37(5) -0.097(19) -0.26(3) 0.091(15) C83 0.124(15) 0.28(3) 0.040(11) 0.132(14) 0.076(11) 0.185(18) C82 0.054(10) 0.024(7) 0.155(19) 0.000(9) 0.017(11) -0.027(7) C80 0.109(17) 0.14(2) 0.14(3) 0.018(17) -0.003(17) 0.046(15) C79 0.47(5) 0.115(16) 0.065(15) 0.040(13) 0.12(2) 0.22(3) C78 0.088(11) 0.062(9) 0.028(9) 0.015(7) 0.027(9) 0.069(9) C71 0.28(5) 0.35(5) 0.12(3) 0.03(3) -0.21(5) -0.09(4) C70 0.041(13) 0.65(8) 0.09(2) -0.23(4) -0.036(15) 0.03(3) N17 0.47(5) 0.14(2) 0.44(5) -0.24(3) 0.46(5) -0.24(3) C69 0.97(19) 1.06(17) 1.05(19) 0.99(17) 0.93(18) 0.67(16) C1 0.052(6) 0.036(5) 0.048(7) 0.004(4) 0.010(5) 0.002(5) C2 0.040(6) 0.049(6) 0.055(7) 0.006(5) -0.002(5) 0.004(5) C3 0.044(6) 0.040(5) 0.046(7) 0.012(4) -0.006(5) -0.001(4) C4 0.045(6) 0.044(5) 0.041(6) 0.005(4) 0.002(5) 0.006(5) C5 0.038(5) 0.059(6) 0.045(7) -0.003(5) 0.005(5) -0.003(5) C6 0.040(6) 0.052(6) 0.043(7) -0.001(5) 0.001(5) -0.004(5) C7 0.045(6) 0.045(5) 0.051(7) 0.008(5) 0.006(6) -0.004(5) C8 0.063(7) 0.034(5) 0.041(6) 0.005(4) 0.004(5) -0.013(5) C9 0.052(7) 0.056(6) 0.079(9) 0.009(6) 0.011(6) -0.012(5) C10 0.066(8) 0.058(7) 0.115(12) 0.013(7) 0.008(8) -0.029(6) C11 0.085(9) 0.051(6) 0.104(11) 0.011(6) 0.015(8) -0.029(7) C12 0.071(8) 0.052(6) 0.072(9) -0.005(5) 0.021(7) -0.010(5) C13 0.046(6) 0.045(5) 0.040(6) 0.009(4) -0.004(5) -0.015(5) C14 0.062(7) 0.024(4) 0.041(6) 0.002(4) 0.012(5) 0.002(4) C15 0.050(6) 0.033(5) 0.033(6) 0.000(4) 0.002(5) 0.005(4) C16 0.078(7) 0.035(5) 0.055(7) -0.016(5) 0.016(6) -0.009(5) C17 0.095(8) 0.054(6) 0.044(7) -0.014(5) 0.026(7) 0.008(6) C18 0.084(8) 0.067(7) 0.044(7) 0.006(5) 0.024(6) 0.013(6) C19 0.071(7) 0.036(5) 0.053(7) 0.003(5) 0.016(6) 0.003(5) C20 0.057(6) 0.033(5) 0.032(6) 0.002(4) 0.008(5) 0.000(4) C21 0.050(6) 0.034(5) 0.032(6) 0.003(4) 0.001(5) 0.000(4) C22 0.059(10) 0.34(3) 0.067(12) -0.078(15) 0.019(9) -0.059(14) C23 0.099(13) 0.36(3) 0.078(14) 0.004(16) 0.035(12) 0.104(17) C24 0.066(7) 0.036(5) 0.057(7) 0.007(5) 0.016(6) 0.004(5) C25 0.049(6) 0.031(5) 0.050(7) 0.000(4) 0.013(5) 0.001(4) C26 0.071(7) 0.041(5) 0.072(8) 0.003(5) 0.028(7) 0.005(5) C27 0.145(12) 0.078(9) 0.103(11) 0.023(8) 0.080(10) 0.039(8) C28 0.186(15) 0.063(8) 0.105(12) 0.024(7) 0.096(12) 0.047(9) C29 0.162(12) 0.031(5) 0.088(10) 0.013(6) 0.069(10) 0.020(7) C30 0.075(7) 0.030(5) 0.054(7) -0.001(4) 0.024(6) 0.005(5) C31 0.052(6) 0.030(5) 0.040(7) 0.001(4) 0.013(5) 0.005(4) C32 0.052(6) 0.035(5) 0.034(6) 0.004(4) 0.003(5) -0.001(4) C33 0.082(7) 0.046(6) 0.044(7) -0.003(5) 0.006(6) 0.002(5) C34 0.094(9) 0.048(6) 0.063(9) 0.017(6) 0.011(7) 0.014(6) C35 0.061(7) 0.083(8) 0.053(8) 0.021(6) 0.011(6) 0.013(6) C36 0.064(7) 0.047(6) 0.046(7) 0.004(5) 0.008(6) 0.011(5) C37 0.052(6) 0.041(5) 0.041(7) 0.002(5) 0.011(5) -0.001(4) C38 0.097(9) 0.056(7) 0.053(8) -0.016(6) -0.024(7) 0.018(7) C39 0.085(8) 0.053(6) 0.040(7) -0.017(5) -0.011(6) 0.021(6) C40 0.075(7) 0.059(6) 0.035(7) -0.002(5) -0.006(6) 0.022(6) C41 0.069(7) 0.058(6) 0.040(7) -0.001(5) -0.002(6) 0.025(5) C42 0.087(8) 0.054(6) 0.047(8) -0.016(5) -0.024(7) 0.023(6) C43 0.140(12) 0.062(7) 0.063(9) -0.015(6) -0.050(9) 0.021(8) C44 0.167(13) 0.059(7) 0.054(9) -0.033(6) -0.064(9) 0.051(8) C45 0.074(8) 0.078(8) 0.093(11) 0.015(7) -0.001(8) 0.019(7) C46 0.086(9) 0.100(10) 0.088(11) 0.025(8) -0.009(8) -0.010(8) C47 0.081(8) 0.058(7) 0.119(12) 0.003(7) -0.023(8) 0.016(6) C48 0.100(11) 0.110(11) 0.151(16) -0.075(11) 0.047(11) -0.036(9) C49 0.36(3) 0.120(14) 0.117(16) -0.057(12) 0.10(2) -0.093(17) C50 0.192(16) 0.087(9) 0.085(11) -0.030(8) 0.058(12) -0.056(10) C51 0.21(2) 0.097(13) 0.46(5) 0.10(2) 0.17(3) 0.020(14) C52 0.48(6) 0.87(10) 0.28(4) 0.37(6) 0.31(5) 0.51(7) C53 0.33(4) 0.043(12) 2.0(2) 0.07(4) -0.40(8) -0.019(19) C54 0.30(3) 0.177(18) 0.074(13) -0.054(12) -0.073(16) 0.140(19) C55 0.187(17) 0.118(12) 0.120(16) -0.054(11) -0.098(13) 0.079(12) C56 0.085(8) 0.072(7) 0.060(9) 0.009(6) 0.005(7) 0.007(6) C57 0.099(10) 0.093(9) 0.083(11) 0.001(8) 0.046(9) -0.016(8) C58 0.133(13) 0.126(12) 0.053(9) 0.017(8) 0.000(9) -0.025(10) C59 0.146(12) 0.072(8) 0.069(9) -0.004(6) 0.024(9) -0.056(8) C60 0.057(8) 0.120(10) 0.085(11) -0.051(8) -0.005(7) -0.009(7) C61 0.078(10) 0.203(17) 0.118(15) -0.086(13) -0.007(10) 0.004(10) C62 0.046(6) 0.098(8) 0.057(8) -0.015(6) -0.016(6) -0.001(6) C63 0.094(9) 0.055(7) 0.087(10) -0.019(6) -0.025(8) -0.015(6) C64 0.081(9) 0.103(10) 0.086(11) -0.029(8) -0.013(8) -0.002(8) C65 0.081(8) 0.081(8) 0.069(9) -0.031(7) 0.004(7) -0.032(6) C66 0.095(9) 0.082(7) 0.055(8) 0.011(6) 0.040(7) 0.017(7) C67 0.141(12) 0.044(6) 0.091(10) -0.003(6) 0.055(9) -0.004(7) C68 0.063(7) 0.053(6) 0.058(7) 0.012(5) 0.021(6) 0.013(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 O1 N1 1.230(10) . ? O2 N1 1.213(9) . ? O3 C7 1.189(10) . ? O4 C14 1.218(10) . ? O5 C21 1.225(9) . ? O6 C24 1.217(10) . ? O7 C31 1.195(10) . ? O8 C38 1.195(13) . ? O9 N14 1.210(11) . ? O10 N14 1.233(11) . ? N1 C1 1.448(11) . ? N2 C7 1.390(11) . ? N2 C4 1.394(10) . ? N3 C8 1.359(10) . ? N3 C7 1.385(11) . ? N4 C14 1.377(10) . ? N4 C13 1.405(10) . ? N5 C14 1.353(11) . ? N5 C15 1.445(10) . ? N6 C21 1.377(10) . ? N6 C20 1.410(10) . ? N7 C21 1.324(10) . ? N7 C22 1.79(2) . ? N8 C24 1.367(11) . ? N8 C23 1.87(2) . ? N9 C24 1.369(10) . ? N9 C25 1.395(10) . ? N10 C31 1.391(11) . ? N10 C30 1.411(11) . ? N11 C31 1.374(10) . ? N11 C32 1.405(11) . ? N12 C38 1.364(12) . ? N12 C37 1.423(10) . ? N13 C39 1.376(12) . ? N13 C38 1.389(13) . ? N14 C42 1.440(12) . ? N15 C54 1.47(2) . ? N15 C48 1.543(16) . ? N15 C51 1.564(15) . ? N15 C45 1.604(14) . ? N16 C57 1.512(13) . ? N16 C66 1.517(11) . ? N16 C63 1.524(13) . ? N16 C60 1.576(14) . ? N18 C75 1.509(19) . ? N18 C72 1.516(18) . ? C72 C73 1.503(14) . ? C73 C74 1.560(17) . ? C75 C76 1.584(15) . ? C76 C77 1.55(2) . ? C81 C69 1.53(4) . ? C81 N17 1.769(17) . ? C81 C82 1.792(17) . ? C83 C82 1.717(15) . ? C80 C79 1.462(16) . ? C79 C78 1.309(14) . ? C78 N17 1.560(14) . ? C71 C70 1.538(13) . ? C70 C69 1.523(14) . ? N17 C69 1.532(14) . ? C1 C2 1.367(12) . ? C1 C6 1.374(12) . ? C2 C3 1.372(11) . ? C3 C4 1.393(12) . ? C4 C5 1.408(12) . ? C5 C6 1.351(11) . ? C8 C9 1.395(12) . ? C8 C13 1.403(12) . ? C9 C10 1.387(14) . ? C10 C11 1.401(15) . ? C11 C12 1.392(14) . ? C12 C13 1.400(12) . ? C15 C20 1.384(10) . ? C15 C16 1.390(11) . ? C16 C17 1.401(12) . ? C17 C18 1.366(13) . ? C18 C19 1.398(12) . ? C19 C20 1.374(11) . ? C22 C23 1.21(2) . ? C25 C26 1.393(12) . ? C25 C30 1.402(11) . ? C26 C27 1.369(13) . ? C27 C28 1.403(15) . ? C28 C29 1.345(14) . ? C29 C30 1.374(12) . ? C32 C37 1.352(12) . ? C32 C33 1.395(11) . ? C33 C34 1.352(14) . ? C34 C35 1.378(14) . ? C35 C36 1.392(13) . ? C36 C37 1.379(13) . ? C39 C44 1.400(14) . ? C39 C40 1.414(13) . ? C40 C41 1.361(12) . ? C41 C42 1.387(13) . ? C42 C43 1.368(14) . ? C43 C44 1.383(14) . ? C45 C46 1.498(15) . ? C46 C47 1.568(16) . ? C48 C49 1.35(2) . ? C49 C50 1.54(2) . ? C51 C52 1.385(16) . ? C52 C53 1.620(18) . ? C54 C55 1.23(2) . ? C55 C56 1.540(19) . ? C57 C58 1.418(18) . ? C58 C59 1.669(16) . ? C60 C61 1.469(17) . ? C61 C62 1.501(18) . ? C63 C64 1.457(15) . ? C64 C65 1.557(16) . ? C66 C67 1.484(15) . ? C67 C68 1.565(14) . ? 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 O2 N1 O1 123.2(8) . . ? O2 N1 C1 118.7(9) . . ? O1 N1 C1 118.1(8) . . ? C7 N2 C4 127.3(8) . . ? C8 N3 C7 125.8(8) . . ? C14 N4 C13 124.2(8) . . ? C14 N5 C15 121.7(8) . . ? C21 N6 C20 127.6(7) . . ? C21 N7 C22 115.9(8) . . ? C24 N8 C23 117.0(8) . . ? C24 N9 C25 126.7(7) . . ? C31 N10 C30 119.8(8) . . ? C31 N11 C32 122.1(8) . . ? C38 N12 C37 125.7(9) . . ? C39 N13 C38 126.3(9) . . ? O9 N14 O10 122.0(9) . . ? O9 N14 C42 118.5(10) . . ? O10 N14 C42 119.4(11) . . ? C54 N15 C48 104.7(13) . . ? C54 N15 C51 123.4(17) . . ? C48 N15 C51 107.8(11) . . ? C54 N15 C45 109.0(10) . . ? C48 N15 C45 114.5(11) . . ? C51 N15 C45 97.9(10) . . ? C57 N16 C66 112.5(8) . . ? C57 N16 C63 111.1(8) . . ? C66 N16 C63 106.4(8) . . ? C57 N16 C60 109.8(9) . . ? C66 N16 C60 107.3(8) . . ? C63 N16 C60 109.5(8) . . ? C75 N18 C72 104.2(18) . . ? C73 C72 N18 114.5(12) . . ? C72 C73 C74 108.9(14) . . ? N18 C75 C76 114.2(14) . . ? C77 C76 C75 107.1(15) . . ? C69 C81 N17 54.8(9) . . ? C69 C81 C82 122.6(14) . . ? N17 C81 C82 175.4(19) . . ? C83 C82 C81 121.7(13) . . ? C78 C79 C80 131(2) . . ? C79 C78 N17 145.5(14) . . ? C69 C70 C71 114.0(13) . . ? C69 N17 C78 113.7(13) . . ? C69 N17 C81 54.7(15) . . ? C78 N17 C81 168.0(16) . . ? C70 C69 C81 119.5(19) . . ? C70 C69 N17 112.9(15) . . ? C81 C69 N17 70.5(13) . . ? C2 C1 C6 121.1(8) . . ? C2 C1 N1 118.7(9) . . ? C6 C1 N1 120.1(8) . . ? C1 C2 C3 120.0(9) . . ? C2 C3 C4 119.9(8) . . ? C3 C4 N2 124.2(8) . . ? C3 C4 C5 118.4(8) . . ? N2 C4 C5 117.3(8) . . ? C6 C5 C4 120.8(9) . . ? C5 C6 C1 119.6(9) . . ? O3 C7 N3 125.2(9) . . ? O3 C7 N2 123.8(9) . . ? N3 C7 N2 111.0(8) . . ? N3 C8 C9 122.6(9) . . ? N3 C8 C13 118.6(8) . . ? C9 C8 C13 118.7(8) . . ? C10 C9 C8 120.4(10) . . ? C9 C10 C11 121.3(10) . . ? C12 C11 C10 118.4(10) . . ? C11 C12 C13 120.6(10) . . ? C12 C13 C8 120.6(8) . . ? C12 C13 N4 118.0(9) . . ? C8 C13 N4 121.4(8) . . ? O4 C14 N5 123.4(8) . . ? O4 C14 N4 122.7(9) . . ? N5 C14 N4 113.9(8) . . ? C20 C15 C16 121.0(8) . . ? C20 C15 N5 122.0(7) . . ? C16 C15 N5 117.0(7) . . ? C15 C16 C17 119.8(8) . . ? C18 C17 C16 119.3(9) . . ? C17 C18 C19 120.1(9) . . ? C20 C19 C18 121.4(8) . . ? C19 C20 C15 118.4(8) . . ? C19 C20 N6 123.7(7) . . ? C15 C20 N6 117.9(7) . . ? O5 C21 N7 122.9(7) . . ? O5 C21 N6 123.1(8) . . ? N7 C21 N6 113.9(8) . . ? C23 C22 N7 87.7(19) . . ? C22 C23 N8 86.0(16) . . ? O6 C24 N8 123.4(8) . . ? O6 C24 N9 125.1(9) . . ? N8 C24 N9 111.6(8) . . ? C26 C25 N9 122.6(7) . . ? C26 C25 C30 118.2(8) . . ? N9 C25 C30 119.2(7) . . ? C27 C26 C25 121.3(9) . . ? C26 C27 C28 119.3(10) . . ? C29 C28 C27 119.5(10) . . ? C28 C29 C30 122.2(9) . . ? C29 C30 C25 119.4(8) . . ? C29 C30 N10 119.1(8) . . ? C25 C30 N10 121.4(8) . . ? O7 C31 N11 125.5(9) . . ? O7 C31 N10 122.5(8) . . ? N11 C31 N10 112.0(8) . . ? C37 C32 C33 118.4(9) . . ? C37 C32 N11 123.8(8) . . ? C33 C32 N11 117.8(8) . . ? C34 C33 C32 122.2(10) . . ? C33 C34 C35 118.4(10) . . ? C34 C35 C36 121.0(10) . . ? C37 C36 C35 118.5(10) . . ? C32 C37 C36 121.6(8) . . ? C32 C37 N12 117.4(9) . . ? C36 C37 N12 120.8(8) . . ? O8 C38 N12 123.3(10) . . ? O8 C38 N13 126.1(10) . . ? N12 C38 N13 110.5(10) . . ? N13 C39 C44 125.4(9) . . ? N13 C39 C40 116.2(10) . . ? C44 C39 C40 118.3(9) . . ? C41 C40 C39 121.2(10) . . ? C40 C41 C42 119.2(9) . . ? C43 C42 C41 121.3(10) . . ? C43 C42 N14 120.3(11) . . ? C41 C42 N14 118.4(10) . . ? C42 C43 C44 120.1(11) . . ? C43 C44 C39 119.9(10) . . ? C46 C45 N15 114.6(9) . . ? C45 C46 C47 104.9(9) . . ? C49 C48 N15 122.1(16) . . ? C48 C49 C50 116(2) . . ? C52 C51 N15 132.4(19) . . ? C51 C52 C53 113.2(16) . . ? C55 C54 N15 137.1(18) . . ? C54 C55 C56 125.6(16) . . ? C58 C57 N16 113.6(11) . . ? C57 C58 C59 108.8(12) . . ? C61 C60 N16 117.8(12) . . ? C60 C61 C62 112.9(12) . . ? C64 C63 N16 119.5(11) . . ? C63 C64 C65 108.0(11) . . ? C67 C66 N16 115.4(10) . . ? C66 C67 C68 110.2(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N13 H13 Cl3 0.88 2.26 3.110(9) 162.8 1_565 N12 H12 Cl3 0.88 2.55 3.364(8) 153.8 1_565 N9 H9 Cl3 0.88 2.61 3.430(7) 155.7 1_565 N8 H8 Cl3 0.88 2.43 3.220(8) 149.3 1_565 N11 H11 Cl2 0.88 2.59 3.247(8) 132.1 1_565 N10 H10 Cl2 0.88 2.83 3.363(7) 120.2 1_565 N5 H5 Cl2 0.88 2.83 3.408(7) 125.0 . N4 H4 Cl2 0.88 2.57 3.231(7) 132.3 . N7 H7 Cl1 0.88 2.42 3.212(7) 150.3 . N6 H6 Cl1 0.88 2.61 3.427(7) 154.3 . N3 H3 Cl1 0.88 2.53 3.344(8) 154.8 . N2 H2 Cl1 0.88 2.28 3.120(8) 160.2 . _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.28 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.821 _refine_diff_density_min -1.216 _refine_diff_density_rms 0.123 ############ data_(TBA)2LCl2 _database_code_depnum_ccdc_archive 'CCDC 849102' #TrackingRef 'complexes 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H124 Cl8 N16 O11' _chemical_formula_weight 1793.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.995(2) _cell_length_b 18.961(3) _cell_length_c 21.692(4) _cell_angle_alpha 101.726(3) _cell_angle_beta 106.372(3) _cell_angle_gamma 102.616(3) _cell_volume 4800.1(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2881 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.35 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.296 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9137 _exptl_absorpt_correction_T_max 0.9681 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24598 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.1687 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 25.11 _reflns_number_total 16924 _reflns_number_gt 8150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.4931P] 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 16924 _refine_ls_number_parameters 1064 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1886 _refine_ls_R_factor_gt 0.1027 _refine_ls_wR_factor_ref 0.3036 _refine_ls_wR_factor_gt 0.2543 _refine_ls_goodness_of_fit_ref 1.221 _refine_ls_restrained_S_all 1.221 _refine_ls_shift/su_max 0.002 _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 Cl1 Cl 0.49237(14) 0.30328(9) 0.23625(8) 0.0291(4) Uani 1 1 d . . . Cl2 Cl 0.75696(13) 0.29801(9) 0.17564(8) 0.0266(4) Uani 1 1 d . . . Cl3 Cl 0.5474(3) 0.2945(2) 0.44410(15) 0.1244(14) Uani 1 1 d . . . Cl4 Cl 0.4718(3) 0.42085(18) 0.4215(2) 0.1260(13) Uani 1 1 d . . . Cl5 Cl 0.3167(2) 0.27381(17) 0.37627(16) 0.0896(9) Uani 1 1 d . . . Cl6 Cl 0.2652(3) 0.8535(2) 0.35635(19) 0.1202(12) Uani 1 1 d . . . Cl7 Cl 0.4507(3) 0.8430(2) 0.4599(3) 0.1573(18) Uani 1 1 d . . . Cl8 Cl 0.4746(3) 0.9687(2) 0.4035(2) 0.1369(14) Uani 1 1 d . . . O1 O 0.7759(6) 0.0721(3) 0.4632(3) 0.077(2) Uani 1 1 d . . . O2 O 0.8042(6) -0.0122(4) 0.3931(3) 0.085(2) Uani 1 1 d . . . O3 O 0.5564(4) 0.0746(2) 0.1016(2) 0.0291(11) Uani 1 1 d . . . O4 O 0.4730(4) 0.3813(2) 0.0194(2) 0.0326(11) Uani 1 1 d . . . O5 O 0.8374(4) 0.5346(2) 0.3289(2) 0.0351(12) Uani 1 1 d . . . O6 O 0.9204(4) 0.2208(3) 0.3782(2) 0.0406(13) Uani 1 1 d . . . O7 O 0.8959(4) 0.1504(2) 0.0632(2) 0.0285(10) Uani 1 1 d . . . O8 O 0.9018(4) 0.3686(2) -0.0048(2) 0.0313(11) Uani 1 1 d . . . O9 O 1.1656(5) 0.7312(3) 0.2132(3) 0.0619(17) Uani 1 1 d . . . O10 O 1.0484(5) 0.7292(3) 0.2680(3) 0.0580(16) Uani 1 1 d . . . O11 O 0.5342(7) 0.7077(5) 0.3253(5) 0.101(3) Uani 1 1 d . . . N1 N 0.7648(6) 0.0390(4) 0.4052(4) 0.0542(19) Uani 1 1 d . . . N2 N 0.5448(4) 0.1449(3) 0.1979(3) 0.0291(13) Uani 1 1 d . . . H2 H 0.5168 0.1808 0.2117 0.035 Uiso 1 1 calc R . . N3 N 0.4813(4) 0.1733(3) 0.1000(3) 0.0239(12) Uani 1 1 d . . . H3 H 0.4717 0.2119 0.1256 0.029 Uiso 1 1 calc R . . N4 N 0.5498(4) 0.2920(3) 0.0543(3) 0.0297(13) Uani 1 1 d . . . H4 H 0.6073 0.2865 0.0840 0.036 Uiso 1 1 calc R . . N5 N 0.6213(5) 0.4127(3) 0.1176(3) 0.0288(13) Uani 1 1 d . . . H5 H 0.6670 0.3935 0.1427 0.035 Uiso 1 1 calc R . . N6 N 0.6634(5) 0.4725(3) 0.2521(2) 0.0297(13) Uani 1 1 d . . . H6 H 0.6034 0.4341 0.2418 0.036 Uiso 1 1 calc R . . N7 N 0.7400(4) 0.4231(3) 0.3356(3) 0.0274(13) Uani 1 1 d . . . H7 H 0.6756 0.3872 0.3192 0.033 Uiso 1 1 calc R . . N8 N 0.8394(5) 0.2995(3) 0.3301(3) 0.0391(16) Uani 1 1 d . . . H8 H 0.8206 0.3148 0.2940 0.047 Uiso 1 1 calc R . . N9 N 0.8774(4) 0.2043(3) 0.2656(3) 0.0271(13) Uani 1 1 d . . . H9 H 0.8317 0.2135 0.2317 0.032 Uiso 1 1 calc R . . N10 N 0.8052(4) 0.1154(3) 0.1333(2) 0.0267(13) Uani 1 1 d . . . H10 H 0.7405 0.1070 0.1401 0.032 Uiso 1 1 calc R . . N11 N 0.7069(4) 0.1319(3) 0.0333(2) 0.0244(12) Uani 1 1 d . . . H11 H 0.6476 0.1229 0.0457 0.029 Uiso 1 1 calc R . . N12 N 0.7980(5) 0.2750(3) 0.0249(3) 0.0310(13) Uani 1 1 d . . . H12 H 0.7858 0.2645 0.0604 0.037 Uiso 1 1 calc R . . N13 N 0.8816(5) 0.3904(3) 0.0985(3) 0.0326(14) Uani 1 1 d . . . H13 H 0.8563 0.3667 0.1246 0.039 Uiso 1 1 calc R . . N14 N 1.0865(6) 0.6989(3) 0.2269(3) 0.0433(16) Uani 1 1 d . . . N15 N 0.0818(5) 0.2389(3) 0.5604(3) 0.0294(13) Uani 1 1 d . . . N16 N 0.1809(4) 0.2883(3) 0.0852(3) 0.0270(13) Uani 1 1 d . . . C1 C 0.7062(6) 0.0647(4) 0.3514(4) 0.0423(19) Uani 1 1 d . . . C2 C 0.6924(6) 0.0287(4) 0.2870(4) 0.042(2) Uani 1 1 d . . . H2A H 0.7206 -0.0131 0.2787 0.051 Uiso 1 1 calc R . . C3 C 0.6381(6) 0.0521(4) 0.2336(4) 0.0342(17) Uani 1 1 d . . . H3A H 0.6283 0.0266 0.1889 0.041 Uiso 1 1 calc R . . C4 C 0.5976(5) 0.1147(4) 0.2474(3) 0.0297(16) Uani 1 1 d . . . C5 C 0.6096(6) 0.1485(4) 0.3115(4) 0.0414(19) Uani 1 1 d . . . H5A H 0.5811 0.1900 0.3206 0.050 Uiso 1 1 calc R . . C6 C 0.6630(7) 0.1232(4) 0.3640(4) 0.049(2) Uani 1 1 d . . . H6A H 0.6694 0.1467 0.4086 0.059 Uiso 1 1 calc R . . C7 C 0.5304(5) 0.1264(4) 0.1306(3) 0.0250(15) Uani 1 1 d . . . C8 C 0.4442(5) 0.1636(3) 0.0282(3) 0.0248(15) Uani 1 1 d . . . C9 C 0.3758(5) 0.0943(4) -0.0169(3) 0.0299(16) Uani 1 1 d . . . H9A H 0.3578 0.0514 -0.0014 0.036 Uiso 1 1 calc R . . C10 C 0.3349(6) 0.0888(4) -0.0839(4) 0.0395(18) Uani 1 1 d . . . H10A H 0.2885 0.0418 -0.1150 0.047 Uiso 1 1 calc R . . C11 C 0.3615(6) 0.1529(4) -0.1067(3) 0.0393(18) Uani 1 1 d . . . H11A H 0.3300 0.1498 -0.1527 0.047 Uiso 1 1 calc R . . C12 C 0.4344(6) 0.2207(4) -0.0614(3) 0.0321(16) Uani 1 1 d . . . H12A H 0.4560 0.2632 -0.0767 0.039 Uiso 1 1 calc R . . C13 C 0.4750(5) 0.2257(3) 0.0059(3) 0.0259(15) Uani 1 1 d . . . C14 C 0.5429(5) 0.3641(4) 0.0602(3) 0.0258(15) Uani 1 1 d . . . C15 C 0.6373(5) 0.4906(4) 0.1412(3) 0.0289(16) Uani 1 1 d . . . C16 C 0.6315(6) 0.5378(4) 0.0995(3) 0.0318(16) Uani 1 1 d . . . H16 H 0.6123 0.5173 0.0526 0.038 Uiso 1 1 calc R . . C17 C 0.6538(6) 0.6142(4) 0.1265(4) 0.0401(19) Uani 1 1 d . . . H17 H 0.6509 0.6464 0.0981 0.048 Uiso 1 1 calc R . . C18 C 0.6801(7) 0.6441(4) 0.1944(4) 0.049(2) Uani 1 1 d . . . H18 H 0.6975 0.6970 0.2126 0.059 Uiso 1 1 calc R . . C19 C 0.6814(6) 0.5982(4) 0.2360(3) 0.0376(18) Uani 1 1 d . . . H19 H 0.6964 0.6191 0.2824 0.045 Uiso 1 1 calc R . . C20 C 0.6608(6) 0.5218(4) 0.2104(3) 0.0290(16) Uani 1 1 d . . . C21 C 0.7531(6) 0.4812(4) 0.3071(3) 0.0274(15) Uani 1 1 d . . . C22 C 0.8275(6) 0.4183(4) 0.3915(3) 0.0362(17) Uani 1 1 d . . . H22A H 0.8197 0.4437 0.4338 0.043 Uiso 1 1 calc R . . H22B H 0.9014 0.4450 0.3907 0.043 Uiso 1 1 calc R . . C23 C 0.8234(7) 0.3381(4) 0.3898(3) 0.0362(18) Uani 1 1 d . . . H23A H 0.8825 0.3373 0.4298 0.043 Uiso 1 1 calc R . . H23B H 0.7498 0.3114 0.3911 0.043 Uiso 1 1 calc R . . C24 C 0.8825(6) 0.2406(3) 0.3281(3) 0.0270(15) Uani 1 1 d . . . C25 C 0.9368(5) 0.1536(3) 0.2491(3) 0.0224(14) Uani 1 1 d . . . C26 C 1.0278(6) 0.1470(4) 0.2940(3) 0.0308(16) Uani 1 1 d . . . H26 H 1.0502 0.1747 0.3397 0.037 Uiso 1 1 calc R . . C27 C 1.0903(6) 0.1000(4) 0.2748(4) 0.0385(18) Uani 1 1 d . . . H27 H 1.1554 0.0975 0.3070 0.046 Uiso 1 1 calc R . . C28 C 1.0566(6) 0.0575(4) 0.2090(3) 0.0327(17) Uani 1 1 d . . . H28 H 1.0985 0.0259 0.1953 0.039 Uiso 1 1 calc R . . C29 C 0.9593(5) 0.0616(4) 0.1623(3) 0.0296(16) Uani 1 1 d . . . H29 H 0.9332 0.0312 0.1172 0.035 Uiso 1 1 calc R . . C30 C 0.9017(5) 0.1101(3) 0.1825(3) 0.0233(14) Uani 1 1 d . . . C31 C 0.8115(6) 0.1335(3) 0.0753(3) 0.0250(15) Uani 1 1 d . . . C32 C 0.6977(5) 0.1454(4) -0.0313(3) 0.0247(15) Uani 1 1 d . . . C33 C 0.6347(6) 0.0862(4) -0.0884(3) 0.0320(16) Uani 1 1 d . . . H33 H 0.5988 0.0388 -0.0845 0.038 Uiso 1 1 calc R . . C34 C 0.6242(6) 0.0966(4) -0.1518(4) 0.0424(19) Uani 1 1 d . . . H34 H 0.5817 0.0568 -0.1915 0.051 Uiso 1 1 calc R . . C35 C 0.6790(6) 0.1684(4) -0.1549(4) 0.0425(19) Uani 1 1 d . . . H35 H 0.6745 0.1762 -0.1973 0.051 Uiso 1 1 calc R . . C36 C 0.7386(6) 0.2269(4) -0.0978(3) 0.0375(18) Uani 1 1 d . . . H36 H 0.7746 0.2746 -0.1011 0.045 Uiso 1 1 calc R . . C37 C 0.7460(5) 0.2162(4) -0.0352(3) 0.0272(15) Uani 1 1 d . . . C38 C 0.8644(5) 0.3458(3) 0.0358(3) 0.0251(15) Uani 1 1 d . . . C39 C 0.9335(5) 0.4680(4) 0.1268(3) 0.0278(15) Uani 1 1 d . . . C40 C 0.9970(5) 0.5129(4) 0.0991(3) 0.0298(16) Uani 1 1 d . . . H40 H 1.0058 0.4921 0.0578 0.036 Uiso 1 1 calc R . . C41 C 1.0470(6) 0.5887(4) 0.1331(3) 0.0351(17) Uani 1 1 d . . . H41 H 1.0927 0.6198 0.1159 0.042 Uiso 1 1 calc R . . C42 C 1.0311(6) 0.6187(4) 0.1910(4) 0.0350(17) Uani 1 1 d . . . C43 C 0.9640(6) 0.5756(4) 0.2176(3) 0.0324(16) Uani 1 1 d . . . H43 H 0.9519 0.5976 0.2574 0.039 Uiso 1 1 calc R . . C44 C 0.9158(6) 0.5004(3) 0.1850(3) 0.0279(15) Uani 1 1 d . . . H44 H 0.8695 0.4700 0.2024 0.033 Uiso 1 1 calc R . . C45 C 0.1203(6) 0.2258(4) 0.6288(3) 0.0311(16) Uani 1 1 d . . . H45A H 0.1151 0.2679 0.6621 0.037 Uiso 1 1 calc R . . H45B H 0.2005 0.2279 0.6404 0.037 Uiso 1 1 calc R . . C46 C 0.0566(7) 0.1523(4) 0.6360(4) 0.0427(19) Uani 1 1 d . . . H46A H 0.0611 0.1092 0.6035 0.051 Uiso 1 1 calc R . . H46B H -0.0234 0.1498 0.6265 0.051 Uiso 1 1 calc R . . C47 C 0.1072(7) 0.1476(4) 0.7071(4) 0.046(2) Uani 1 1 d . . . H47A H 0.1882 0.1534 0.7170 0.056 Uiso 1 1 calc R . . H47B H 0.0996 0.1899 0.7390 0.056 Uiso 1 1 calc R . . C48 C 0.0524(8) 0.0745(5) 0.7175(4) 0.065(3) Uani 1 1 d . . . H48A H -0.0286 0.0671 0.7056 0.098 Uiso 1 1 calc R . . H48B H 0.0841 0.0760 0.7646 0.098 Uiso 1 1 calc R . . H48C H 0.0659 0.0327 0.6891 0.098 Uiso 1 1 calc R . . C49 C 0.0727(6) 0.1722(4) 0.5045(3) 0.0358(17) Uani 1 1 d . . . H49A H 0.0174 0.1272 0.5048 0.043 Uiso 1 1 calc R . . H49B H 0.0435 0.1827 0.4610 0.043 Uiso 1 1 calc R . . C50 C 0.1813(8) 0.1540(4) 0.5092(4) 0.053(2) Uani 1 1 d . . . H50A H 0.2158 0.1481 0.5540 0.064 Uiso 1 1 calc R . . H50B H 0.2344 0.1955 0.5025 0.064 Uiso 1 1 calc R . . C51 C 0.1565(9) 0.0802(5) 0.4546(4) 0.075(3) Uani 1 1 d . . . H51A H 0.1113 0.0384 0.4655 0.090 Uiso 1 1 calc R . . H51B H 0.1104 0.0842 0.4113 0.090 Uiso 1 1 calc R . . C52 C 0.2549(10) 0.0612(6) 0.4466(6) 0.096(4) Uani 1 1 d . . . H52A H 0.2945 0.0982 0.4292 0.144 Uiso 1 1 calc R . . H52B H 0.2321 0.0109 0.4152 0.144 Uiso 1 1 calc R . . H52C H 0.3048 0.0616 0.4901 0.144 Uiso 1 1 calc R . . C53 C 0.1625(6) 0.3108(4) 0.5653(3) 0.0324(16) Uani 1 1 d . . . H53A H 0.2384 0.3041 0.5760 0.039 Uiso 1 1 calc R . . H53B H 0.1639 0.3504 0.6034 0.039 Uiso 1 1 calc R . . C54 C 0.1392(6) 0.3389(4) 0.5038(4) 0.0441(19) Uani 1 1 d . . . H54A H 0.0677 0.3519 0.4955 0.053 Uiso 1 1 calc R . . H54B H 0.1313 0.2985 0.4643 0.053 Uiso 1 1 calc R . . C55 C 0.2337(7) 0.4080(4) 0.5127(4) 0.0399(18) Uani 1 1 d . . . H55A H 0.3029 0.3933 0.5149 0.048 Uiso 1 1 calc R . . H55B H 0.2485 0.4457 0.5555 0.048 Uiso 1 1 calc R . . C56 C 0.2031(8) 0.4438(5) 0.4538(4) 0.058(2) Uani 1 1 d . . . H56A H 0.1931 0.4076 0.4118 0.087 Uiso 1 1 calc R . . H56B H 0.2636 0.4894 0.4620 0.087 Uiso 1 1 calc R . . H56C H 0.1332 0.4568 0.4508 0.087 Uiso 1 1 calc R . . C57 C -0.0392(5) 0.2470(4) 0.5421(3) 0.0318(16) Uani 1 1 d . . . H57A H -0.0617 0.2524 0.4962 0.038 Uiso 1 1 calc R . . H57B H -0.0907 0.1996 0.5413 0.038 Uiso 1 1 calc R . . C58 C -0.0560(6) 0.3111(4) 0.5874(3) 0.0376(18) Uani 1 1 d . . . H58A H -0.0045 0.3590 0.5892 0.045 Uiso 1 1 calc R . . H58B H -0.0368 0.3054 0.6333 0.045 Uiso 1 1 calc R . . C59 C -0.1750(7) 0.3151(5) 0.5645(4) 0.050(2) Uani 1 1 d . . . H59A H -0.1924 0.3236 0.5196 0.060 Uiso 1 1 calc R . . H59B H -0.2265 0.2659 0.5600 0.060 Uiso 1 1 calc R . . C60 C -0.1966(8) 0.3762(5) 0.6110(4) 0.064(3) Uani 1 1 d . . . H60A H -0.1897 0.3645 0.6537 0.095 Uiso 1 1 calc R . . H60B H -0.2725 0.3793 0.5907 0.095 Uiso 1 1 calc R . . H60C H -0.1418 0.4245 0.6188 0.095 Uiso 1 1 calc R . . C61 C 0.2335(5) 0.2252(4) 0.0942(3) 0.0294(16) Uani 1 1 d . . . H61A H 0.2850 0.2245 0.0681 0.035 Uiso 1 1 calc R . . H61B H 0.2794 0.2370 0.1420 0.035 Uiso 1 1 calc R . . C62 C 0.1522(6) 0.1471(4) 0.0732(4) 0.0353(17) Uani 1 1 d . . . H62A H 0.1206 0.1286 0.0236 0.042 Uiso 1 1 calc R . . H62B H 0.0895 0.1492 0.0902 0.042 Uiso 1 1 calc R . . C63 C 0.2115(6) 0.0918(4) 0.1007(4) 0.0360(17) Uani 1 1 d . . . H63A H 0.2856 0.1008 0.0948 0.043 Uiso 1 1 calc R . . H63B H 0.2243 0.1024 0.1493 0.043 Uiso 1 1 calc R . . C64 C 0.1455(6) 0.0106(4) 0.0668(4) 0.0440(19) Uani 1 1 d . . . H64A H 0.0685 0.0028 0.0669 0.066 Uiso 1 1 calc R . . H64B H 0.1806 -0.0213 0.0909 0.066 Uiso 1 1 calc R . . H64C H 0.1444 -0.0028 0.0205 0.066 Uiso 1 1 calc R . . C65 C 0.1015(6) 0.2688(4) 0.0133(3) 0.0341(17) Uani 1 1 d . . . H65A H 0.0422 0.2213 0.0040 0.041 Uiso 1 1 calc R . . H65B H 0.0646 0.3089 0.0093 0.041 Uiso 1 1 calc R . . C66 C 0.1563(6) 0.2595(4) -0.0399(4) 0.0444(19) Uani 1 1 d . . . H66A H 0.2130 0.3074 -0.0330 0.053 Uiso 1 1 calc R . . H66B H 0.1948 0.2201 -0.0363 0.053 Uiso 1 1 calc R . . C67 C 0.0683(8) 0.2376(5) -0.1084(4) 0.059(2) Uani 1 1 d . . . H67A H 0.1064 0.2410 -0.1417 0.071 Uiso 1 1 calc R . . H67B H 0.0250 0.2746 -0.1094 0.071 Uiso 1 1 calc R . . C68 C -0.0136(8) 0.1587(5) -0.1295(4) 0.068(3) Uani 1 1 d . . . H68A H 0.0286 0.1219 -0.1248 0.103 Uiso 1 1 calc R . . H68B H -0.0618 0.1466 -0.1763 0.103 Uiso 1 1 calc R . . H68C H -0.0600 0.1568 -0.1009 0.103 Uiso 1 1 calc R . . C69 C 0.2764(5) 0.3594(4) 0.1024(4) 0.0327(16) Uani 1 1 d . . . H69A H 0.3232 0.3708 0.1499 0.039 Uiso 1 1 calc R . . H69B H 0.3238 0.3489 0.0751 0.039 Uiso 1 1 calc R . . C70 C 0.2437(6) 0.4287(4) 0.0919(4) 0.043(2) Uani 1 1 d . . . H70A H 0.2037 0.4436 0.1227 0.052 Uiso 1 1 calc R . . H70B H 0.1922 0.4173 0.0454 0.052 Uiso 1 1 calc R . . C71 C 0.3472(6) 0.4941(4) 0.1047(4) 0.050(2) Uani 1 1 d . . . H71A H 0.3969 0.5067 0.1518 0.060 Uiso 1 1 calc R . . H71B H 0.3892 0.4779 0.0755 0.060 Uiso 1 1 calc R . . C72 C 0.3177(8) 0.5642(5) 0.0914(6) 0.078(3) Uani 1 1 d . . . H72A H 0.2625 0.5510 0.0463 0.116 Uiso 1 1 calc R . . H72B H 0.3855 0.6020 0.0949 0.116 Uiso 1 1 calc R . . H72C H 0.2860 0.5848 0.1245 0.116 Uiso 1 1 calc R . . C73 C 0.1123(5) 0.2991(4) 0.1308(3) 0.0315(16) Uani 1 1 d . . . H73A H 0.0928 0.3466 0.1301 0.038 Uiso 1 1 calc R . . H73B H 0.0412 0.2575 0.1116 0.038 Uiso 1 1 calc R . . C74 C 0.1664(6) 0.3017(4) 0.2030(3) 0.0383(18) Uani 1 1 d . . . H74A H 0.2458 0.3329 0.2200 0.046 Uiso 1 1 calc R . . H74B H 0.1643 0.2503 0.2066 0.046 Uiso 1 1 calc R . . C75 C 0.1023(7) 0.3358(4) 0.2446(4) 0.045(2) Uani 1 1 d . . . H75A H 0.0210 0.3156 0.2187 0.054 Uiso 1 1 calc R . . H75B H 0.1156 0.3193 0.2859 0.054 Uiso 1 1 calc R . . C76 C 0.1337(8) 0.4196(5) 0.2638(4) 0.063(3) Uani 1 1 d . . . H76A H 0.2146 0.4403 0.2882 0.095 Uiso 1 1 calc R . . H76B H 0.0927 0.4371 0.2924 0.095 Uiso 1 1 calc R . . H76C H 0.1146 0.4365 0.2233 0.095 Uiso 1 1 calc R . . C77 C 0.4548(7) 0.3259(5) 0.3907(4) 0.058(2) Uani 1 1 d . . . H77 H 0.4683 0.3176 0.3470 0.069 Uiso 1 1 calc R . . C78 C 0.3552(15) 0.9010(6) 0.4266(6) 0.157(8) Uani 1 1 d . . . H78 H 0.3255 0.9274 0.4595 0.188 Uiso 1 1 calc R . . C79 C 0.5744(12) 0.8202(9) 0.2985(8) 0.137(6) Uani 1 1 d . . . H79A H 0.5437 0.8605 0.3139 0.206 Uiso 1 1 calc R . . H79B H 0.5915 0.8256 0.2582 0.206 Uiso 1 1 calc R . . H79C H 0.6431 0.8233 0.3338 0.206 Uiso 1 1 calc R . . C80 C 0.4896(12) 0.7450(9) 0.2825(8) 0.126(5) Uani 1 1 d . . . H80A H 0.4191 0.7522 0.2881 0.151 Uiso 1 1 calc R . . H80B H 0.4724 0.7158 0.2357 0.151 Uiso 1 1 calc R . . C81 C 0.4567(14) 0.6357(12) 0.3099(9) 0.161(7) Uani 1 1 d . . . H81A H 0.3841 0.6428 0.3114 0.194 Uiso 1 1 calc R . . H81B H 0.4443 0.6076 0.2634 0.194 Uiso 1 1 calc R . . C82 C 0.4880(11) 0.5921(10) 0.3515(9) 0.159(8) Uani 1 1 d . . . H82A H 0.5700 0.6055 0.3696 0.238 Uiso 1 1 calc R . . H82B H 0.4575 0.5388 0.3260 0.238 Uiso 1 1 calc R . . H82C H 0.4588 0.6012 0.3885 0.238 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 Cl1 0.0275(9) 0.0249(9) 0.0302(9) 0.0046(7) 0.0057(8) 0.0066(7) Cl2 0.0279(9) 0.0302(9) 0.0248(9) 0.0127(7) 0.0082(7) 0.0110(7) Cl3 0.095(2) 0.230(4) 0.069(2) 0.046(2) 0.0163(18) 0.100(3) Cl4 0.146(3) 0.069(2) 0.157(3) 0.007(2) 0.082(3) 0.005(2) Cl5 0.0511(15) 0.096(2) 0.111(2) 0.0276(17) 0.0244(16) 0.0063(14) Cl6 0.108(3) 0.100(2) 0.121(3) 0.009(2) 0.010(2) 0.027(2) Cl7 0.101(3) 0.134(3) 0.214(5) 0.067(3) 0.013(3) 0.028(3) Cl8 0.124(3) 0.114(3) 0.187(4) 0.054(3) 0.072(3) 0.027(2) O1 0.090(5) 0.054(4) 0.059(5) 0.026(4) -0.014(4) 0.007(4) O2 0.099(6) 0.097(6) 0.077(5) 0.048(4) 0.014(4) 0.061(5) O3 0.031(3) 0.021(2) 0.038(3) 0.008(2) 0.016(2) 0.008(2) O4 0.034(3) 0.027(3) 0.029(3) 0.008(2) -0.003(2) 0.011(2) O5 0.036(3) 0.024(3) 0.036(3) 0.007(2) 0.004(2) 0.003(2) O6 0.056(3) 0.040(3) 0.025(3) 0.010(2) 0.003(2) 0.024(3) O7 0.020(2) 0.032(3) 0.036(3) 0.012(2) 0.013(2) 0.005(2) O8 0.033(3) 0.028(3) 0.030(3) 0.005(2) 0.017(2) -0.001(2) O9 0.082(4) 0.039(3) 0.052(4) 0.009(3) 0.031(3) -0.016(3) O10 0.096(5) 0.029(3) 0.052(4) 0.003(3) 0.042(4) 0.011(3) O11 0.089(6) 0.098(6) 0.134(7) 0.045(6) 0.050(6) 0.035(5) N1 0.049(5) 0.051(5) 0.055(5) 0.026(4) 0.003(4) 0.008(4) N2 0.031(3) 0.028(3) 0.033(3) 0.010(3) 0.012(3) 0.014(3) N3 0.024(3) 0.020(3) 0.030(3) 0.008(2) 0.011(3) 0.009(2) N4 0.028(3) 0.024(3) 0.028(3) 0.010(3) -0.004(3) 0.005(3) N5 0.033(3) 0.020(3) 0.026(3) 0.005(2) -0.001(3) 0.009(3) N6 0.028(3) 0.027(3) 0.020(3) 0.011(2) -0.006(3) -0.004(3) N7 0.022(3) 0.031(3) 0.025(3) 0.012(3) 0.001(3) 0.007(2) N8 0.062(4) 0.037(4) 0.028(3) 0.014(3) 0.013(3) 0.033(3) N9 0.031(3) 0.028(3) 0.025(3) 0.012(2) 0.007(3) 0.014(3) N10 0.025(3) 0.030(3) 0.023(3) 0.007(2) 0.003(3) 0.010(3) N11 0.018(3) 0.034(3) 0.025(3) 0.015(3) 0.008(2) 0.009(2) N12 0.041(4) 0.022(3) 0.029(3) 0.008(3) 0.015(3) 0.003(3) N13 0.049(4) 0.020(3) 0.031(3) 0.008(3) 0.022(3) 0.004(3) N14 0.067(5) 0.028(3) 0.033(4) 0.010(3) 0.018(4) 0.005(3) N15 0.035(3) 0.033(3) 0.023(3) 0.010(3) 0.007(3) 0.017(3) N16 0.021(3) 0.025(3) 0.035(3) 0.011(3) 0.009(3) 0.008(2) C1 0.038(5) 0.040(5) 0.039(5) 0.017(4) -0.003(4) 0.008(4) C2 0.030(4) 0.033(4) 0.073(6) 0.026(4) 0.021(4) 0.012(3) C3 0.037(4) 0.026(4) 0.041(4) 0.015(3) 0.015(4) 0.008(3) C4 0.024(4) 0.026(4) 0.038(4) 0.013(3) 0.010(3) 0.002(3) C5 0.050(5) 0.037(4) 0.038(5) 0.014(4) 0.009(4) 0.019(4) C6 0.060(6) 0.031(4) 0.037(5) 0.001(4) 0.002(4) 0.003(4) C7 0.015(3) 0.024(4) 0.028(4) 0.007(3) 0.002(3) -0.003(3) C8 0.021(3) 0.024(4) 0.031(4) 0.010(3) 0.007(3) 0.009(3) C9 0.025(4) 0.026(4) 0.034(4) 0.004(3) 0.010(3) 0.004(3) C10 0.039(5) 0.033(4) 0.034(5) -0.005(3) 0.009(4) 0.004(3) C11 0.049(5) 0.034(4) 0.025(4) 0.003(3) 0.003(4) 0.010(4) C12 0.034(4) 0.028(4) 0.034(4) 0.008(3) 0.011(4) 0.010(3) C13 0.017(3) 0.024(4) 0.033(4) 0.006(3) 0.004(3) 0.006(3) C14 0.026(4) 0.026(4) 0.027(4) 0.010(3) 0.010(3) 0.007(3) C15 0.018(4) 0.026(4) 0.033(4) 0.007(3) 0.000(3) 0.001(3) C16 0.033(4) 0.029(4) 0.028(4) 0.012(3) 0.003(3) 0.005(3) C17 0.047(5) 0.029(4) 0.034(5) 0.017(3) 0.000(4) 0.003(3) C18 0.072(6) 0.020(4) 0.039(5) 0.008(3) -0.002(4) 0.009(4) C19 0.054(5) 0.025(4) 0.025(4) 0.003(3) 0.004(4) 0.012(4) C20 0.031(4) 0.028(4) 0.024(4) 0.010(3) 0.004(3) 0.005(3) C21 0.034(4) 0.024(4) 0.025(4) 0.001(3) 0.010(3) 0.016(3) C22 0.040(4) 0.033(4) 0.029(4) 0.005(3) 0.003(4) 0.011(3) C23 0.049(5) 0.036(4) 0.023(4) 0.011(3) 0.007(4) 0.016(4) C24 0.034(4) 0.023(4) 0.019(4) 0.003(3) 0.004(3) 0.007(3) C25 0.019(3) 0.019(3) 0.031(4) 0.011(3) 0.009(3) 0.006(3) C26 0.036(4) 0.030(4) 0.026(4) 0.010(3) 0.007(3) 0.011(3) C27 0.036(4) 0.043(4) 0.037(5) 0.018(4) 0.006(4) 0.016(4) C28 0.037(4) 0.034(4) 0.038(4) 0.019(3) 0.018(4) 0.018(3) C29 0.031(4) 0.031(4) 0.031(4) 0.010(3) 0.014(3) 0.014(3) C30 0.016(3) 0.026(3) 0.032(4) 0.015(3) 0.008(3) 0.008(3) C31 0.029(4) 0.018(3) 0.025(4) 0.002(3) 0.006(3) 0.008(3) C32 0.019(3) 0.032(4) 0.027(4) 0.011(3) 0.010(3) 0.012(3) C33 0.028(4) 0.030(4) 0.030(4) 0.010(3) 0.004(3) -0.001(3) C34 0.036(4) 0.046(5) 0.032(4) 0.010(4) 0.004(4) -0.002(4) C35 0.044(5) 0.048(5) 0.028(4) 0.017(4) 0.011(4) -0.003(4) C36 0.037(4) 0.032(4) 0.029(4) 0.006(3) 0.003(4) -0.006(3) C37 0.021(4) 0.029(4) 0.031(4) 0.013(3) 0.007(3) 0.003(3) C38 0.024(4) 0.025(4) 0.025(4) 0.010(3) 0.005(3) 0.007(3) C39 0.029(4) 0.024(4) 0.030(4) 0.010(3) 0.009(3) 0.005(3) C40 0.033(4) 0.030(4) 0.025(4) 0.003(3) 0.013(3) 0.005(3) C41 0.047(5) 0.025(4) 0.034(4) 0.008(3) 0.021(4) 0.002(3) C42 0.037(4) 0.024(4) 0.038(4) 0.010(3) 0.010(4) 0.001(3) C43 0.043(4) 0.030(4) 0.026(4) 0.007(3) 0.015(4) 0.011(3) C44 0.037(4) 0.021(3) 0.027(4) 0.007(3) 0.016(3) 0.004(3) C45 0.033(4) 0.039(4) 0.024(4) 0.012(3) 0.007(3) 0.016(3) C46 0.048(5) 0.039(4) 0.037(5) 0.012(4) 0.009(4) 0.012(4) C47 0.059(5) 0.040(5) 0.043(5) 0.019(4) 0.017(4) 0.014(4) C48 0.069(6) 0.072(6) 0.063(6) 0.045(5) 0.024(5) 0.010(5) C49 0.047(5) 0.031(4) 0.027(4) 0.004(3) 0.008(4) 0.016(4) C50 0.082(7) 0.043(5) 0.051(5) 0.019(4) 0.033(5) 0.032(5) C51 0.129(9) 0.090(7) 0.043(5) 0.029(5) 0.036(6) 0.088(7) C52 0.128(10) 0.101(9) 0.104(9) 0.043(7) 0.066(8) 0.072(8) C53 0.028(4) 0.036(4) 0.033(4) 0.009(3) 0.009(3) 0.010(3) C54 0.043(5) 0.049(5) 0.041(5) 0.020(4) 0.012(4) 0.011(4) C55 0.054(5) 0.037(4) 0.036(4) 0.012(3) 0.021(4) 0.018(4) C56 0.091(7) 0.045(5) 0.055(6) 0.028(4) 0.038(5) 0.025(5) C57 0.026(4) 0.030(4) 0.031(4) 0.007(3) 0.001(3) 0.005(3) C58 0.047(5) 0.028(4) 0.032(4) 0.006(3) 0.009(4) 0.007(3) C59 0.046(5) 0.061(6) 0.043(5) 0.017(4) 0.009(4) 0.023(4) C60 0.063(6) 0.078(7) 0.060(6) 0.019(5) 0.020(5) 0.045(5) C61 0.016(3) 0.033(4) 0.035(4) 0.004(3) 0.005(3) 0.009(3) C62 0.034(4) 0.033(4) 0.036(4) 0.010(3) 0.010(4) 0.008(3) C63 0.026(4) 0.044(4) 0.049(5) 0.019(4) 0.018(4) 0.018(3) C64 0.039(4) 0.037(4) 0.063(5) 0.012(4) 0.021(4) 0.020(4) C65 0.024(4) 0.034(4) 0.031(4) 0.003(3) -0.003(3) 0.005(3) C66 0.042(5) 0.048(5) 0.036(5) 0.013(4) 0.010(4) 0.002(4) C67 0.077(7) 0.051(5) 0.030(5) 0.006(4) 0.000(5) 0.009(5) C68 0.079(7) 0.060(6) 0.047(6) -0.004(5) 0.008(5) 0.018(5) C69 0.021(4) 0.032(4) 0.039(4) 0.010(3) 0.007(3) 0.001(3) C70 0.021(4) 0.035(4) 0.078(6) 0.025(4) 0.019(4) 0.008(3) C71 0.037(5) 0.037(5) 0.073(6) 0.018(4) 0.017(5) 0.002(4) C72 0.051(6) 0.034(5) 0.141(10) 0.026(6) 0.031(6) 0.002(4) C73 0.022(4) 0.031(4) 0.044(4) 0.009(3) 0.015(3) 0.010(3) C74 0.040(4) 0.046(5) 0.032(4) 0.012(4) 0.013(4) 0.015(4) C75 0.046(5) 0.053(5) 0.038(5) 0.011(4) 0.017(4) 0.017(4) C76 0.082(7) 0.064(6) 0.039(5) 0.009(4) 0.010(5) 0.033(5) C77 0.046(5) 0.085(7) 0.044(5) 0.019(5) 0.017(4) 0.021(5) C78 0.27(2) 0.039(6) 0.064(8) -0.003(6) -0.045(10) 0.016(9) C79 0.097(11) 0.157(14) 0.179(15) 0.107(13) 0.028(11) 0.050(11) C80 0.100(11) 0.140(14) 0.170(15) 0.077(12) 0.056(11) 0.056(11) C81 0.117(14) 0.20(2) 0.188(18) 0.101(16) 0.050(13) 0.053(15) C82 0.068(9) 0.225(18) 0.240(19) 0.174(17) 0.059(11) 0.045(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 Cl3 C77 1.719(9) . ? Cl4 C77 1.728(9) . ? Cl5 C77 1.754(9) . ? Cl6 C78 1.575(11) . ? Cl7 C78 1.921(14) . ? Cl8 C78 2.034(17) . ? O1 N1 1.238(9) . ? O2 N1 1.210(9) . ? O3 C7 1.219(7) . ? O4 C14 1.229(7) . ? O5 C21 1.216(8) . ? O6 C24 1.230(7) . ? O7 C31 1.191(7) . ? O8 C38 1.226(7) . ? O9 N14 1.222(8) . ? O10 N14 1.238(8) . ? O11 C80 1.357(14) . ? O11 C81 1.419(18) . ? N1 C1 1.440(9) . ? N2 C7 1.377(8) . ? N2 C4 1.400(8) . ? N3 C7 1.374(8) . ? N3 C8 1.453(8) . ? N4 C14 1.372(8) . ? N4 C13 1.407(8) . ? N5 C14 1.359(8) . ? N5 C15 1.409(8) . ? N6 C21 1.363(8) . ? N6 C20 1.428(8) . ? N7 C21 1.372(8) . ? N7 C22 1.444(8) . ? N8 C24 1.352(8) . ? N8 C23 1.445(8) . ? N9 C24 1.366(8) . ? N9 C25 1.410(7) . ? N10 C31 1.389(8) . ? N10 C30 1.437(7) . ? N11 C31 1.398(8) . ? N11 C32 1.451(8) . ? N12 C38 1.360(8) . ? N12 C37 1.408(8) . ? N13 C38 1.377(8) . ? N13 C39 1.400(8) . ? N14 C42 1.470(9) . ? N15 C53 1.491(8) . ? N15 C45 1.516(8) . ? N15 C49 1.523(8) . ? N15 C57 1.559(8) . ? N16 C69 1.517(8) . ? N16 C73 1.520(8) . ? N16 C61 1.522(8) . ? N16 C65 1.525(8) . ? C1 C6 1.363(10) . ? C1 C2 1.366(10) . ? C2 C3 1.386(10) . ? C3 C4 1.412(9) . ? C4 C5 1.355(9) . ? C5 C6 1.390(10) . ? C8 C13 1.384(9) . ? C8 C9 1.397(9) . ? C9 C10 1.373(9) . ? C10 C11 1.414(10) . ? C11 C12 1.395(9) . ? C12 C13 1.381(9) . ? C15 C16 1.395(9) . ? C15 C20 1.412(9) . ? C16 C17 1.379(9) . ? C17 C18 1.379(10) . ? C18 C19 1.374(9) . ? C19 C20 1.377(9) . ? C22 C23 1.502(9) . ? C25 C26 1.353(8) . ? C25 C30 1.398(9) . ? C26 C27 1.408(9) . ? C27 C28 1.380(9) . ? C28 C29 1.408(9) . ? C29 C30 1.385(8) . ? C32 C37 1.383(9) . ? C32 C33 1.388(9) . ? C33 C34 1.404(9) . ? C34 C35 1.414(10) . ? C35 C36 1.375(10) . ? C36 C37 1.393(9) . ? C39 C44 1.391(9) . ? C39 C40 1.398(9) . ? C40 C41 1.386(9) . ? C41 C42 1.361(9) . ? C42 C43 1.389(9) . ? C43 C44 1.368(9) . ? C45 C46 1.520(9) . ? C46 C47 1.525(10) . ? C47 C48 1.507(10) . ? C49 C50 1.504(10) . ? C50 C51 1.542(11) . ? C51 C52 1.448(13) . ? C53 C54 1.513(9) . ? C54 C55 1.523(10) . ? C55 C56 1.560(10) . ? C57 C58 1.498(9) . ? C58 C59 1.508(10) . ? C59 C60 1.506(11) . ? C61 C62 1.513(9) . ? C62 C63 1.547(9) . ? C63 C64 1.502(10) . ? C65 C66 1.517(10) . ? C66 C67 1.507(10) . ? C67 C68 1.528(12) . ? C69 C70 1.508(9) . ? C70 C71 1.531(9) . ? C71 C72 1.520(10) . ? C73 C74 1.511(9) . ? C74 C75 1.532(10) . ? C75 C76 1.489(11) . ? C79 C80 1.505(17) . ? C81 C82 1.380(17) . ? 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 C80 O11 C81 108.7(12) . . ? O2 N1 O1 122.1(7) . . ? O2 N1 C1 119.7(8) . . ? O1 N1 C1 118.1(8) . . ? C7 N2 C4 129.4(5) . . ? C7 N3 C8 124.6(5) . . ? C14 N4 C13 127.2(5) . . ? C14 N5 C15 126.9(5) . . ? C21 N6 C20 124.0(5) . . ? C21 N7 C22 122.7(6) . . ? C24 N8 C23 122.2(5) . . ? C24 N9 C25 127.5(5) . . ? C31 N10 C30 121.6(5) . . ? C31 N11 C32 118.8(5) . . ? C38 N12 C37 129.1(5) . . ? C38 N13 C39 129.5(5) . . ? O9 N14 O10 124.6(6) . . ? O9 N14 C42 117.6(6) . . ? O10 N14 C42 117.8(6) . . ? C53 N15 C45 105.6(5) . . ? C53 N15 C49 114.1(5) . . ? C45 N15 C49 112.2(5) . . ? C53 N15 C57 109.6(5) . . ? C45 N15 C57 111.6(5) . . ? C49 N15 C57 104.0(5) . . ? C69 N16 C73 110.2(5) . . ? C69 N16 C61 106.9(5) . . ? C73 N16 C61 111.1(5) . . ? C69 N16 C65 111.5(5) . . ? C73 N16 C65 107.4(5) . . ? C61 N16 C65 109.9(5) . . ? C6 C1 C2 120.1(7) . . ? C6 C1 N1 120.7(8) . . ? C2 C1 N1 119.2(7) . . ? C1 C2 C3 121.3(7) . . ? C2 C3 C4 118.2(7) . . ? C5 C4 N2 117.0(6) . . ? C5 C4 C3 119.7(6) . . ? N2 C4 C3 123.3(6) . . ? C4 C5 C6 120.9(7) . . ? C1 C6 C5 119.7(7) . . ? O3 C7 N3 124.2(6) . . ? O3 C7 N2 124.6(6) . . ? N3 C7 N2 111.2(6) . . ? C13 C8 C9 120.9(6) . . ? C13 C8 N3 118.1(6) . . ? C9 C8 N3 120.9(6) . . ? C10 C9 C8 119.3(6) . . ? C9 C10 C11 120.1(6) . . ? C12 C11 C10 119.7(6) . . ? C13 C12 C11 119.7(6) . . ? C12 C13 C8 120.1(6) . . ? C12 C13 N4 122.7(6) . . ? C8 C13 N4 117.1(6) . . ? O4 C14 N5 125.1(6) . . ? O4 C14 N4 123.9(6) . . ? N5 C14 N4 111.0(5) . . ? C16 C15 N5 122.9(6) . . ? C16 C15 C20 119.0(6) . . ? N5 C15 C20 118.1(5) . . ? C17 C16 C15 119.9(6) . . ? C16 C17 C18 120.4(6) . . ? C19 C18 C17 120.6(7) . . ? C18 C19 C20 120.0(7) . . ? C19 C20 C15 120.0(6) . . ? C19 C20 N6 121.7(6) . . ? C15 C20 N6 118.3(6) . . ? O5 C21 N6 124.0(6) . . ? O5 C21 N7 122.5(6) . . ? N6 C21 N7 113.5(6) . . ? N7 C22 C23 112.0(6) . . ? N8 C23 C22 111.3(6) . . ? O6 C24 N8 122.4(6) . . ? O6 C24 N9 123.3(6) . . ? N8 C24 N9 114.3(5) . . ? C26 C25 C30 118.8(6) . . ? C26 C25 N9 123.1(6) . . ? C30 C25 N9 118.0(5) . . ? C25 C26 C27 121.7(6) . . ? C28 C27 C26 119.7(6) . . ? C27 C28 C29 119.0(6) . . ? C30 C29 C28 119.8(6) . . ? C29 C30 C25 121.0(6) . . ? C29 C30 N10 118.6(6) . . ? C25 C30 N10 120.4(5) . . ? O7 C31 N10 124.6(6) . . ? O7 C31 N11 123.6(6) . . ? N10 C31 N11 111.8(6) . . ? C37 C32 C33 121.5(6) . . ? C37 C32 N11 120.6(6) . . ? C33 C32 N11 117.8(6) . . ? C32 C33 C34 119.7(6) . . ? C33 C34 C35 117.9(7) . . ? C36 C35 C34 121.5(7) . . ? C35 C36 C37 119.9(7) . . ? C32 C37 C36 119.2(6) . . ? C32 C37 N12 117.8(6) . . ? C36 C37 N12 123.0(6) . . ? O8 C38 N12 125.5(6) . . ? O8 C38 N13 123.5(6) . . ? N12 C38 N13 110.9(5) . . ? C44 C39 C40 119.9(6) . . ? C44 C39 N13 116.1(6) . . ? C40 C39 N13 124.0(6) . . ? C41 C40 C39 118.5(6) . . ? C42 C41 C40 120.4(6) . . ? C41 C42 C43 121.8(6) . . ? C41 C42 N14 119.6(6) . . ? C43 C42 N14 118.6(6) . . ? C44 C43 C42 118.2(6) . . ? C43 C44 C39 121.1(6) . . ? N15 C45 C46 116.4(6) . . ? C45 C46 C47 109.5(6) . . ? C48 C47 C46 112.9(7) . . ? C50 C49 N15 114.6(6) . . ? C49 C50 C51 108.6(7) . . ? C52 C51 C50 114.9(10) . . ? N15 C53 C54 116.2(6) . . ? C53 C54 C55 110.9(6) . . ? C54 C55 C56 111.2(6) . . ? C58 C57 N15 116.5(5) . . ? C57 C58 C59 112.4(6) . . ? C60 C59 C58 113.8(7) . . ? C62 C61 N16 115.7(5) . . ? C61 C62 C63 110.8(6) . . ? C64 C63 C62 113.1(6) . . ? C66 C65 N16 115.2(5) . . ? C67 C66 C65 109.7(7) . . ? C66 C67 C68 114.7(7) . . ? C70 C69 N16 116.4(5) . . ? C69 C70 C71 111.0(6) . . ? C72 C71 C70 112.8(6) . . ? C74 C73 N16 116.8(5) . . ? C73 C74 C75 108.8(6) . . ? C76 C75 C74 114.4(7) . . ? Cl3 C77 Cl4 112.1(5) . . ? Cl3 C77 Cl5 109.8(5) . . ? Cl4 C77 Cl5 109.8(5) . . ? Cl6 C78 Cl7 110.0(7) . . ? Cl6 C78 Cl8 103.8(8) . . ? Cl7 C78 Cl8 93.9(8) . . ? O11 C80 C79 107.7(12) . . ? C82 C81 O11 115.5(15) . . ? 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 O2 N1 C1 C6 -178.7(8) . . . . ? O1 N1 C1 C6 -0.9(11) . . . . ? O2 N1 C1 C2 2.5(12) . . . . ? O1 N1 C1 C2 -179.7(7) . . . . ? C6 C1 C2 C3 2.1(11) . . . . ? N1 C1 C2 C3 -179.0(7) . . . . ? C1 C2 C3 C4 0.4(10) . . . . ? C7 N2 C4 C5 173.8(7) . . . . ? C7 N2 C4 C3 -6.1(10) . . . . ? C2 C3 C4 C5 -2.0(10) . . . . ? C2 C3 C4 N2 177.8(6) . . . . ? N2 C4 C5 C6 -178.7(7) . . . . ? C3 C4 C5 C6 1.1(11) . . . . ? C2 C1 C6 C5 -3.0(12) . . . . ? N1 C1 C6 C5 178.1(7) . . . . ? C4 C5 C6 C1 1.4(12) . . . . ? C8 N3 C7 O3 6.0(9) . . . . ? C8 N3 C7 N2 -173.2(5) . . . . ? C4 N2 C7 O3 5.4(10) . . . . ? C4 N2 C7 N3 -175.4(6) . . . . ? C7 N3 C8 C13 -132.1(6) . . . . ? C7 N3 C8 C9 50.3(9) . . . . ? C13 C8 C9 C10 -2.8(10) . . . . ? N3 C8 C9 C10 174.7(6) . . . . ? C8 C9 C10 C11 -0.3(10) . . . . ? C9 C10 C11 C12 3.4(11) . . . . ? C10 C11 C12 C13 -3.5(10) . . . . ? C11 C12 C13 C8 0.5(10) . . . . ? C11 C12 C13 N4 179.2(6) . . . . ? C9 C8 C13 C12 2.7(9) . . . . ? N3 C8 C13 C12 -174.9(6) . . . . ? C9 C8 C13 N4 -176.0(5) . . . . ? N3 C8 C13 N4 6.4(8) . . . . ? C14 N4 C13 C12 45.2(10) . . . . ? C14 N4 C13 C8 -136.1(6) . . . . ? C15 N5 C14 O4 0.2(11) . . . . ? C15 N5 C14 N4 -178.2(6) . . . . ? C13 N4 C14 O4 -6.2(10) . . . . ? C13 N4 C14 N5 172.2(6) . . . . ? C14 N5 C15 C16 -41.5(10) . . . . ? C14 N5 C15 C20 138.9(7) . . . . ? N5 C15 C16 C17 -176.6(6) . . . . ? C20 C15 C16 C17 3.0(10) . . . . ? C15 C16 C17 C18 -1.0(11) . . . . ? C16 C17 C18 C19 -1.9(13) . . . . ? C17 C18 C19 C20 2.7(13) . . . . ? C18 C19 C20 C15 -0.7(11) . . . . ? C18 C19 C20 N6 178.9(7) . . . . ? C16 C15 C20 C19 -2.2(10) . . . . ? N5 C15 C20 C19 177.5(6) . . . . ? C16 C15 C20 N6 178.3(6) . . . . ? N5 C15 C20 N6 -2.1(9) . . . . ? C21 N6 C20 C19 -55.9(9) . . . . ? C21 N6 C20 C15 123.7(7) . . . . ? C20 N6 C21 O5 5.2(10) . . . . ? C20 N6 C21 N7 -174.2(6) . . . . ? C22 N7 C21 O5 -3.6(9) . . . . ? C22 N7 C21 N6 175.8(6) . . . . ? C21 N7 C22 C23 -148.2(6) . . . . ? C24 N8 C23 C22 153.3(6) . . . . ? N7 C22 C23 N8 61.4(8) . . . . ? C23 N8 C24 O6 -7.0(11) . . . . ? C23 N8 C24 N9 171.3(6) . . . . ? C25 N9 C24 O6 -17.7(11) . . . . ? C25 N9 C24 N8 164.0(6) . . . . ? C24 N9 C25 C26 -16.1(10) . . . . ? C24 N9 C25 C30 166.2(6) . . . . ? C30 C25 C26 C27 2.7(9) . . . . ? N9 C25 C26 C27 -175.1(6) . . . . ? C25 C26 C27 C28 -2.1(10) . . . . ? C26 C27 C28 C29 -0.6(10) . . . . ? C27 C28 C29 C30 2.5(10) . . . . ? C28 C29 C30 C25 -1.9(9) . . . . ? C28 C29 C30 N10 177.6(6) . . . . ? C26 C25 C30 C29 -0.6(9) . . . . ? N9 C25 C30 C29 177.2(6) . . . . ? C26 C25 C30 N10 179.9(6) . . . . ? N9 C25 C30 N10 -2.3(8) . . . . ? C31 N10 C30 C29 -55.7(8) . . . . ? C31 N10 C30 C25 123.8(6) . . . . ? C30 N10 C31 O7 -4.9(9) . . . . ? C30 N10 C31 N11 177.1(5) . . . . ? C32 N11 C31 O7 5.3(9) . . . . ? C32 N11 C31 N10 -176.6(5) . . . . ? C31 N11 C32 C37 -69.6(7) . . . . ? C31 N11 C32 C33 113.5(6) . . . . ? C37 C32 C33 C34 3.5(10) . . . . ? N11 C32 C33 C34 -179.6(6) . . . . ? C32 C33 C34 C35 -0.2(10) . . . . ? C33 C34 C35 C36 -1.6(11) . . . . ? C34 C35 C36 C37 0.1(12) . . . . ? C33 C32 C37 C36 -5.0(10) . . . . ? N11 C32 C37 C36 178.2(6) . . . . ? C33 C32 C37 N12 173.2(6) . . . . ? N11 C32 C37 N12 -3.7(9) . . . . ? C35 C36 C37 C32 3.2(10) . . . . ? C35 C36 C37 N12 -174.9(6) . . . . ? C38 N12 C37 C32 169.5(6) . . . . ? C38 N12 C37 C36 -12.4(11) . . . . ? C37 N12 C38 O8 -8.9(11) . . . . ? C37 N12 C38 N13 168.9(6) . . . . ? C39 N13 C38 O8 5.8(11) . . . . ? C39 N13 C38 N12 -172.1(6) . . . . ? C38 N13 C39 C44 165.5(6) . . . . ? C38 N13 C39 C40 -12.4(11) . . . . ? C44 C39 C40 C41 4.1(10) . . . . ? N13 C39 C40 C41 -178.1(6) . . . . ? C39 C40 C41 C42 -2.2(10) . . . . ? C40 C41 C42 C43 -0.7(11) . . . . ? C40 C41 C42 N14 178.9(6) . . . . ? O9 N14 C42 C41 -17.6(10) . . . . ? O10 N14 C42 C41 160.9(7) . . . . ? O9 N14 C42 C43 162.0(6) . . . . ? O10 N14 C42 C43 -19.5(10) . . . . ? C41 C42 C43 C44 1.7(10) . . . . ? N14 C42 C43 C44 -177.8(6) . . . . ? C42 C43 C44 C39 0.2(10) . . . . ? C40 C39 C44 C43 -3.1(10) . . . . ? N13 C39 C44 C43 178.9(6) . . . . ? C53 N15 C45 C46 -175.6(6) . . . . ? C49 N15 C45 C46 -50.8(8) . . . . ? C57 N15 C45 C46 65.4(7) . . . . ? N15 C45 C46 C47 179.0(6) . . . . ? C45 C46 C47 C48 -177.1(7) . . . . ? C53 N15 C49 C50 58.6(7) . . . . ? C45 N15 C49 C50 -61.4(8) . . . . ? C57 N15 C49 C50 178.0(6) . . . . ? N15 C49 C50 C51 173.3(6) . . . . ? C49 C50 C51 C52 171.5(8) . . . . ? C45 N15 C53 C54 -177.2(6) . . . . ? C49 N15 C53 C54 59.2(8) . . . . ? C57 N15 C53 C54 -56.9(7) . . . . ? N15 C53 C54 C55 -174.3(6) . . . . ? C53 C54 C55 C56 -172.3(6) . . . . ? C53 N15 C57 C58 -55.3(7) . . . . ? C45 N15 C57 C58 61.2(7) . . . . ? C49 N15 C57 C58 -177.7(6) . . . . ? N15 C57 C58 C59 178.6(6) . . . . ? C57 C58 C59 C60 176.7(7) . . . . ? C69 N16 C61 C62 -174.4(6) . . . . ? C73 N16 C61 C62 65.4(7) . . . . ? C65 N16 C61 C62 -53.3(7) . . . . ? N16 C61 C62 C63 -165.6(5) . . . . ? C61 C62 C63 C64 -164.2(6) . . . . ? C69 N16 C65 C66 56.4(7) . . . . ? C73 N16 C65 C66 177.2(6) . . . . ? C61 N16 C65 C66 -61.8(7) . . . . ? N16 C65 C66 C67 177.9(6) . . . . ? C65 C66 C67 C68 -68.6(10) . . . . ? C73 N16 C69 C70 -63.7(7) . . . . ? C61 N16 C69 C70 175.5(6) . . . . ? C65 N16 C69 C70 55.4(8) . . . . ? N16 C69 C70 C71 -174.6(6) . . . . ? C69 C70 C71 C72 177.3(7) . . . . ? C69 N16 C73 C74 -71.6(7) . . . . ? C61 N16 C73 C74 46.7(7) . . . . ? C65 N16 C73 C74 166.8(6) . . . . ? N16 C73 C74 C75 163.2(6) . . . . ? C73 C74 C75 C76 -81.1(8) . . . . ? C81 O11 C80 C79 -178.4(13) . . . . ? C80 O11 C81 C82 -177.0(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 Cl1 0.88 2.39 3.222(5) 158.8 . N3 H3 Cl1 0.88 2.56 3.388(5) 156.1 . N6 H6 Cl1 0.88 2.54 3.370(5) 156.7 . N7 H7 Cl1 0.88 2.49 3.327(6) 158.8 . C77 H77 Cl1 1.00 2.48 3.475(9) 175.5 . C61 H61B Cl1 0.99 2.77 3.624(7) 144.9 . N4 H4 Cl2 0.88 2.29 3.153(5) 167.0 . N5 H5 Cl2 0.88 2.48 3.310(5) 158.2 . N8 H8 Cl2 0.88 2.39 3.210(6) 154.4 . N9 H9 Cl2 0.88 2.41 3.212(5) 152.2 . N12 H12 Cl2 0.88 2.60 3.417(6) 153.9 . N13 H13 Cl2 0.88 2.29 3.158(6) 168.6 . N10 H10 O3 0.88 2.20 2.995(7) 150.6 . N11 H11 O3 0.88 2.12 2.927(7) 151.8 . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.022 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.112 ############ data_(TEA)4LBr4 _database_code_depnum_ccdc_archive 'CCDC 849103' #TrackingRef 'complexes 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H120 Br4 N18 O10' _chemical_formula_weight 1765.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.952(3) _cell_length_b 28.436(8) _cell_length_c 12.614(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.341(4) _cell_angle_gamma 90.00 _cell_volume 4283(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6388 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 24.52 _exptl_crystal_description Blocl _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 1.944 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5932 _exptl_absorpt_correction_T_max 0.6219 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27516 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7455 _reflns_number_gt 5464 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+1.1780P] 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 7455 _refine_ls_number_parameters 495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _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 Br1 Br 0.69161(3) 0.606062(12) 0.52999(3) 0.03127(12) Uani 1 1 d . . . Br2 Br 0.95578(3) 0.580697(11) 0.76265(3) 0.03253(12) Uani 1 1 d . . . O1 O 0.7570(2) 0.33393(9) 0.8212(2) 0.0498(8) Uani 1 1 d . . . O2 O 0.6343(3) 0.34080(9) 0.9393(3) 0.0514(8) Uani 1 1 d . . . O3 O 0.5824(2) 0.58119(8) 0.9178(2) 0.0333(6) Uani 1 1 d . . . O4 O 0.8747(2) 0.75758(7) 0.6875(2) 0.0326(6) Uani 1 1 d . . . O5 O 1.09985(19) 0.58761(7) 0.4196(2) 0.0279(6) Uani 1 1 d . . . N1 N 0.6905(3) 0.35713(10) 0.8695(3) 0.0327(8) Uani 1 1 d . . . N2 N 0.6590(3) 0.54937(9) 0.7717(2) 0.0300(7) Uani 1 1 d . . . H2 H 0.6788 0.5566 0.7072 0.036 Uiso 1 1 calc R . . N3 N 0.6634(2) 0.62840(9) 0.7964(2) 0.0244(7) Uani 1 1 d . . . H3 H 0.6869 0.6287 0.7311 0.029 Uiso 1 1 calc R . . N4 N 0.8382(2) 0.68822(9) 0.7715(2) 0.0240(7) Uani 1 1 d . . . H4 H 0.8591 0.6586 0.7771 0.029 Uiso 1 1 calc R . . N5 N 0.9700(2) 0.69034(9) 0.6475(2) 0.0245(7) Uani 1 1 d . . . H5 H 0.9885 0.6622 0.6717 0.029 Uiso 1 1 calc R . . N6 N 0.9568(2) 0.63510(9) 0.4678(2) 0.0231(7) Uani 1 1 d . . . H6 H 0.8860 0.6360 0.4843 0.028 Uiso 1 1 calc R . . N7 N 0.9314(2) 0.55609(9) 0.4544(2) 0.0227(6) Uani 1 1 d . . . H7 H 0.8600 0.5616 0.4634 0.027 Uiso 1 1 calc R . . N8 N 0.6551(2) 0.36109(10) 0.3759(3) 0.0318(7) Uani 1 1 d . . . N9 N 0.1719(3) 0.09130(11) 0.3582(3) 0.0456(9) Uani 1 1 d . . . C1 C 0.6773(3) 0.40719(11) 0.8435(3) 0.0263(8) Uani 1 1 d . . . C2 C 0.6100(3) 0.43479(12) 0.9033(3) 0.0303(9) Uani 1 1 d . . . H2A H 0.5701 0.4215 0.9596 0.036 Uiso 1 1 calc R . . C3 C 0.6011(3) 0.48251(11) 0.8804(3) 0.0306(9) Uani 1 1 d . . . H3A H 0.5545 0.5020 0.9209 0.037 Uiso 1 1 calc R . . C4 C 0.6601(3) 0.50162(11) 0.7986(3) 0.0251(8) Uani 1 1 d . . . C5 C 0.7256(3) 0.47198(11) 0.7371(3) 0.0294(9) Uani 1 1 d . . . H5A H 0.7640 0.4846 0.6790 0.035 Uiso 1 1 calc R . . C6 C 0.7345(3) 0.42494(12) 0.7604(3) 0.0308(9) Uani 1 1 d . . . H6A H 0.7797 0.4050 0.7195 0.037 Uiso 1 1 calc R . . C7 C 0.6303(3) 0.58614(11) 0.8357(3) 0.0224(8) Uani 1 1 d . . . C8 C 0.6633(3) 0.67180(11) 0.8515(3) 0.0227(8) Uani 1 1 d . . . C9 C 0.5795(3) 0.68406(12) 0.9189(3) 0.0282(8) Uani 1 1 d . . . H9 H 0.5196 0.6629 0.9301 0.034 Uiso 1 1 calc R . . C10 C 0.5828(3) 0.72719(12) 0.9701(3) 0.0342(9) Uani 1 1 d . . . H10 H 0.5255 0.7355 1.0167 0.041 Uiso 1 1 calc R . . C11 C 0.6693(3) 0.75815(13) 0.9535(3) 0.0401(10) Uani 1 1 d . . . H11 H 0.6709 0.7878 0.9882 0.048 Uiso 1 1 calc R . . C12 C 0.7533(3) 0.74639(11) 0.8870(3) 0.0327(9) Uani 1 1 d . . . H12 H 0.8126 0.7679 0.8763 0.039 Uiso 1 1 calc R . . C13 C 0.7516(3) 0.70309(11) 0.8355(3) 0.0253(8) Uani 1 1 d . . . C14 C 0.8928(3) 0.71563(11) 0.7016(3) 0.0238(8) Uani 1 1 d . . . C15 C 1.0216(3) 0.70635(10) 0.5561(3) 0.0211(7) Uani 1 1 d . . . C16 C 1.0786(3) 0.74902(11) 0.5545(3) 0.0290(9) Uani 1 1 d . . . H16 H 1.0823 0.7684 0.6159 0.035 Uiso 1 1 calc R . . C17 C 1.1293(3) 0.76312(12) 0.4644(3) 0.0336(9) Uani 1 1 d . . . H17 H 1.1678 0.7923 0.4636 0.040 Uiso 1 1 calc R . . C18 C 1.1249(3) 0.73521(12) 0.3743(3) 0.0337(9) Uani 1 1 d . . . H18 H 1.1602 0.7452 0.3120 0.040 Uiso 1 1 calc R . . C19 C 1.0687(3) 0.69267(11) 0.3753(3) 0.0266(8) Uani 1 1 d . . . H19 H 1.0658 0.6734 0.3138 0.032 Uiso 1 1 calc R . . C20 C 1.0170(3) 0.67820(10) 0.4651(3) 0.0225(8) Uani 1 1 d . . . C21 C 1.0026(3) 0.59232(11) 0.4460(3) 0.0227(8) Uani 1 1 d . . . C22 C 0.9710(3) 0.50766(10) 0.4487(3) 0.0245(8) Uani 1 1 d . . . H22A H 1.0237 0.5048 0.3905 0.029 Uiso 1 1 calc R . . H22B H 0.9067 0.4866 0.4323 0.029 Uiso 1 1 calc R . . C23 C 0.5947(3) 0.40798(13) 0.3805(4) 0.0370(10) Uani 1 1 d . . . H23A H 0.5752 0.4182 0.3071 0.044 Uiso 1 1 calc R . . H23B H 0.5237 0.4033 0.4170 0.044 Uiso 1 1 calc R . . C24 C 0.6598(4) 0.44691(14) 0.4364(4) 0.0512(12) Uani 1 1 d . . . H24A H 0.6763 0.4379 0.5104 0.077 Uiso 1 1 calc R . . H24B H 0.6152 0.4758 0.4342 0.077 Uiso 1 1 calc R . . H24C H 0.7301 0.4522 0.4007 0.077 Uiso 1 1 calc R . . C25 C 0.7593(3) 0.36465(16) 0.3116(4) 0.0435(11) Uani 1 1 d . . . H25A H 0.8091 0.3889 0.3442 0.052 Uiso 1 1 calc R . . H25B H 0.7995 0.3343 0.3164 0.052 Uiso 1 1 calc R . . C26 C 0.7387(4) 0.37659(17) 0.1962(4) 0.0539(12) Uani 1 1 d . . . H26A H 0.6951 0.3514 0.1612 0.081 Uiso 1 1 calc R . . H26B H 0.8105 0.3800 0.1622 0.081 Uiso 1 1 calc R . . H26C H 0.6969 0.4062 0.1900 0.081 Uiso 1 1 calc R . . C27 C 0.5709(3) 0.32679(13) 0.3261(3) 0.0367(10) Uani 1 1 d . . . H27A H 0.5059 0.3249 0.3721 0.044 Uiso 1 1 calc R . . H27B H 0.5437 0.3397 0.2569 0.044 Uiso 1 1 calc R . . C28 C 0.6140(4) 0.27759(14) 0.3086(4) 0.0509(12) Uani 1 1 d . . . H28A H 0.6765 0.2787 0.2607 0.076 Uiso 1 1 calc R . . H28B H 0.5538 0.2581 0.2770 0.076 Uiso 1 1 calc R . . H28C H 0.6398 0.2640 0.3767 0.076 Uiso 1 1 calc R . . C29 C 0.6936(3) 0.34508(13) 0.4860(3) 0.0358(9) Uani 1 1 d . . . H29A H 0.7310 0.3142 0.4798 0.043 Uiso 1 1 calc R . . H29B H 0.7502 0.3677 0.5145 0.043 Uiso 1 1 calc R . . C30 C 0.6030(3) 0.34057(14) 0.5647(4) 0.0435(11) Uani 1 1 d . . . H30A H 0.5669 0.3712 0.5737 0.065 Uiso 1 1 calc R . . H30B H 0.6358 0.3300 0.6330 0.065 Uiso 1 1 calc R . . H30C H 0.5472 0.3176 0.5386 0.065 Uiso 1 1 calc R . . C31 C 0.2078(4) 0.12620(16) 0.2749(4) 0.0522(12) Uani 1 1 d . . . H31A H 0.2068 0.1100 0.2054 0.063 Uiso 1 1 calc R . . H31B H 0.1516 0.1518 0.2698 0.063 Uiso 1 1 calc R . . C32 C 0.3215(4) 0.14790(19) 0.2947(4) 0.0705(15) Uani 1 1 d . . . H32A H 0.3243 0.1637 0.3638 0.106 Uiso 1 1 calc R . . H32B H 0.3355 0.1709 0.2388 0.106 Uiso 1 1 calc R . . H32C H 0.3789 0.1233 0.2943 0.106 Uiso 1 1 calc R . . C33 C 0.1599(4) 0.11551(13) 0.4638(3) 0.0411(10) Uani 1 1 d . . . H33A H 0.1455 0.0913 0.5181 0.049 Uiso 1 1 calc R . . H33B H 0.2318 0.1309 0.4843 0.049 Uiso 1 1 calc R . . C34 C 0.0684(4) 0.15171(13) 0.4658(4) 0.0436(11) Uani 1 1 d . . . H34A H 0.0831 0.1766 0.4144 0.065 Uiso 1 1 calc R . . H34B H 0.0661 0.1653 0.5370 0.065 Uiso 1 1 calc R . . H34C H -0.0037 0.1368 0.4472 0.065 Uiso 1 1 calc R . . C35 C 0.2582(5) 0.05265(16) 0.3758(4) 0.0662(16) Uani 1 1 d . . . H35A H 0.3293 0.0670 0.4028 0.079 Uiso 1 1 calc R . . H35B H 0.2322 0.0311 0.4313 0.079 Uiso 1 1 calc R . . C36 C 0.2814(6) 0.0241(2) 0.2777(5) 0.098(2) Uani 1 1 d . . . H36A H 0.2134 0.0072 0.2542 0.148 Uiso 1 1 calc R . . H36B H 0.3414 0.0015 0.2944 0.148 Uiso 1 1 calc R . . H36C H 0.3044 0.0452 0.2211 0.148 Uiso 1 1 calc R . . C37 C 0.0612(4) 0.07091(15) 0.3180(4) 0.0543(13) Uani 1 1 d . . . H37A H 0.0087 0.0971 0.3018 0.065 Uiso 1 1 calc R . . H37B H 0.0731 0.0540 0.2508 0.065 Uiso 1 1 calc R . . C38 C 0.0071(5) 0.03761(16) 0.3942(4) 0.0749(17) Uani 1 1 d . . . H38A H 0.0588 0.0117 0.4118 0.112 Uiso 1 1 calc R . . H38B H -0.0620 0.0249 0.3609 0.112 Uiso 1 1 calc R . . H38C H -0.0104 0.0546 0.4590 0.112 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 Br1 0.0292(2) 0.0332(2) 0.0321(2) 0.00570(17) 0.00970(16) 0.00275(16) Br2 0.0449(2) 0.01664(17) 0.0368(3) 0.00091(16) 0.01018(18) 0.00476(16) O1 0.071(2) 0.0253(14) 0.055(2) 0.0084(13) 0.0337(17) 0.0188(14) O2 0.077(2) 0.0215(13) 0.059(2) 0.0126(14) 0.0402(18) 0.0070(14) O3 0.0498(16) 0.0197(12) 0.0317(17) 0.0000(11) 0.0192(13) -0.0022(11) O4 0.0498(16) 0.0117(12) 0.0376(17) 0.0040(11) 0.0163(13) 0.0038(11) O5 0.0300(14) 0.0183(12) 0.0363(16) -0.0026(11) 0.0127(12) 0.0015(10) N1 0.046(2) 0.0174(15) 0.035(2) 0.0040(14) 0.0127(17) 0.0036(14) N2 0.056(2) 0.0098(13) 0.0255(18) -0.0008(12) 0.0191(15) -0.0014(13) N3 0.0391(17) 0.0154(13) 0.0197(17) 0.0007(12) 0.0121(13) -0.0013(12) N4 0.0330(16) 0.0112(13) 0.0289(18) 0.0029(12) 0.0159(14) 0.0022(12) N5 0.0376(17) 0.0090(12) 0.0279(18) 0.0026(12) 0.0121(14) 0.0032(12) N6 0.0257(15) 0.0123(13) 0.0320(19) -0.0035(12) 0.0094(13) -0.0008(11) N7 0.0244(15) 0.0122(13) 0.0321(18) -0.0010(12) 0.0068(13) -0.0006(11) N8 0.0288(16) 0.0298(16) 0.037(2) 0.0010(14) 0.0061(14) 0.0006(13) N9 0.072(3) 0.0334(18) 0.030(2) -0.0075(15) -0.0121(19) 0.0136(17) C1 0.036(2) 0.0134(16) 0.030(2) 0.0027(15) 0.0085(17) -0.0001(15) C2 0.043(2) 0.0225(18) 0.027(2) 0.0025(16) 0.0208(18) -0.0033(16) C3 0.041(2) 0.0191(17) 0.033(2) -0.0011(16) 0.0205(18) 0.0017(16) C4 0.034(2) 0.0150(16) 0.027(2) -0.0002(15) 0.0078(16) -0.0023(15) C5 0.040(2) 0.0199(17) 0.030(2) -0.0009(16) 0.0185(17) -0.0026(16) C6 0.037(2) 0.0205(18) 0.036(2) -0.0010(16) 0.0160(18) 0.0007(16) C7 0.0282(18) 0.0173(16) 0.022(2) 0.0018(15) 0.0060(16) 0.0020(14) C8 0.0318(19) 0.0159(16) 0.021(2) 0.0004(14) 0.0068(15) 0.0043(14) C9 0.034(2) 0.0206(17) 0.031(2) 0.0008(16) 0.0103(17) 0.0043(15) C10 0.042(2) 0.0229(18) 0.039(3) -0.0016(17) 0.0192(19) 0.0050(17) C11 0.053(3) 0.0228(19) 0.045(3) -0.0101(18) 0.015(2) 0.0049(18) C12 0.044(2) 0.0170(17) 0.038(2) -0.0052(16) 0.0114(19) -0.0042(16) C13 0.0315(19) 0.0164(16) 0.029(2) 0.0024(15) 0.0087(16) 0.0048(15) C14 0.0283(19) 0.0187(17) 0.025(2) -0.0017(15) 0.0027(16) -0.0009(15) C15 0.0239(17) 0.0129(15) 0.027(2) 0.0008(14) 0.0088(15) 0.0017(13) C16 0.039(2) 0.0159(16) 0.033(2) -0.0042(16) 0.0102(18) -0.0038(15) C17 0.041(2) 0.0164(17) 0.044(3) 0.0035(17) 0.0098(19) -0.0073(16) C18 0.045(2) 0.0247(19) 0.032(2) 0.0054(17) 0.0156(18) -0.0049(17) C19 0.035(2) 0.0174(17) 0.028(2) -0.0026(15) 0.0070(17) -0.0002(15) C20 0.0254(18) 0.0125(15) 0.030(2) 0.0022(15) 0.0042(16) -0.0008(14) C21 0.032(2) 0.0155(16) 0.021(2) -0.0009(14) 0.0048(16) 0.0009(15) C22 0.0332(19) 0.0111(15) 0.030(2) -0.0037(14) 0.0074(16) -0.0014(14) C23 0.029(2) 0.031(2) 0.051(3) 0.0034(19) 0.0066(19) 0.0040(17) C24 0.061(3) 0.029(2) 0.062(3) 0.008(2) -0.005(2) -0.007(2) C25 0.028(2) 0.053(3) 0.050(3) 0.002(2) 0.012(2) 0.0020(19) C26 0.042(3) 0.070(3) 0.051(3) 0.007(3) 0.018(2) 0.003(2) C27 0.033(2) 0.038(2) 0.039(3) -0.0063(19) 0.0056(18) -0.0045(17) C28 0.054(3) 0.040(2) 0.060(3) -0.010(2) 0.012(2) 0.002(2) C29 0.034(2) 0.035(2) 0.038(3) 0.0028(19) 0.0003(18) 0.0012(17) C30 0.048(2) 0.040(2) 0.043(3) 0.005(2) 0.004(2) -0.0061(19) C31 0.075(3) 0.049(3) 0.032(3) 0.002(2) 0.001(2) 0.015(2) C32 0.082(4) 0.074(4) 0.055(4) 0.008(3) 0.005(3) 0.000(3) C33 0.070(3) 0.0262(19) 0.027(2) -0.0055(17) -0.007(2) 0.0049(19) C34 0.066(3) 0.025(2) 0.040(3) 0.0015(18) 0.004(2) 0.0030(19) C35 0.102(4) 0.040(3) 0.055(3) -0.012(2) -0.025(3) 0.036(3) C36 0.142(6) 0.074(4) 0.077(5) -0.039(3) -0.024(4) 0.057(4) C37 0.079(3) 0.039(2) 0.043(3) -0.008(2) -0.020(3) -0.003(2) C38 0.112(4) 0.039(3) 0.072(4) 0.001(3) -0.022(3) -0.027(3) _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 O1 N1 1.216(4) . ? O2 N1 1.220(4) . ? O3 C7 1.213(4) . ? O4 C14 1.224(4) . ? O5 C21 1.229(4) . ? N1 C1 1.468(4) . ? N2 C7 1.373(4) . ? N2 C4 1.400(4) . ? N3 C7 1.365(4) . ? N3 C8 1.417(4) . ? N4 C14 1.364(4) . ? N4 C13 1.403(4) . ? N5 C14 1.373(4) . ? N5 C15 1.405(4) . ? N6 C21 1.367(4) . ? N6 C20 1.422(4) . ? N7 C21 1.343(4) . ? N7 C22 1.459(4) . ? N8 C29 1.515(5) . ? N8 C25 1.518(5) . ? N8 C23 1.518(4) . ? N8 C27 1.518(5) . ? N9 C33 1.512(5) . ? N9 C37 1.514(5) . ? N9 C35 1.518(5) . ? N9 C31 1.520(5) . ? C1 C2 1.372(5) . ? C1 C6 1.372(5) . ? C2 C3 1.391(5) . ? C3 C4 1.384(5) . ? C4 C5 1.405(5) . ? C5 C6 1.373(5) . ? C8 C9 1.385(5) . ? C8 C13 1.401(5) . ? C9 C10 1.386(5) . ? C10 C11 1.381(5) . ? C11 C12 1.374(5) . ? C12 C13 1.392(5) . ? C15 C16 1.392(4) . ? C15 C20 1.398(5) . ? C16 C17 1.370(5) . ? C17 C18 1.386(5) . ? C18 C19 1.384(5) . ? C19 C20 1.375(5) . ? C22 C22 1.507(7) 3_766 ? C23 C24 1.511(5) . ? C25 C26 1.505(6) . ? C27 C28 1.511(5) . ? C29 C30 1.504(6) . ? C31 C32 1.504(7) . ? C33 C34 1.502(5) . ? C35 C36 1.514(7) . ? C37 C38 1.512(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 N1 O2 123.0(3) . . ? O1 N1 C1 118.7(3) . . ? O2 N1 C1 118.2(3) . . ? C7 N2 C4 126.6(3) . . ? C7 N3 C8 125.6(3) . . ? C14 N4 C13 125.7(3) . . ? C14 N5 C15 124.3(3) . . ? C21 N6 C20 123.7(3) . . ? C21 N7 C22 120.8(3) . . ? C29 N8 C25 106.5(3) . . ? C29 N8 C23 110.9(3) . . ? C25 N8 C23 111.3(3) . . ? C29 N8 C27 111.0(3) . . ? C25 N8 C27 111.4(3) . . ? C23 N8 C27 105.8(3) . . ? C33 N9 C37 110.9(4) . . ? C33 N9 C35 106.9(3) . . ? C37 N9 C35 110.6(3) . . ? C33 N9 C31 110.6(3) . . ? C37 N9 C31 106.6(3) . . ? C35 N9 C31 111.4(4) . . ? C2 C1 C6 122.1(3) . . ? C2 C1 N1 119.5(3) . . ? C6 C1 N1 118.4(3) . . ? C1 C2 C3 119.0(3) . . ? C4 C3 C2 120.1(3) . . ? C3 C4 N2 124.2(3) . . ? C3 C4 C5 119.2(3) . . ? N2 C4 C5 116.6(3) . . ? C6 C5 C4 120.4(3) . . ? C1 C6 C5 119.0(3) . . ? O3 C7 N3 124.5(3) . . ? O3 C7 N2 123.5(3) . . ? N3 C7 N2 111.9(3) . . ? C9 C8 C13 119.8(3) . . ? C9 C8 N3 122.4(3) . . ? C13 C8 N3 117.8(3) . . ? C8 C9 C10 120.0(3) . . ? C11 C10 C9 120.1(3) . . ? C12 C11 C10 120.5(3) . . ? C11 C12 C13 120.2(3) . . ? C12 C13 C8 119.4(3) . . ? C12 C13 N4 122.5(3) . . ? C8 C13 N4 118.0(3) . . ? O4 C14 N4 124.4(3) . . ? O4 C14 N5 123.8(3) . . ? N4 C14 N5 111.8(3) . . ? C16 C15 C20 119.3(3) . . ? C16 C15 N5 121.7(3) . . ? C20 C15 N5 118.9(3) . . ? C17 C16 C15 120.0(3) . . ? C16 C17 C18 120.6(3) . . ? C19 C18 C17 119.7(3) . . ? C20 C19 C18 120.3(3) . . ? C19 C20 C15 120.1(3) . . ? C19 C20 N6 121.5(3) . . ? C15 C20 N6 118.5(3) . . ? O5 C21 N7 123.2(3) . . ? O5 C21 N6 122.9(3) . . ? N7 C21 N6 114.0(3) . . ? N7 C22 C22 111.7(3) . 3_766 ? C24 C23 N8 115.1(3) . . ? C26 C25 N8 115.3(3) . . ? C28 C27 N8 115.6(3) . . ? C30 C29 N8 115.5(3) . . ? C32 C31 N9 115.6(4) . . ? C34 C33 N9 115.0(3) . . ? C36 C35 N9 114.5(4) . . ? C38 C37 N9 114.7(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 O1 N1 C1 C2 -174.4(4) . . . . ? O2 N1 C1 C2 5.3(5) . . . . ? O1 N1 C1 C6 4.7(5) . . . . ? O2 N1 C1 C6 -175.6(4) . . . . ? C6 C1 C2 C3 -1.3(6) . . . . ? N1 C1 C2 C3 177.8(3) . . . . ? C1 C2 C3 C4 -0.4(6) . . . . ? C2 C3 C4 N2 -178.0(3) . . . . ? C2 C3 C4 C5 2.2(6) . . . . ? C7 N2 C4 C3 20.7(6) . . . . ? C7 N2 C4 C5 -159.5(4) . . . . ? C3 C4 C5 C6 -2.5(6) . . . . ? N2 C4 C5 C6 177.7(3) . . . . ? C2 C1 C6 C5 1.0(6) . . . . ? N1 C1 C6 C5 -178.1(3) . . . . ? C4 C5 C6 C1 0.9(6) . . . . ? C8 N3 C7 O3 10.4(6) . . . . ? C8 N3 C7 N2 -168.8(3) . . . . ? C4 N2 C7 O3 -14.1(6) . . . . ? C4 N2 C7 N3 165.1(3) . . . . ? C7 N3 C8 C9 -37.9(5) . . . . ? C7 N3 C8 C13 142.6(3) . . . . ? C13 C8 C9 C10 0.1(5) . . . . ? N3 C8 C9 C10 -179.3(3) . . . . ? C8 C9 C10 C11 0.4(6) . . . . ? C9 C10 C11 C12 -0.6(6) . . . . ? C10 C11 C12 C13 0.2(6) . . . . ? C11 C12 C13 C8 0.3(6) . . . . ? C11 C12 C13 N4 -176.4(4) . . . . ? C9 C8 C13 C12 -0.5(5) . . . . ? N3 C8 C13 C12 179.0(3) . . . . ? C9 C8 C13 N4 176.3(3) . . . . ? N3 C8 C13 N4 -4.2(5) . . . . ? C14 N4 C13 C12 -41.2(5) . . . . ? C14 N4 C13 C8 142.1(3) . . . . ? C13 N4 C14 O4 1.9(6) . . . . ? C13 N4 C14 N5 -177.3(3) . . . . ? C15 N5 C14 O4 -13.1(5) . . . . ? C15 N5 C14 N4 166.1(3) . . . . ? C14 N5 C15 C16 54.6(5) . . . . ? C14 N5 C15 C20 -126.5(3) . . . . ? C20 C15 C16 C17 0.2(5) . . . . ? N5 C15 C16 C17 179.0(3) . . . . ? C15 C16 C17 C18 -0.2(6) . . . . ? C16 C17 C18 C19 0.0(6) . . . . ? C17 C18 C19 C20 0.3(5) . . . . ? C18 C19 C20 C15 -0.4(5) . . . . ? C18 C19 C20 N6 178.7(3) . . . . ? C16 C15 C20 C19 0.1(5) . . . . ? N5 C15 C20 C19 -178.7(3) . . . . ? C16 C15 C20 N6 -179.0(3) . . . . ? N5 C15 C20 N6 2.2(4) . . . . ? C21 N6 C20 C19 57.1(5) . . . . ? C21 N6 C20 C15 -123.9(4) . . . . ? C22 N7 C21 O5 9.8(5) . . . . ? C22 N7 C21 N6 -171.2(3) . . . . ? C20 N6 C21 O5 -1.8(5) . . . . ? C20 N6 C21 N7 179.2(3) . . . . ? C21 N7 C22 C22 77.7(5) . . . 3_766 ? C29 N8 C23 C24 54.6(4) . . . . ? C25 N8 C23 C24 -63.8(5) . . . . ? C27 N8 C23 C24 175.0(4) . . . . ? C29 N8 C25 C26 175.5(4) . . . . ? C23 N8 C25 C26 -63.5(5) . . . . ? C27 N8 C25 C26 54.3(5) . . . . ? C29 N8 C27 C28 -62.3(4) . . . . ? C25 N8 C27 C28 56.2(5) . . . . ? C23 N8 C27 C28 177.4(4) . . . . ? C25 N8 C29 C30 178.3(3) . . . . ? C23 N8 C29 C30 57.0(4) . . . . ? C27 N8 C29 C30 -60.3(4) . . . . ? C33 N9 C31 C32 64.3(5) . . . . ? C37 N9 C31 C32 -175.1(4) . . . . ? C35 N9 C31 C32 -54.4(5) . . . . ? C37 N9 C33 C34 -53.0(5) . . . . ? C35 N9 C33 C34 -173.6(4) . . . . ? C31 N9 C33 C34 65.0(5) . . . . ? C33 N9 C35 C36 179.8(5) . . . . ? C37 N9 C35 C36 59.0(6) . . . . ? C31 N9 C35 C36 -59.3(6) . . . . ? C33 N9 C37 C38 -55.4(5) . . . . ? C35 N9 C37 C38 62.9(5) . . . . ? C31 N9 C37 C38 -175.9(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5 Br2 0.88 2.62 3.447(3) 156.1 . N4 H4 Br2 0.88 2.51 3.369(3) 165.7 . N7 H7 Br1 0.88 2.55 3.372(3) 156.2 . N6 H6 Br1 0.88 2.56 3.398(3) 158.8 . N3 H3 Br1 0.88 2.62 3.449(3) 157.4 . N2 H2 Br1 0.88 2.65 3.485(3) 158.3 . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.760 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.081 ############ data_(TPA)3LBr3 _database_code_depnum_ccdc_archive 'CCDC 849104' #TrackingRef 'complexes 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H124 Br3 N17 O10' _chemical_formula_weight 1723.69 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 32.939(3) _cell_length_b 19.383(2) _cell_length_c 28.226(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.879(2) _cell_angle_gamma 90.00 _cell_volume 17851(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 23.14 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7264 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6756 _exptl_absorpt_correction_T_max 0.6921 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 58826 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15689 _reflns_number_gt 10078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1379P)^2^+138.1218P] 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 15689 _refine_ls_number_parameters 1073 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1238 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.2626 _refine_ls_wR_factor_gt 0.2230 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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 Br1 Br 0.13450(2) 0.27815(3) 0.47159(2) 0.0404(2) Uani 1 1 d . . . Br2 Br 0.21172(2) 0.71706(4) 0.35104(3) 0.0428(2) Uani 1 1 d . . . Br3 Br 0.18803(2) 0.99855(3) 0.42785(3) 0.0477(2) Uani 1 1 d . . . C1 C -0.0037(2) 0.5109(4) 0.4361(3) 0.0444(17) Uani 1 1 d . . . C2 C 0.0363(2) 0.4960(4) 0.4538(3) 0.0454(17) Uani 1 1 d . . . H2 H 0.0549 0.5316 0.4652 0.055 Uiso 1 1 calc R . . C3 C 0.0487(2) 0.4288(4) 0.4545(3) 0.0466(17) Uani 1 1 d . . . H3 H 0.0763 0.4178 0.4667 0.056 Uiso 1 1 calc R . . C4 C 0.0217(2) 0.3755(4) 0.4376(3) 0.0456(17) Uani 1 1 d . . . C5 C -0.0190(2) 0.3923(4) 0.4204(3) 0.0503(19) Uani 1 1 d . . . H5 H -0.0379 0.3570 0.4091 0.060 Uiso 1 1 calc R . . C6 C -0.0316(2) 0.4599(4) 0.4197(3) 0.0511(19) Uani 1 1 d . . . H6 H -0.0592 0.4715 0.4082 0.061 Uiso 1 1 calc R . . C7 C 0.0197(2) 0.2509(4) 0.4161(3) 0.0462(17) Uani 1 1 d . . . C8 C 0.0370(2) 0.1294(4) 0.4027(3) 0.0470(18) Uani 1 1 d . . . C9 C -0.0032(3) 0.1024(4) 0.3981(3) 0.059(2) Uani 1 1 d . . . H9 H -0.0256 0.1311 0.4031 0.071 Uiso 1 1 calc R . . C10 C -0.0093(3) 0.0336(5) 0.3862(4) 0.078(3) Uani 1 1 d . . . H10 H -0.0363 0.0153 0.3834 0.093 Uiso 1 1 calc R . . C11 C 0.0224(4) -0.0090(5) 0.3783(4) 0.078(3) Uani 1 1 d . . . H11 H 0.0174 -0.0561 0.3703 0.094 Uiso 1 1 calc R . . C12 C 0.0616(3) 0.0176(4) 0.3821(3) 0.063(2) Uani 1 1 d . . . H12 H 0.0837 -0.0116 0.3768 0.075 Uiso 1 1 calc R . . C13 C 0.0689(2) 0.0874(4) 0.3936(3) 0.0467(18) Uani 1 1 d . . . C14 C 0.1245(2) 0.1574(3) 0.3684(2) 0.0411(16) Uani 1 1 d . . . C15 C 0.1864(2) 0.1879(4) 0.3350(2) 0.0439(17) Uani 1 1 d . . . C16 C 0.2012(3) 0.1414(4) 0.3041(3) 0.059(2) Uani 1 1 d . . . H16 H 0.1971 0.0933 0.3081 0.071 Uiso 1 1 calc R . . C17 C 0.2219(3) 0.1641(5) 0.2677(3) 0.068(3) Uani 1 1 d . . . H17 H 0.2323 0.1320 0.2470 0.081 Uiso 1 1 calc R . . C18 C 0.2271(3) 0.2336(5) 0.2619(3) 0.064(2) Uani 1 1 d . . . H18 H 0.2408 0.2497 0.2365 0.076 Uiso 1 1 calc R . . C19 C 0.2127(3) 0.2803(4) 0.2923(3) 0.055(2) Uani 1 1 d . . . H19 H 0.2166 0.3283 0.2877 0.066 Uiso 1 1 calc R . . C20 C 0.1923(2) 0.2580(3) 0.3299(2) 0.0431(17) Uani 1 1 d . . . C21 C 0.1837(2) 0.3735(3) 0.3670(2) 0.0395(16) Uani 1 1 d . . . C24 C 0.1387(3) 0.6260(4) 0.4358(3) 0.056(2) Uani 1 1 d . . . C25 C 0.1108(2) 0.7408(4) 0.4514(3) 0.0442(17) Uani 1 1 d . . . C26 C 0.0837(3) 0.7198(4) 0.4819(3) 0.060(2) Uani 1 1 d . A . H26 H 0.0815 0.6721 0.4889 0.073 Uiso 1 1 calc R . . C27 C 0.0600(4) 0.7667(5) 0.5021(4) 0.097(4) Uani 1 1 d . . . H27 H 0.0415 0.7512 0.5227 0.116 Uiso 1 1 calc R A . C28 C 0.0628(4) 0.8365(6) 0.4926(4) 0.113(5) Uani 1 1 d . A . H28 H 0.0466 0.8689 0.5070 0.135 Uiso 1 1 calc R . . C29 C 0.0892(4) 0.8581(4) 0.4624(4) 0.087(4) Uani 1 1 d . . . H29 H 0.0911 0.9059 0.4557 0.104 Uiso 1 1 calc R A . C30 C 0.1132(3) 0.8117(4) 0.4412(3) 0.052(2) Uani 1 1 d . A . C31 C 0.1271(2) 0.8424(3) 0.3619(2) 0.0384(16) Uani 1 1 d . A . C32 C 0.1356(2) 0.9133(4) 0.2923(3) 0.0432(17) Uani 1 1 d . A . C33 C 0.1267(3) 0.9833(4) 0.2858(3) 0.055(2) Uani 1 1 d . . . H33 H 0.1299 1.0134 0.3125 0.066 Uiso 1 1 calc R . . C34 C 0.1135(3) 1.0090(4) 0.2413(3) 0.066(2) Uani 1 1 d . . . H34 H 0.1075 1.0567 0.2371 0.079 Uiso 1 1 calc R . . C35 C 0.1088(3) 0.9657(5) 0.2027(3) 0.065(2) Uani 1 1 d . . . H35 H 0.0988 0.9835 0.1720 0.078 Uiso 1 1 calc R . . C36 C 0.1186(3) 0.8962(4) 0.2078(3) 0.055(2) Uani 1 1 d . . . H36 H 0.1155 0.8665 0.1808 0.066 Uiso 1 1 calc R . . C37 C 0.1328(2) 0.8708(4) 0.2527(3) 0.0448(17) Uani 1 1 d . . . C38 C 0.1338(4) 0.7469(5) 0.2334(3) 0.082(3) Uani 1 1 d . . . C39 C 0.1411(4) 0.6190(4) 0.2373(3) 0.076(3) Uani 1 1 d . . . C40 C 0.1619(3) 0.5663(4) 0.2644(3) 0.057(2) Uani 1 1 d . . . H40 H 0.1827 0.5779 0.2898 0.068 Uiso 1 1 calc R . . C41 C 0.1527(3) 0.4983(4) 0.2551(3) 0.058(2) Uani 1 1 d . . . H41 H 0.1665 0.4629 0.2743 0.069 Uiso 1 1 calc R . . C42 C 0.1236(3) 0.4825(4) 0.2178(3) 0.070(3) Uani 1 1 d . . . C43 C 0.1029(4) 0.5328(5) 0.1897(4) 0.111(5) Uani 1 1 d . . . H43 H 0.0828 0.5201 0.1636 0.133 Uiso 1 1 calc R . . C44 C 0.1112(4) 0.6017(5) 0.1994(4) 0.115(5) Uani 1 1 d . . . H44 H 0.0967 0.6368 0.1805 0.138 Uiso 1 1 calc R . . C45 C 0.1930(3) 0.0565(5) 0.6141(3) 0.070(3) Uani 1 1 d . . . C46 C 0.1994(3) -0.0178(5) 0.6040(4) 0.071(3) Uani 1 1 d . . . C47 C 0.2132(3) -0.0539(5) 0.6526(4) 0.077(3) Uani 1 1 d . . . C48 C 0.1715(3) 0.1754(5) 0.5864(3) 0.079(3) Uani 1 1 d . . . C49 C 0.2060(5) 0.2114(6) 0.6177(4) 0.102(4) Uani 1 1 d . . . C50 C 0.1911(5) 0.2876(5) 0.6280(4) 0.111(5) Uani 1 1 d . . . C51 C 0.2187(3) 0.1052(4) 0.5432(3) 0.062(2) Uani 1 1 d . . . C52 C 0.2171(3) 0.1571(4) 0.5032(3) 0.062(2) Uani 1 1 d . . . C53 C 0.2549(3) 0.1500(4) 0.4773(3) 0.060(2) Uani 1 1 d . . . C54 C 0.1455(3) 0.0750(6) 0.5356(3) 0.077(3) Uani 1 1 d . . . C55 C 0.1085(3) 0.0567(9) 0.5587(4) 0.120(5) Uani 1 1 d . . . C56 C 0.0725(3) 0.0438(6) 0.5197(3) 0.079(3) Uani 1 1 d . . . C57 C 0.1853(7) 0.3127(14) 0.1068(8) 0.181(9) Uani 1 1 d . . . C58 C 0.1576(7) 0.2937(12) 0.0776(17) 0.36(3) Uani 1 1 d D . . C59 C 0.1587(11) 0.2143(14) 0.0908(14) 0.38(3) Uani 1 1 d D . . C60 C 0.2279(5) 0.3702(8) 0.0634(7) 0.160(8) Uani 1 1 d . . . C61 C 0.2328(13) 0.3434(10) 0.0291(11) 0.34(3) Uani 1 1 d . . . C62 C 0.2648(6) 0.3433(7) -0.0045(5) 0.145(7) Uani 1 1 d . . . C63 C 0.1647(3) 0.4333(6) 0.0869(4) 0.086(3) Uani 1 1 d . . . C64 C 0.1805(4) 0.5024(6) 0.0744(5) 0.101(4) Uani 1 1 d . . . C65 C 0.1423(3) 0.5458(5) 0.0571(4) 0.090(3) Uani 1 1 d . . . C66 C 0.2242(8) 0.3909(11) 0.1437(7) 0.239(15) Uani 1 1 d . . . C67 C 0.2263(6) 0.4308(10) 0.1741(7) 0.181(10) Uani 1 1 d . . . C68 C 0.2562(3) 0.4357(6) 0.2212(3) 0.078(3) Uani 1 1 d . . . N1 N -0.0168(2) 0.5825(3) 0.4330(2) 0.0516(16) Uani 1 1 d . . . N2 N 0.03765(19) 0.3096(3) 0.4380(2) 0.0506(16) Uani 1 1 d . . . H2A H 0.0622 0.3042 0.4542 0.061 Uiso 1 1 calc R . . N3 N 0.04582(18) 0.1963(3) 0.4191(2) 0.0444(14) Uani 1 1 d . . . H3A H 0.0710 0.2040 0.4329 0.053 Uiso 1 1 calc R . . N4 N 0.10994(19) 0.1105(3) 0.3992(2) 0.0431(14) Uani 1 1 d . . . H4 H 0.1271 0.0944 0.4233 0.052 Uiso 1 1 calc R . . N5 N 0.16613(18) 0.1606(3) 0.37318(19) 0.0383(13) Uani 1 1 d . . . H5A H 0.1808 0.1458 0.3997 0.046 Uiso 1 1 calc R . . N6 N 0.17877(19) 0.3030(3) 0.3635(2) 0.0439(14) Uani 1 1 d . A . H6A H 0.1654 0.2838 0.3850 0.053 Uiso 1 1 calc R . . N7 N 0.1660(2) 0.4021(3) 0.4026(2) 0.0536(17) Uani 0.58(3) 1 d P A 1 N8 N 0.1639(3) 0.5951(3) 0.4074(3) 0.103(4) Uani 0.58(3) 1 d P A 1 H8 H 0.1686 0.6156 0.3809 0.123 Uiso 0.58(3) 1 calc PR A 1 C22 C 0.1505(5) 0.4765(9) 0.3970(6) 0.042(4) Uani 0.58(3) 1 d P A 1 C23 C 0.1842(4) 0.5247(8) 0.4214(5) 0.051(5) Uani 0.58(3) 1 d P A 1 N7A N 0.1660(2) 0.4021(3) 0.4026(2) 0.0536(17) Uani 0.42(3) 1 d P A 2 H7A H 0.1482 0.3787 0.4167 0.064 Uiso 0.42(3) 1 calc PR A 2 N8A N 0.1639(3) 0.5951(3) 0.4074(3) 0.103(4) Uani 0.42(3) 1 d P A 2 C22A C 0.1773(8) 0.4748(12) 0.4177(7) 0.047(7) Uani 0.42(3) 1 d P A 2 C23A C 0.1452(6) 0.5197(12) 0.3894(6) 0.044(6) Uani 0.42(3) 1 d P A 2 N9 N 0.13558(18) 0.6962(3) 0.4288(2) 0.0398(13) Uani 1 1 d . A . H9A H 0.1504 0.7145 0.4084 0.048 Uiso 1 1 calc R . . N10 N 0.1411(2) 0.8370(3) 0.4100(2) 0.0452(14) Uani 1 1 d . . . H10A H 0.1664 0.8487 0.4214 0.054 Uiso 1 1 calc R A . N11 N 0.14958(19) 0.8893(3) 0.33913(19) 0.0414(14) Uani 1 1 d . . . H11A H 0.1731 0.9045 0.3541 0.050 Uiso 1 1 calc R A . N12 N 0.1466(2) 0.8021(3) 0.2599(2) 0.0489(15) Uani 1 1 d . . . H12A H 0.1656 0.7947 0.2844 0.059 Uiso 1 1 calc R . . N13 N 0.1513(3) 0.6858(4) 0.2513(2) 0.082(3) Uani 1 1 d . . . H13 H 0.1718 0.6900 0.2747 0.098 Uiso 1 1 calc R . . N14 N 0.1134(3) 0.4103(4) 0.2064(3) 0.085(3) Uani 1 1 d . . . N15 N 0.1999(3) 0.3787(5) 0.0979(4) 0.091(3) Uani 1 1 d . . . N16 N 0.18219(19) 0.1046(3) 0.5705(2) 0.0475(15) Uani 1 1 d . . . N17 N 0.9643(4) 0.6855(8) 0.2499(6) 0.071(4) Uani 0.50 1 d P B -1 N18 N 0.0136(3) 0.2709(5) 0.2469(5) 0.047(3) Uani 0.50 1 d PD C -1 C69 C 0.9968(3) 0.7218(6) 0.2870(4) 0.049(3) Uani 0.67 1 d P B -1 C70 C 0.9847(5) 0.8020(19) 0.2387(8) 0.164(14) Uani 0.67 1 d P D -1 C71 C 0.9926(9) 0.889(2) 0.2631(9) 0.195(16) Uani 0.67 1 d P D -1 C72 C 0.9750(4) 0.7396(9) 0.3287(5) 0.075(4) Uani 0.67 1 d P B -1 C73 C 0.9998(4) 0.7759(6) 0.3765(5) 0.060(3) Uani 0.67 1 d P B -1 C74 C 0.9616(5) 0.8255(13) 0.4000(5) 0.161(12) Uani 0.67 1 d P B -1 C75 C 1.0276(4) 0.6648(7) 0.2973(4) 0.066(4) Uani 0.67 1 d P B -1 C76 C 1.0402(11) 0.6222(11) 0.3274(6) 0.213(18) Uani 0.67 1 d P B -1 C77 C 1.0639(7) 0.5702(14) 0.3340(8) 0.137(9) Uani 0.67 1 d P B -1 C78 C 0.0328(5) 0.3112(8) 0.2780(4) 0.080(5) Uani 0.67 1 d P C -1 C79 C 0.0220(5) 0.3615(8) 0.3078(5) 0.079(4) Uani 0.67 1 d P C -1 C80 C 0.0653(10) 0.394(2) 0.3296(8) 0.28(3) Uani 0.67 1 d P C -1 C81 C -0.0039(6) 0.2066(8) 0.2222(8) 0.123(8) Uani 0.67 1 d PD C -1 C82 C 0.0171(9) 0.1427(9) 0.2460(19) 0.38(4) Uani 0.67 1 d PD C -1 C83 C -0.0123(13) 0.0833(13) 0.252(3) 0.22(3) Uani 0.67 1 d PD C -1 C84 C 0.0403(8) 0.2459(11) 0.2095(6) 0.122(8) Uani 0.67 1 d P C -1 C85 C 0.0845(8) 0.2128(9) 0.2326(7) 0.116(8) Uani 0.67 1 d P C -1 C86 C 0.1062(11) 0.1913(14) 0.1906(10) 0.197(16) Uani 0.67 1 d P C -1 O1 O -0.0504(2) 0.5966(3) 0.4104(2) 0.0715(17) Uani 1 1 d . . . O2 O 0.00521(19) 0.6265(3) 0.4533(2) 0.0705(17) Uani 1 1 d . . . O3 O -0.01590(16) 0.2488(3) 0.3969(2) 0.0574(14) Uani 1 1 d . . . O4 O 0.10176(16) 0.1934(3) 0.34057(19) 0.0525(13) Uani 1 1 d . . . O5 O 0.20258(17) 0.4076(2) 0.34067(18) 0.0501(13) Uani 1 1 d . A . O6 O 0.1220(2) 0.5933(3) 0.4653(2) 0.0671(17) Uani 1 1 d . A . O7 O 0.09917(16) 0.8082(3) 0.34181(18) 0.0504(13) Uani 1 1 d . . . O8 O 0.1075(4) 0.7502(4) 0.1989(3) 0.184(7) Uani 1 1 d . . . O9 O 0.1318(2) 0.3663(3) 0.2317(3) 0.095(2) Uani 1 1 d . . . O10 O 0.0883(3) 0.3966(4) 0.1722(3) 0.133(4) 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 Br1 0.0390(4) 0.0401(4) 0.0400(4) 0.0050(3) -0.0018(3) 0.0007(3) Br2 0.0393(4) 0.0425(4) 0.0448(4) -0.0013(3) -0.0006(3) -0.0033(3) Br3 0.0644(5) 0.0279(3) 0.0477(4) -0.0049(3) -0.0035(3) 0.0007(3) C1 0.047(4) 0.046(4) 0.041(4) 0.005(3) 0.008(3) 0.000(3) C2 0.042(4) 0.052(4) 0.041(4) -0.003(3) 0.002(3) -0.004(3) C3 0.033(4) 0.055(5) 0.050(4) 0.000(4) -0.002(3) 0.002(3) C4 0.041(4) 0.048(4) 0.047(4) 0.008(3) 0.005(3) 0.000(3) C5 0.039(4) 0.048(4) 0.060(5) 0.009(4) -0.006(4) -0.005(3) C6 0.040(4) 0.052(5) 0.059(5) 0.010(4) 0.000(4) 0.002(3) C7 0.040(4) 0.051(4) 0.045(4) 0.009(3) 0.001(3) -0.006(3) C8 0.051(5) 0.045(4) 0.044(4) 0.004(3) 0.001(3) -0.008(4) C9 0.052(5) 0.059(5) 0.064(5) 0.005(4) -0.002(4) -0.017(4) C10 0.075(7) 0.073(6) 0.083(7) 0.004(5) 0.004(5) -0.033(6) C11 0.097(8) 0.047(5) 0.090(7) 0.001(5) 0.008(6) -0.036(5) C12 0.076(6) 0.043(4) 0.067(6) 0.002(4) 0.005(5) -0.011(4) C13 0.056(5) 0.038(4) 0.044(4) 0.004(3) 0.001(4) -0.015(3) C14 0.056(5) 0.029(3) 0.037(4) -0.001(3) 0.002(3) -0.001(3) C15 0.054(5) 0.039(4) 0.039(4) -0.004(3) 0.008(3) -0.008(3) C16 0.076(6) 0.045(4) 0.059(5) -0.019(4) 0.020(4) -0.003(4) C17 0.094(7) 0.056(5) 0.057(5) -0.023(4) 0.027(5) 0.002(5) C18 0.087(7) 0.068(6) 0.039(4) -0.001(4) 0.024(4) 0.001(5) C19 0.077(6) 0.044(4) 0.046(4) 0.002(3) 0.014(4) 0.001(4) C20 0.056(5) 0.035(4) 0.039(4) 0.000(3) 0.011(3) 0.003(3) C21 0.047(4) 0.029(3) 0.041(4) 0.005(3) 0.002(3) 0.000(3) C24 0.085(6) 0.027(4) 0.060(5) 0.000(3) 0.025(5) -0.001(4) C25 0.055(5) 0.036(4) 0.043(4) -0.001(3) 0.013(4) 0.001(3) C26 0.075(6) 0.042(4) 0.068(5) 0.013(4) 0.025(5) 0.009(4) C27 0.135(10) 0.068(6) 0.105(9) 0.020(6) 0.075(8) 0.018(6) C28 0.176(13) 0.068(7) 0.116(9) 0.021(6) 0.099(10) 0.044(7) C29 0.139(10) 0.039(5) 0.093(7) 0.013(5) 0.058(7) 0.032(5) C30 0.076(6) 0.039(4) 0.045(4) 0.002(3) 0.019(4) 0.012(4) C31 0.049(4) 0.028(3) 0.039(4) -0.004(3) 0.011(3) 0.002(3) C32 0.046(4) 0.041(4) 0.043(4) 0.002(3) 0.006(3) 0.002(3) C33 0.068(6) 0.044(4) 0.053(5) 0.007(4) 0.007(4) 0.009(4) C34 0.084(7) 0.052(5) 0.064(6) 0.015(4) 0.015(5) 0.015(4) C35 0.075(6) 0.070(6) 0.049(5) 0.021(4) 0.004(4) 0.018(5) C36 0.061(5) 0.063(5) 0.043(4) 0.002(4) 0.009(4) 0.014(4) C37 0.044(4) 0.051(4) 0.041(4) 0.003(3) 0.009(3) 0.004(3) C38 0.131(9) 0.058(5) 0.046(5) -0.021(4) -0.029(6) 0.042(6) C39 0.126(9) 0.054(5) 0.040(5) -0.016(4) -0.019(5) 0.032(5) C40 0.075(6) 0.060(5) 0.033(4) -0.006(4) -0.005(4) 0.018(4) C41 0.076(6) 0.054(5) 0.042(4) -0.002(4) 0.003(4) 0.019(4) C42 0.099(7) 0.057(5) 0.047(5) -0.013(4) -0.018(5) 0.028(5) C43 0.166(12) 0.069(6) 0.076(7) -0.031(6) -0.064(7) 0.051(7) C44 0.185(13) 0.056(6) 0.078(7) -0.034(5) -0.079(8) 0.058(7) C45 0.075(6) 0.070(6) 0.059(5) 0.014(4) -0.011(5) 0.019(5) C46 0.071(6) 0.063(6) 0.077(6) 0.007(5) 0.000(5) 0.013(5) C47 0.087(7) 0.075(6) 0.070(6) 0.025(5) 0.011(5) 0.023(5) C48 0.102(8) 0.076(6) 0.061(6) -0.003(5) 0.014(6) 0.043(6) C49 0.161(12) 0.077(7) 0.059(6) -0.014(5) -0.013(7) 0.038(7) C50 0.190(14) 0.063(6) 0.079(7) -0.012(5) 0.014(8) 0.057(8) C51 0.071(6) 0.057(5) 0.060(5) -0.011(4) 0.018(4) -0.001(4) C52 0.074(6) 0.049(5) 0.061(5) -0.006(4) 0.006(4) 0.003(4) C53 0.048(5) 0.064(5) 0.069(5) -0.012(4) 0.016(4) -0.006(4) C54 0.053(5) 0.118(8) 0.057(5) 0.021(5) -0.001(4) 0.013(5) C55 0.061(7) 0.222(17) 0.075(7) 0.047(9) 0.000(6) 0.017(8) C56 0.052(5) 0.117(8) 0.067(6) 0.011(6) 0.004(5) -0.015(5) C57 0.138(18) 0.23(3) 0.18(2) 0.032(19) 0.048(15) 0.065(18) C58 0.126(18) 0.18(2) 0.69(8) 0.17(3) -0.17(3) -0.017(16) C59 0.44(5) 0.31(4) 0.44(5) 0.27(4) 0.21(4) 0.29(4) C60 0.113(11) 0.139(13) 0.24(2) -0.130(14) 0.082(13) -0.049(10) C61 0.68(7) 0.115(15) 0.31(3) -0.115(19) 0.33(4) -0.18(3) C62 0.28(2) 0.085(9) 0.076(8) -0.025(7) 0.046(11) -0.059(11) C63 0.077(7) 0.082(7) 0.095(8) 0.009(6) -0.004(6) 0.010(6) C64 0.084(8) 0.105(9) 0.108(9) 0.037(7) -0.011(7) -0.012(7) C65 0.082(7) 0.062(6) 0.116(9) 0.020(6) -0.018(6) 0.013(5) C66 0.33(3) 0.207(19) 0.134(14) -0.096(14) -0.144(17) 0.20(2) C67 0.185(17) 0.181(17) 0.144(14) -0.070(13) -0.094(13) 0.110(14) C68 0.064(6) 0.105(8) 0.065(6) 0.017(6) 0.004(5) 0.000(5) N1 0.052(4) 0.045(4) 0.057(4) 0.006(3) 0.003(3) 0.004(3) N2 0.037(3) 0.047(4) 0.063(4) 0.003(3) -0.008(3) 0.003(3) N3 0.038(3) 0.039(3) 0.054(4) 0.003(3) -0.001(3) -0.006(3) N4 0.052(4) 0.033(3) 0.042(3) 0.007(3) 0.000(3) -0.002(3) N5 0.045(4) 0.033(3) 0.036(3) -0.001(2) 0.003(3) -0.001(2) N6 0.065(4) 0.028(3) 0.042(3) 0.004(2) 0.018(3) 0.003(3) N7 0.083(5) 0.026(3) 0.056(4) -0.001(3) 0.025(4) -0.001(3) N8 0.183(10) 0.029(4) 0.120(7) 0.006(4) 0.104(7) 0.015(5) C22 0.045(9) 0.030(10) 0.052(9) 0.007(7) 0.002(7) 0.007(7) C23 0.051(9) 0.029(10) 0.070(10) -0.004(6) -0.001(7) -0.005(6) N7A 0.083(5) 0.026(3) 0.056(4) -0.001(3) 0.025(4) -0.001(3) N8A 0.183(10) 0.029(4) 0.120(7) 0.006(4) 0.104(7) 0.015(5) C22A 0.052(14) 0.046(17) 0.041(11) -0.005(9) 0.001(10) 0.003(10) C23A 0.060(13) 0.024(12) 0.042(10) 0.004(8) -0.009(8) 0.001(9) N9 0.047(4) 0.026(3) 0.046(3) 0.002(2) 0.007(3) 0.001(2) N10 0.061(4) 0.036(3) 0.039(3) -0.001(3) 0.006(3) -0.003(3) N11 0.052(4) 0.034(3) 0.035(3) 0.003(2) -0.002(3) -0.006(3) N12 0.057(4) 0.050(4) 0.038(3) 0.000(3) -0.001(3) 0.009(3) N13 0.129(7) 0.057(4) 0.047(4) -0.017(3) -0.030(4) 0.041(5) N14 0.107(7) 0.065(5) 0.075(6) -0.007(4) -0.021(5) 0.028(5) N15 0.087(7) 0.065(5) 0.109(8) 0.003(5) -0.026(6) 0.020(5) N16 0.049(4) 0.054(4) 0.038(3) 0.000(3) 0.002(3) 0.018(3) N17 0.049(9) 0.068(9) 0.093(12) 0.008(8) 0.003(8) 0.001(7) N18 0.047(9) 0.040(6) 0.052(7) 0.013(6) -0.001(8) 0.006(5) C69 0.036(6) 0.051(7) 0.060(7) -0.008(6) 0.005(5) 0.001(5) C70 0.045(9) 0.35(4) 0.087(15) 0.13(2) -0.021(9) -0.052(17) C71 0.10(2) 0.39(5) 0.09(2) 0.09(2) 0.033(14) 0.11(3) C72 0.050(8) 0.103(11) 0.071(9) -0.007(8) 0.006(7) 0.013(8) C73 0.056(8) 0.037(6) 0.083(9) -0.012(6) -0.002(7) 0.019(5) C74 0.105(12) 0.34(3) 0.054(8) -0.138(14) 0.068(9) -0.168(17) C75 0.088(10) 0.083(9) 0.032(6) 0.029(6) 0.025(6) 0.066(8) C76 0.48(5) 0.121(15) 0.050(9) 0.039(10) 0.077(17) 0.22(2) C77 0.099(15) 0.18(2) 0.128(18) 0.008(16) 0.005(13) 0.069(15) C78 0.087(10) 0.090(10) 0.045(7) -0.037(7) -0.057(7) 0.054(8) C79 0.086(11) 0.094(11) 0.059(8) -0.013(8) 0.015(8) -0.037(9) C80 0.25(3) 0.50(6) 0.092(15) -0.15(3) 0.060(18) -0.31(4) C81 0.070(12) 0.111(15) 0.18(2) -0.051(14) -0.023(14) 0.032(11) C82 0.20(4) 0.099(19) 0.74(10) -0.11(4) -0.29(6) 0.05(2) C83 0.22(7) 0.094(15) 0.32(4) 0.01(4) -0.09(6) 0.05(2) C84 0.18(2) 0.129(16) 0.061(10) 0.004(10) 0.024(12) 0.077(16) C85 0.18(2) 0.092(12) 0.082(12) 0.029(10) 0.052(13) 0.049(13) C86 0.31(4) 0.15(2) 0.15(2) 0.066(18) 0.13(3) 0.13(3) O1 0.067(4) 0.053(3) 0.087(4) 0.006(3) -0.013(3) 0.011(3) O2 0.065(4) 0.052(3) 0.090(5) -0.010(3) -0.005(3) -0.001(3) O3 0.041(3) 0.062(3) 0.068(4) 0.000(3) 0.000(3) -0.004(3) O4 0.055(3) 0.047(3) 0.054(3) 0.017(3) 0.001(3) -0.002(3) O5 0.069(4) 0.032(2) 0.052(3) 0.005(2) 0.018(3) -0.005(2) O6 0.106(5) 0.035(3) 0.069(4) 0.009(3) 0.043(4) 0.000(3) O7 0.052(3) 0.051(3) 0.049(3) -0.005(2) 0.010(3) -0.011(3) O8 0.325(15) 0.069(5) 0.109(7) -0.046(5) -0.148(9) 0.080(7) O9 0.109(6) 0.057(4) 0.109(6) 0.006(4) -0.026(5) 0.009(4) O10 0.204(10) 0.066(5) 0.100(6) -0.022(4) -0.083(7) 0.021(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 C2 1.372(10) . ? C1 C6 1.386(10) . ? C1 N1 1.454(9) . ? C2 C3 1.365(10) . ? C3 C4 1.404(10) . ? C4 N2 1.380(9) . ? C4 C5 1.399(10) . ? C5 C6 1.372(10) . ? C7 O3 1.222(9) . ? C7 N3 1.360(10) . ? C7 N2 1.390(10) . ? C8 C13 1.381(11) . ? C8 N3 1.395(9) . ? C8 C9 1.411(11) . ? C9 C10 1.384(13) . ? C10 C11 1.374(15) . ? C11 C12 1.380(13) . ? C12 C13 1.406(10) . ? C13 N4 1.411(9) . ? C14 O4 1.226(8) . ? C14 N5 1.360(9) . ? C14 N4 1.389(9) . ? C15 C20 1.382(10) . ? C15 C16 1.389(10) . ? C15 N5 1.443(9) . ? C16 C17 1.381(12) . ? C17 C18 1.372(12) . ? C18 C19 1.376(11) . ? C19 C20 1.401(10) . ? C20 N6 1.405(9) . ? C21 O5 1.224(8) . ? C21 N7 1.348(9) . ? C21 N6 1.378(8) . ? C24 O6 1.234(9) . ? C24 N8 1.367(10) . ? C24 N9 1.376(8) . ? C25 C26 1.381(11) . ? C25 N9 1.402(9) . ? C25 C30 1.409(10) . ? C26 C27 1.374(12) . ? C27 C28 1.383(14) . ? C28 C29 1.364(14) . ? C29 C30 1.386(11) . ? C30 N10 1.443(10) . ? C31 O7 1.210(8) . ? C31 N10 1.376(9) . ? C31 N11 1.385(9) . ? C32 C37 1.380(10) . ? C32 C33 1.394(10) . ? C32 N11 1.418(9) . ? C33 C34 1.366(12) . ? C34 C35 1.365(13) . ? C35 C36 1.388(12) . ? C36 C37 1.381(10) . ? C37 N12 1.414(9) . ? C38 O8 1.212(11) . ? C38 N12 1.339(11) . ? C38 N13 1.384(11) . ? C39 N13 1.383(11) . ? C39 C44 1.390(13) . ? C39 C40 1.397(11) . ? C40 C41 1.370(11) . ? C41 C42 1.359(12) . ? C42 C43 1.377(13) . ? C42 N14 1.465(12) . ? C43 C44 1.385(14) . ? C45 C46 1.490(13) . ? C45 N16 1.545(10) . ? C46 C47 1.552(13) . ? C48 N16 1.500(11) . ? C48 C49 1.509(17) . ? C49 C50 1.595(13) . ? C51 C52 1.506(12) . ? C51 N16 1.517(10) . ? C52 C53 1.533(12) . ? C54 C55 1.503(15) . ? C54 N16 1.560(12) . ? C55 C56 1.524(15) . ? C57 C58 1.20(3) . ? C57 N15 1.40(3) . ? C58 C59 1.582(18) . ? C60 C61 1.13(2) . ? C60 N15 1.439(17) . ? C61 C62 1.51(3) . ? C63 C64 1.497(15) . ? C63 N15 1.569(13) . ? C64 C65 1.537(15) . ? C66 C67 1.150(18) . ? C66 N15 1.442(17) . ? C67 C68 1.546(17) . ? N1 O2 1.211(8) . ? N1 O1 1.231(8) . ? N7 C22 1.531(19) . ? N8 C23 1.548(17) . ? C22 C23 1.54(2) . ? C22A C23A 1.51(3) . ? N14 O10 1.212(10) . ? N14 O9 1.220(10) . ? N17 C69 1.556(19) . ? N18 C78 1.277(17) . ? N18 C81 1.504(15) . ? N18 C84 1.54(2) . ? C69 C72 1.499(18) . ? C69 C75 1.502(15) . ? C70 C71 1.82(4) . ? C72 C73 1.64(2) . ? C73 C74 1.78(2) . ? C75 C76 1.216(17) . ? C76 C77 1.27(2) . ? C78 C79 1.367(19) . ? C79 C80 1.60(2) . ? C81 C82 1.529(17) . ? C82 C83 1.529(19) . ? C84 C85 1.64(3) . ? C85 C86 1.52(3) . ? 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 C6 122.0(7) . . ? C2 C1 N1 119.1(7) . . ? C6 C1 N1 118.8(7) . . ? C3 C2 C1 118.5(7) . . ? C2 C3 C4 121.5(7) . . ? N2 C4 C5 124.4(7) . . ? N2 C4 C3 117.0(7) . . ? C5 C4 C3 118.6(7) . . ? C6 C5 C4 120.0(7) . . ? C5 C6 C1 119.4(7) . . ? O3 C7 N3 124.2(7) . . ? O3 C7 N2 123.3(7) . . ? N3 C7 N2 112.4(6) . . ? C13 C8 N3 118.6(7) . . ? C13 C8 C9 119.6(7) . . ? N3 C8 C9 121.7(7) . . ? C10 C9 C8 118.9(9) . . ? C11 C10 C9 122.0(9) . . ? C10 C11 C12 119.2(9) . . ? C11 C12 C13 120.5(9) . . ? C8 C13 C12 119.9(7) . . ? C8 C13 N4 122.3(6) . . ? C12 C13 N4 117.6(7) . . ? O4 C14 N5 123.9(6) . . ? O4 C14 N4 122.7(7) . . ? N5 C14 N4 113.4(6) . . ? C20 C15 C16 120.4(7) . . ? C20 C15 N5 121.7(6) . . ? C16 C15 N5 117.9(6) . . ? C17 C16 C15 120.8(7) . . ? C18 C17 C16 119.0(7) . . ? C17 C18 C19 120.8(8) . . ? C18 C19 C20 120.8(7) . . ? C15 C20 C19 118.2(6) . . ? C15 C20 N6 118.5(6) . . ? C19 C20 N6 123.2(6) . . ? O5 C21 N7 122.6(6) . . ? O5 C21 N6 123.7(6) . . ? N7 C21 N6 113.7(6) . . ? O6 C24 N8 122.3(7) . . ? O6 C24 N9 125.0(7) . . ? N8 C24 N9 112.7(7) . . ? C26 C25 N9 124.5(6) . . ? C26 C25 C30 118.3(7) . . ? N9 C25 C30 117.2(6) . . ? C27 C26 C25 121.0(8) . . ? C26 C27 C28 120.7(9) . . ? C29 C28 C27 119.1(9) . . ? C28 C29 C30 121.4(8) . . ? C29 C30 C25 119.6(7) . . ? C29 C30 N10 119.4(7) . . ? C25 C30 N10 121.0(6) . . ? O7 C31 N10 123.4(6) . . ? O7 C31 N11 124.2(6) . . ? N10 C31 N11 112.3(6) . . ? C37 C32 C33 118.9(7) . . ? C37 C32 N11 122.4(6) . . ? C33 C32 N11 118.6(7) . . ? C34 C33 C32 120.7(8) . . ? C35 C34 C33 119.7(8) . . ? C34 C35 C36 121.0(8) . . ? C37 C36 C35 119.0(8) . . ? C32 C37 C36 120.5(7) . . ? C32 C37 N12 117.5(6) . . ? C36 C37 N12 121.9(7) . . ? O8 C38 N12 122.8(8) . . ? O8 C38 N13 123.7(9) . . ? N12 C38 N13 113.3(8) . . ? N13 C39 C44 124.4(8) . . ? N13 C39 C40 116.5(8) . . ? C44 C39 C40 119.2(8) . . ? C41 C40 C39 121.4(8) . . ? C42 C41 C40 118.5(8) . . ? C41 C42 C43 122.0(9) . . ? C41 C42 N14 120.1(8) . . ? C43 C42 N14 117.9(8) . . ? C42 C43 C44 119.9(9) . . ? C43 C44 C39 119.0(9) . . ? C46 C45 N16 117.1(8) . . ? C45 C46 C47 107.4(8) . . ? N16 C48 C49 114.2(8) . . ? C48 C49 C50 108.0(10) . . ? C52 C51 N16 115.9(7) . . ? C51 C52 C53 110.5(7) . . ? C55 C54 N16 114.6(8) . . ? C54 C55 C56 108.8(9) . . ? C58 C57 N15 114(2) . . ? C57 C58 C59 98(3) . . ? C61 C60 N15 144(2) . . ? C60 C61 C62 137(3) . . ? C64 C63 N15 112.3(10) . . ? C63 C64 C65 105.7(9) . . ? C67 C66 N15 138.5(14) . . ? C66 C67 C68 130.5(14) . . ? O2 N1 O1 121.8(7) . . ? O2 N1 C1 119.3(7) . . ? O1 N1 C1 118.9(7) . . ? C4 N2 C7 127.9(6) . . ? C7 N3 C8 126.9(6) . . ? C14 N4 C13 123.0(6) . . ? C14 N5 C15 120.3(6) . . ? C21 N6 C20 128.3(6) . . ? C21 N7 C22 118.8(7) . . ? C24 N8 C23 120.9(8) . . ? N7 C22 C23 108.4(14) . . ? C22 C23 N8 99.3(11) . . ? C24 N9 C25 125.5(6) . . ? C31 N10 C30 118.2(6) . . ? C31 N11 C32 121.5(6) . . ? C38 N12 C37 127.1(7) . . ? C39 N13 C38 128.6(8) . . ? O10 N14 O9 122.9(9) . . ? O10 N14 C42 119.7(8) . . ? O9 N14 C42 117.4(8) . . ? C57 N15 C60 106.5(12) . . ? C57 N15 C66 98.8(17) . . ? C60 N15 C66 107.4(15) . . ? C57 N15 C63 112.9(12) . . ? C60 N15 C63 117.8(12) . . ? C66 N15 C63 111.7(9) . . ? C48 N16 C51 112.4(7) . . ? C48 N16 C45 110.6(6) . . ? C51 N16 C45 107.3(6) . . ? C48 N16 C54 109.5(7) . . ? C51 N16 C54 106.2(6) . . ? C45 N16 C54 110.7(7) . . ? C78 N18 C81 161.4(13) . . ? C78 N18 C84 112.7(15) . . ? C81 N18 C84 68.9(14) . . ? C72 C69 C75 113.5(11) . . ? C72 C69 N17 105.9(11) . . ? C75 C69 N17 100.5(10) . . ? C69 C72 C73 120.5(11) . . ? C72 C73 C74 103.9(9) . . ? C76 C75 C69 142.5(14) . . ? C75 C76 C77 142(2) . . ? N18 C78 C79 135.5(14) . . ? C78 C79 C80 103.1(18) . . ? N18 C81 C82 110.3(14) . . ? C81 C82 C83 113.8(17) . . ? N18 C84 C85 114.3(14) . . ? C86 C85 C84 106.5(18) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N11 H11A Br3 0.88 2.76 3.390(6) 129.6 . N10 H10A Br3 0.88 2.99 3.497(6) 118.6 . N13 H13 Br2 0.88 2.42 3.273(7) 162.5 . N12 H12A Br2 0.88 2.71 3.526(6) 155.3 . N9 H9A Br2 0.88 2.76 3.575(6) 155.3 . N8 H8 Br2 0.88 2.63 3.361(7) 140.9 . N6 H6A Br1 0.88 2.78 3.591(6) 154.5 . N3 H3A Br1 0.88 2.65 3.473(6) 156.8 . N2 H2A Br1 0.88 2.42 3.258(6) 160.2 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.140 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.126 ############ data_(TBA)4LBr4 _database_code_depnum_ccdc_archive 'CCDC 849105' #TrackingRef 'complexes 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H186 Br4 N18 O11' _chemical_formula_weight 2232.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 12.2557(18) _cell_length_b 37.945(6) _cell_length_c 13.0316(19) _cell_angle_alpha 90.00 _cell_angle_beta 96.945(2) _cell_angle_gamma 90.00 _cell_volume 6015.8(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5980 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 50.93 _exptl_crystal_description Flack _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 1.399 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6710 _exptl_absorpt_correction_T_max 0.8391 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39385 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10560 _reflns_number_gt 6046 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0200P] 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 10560 _refine_ls_number_parameters 659 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1721 _refine_ls_R_factor_gt 0.1089 _refine_ls_wR_factor_ref 0.2947 _refine_ls_wR_factor_gt 0.2730 _refine_ls_goodness_of_fit_ref 1.688 _refine_ls_restrained_S_all 1.692 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br2 Br 0.19825(8) 0.21852(2) 0.69107(7) 0.0748(4) Uani 1 1 d . . . Br1 Br 0.00861(7) 0.09100(2) 0.19268(7) 0.0669(3) Uani 1 1 d . . . N1 N 0.4587(16) -0.0382(5) 0.356(3) 0.26(3) Uani 0.58(3) 1 d PD A 1 O1 O 0.5503(16) -0.0383(8) 0.393(4) 0.33(3) Uani 0.50 1 d PD A 1 O2 O 0.3983(9) -0.0629(3) 0.3401(17) 0.305(12) Uani 0.58(3) 1 d PD A 1 N1A N 0.449(3) -0.0473(5) 0.272(2) 0.095(11) Uani 0.42(3) 1 d PD A 2 O1A O 0.529(4) -0.0540(9) 0.261(4) 0.25(3) Uani 0.42(3) 1 d P A 2 O2A O 0.3983(9) -0.0629(3) 0.3401(17) 0.305(12) Uani 0.42(3) 1 d P A 2 N2 N 0.2785(6) 0.08736(17) 0.1753(6) 0.080(2) Uani 1 1 d . . . H2 H 0.2062 0.0881 0.1662 0.096 Uiso 1 1 calc R . . N3 N 0.2632(5) 0.14485(15) 0.1237(5) 0.0599(17) Uani 1 1 d . . . H3 H 0.1919 0.1409 0.1144 0.072 Uiso 1 1 calc R . . N4 N 0.2112(6) 0.18220(15) -0.0741(5) 0.0597(17) Uani 1 1 d . . . H4 H 0.2383 0.1840 -0.1334 0.072 Uiso 1 1 calc R . . N5 N 0.0641(5) 0.16308(14) -0.1782(5) 0.0556(16) Uani 1 1 d . . . H5 H 0.1056 0.1686 -0.2264 0.067 Uiso 1 1 calc R . . N6 N -0.0304(5) 0.09813(14) -0.1090(5) 0.0534(16) Uani 1 1 d . . . H6 H 0.0011 0.1086 -0.0528 0.064 Uiso 1 1 calc R . . N7 N 0.0270(5) 0.04749(14) -0.0283(5) 0.0585(17) Uani 1 1 d . . . H7 H 0.0469 0.0608 0.0261 0.070 Uiso 1 1 calc R . . N9 N 0.1360(9) 0.0999(4) 0.5402(9) 0.160(6) Uani 1 1 d D . . O3 O 0.4333(6) 0.12072(16) 0.1640(6) 0.096(2) Uani 1 1 d . . . O4 O 0.0694(4) 0.15569(11) -0.0029(4) 0.0532(13) Uani 1 1 d . . . O5 O -0.0508(4) 0.04578(13) -0.1954(4) 0.0631(14) Uani 1 1 d . . . O6 O 0.0044(9) 0.9916(2) 0.6840(7) 0.059(3) Uani 0.50 1 d P . . C1 C 0.4059(11) -0.0077(3) 0.2783(16) 0.198(10) Uani 1 1 d D . . C2 C 0.2995(9) -0.0026(3) 0.2694(10) 0.113(4) Uani 1 1 d . A . H2A H 0.2517 -0.0206 0.2883 0.136 Uiso 1 1 calc R . . C3 C 0.2578(7) 0.0295(2) 0.2317(8) 0.080(3) Uani 1 1 d . . . H3A H 0.1806 0.0333 0.2229 0.095 Uiso 1 1 calc R A . C4 C 0.3258(8) 0.0555(2) 0.2073(9) 0.095(3) Uani 1 1 d . A . C5 C 0.4338(11) 0.0488(4) 0.2181(18) 0.223(11) Uani 1 1 d . . . H5A H 0.4827 0.0671 0.2036 0.268 Uiso 1 1 calc R A . C6 C 0.4777(12) 0.0160(4) 0.250(2) 0.306(17) Uani 1 1 d . A . H6A H 0.5537 0.0108 0.2507 0.367 Uiso 1 1 calc R . . C7 C 0.3334(8) 0.1184(2) 0.1558(7) 0.072(2) Uani 1 1 d . . . C8 C 0.3049(7) 0.17909(18) 0.1048(7) 0.058(2) Uani 1 1 d . . . C9 C 0.3786(8) 0.1947(2) 0.1823(7) 0.076(3) Uani 1 1 d . . . H9 H 0.3947 0.1837 0.2478 0.092 Uiso 1 1 calc R . . C10 C 0.4282(8) 0.2268(2) 0.1619(9) 0.088(3) Uani 1 1 d . . . H10 H 0.4793 0.2373 0.2136 0.106 Uiso 1 1 calc R . . C11 C 0.4044(9) 0.2430(2) 0.0704(8) 0.079(3) Uani 1 1 d . . . H11 H 0.4399 0.2645 0.0569 0.095 Uiso 1 1 calc R . . C12 C 0.3298(8) 0.2287(2) -0.0025(8) 0.081(3) Uani 1 1 d . . . H12 H 0.3121 0.2406 -0.0664 0.098 Uiso 1 1 calc R . . C13 C 0.2773(7) 0.19617(18) 0.0138(6) 0.057(2) Uani 1 1 d . . . C14 C 0.1132(6) 0.16670(17) -0.0776(7) 0.0493(19) Uani 1 1 d . . . C15 C -0.0439(7) 0.15173(19) -0.2145(6) 0.059(2) Uani 1 1 d . . . C16 C -0.1026(9) 0.1729(2) -0.2861(7) 0.080(3) Uani 1 1 d . . . H16 H -0.0744 0.1954 -0.3010 0.096 Uiso 1 1 calc R . . C17 C -0.2029(9) 0.1620(2) -0.3373(8) 0.094(3) Uani 1 1 d . . . H17 H -0.2410 0.1762 -0.3899 0.113 Uiso 1 1 calc R . . C18 C -0.2463(8) 0.1305(2) -0.3113(8) 0.091(3) Uani 1 1 d . . . H18 H -0.3154 0.1230 -0.3452 0.109 Uiso 1 1 calc R . . C19 C -0.1907(7) 0.1096(2) -0.2365(7) 0.076(3) Uani 1 1 d . . . H19 H -0.2229 0.0881 -0.2178 0.091 Uiso 1 1 calc R . . C20 C -0.0862(7) 0.11949(18) -0.1867(6) 0.058(2) Uani 1 1 d . . . C21 C -0.0217(6) 0.06262(18) -0.1145(7) 0.054(2) Uani 1 1 d . . . C22 C 0.0485(6) 0.00926(17) -0.0213(6) 0.056(2) Uani 1 1 d . . . H22A H 0.1173 0.0048 0.0250 0.067 Uiso 1 1 calc R . . H22B H 0.0575 -0.0002 -0.0906 0.067 Uiso 1 1 calc R . . C23 C 0.2208(16) 0.0986(5) 0.4693(14) 0.183(9) Uani 1 1 d D . . C24 C 0.3289(14) 0.1184(5) 0.5004(18) 0.32(2) Uani 1 1 d D . . C25 C 0.4161(19) 0.1070(7) 0.428(3) 1.54(17) Uani 1 1 d D . . C26 C 0.774(3) 0.1666(9) 0.223(3) 0.32(2) Uani 1 1 d . . . C27 C 0.1785(15) 0.1027(7) 0.6543(11) 0.216(11) Uani 1 1 d . . . C28 C 0.212(2) 0.0760(10) 0.708(3) 0.32(2) Uani 1 1 d . . . C29 C 0.285(3) 0.0851(6) 0.838(3) 0.31(2) Uani 1 1 d . . . C30 C 0.264(2) 0.0513(8) 0.846(3) 0.306(17) Uani 1 1 d . . . C31 C 0.0393(16) 0.0756(6) 0.4919(15) 0.309(18) Uani 1 1 d D . . C32 C -0.1694(16) 0.0670(7) 0.470(2) 0.44(3) Uani 1 1 d D . . C33 C -0.0671(18) 0.0831(9) 0.5366(17) 0.75(8) Uani 1 1 d D . . C34 C 0.1042(17) 0.1453(5) 0.502(2) 0.223(12) Uani 1 1 d . . . C35 C 0.106(2) 0.1597(6) 0.3991(16) 0.248(14) Uani 1 1 d . . . C36 C 0.071(2) 0.1978(7) 0.380(2) 0.235(11) Uani 1 1 d . . . C37 C 0.0742(17) 0.2088(7) 0.2771(19) 0.220(10) Uani 1 1 d . . . C38 C 0.8054(11) 0.1814(3) 0.0087(13) 0.149(6) Uani 1 1 d . . . C39 C 0.7864(16) 0.2204(3) -0.0077(14) 0.198(10) Uani 1 1 d . . . C40 C 0.925(3) 0.2362(4) 0.004(3) 0.33(2) Uani 1 1 d . . . C41 C 0.928(4) 0.2510(11) -0.038(2) 0.45(4) Uani 1 1 d . . . C42 C 0.5976(12) 0.1717(4) -0.0152(14) 0.148(6) Uani 1 1 d . . . C43 C 0.5998(15) 0.1640(5) -0.1361(16) 0.206(8) Uani 1 1 d . . . C44 C 0.4798(15) 0.1767(7) -0.1879(14) 0.204(11) Uani 1 1 d . . . C45 C 0.4724(15) 0.1653(5) -0.294(3) 0.232(11) Uani 1 1 d . . . C46 C 0.7406(8) 0.1249(3) 0.0365(11) 0.110(4) Uani 1 1 d . . . C47 C 0.6543(11) 0.0991(3) 0.0724(14) 0.151(6) Uani 1 1 d . . . C48 C 0.7052(15) 0.0613(4) 0.051(3) 0.239(15) Uani 1 1 d . . . C49 C 0.656(3) 0.0413(8) 0.017(3) 0.35(2) Uani 1 1 d . . . N8 N 0.7085(7) 0.1631(2) 0.0469(9) 0.105(3) Uani 1 1 d . . . C51 C 0.6845(10) 0.1732(3) 0.1556(13) 0.112(4) Uani 1 1 d . . . C52 C 0.751(4) 0.1797(11) 0.311(5) 0.52(6) Uani 1 1 d . . . C53 C 0.756(5) 0.1679(15) 0.357(3) 0.50(5) Uani 1 1 d . . . C54 C -0.170(2) 0.0270(6) 0.479(2) 1.48(13) Uani 1 1 d D . . C50 C 0.520(4) 0.130(2) 0.451(6) 1.28(16) Uani 1 1 d 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 Br2 0.1005(7) 0.0583(5) 0.0652(7) 0.0222(4) 0.0084(5) -0.0053(4) Br1 0.0758(6) 0.0752(6) 0.0497(6) -0.0061(4) 0.0076(4) 0.0018(4) N1 0.08(2) 0.17(3) 0.56(8) 0.26(4) 0.11(3) 0.055(18) O1 0.049(11) 0.22(3) 0.71(8) 0.34(4) 0.04(2) 0.032(13) O2 0.111(8) 0.133(9) 0.65(3) 0.213(15) -0.042(13) -0.009(7) N1A 0.15(3) 0.043(12) 0.092(19) 0.011(12) 0.005(18) -0.005(13) O1A 0.30(5) 0.20(3) 0.28(5) 0.07(3) 0.17(4) 0.20(3) O2A 0.111(8) 0.133(9) 0.65(3) 0.213(15) -0.042(13) -0.009(7) N2 0.059(4) 0.063(4) 0.118(7) 0.035(4) 0.016(4) 0.008(3) N3 0.060(4) 0.054(4) 0.066(5) 0.013(3) 0.011(3) -0.001(3) N4 0.084(5) 0.046(3) 0.049(4) 0.000(3) 0.009(4) -0.006(3) N5 0.077(5) 0.049(4) 0.042(4) 0.011(3) 0.012(4) -0.002(3) N6 0.075(4) 0.038(3) 0.044(4) 0.008(3) -0.002(3) 0.004(3) N7 0.102(5) 0.032(3) 0.036(4) 0.007(3) -0.014(3) 0.001(3) N9 0.104(8) 0.288(17) 0.084(8) -0.103(10) -0.010(6) 0.017(9) O3 0.070(5) 0.079(4) 0.140(7) 0.043(4) 0.022(4) 0.012(3) O4 0.073(3) 0.040(3) 0.048(3) 0.007(2) 0.014(3) 0.003(2) O5 0.091(4) 0.047(3) 0.048(3) -0.001(3) -0.009(3) 0.012(3) O6 0.100(8) 0.042(5) 0.042(6) 0.000(4) 0.032(6) 0.007(5) C1 0.104(10) 0.097(9) 0.40(3) 0.142(14) 0.068(13) 0.025(8) C2 0.079(7) 0.070(6) 0.185(13) 0.059(7) -0.007(7) -0.009(5) C3 0.070(6) 0.064(5) 0.098(8) 0.021(5) -0.012(5) -0.005(5) C4 0.078(7) 0.080(7) 0.132(10) 0.055(6) 0.035(6) 0.014(5) C5 0.112(11) 0.114(10) 0.47(3) 0.148(15) 0.128(15) 0.038(8) C6 0.101(11) 0.165(15) 0.68(5) 0.24(2) 0.142(19) 0.064(10) C7 0.072(6) 0.069(6) 0.075(7) 0.034(5) 0.009(5) 0.012(5) C8 0.072(5) 0.045(4) 0.059(6) -0.002(4) 0.017(4) 0.000(4) C9 0.096(7) 0.065(6) 0.065(6) -0.003(5) -0.001(5) 0.002(5) C10 0.094(7) 0.068(6) 0.102(9) -0.026(6) 0.012(6) -0.016(5) C11 0.121(8) 0.045(5) 0.070(7) -0.014(5) 0.010(6) -0.005(5) C12 0.132(8) 0.041(5) 0.071(7) 0.000(4) 0.012(6) -0.016(5) C13 0.090(6) 0.036(4) 0.048(5) -0.008(4) 0.016(4) 0.004(4) C14 0.062(5) 0.028(3) 0.057(6) 0.003(3) 0.004(4) 0.004(3) C15 0.087(6) 0.042(4) 0.049(5) 0.016(4) 0.011(4) 0.012(4) C16 0.118(8) 0.050(5) 0.064(6) 0.018(4) -0.022(6) 0.006(5) C17 0.112(8) 0.065(6) 0.096(8) 0.025(6) -0.022(7) 0.028(6) C18 0.086(7) 0.072(6) 0.105(8) 0.017(6) -0.027(6) 0.023(5) C19 0.083(6) 0.052(5) 0.086(7) 0.017(5) -0.019(5) 0.008(4) C20 0.079(6) 0.040(4) 0.053(5) 0.009(4) 0.001(4) 0.015(4) C21 0.069(5) 0.034(4) 0.059(6) 0.011(4) 0.005(4) 0.000(3) C22 0.082(6) 0.040(4) 0.043(5) 0.010(3) -0.008(4) 0.012(3) C23 0.23(2) 0.166(15) 0.171(18) -0.049(13) 0.099(17) -0.065(14) C24 0.46(5) 0.22(3) 0.25(3) -0.02(2) -0.13(3) 0.21(3) C25 2.0(2) 2.0(2) 0.49(8) -0.40(11) -0.40(11) 2.0(2) C26 0.28(3) 0.36(4) 0.30(4) -0.27(3) -0.02(3) 0.12(3) C27 0.197(17) 0.40(3) 0.045(8) -0.054(13) -0.002(9) 0.110(19) C28 0.23(3) 0.46(5) 0.29(4) 0.26(4) 0.13(3) 0.18(3) C29 0.42(5) 0.136(17) 0.44(5) 0.06(2) 0.30(4) 0.09(2) C30 0.23(2) 0.21(3) 0.51(6) 0.02(3) 0.16(3) 0.02(2) C31 0.60(6) 0.24(2) 0.068(13) 0.007(14) 0.00(2) 0.00(3) C32 0.43(5) 0.26(3) 0.71(9) 0.09(4) 0.42(6) 0.13(3) C33 1.14(15) 1.01(15) 0.16(3) 0.27(5) 0.39(6) 0.62(12) C34 0.23(2) 0.173(17) 0.24(3) -0.120(18) -0.082(19) 0.091(15) C35 0.38(3) 0.188(18) 0.133(16) -0.088(14) -0.127(19) 0.139(19) C36 0.31(3) 0.22(2) 0.18(2) -0.096(19) 0.03(2) 0.01(2) C37 0.181(18) 0.32(3) 0.157(19) -0.09(2) 0.015(15) 0.018(16) C38 0.141(10) 0.060(7) 0.268(18) -0.026(8) 0.119(11) -0.016(6) C39 0.30(2) 0.108(10) 0.236(19) -0.076(10) 0.226(18) -0.054(11) C40 0.40(3) 0.045(8) 0.62(6) -0.022(16) 0.40(4) -0.007(12) C41 0.75(8) 0.49(6) 0.16(2) -0.04(3) 0.23(4) -0.33(6) C42 0.127(11) 0.180(14) 0.144(14) 0.019(11) 0.048(10) 0.071(10) C43 0.200(18) 0.227(19) 0.184(19) 0.019(15) -0.010(14) 0.122(15) C44 0.137(13) 0.35(3) 0.122(14) 0.000(16) -0.009(11) 0.129(16) C45 0.135(14) 0.171(17) 0.38(4) 0.05(2) -0.02(2) 0.041(12) C46 0.076(7) 0.079(7) 0.179(13) -0.012(7) 0.038(7) 0.004(5) C47 0.139(11) 0.078(8) 0.245(19) -0.023(9) 0.057(11) -0.016(7) C48 0.133(13) 0.068(10) 0.51(5) -0.056(15) 0.001(19) -0.008(9) C49 0.36(4) 0.20(3) 0.45(5) -0.18(3) -0.12(4) 0.14(3) N8 0.098(7) 0.077(6) 0.146(10) 0.001(6) 0.043(6) 0.003(5) C51 0.090(8) 0.096(8) 0.146(13) -0.031(8) 0.000(8) 0.015(6) C52 0.41(6) 0.32(4) 0.71(11) 0.30(6) -0.40(7) -0.19(4) C53 0.71(9) 0.64(9) 0.15(2) 0.01(4) 0.03(4) 0.52(8) C54 2.0(2) 2.00(19) 0.32(4) -0.24(7) -0.40(7) 2.00(19) C50 2.0(4) 1.0(2) 0.7(2) -0.14(17) -0.4(3) 0.6(3) _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 N1 O1 1.165(17) . ? N1 O2 1.197(18) . ? N1 C1 1.623(16) . ? N1A O1A 1.05(4) . ? N1A C1 1.600(17) . ? N2 C4 1.382(10) . ? N2 C7 1.396(11) . ? N3 C7 1.354(10) . ? N3 C8 1.429(9) . ? N4 C14 1.333(9) . ? N4 C13 1.424(10) . ? N5 C14 1.381(9) . ? N5 C15 1.418(10) . ? N6 C21 1.354(8) . ? N6 C20 1.408(9) . ? N7 C21 1.337(9) . ? N7 C22 1.475(8) . ? N9 C23 1.472(14) . ? N9 C27 1.518(17) . ? N9 C31 1.574(15) . ? N9 C34 1.82(3) . ? O3 C7 1.220(10) . ? O4 C14 1.240(9) . ? O5 C21 1.247(9) . ? C1 C2 1.310(14) . ? C1 C6 1.342(16) . ? C2 C3 1.389(12) . ? C3 C4 1.354(11) . ? C4 C5 1.338(15) . ? C5 C6 1.398(16) . ? C8 C13 1.357(10) . ? C8 C9 1.402(11) . ? C9 C10 1.402(12) . ? C10 C11 1.342(13) . ? C11 C12 1.351(12) . ? C12 C13 1.420(11) . ? C15 C16 1.369(11) . ? C15 C20 1.393(10) . ? C16 C17 1.390(12) . ? C17 C18 1.368(13) . ? C18 C19 1.372(11) . ? C19 C20 1.415(11) . ? C22 C22 1.541(15) 3 ? C23 C24 1.534(16) . ? C24 C25 1.571(18) . ? C25 C50 1.54(2) . ? C26 C52 1.31(9) . ? C26 C51 1.35(3) . ? C26 C53 1.78(5) . ? C27 C28 1.27(3) . ? C28 C29 1.85(5) . ? C29 C30 1.31(3) . ? C31 C33 1.518(18) . ? C32 C54 1.521(19) . ? C32 C33 1.560(19) . ? C34 C35 1.44(3) . ? C35 C36 1.52(3) . ? C36 C37 1.41(3) . ? C38 C39 1.510(17) . ? C38 N8 1.511(13) . ? C39 C40 1.79(3) . ? C40 C41 0.79(4) . ? C42 N8 1.530(16) . ? C42 C43 1.61(2) . ? C43 C44 1.62(2) . ? C44 C45 1.44(3) . ? C46 N8 1.513(12) . ? C46 C47 1.554(16) . ? C47 C48 1.60(2) . ? C48 C49 1.03(3) . ? N8 C51 1.530(16) . ? C52 C53 0.74(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 N1 O2 128(2) . . ? O1 N1 C1 123.4(16) . . ? O2 N1 C1 104.9(16) . . ? O1A N1A C1 124(3) . . ? C4 N2 C7 126.8(8) . . ? C7 N3 C8 119.9(7) . . ? C14 N4 C13 127.9(7) . . ? C14 N5 C15 128.9(7) . . ? C21 N6 C20 124.7(6) . . ? C21 N7 C22 122.2(6) . . ? C23 N9 C27 115.6(12) . . ? C23 N9 C31 106.4(11) . . ? C27 N9 C31 125.8(16) . . ? C23 N9 C34 90.2(15) . . ? C27 N9 C34 103.9(14) . . ? C31 N9 C34 108.6(12) . . ? C2 C1 C6 123.8(10) . . ? C2 C1 N1A 117.7(17) . . ? C6 C1 N1A 112.7(17) . . ? C2 C1 N1 118.5(13) . . ? C6 C1 N1 115.3(14) . . ? N1A C1 N1 41.4(15) . . ? C1 C2 C3 118.7(9) . . ? C4 C3 C2 120.8(9) . . ? C5 C4 C3 117.8(9) . . ? C5 C4 N2 124.8(9) . . ? C3 C4 N2 117.4(9) . . ? C4 C5 C6 122.7(12) . . ? C1 C6 C5 115.9(12) . . ? O3 C7 N3 124.6(8) . . ? O3 C7 N2 123.0(7) . . ? N3 C7 N2 112.3(8) . . ? C13 C8 C9 119.9(7) . . ? C13 C8 N3 121.8(7) . . ? C9 C8 N3 118.3(7) . . ? C8 C9 C10 119.2(9) . . ? C11 C10 C9 120.9(9) . . ? C10 C11 C12 119.8(9) . . ? C11 C12 C13 121.7(9) . . ? C8 C13 C12 118.4(8) . . ? C8 C13 N4 125.7(7) . . ? C12 C13 N4 115.2(7) . . ? O4 C14 N4 126.5(7) . . ? O4 C14 N5 122.1(7) . . ? N4 C14 N5 111.3(7) . . ? C16 C15 C20 120.8(8) . . ? C16 C15 N5 116.2(7) . . ? C20 C15 N5 122.8(7) . . ? C15 C16 C17 120.9(8) . . ? C18 C17 C16 119.3(8) . . ? C17 C18 C19 120.5(9) . . ? C18 C19 C20 121.1(8) . . ? C15 C20 N6 121.9(7) . . ? C15 C20 C19 117.3(7) . . ? N6 C20 C19 120.7(7) . . ? O5 C21 N7 122.9(6) . . ? O5 C21 N6 122.6(7) . . ? N7 C21 N6 114.3(7) . . ? N7 C22 C22 109.3(7) . 3 ? N9 C23 C24 118.0(13) . . ? C23 C24 C25 109.6(16) . . ? C50 C25 C24 109.6(19) . . ? C52 C26 C51 105(3) . . ? C52 C26 C53 22(2) . . ? C51 C26 C53 116(3) . . ? C28 C27 N9 122(3) . . ? C27 C28 C29 117(4) . . ? C30 C29 C28 79(3) . . ? C33 C31 N9 112.1(14) . . ? C54 C32 C33 111.2(17) . . ? C31 C33 C32 112.5(16) . . ? C35 C34 N9 125.8(15) . . ? C34 C35 C36 118.5(19) . . ? C37 C36 C35 114(2) . . ? C39 C38 N8 112.6(10) . . ? C38 C39 C40 100.8(14) . . ? C41 C40 C39 108(6) . . ? N8 C42 C43 111.2(10) . . ? C42 C43 C44 103.5(14) . . ? C45 C44 C43 105.1(15) . . ? N8 C46 C47 112.5(8) . . ? C46 C47 C48 102.5(12) . . ? C49 C48 C47 121(3) . . ? C38 N8 C46 100.8(8) . . ? C38 N8 C42 114.3(11) . . ? C46 N8 C42 112.4(10) . . ? C38 N8 C51 115.8(10) . . ? C46 N8 C51 113.9(9) . . ? C42 N8 C51 100.3(9) . . ? C26 C51 N8 108.9(15) . . ? C53 C52 C26 118(9) . . ? C52 C53 C26 40(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5 Br2 0.88 2.52 3.272(6) 144.4 1_554 N4 H4 Br2 0.88 2.63 3.342(6) 138.8 1_554 N2 H2 Br1 0.88 2.49 3.346(7) 164.4 . N3 H3 Br1 0.88 3.20 3.924(6) 141.3 . N6 H6 Br1 0.88 3.26 3.912(6) 133.0 . N7 H7 Br1 0.88 2.55 3.350(6) 152.0 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.811 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.108 ####END